Thermo-Mechanical Investigation ofNanoreinforcements Doped Elastomeric

Nanocomposite Thermal Insulations

By

Srdia Slgar

School of Chemlcsl rnd Mrterisls Englrcering (SCME)N.tionsl Uniyerrity of Scieoccs & Tccbnologr (NUST)

2m4

Thermo-Mechanical Investigation ofNanoreinforcements Doped Elastomeric

Nanocomposite Thermal Insulations

Sadia Sagtr 2OO9-NUST-TftPhDMSE.83

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Supen'tuor: Merltorlous Prof. Dr. Arghri Mrqsood (SI)

co4upervtuor: Prof. Dr. MuhrDmrd Shrhid

Deprrtment of M.t€rhb Elgircerirg (Mn)

School ofChemicd.od M.t rtd! ElgtDeering (SCME)

Nrtionrl UDiverrlty of S{iencci & Tecimlos/ (NUST)

H-12 klim.b.4 Prkirt rOctober, 2014

Thesis Submission Certificate

It 15 to certify th.t u/ork in this thesis ha5 been carried out by

Ms. Sadia Sagar (R€9, 200$NUST -TtrPhD-MS-E-83) and compl€t€d under

my supervision at the School of Chemical and Materials EnSineering,

National Univelslty of S€iencesand Technology, H-12, lslamabad, Paklstan,

S!perul$r

oepr, of Phvti6, Ai. UniErsity,PAF Complex, lslamabad,

Pak|3lan

lt,\j{tiil-Prof. Dr. i/rohanm.d M4.hid

School of chehical and Materialr Engln..nngNational UniveBlty ot Sciences and Technologt,H-12, lslamabad, P.tistan

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Li,ftX?ubl'1u71'otw> Inlen lo!.1Prblietiou

l M asyoui, Nld€m Iqbal, SrdL St8.r, Mohmad Bilal Kho, Umair Javaid

Abladon &d $mo_m4heicd investiSation of shod e6on fibs inpEgnare<l

elstomedc ablativ€s for ult ltiSh imPetllu€ applicalions Polvner DegBdaton

md subi|ny, DOI: ors/l0.l0l64.polymdegodstab 20l4.0E 012

2sadi, So!!r. \adeem lqbal, A.smri M.q"ood VuhmMd Shat'd N@ Abbdt

\han, l;tr lmil dd Moh;cd lsnail Bssvoui Fdbrication dd rhemdl

chd*t*istics of nedonalizd cdbon 'molub's impr€gnaFd

polydindlylsiloMe nm@odposil€s, Jounal of Composit' Malerials DOl:

t 0.l I 7710021998114528?lll.s;it S.c.r. Nadam lqb.t, Assh&i Maqsood dd M Bsvoui MwC\Ts' -l'."*rfu rl.trl rub|;.' con-posires: ftmal lnsulation PhN rtusirion dd

Meclidical Pbo€nies.lAcslT lni J EDS T4h Dol: 10 7763/UET2014 V66E9'

Vol.6. No l.Jue 2014

4.Sadi. S.s.r, Nadeem lqbol. Arghei Vaq$od. Umair Ja\ard lhemoe-a rmellc

I'ii."*'.'r ***e tul.,i.dic *d e\penmenbl tnema' truspon rld\ of

VWCNTAIAn **o-p.til.i J Thcm Anal Calorin, DOI 10 1007/sl 09?l_01 l_

2949.'j5.S..1i. S.srn Node€m lqbal, Asgh& Ma$ood'

rmptsgnlu.d rubber n4@omposiles lhemaldril@null samA calorim.tic srudY. Il0.lt?70?31684411484184

Muhisnlled cdbon @orub€stanspofl/de.onposilion dd

Rei or PIsl ConP, DOI:

6srdi, s.ctr. Nadem lqbdl, Asghd Maqsood Dielectric elechc

o,o*n,es;lcffbo{vl,c tudiontltred muluv€lled cebon nanotub'"

ooli d,n.$J h,lorde ndcomposik. J Phls: Confeence series 439 (20r1)

012024, DOI:10.1088/1742-6596/439/l/012024?-NJ;m '

hbol, S.dit Sts.r, Mohdmad Bilal K}|!' Mohmed lsmil BdsvouiTrrd M. Kha Almi;u siliotc Fibe6 InpEsdted Acryloniuile Buuditrn it". i".*litet, Ablation, Th.dd T@pofl/stabilnv. md M$heicalltuKtion. J ;\DDl. Polvn Sci zoll. DOI l0 |00,APP lq?17

s.NJ;. tqUal, vohd-.ud Bilal Khd. S.di" s's'r' Aselu \l"qsood'

r,i'i""i"" *ir chdel€dadon of MultiMlled carbon NMolubetsilicotre

RLbber Conoosirrs, J ApDI Polvm So 20ll DOI l01002APPIS'll0sNadeem lqb;I. Srdit stsrr. Vohama giti Kno Hunz Muhmmdd Rai:'lu(- -

el,"i...iiL eLr",i* r"'i".omoosh* Usd i! E ?enlemd Envionnenrs Polvm

Enc Sci, DOI 10.l00ZP€n.235?l10- Nai*d lqbnl. s.di. Srgl', MohMnad Bilal Krun tnd Haliz Multomad

iuo*". itu",i-, ,t'.*"r tr"bilirv/tasPon od necbdicsl inte$igarions ol

nodifr; ndokelinne inprcsttrted scrylonirile buradiene rubbcr composircs'

Jouhal of CoDposirc Matdah. DOI: l0 l l ?7/002199831 3484948

r r . il'J*. lot"r, !"0i" s"g"., sd Moh@hld Bilal Khe' conprehensive Ablation- cii.itil!,i.i "tc"*i" ribers tnpEenat€d Rubb€r conposit$, IAcslr lnt J

Ene rdh, Vol 6,No l, Ju€ 2014, DOI: I0 7763^JET 2014 V6 688

1.

2.

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Submitied research orticles to Internrtiooal Journalssadi:s{ar, Nadeem lqbal, AsSh.riMrqsood, Expe menlalthenaltraispott evo ution

otnaio.Lav rcinlorc€d polvmer(ompoeltes Expe nenialHeatt€nsfer,lssN:0391 6152

s.dla 5.3ar, Nadeem lqbal, tuSharlMa$ood, A Novel Roure lo svnlhesire Nanokaollnile

and its Effeds on the Th€.mo.M€chanlcal P.openies ofAcrylonivile sutadiene Robber

Nano.ompositercomposite gi€nce rndTechholqv, l95N:0266'3533

N.dem lqbal, sadl. s4rr, M.3. Xhan, z.ifar M (han, sp€d.a tibeu InpreSnaied

Polm€r com{sit€s: ablation, Thehal conduciivitv/D€compdition and Me(hanictl

rNesriSarion, c.mp6ite scieRe and LchnolSv. lSsN: 026e3533tadeem rqb.l, 5.d1. s.a.., Mohamm.d silal xhan, agha.i Maqsood, 'lhe rcle olM u hiwalbn c2 lbon Nahotuber ro e nht ice Ablation, M echa n ial a.d ltema I P.ope fties

ol Nilrile Butadiene Rubb.. cr.b.n, ISSN:000452?3

Nade€m lqbal, S:di. 5.!rt1 Mohamd.d Silal$:n, NBR/Phenoli. rcsin ble.ded abl.lve.ofi posn€s,loumal otApplied Polymerscieice, ISSN: 1097_4623

6. Nadeem lqbal, s.dla s.s.r,laimoor A. Khan, Faiellqbal, Saad Mehfoo:, ttlohammad H

( Tareen, Nasir M. Ahmad, €fted of que.chim Temperatures on lhe Propedies and

Perfoman.e of Kevlar SuDF ed IPP MembEnes, Joumal of Appli€d Polvfr.r soen.e,

> Internrtional Conference Prpersl.Srdi. s.e'r, Nadeeh lqb6l, Asddi Maqsood, Ill€mo'mahrnicol aid

dilleEndal calodm.lnc snl(ly of thc gBphede oxide impEssted EPDM rubber

no@orosres, N{oTeh2Ol4. Wshingon DC, USA (Windng BBt

Prcstrririon Arrd)z.S.dir stg$, Nadm tqb6l. Asghdi M.qs4 MVCNTS lMryodrcd N.$tal

Rubber CiDposiles: Theml lisul,rio!, PhN Ttusnioo md Mochaniql

Pop€rties, ICCEM 20l3.Chin!, (Winning Bsr Pres.rt.tion Awrrd)l.Srdi. Srgrr, Zalier M Knd, Nad*m lqbal, AsghEi Moqsood,

Themomechei@l study of Ndoclay-Nilrile buladiene rubbe! conPosilcs

IBCAST, klmabad. (2011) (Dort Polrer Prc3eniltion Avtrd)4,Sdir Sqrr, Nadeem lqbal, Asgahri Ma$ood, Dieleclic, electric ud Thedd

proFdies of Cdboxylic Fundionalized Muhi*alled Cdbon Nanolubes

InpEcEted Polydimerhylsiloxd. (PDMS) conposite. vAsscAA _6 (2012)

(WiltringS.@!d Priz4 i! Po.t.rPB.ltltior).s.Srdil S.g& N.dan lqb.l, Shabib AFI& Gu6al, AsSndi Maqsd

functio.olizalion & uifofr disp.Gio. of MWCNTS into PDMS, Nmo Africr,south Aft€ {201D GiBt Priz. i! Onl Pro.ll.tior)

6.Nadeem lqbal, Srdit sigr., Mohann d Bilal Khe, CompEhe.sile Ablalion

Ch@deristics of Cemic Fibe^ lmprc$ded Rubbs Composnes, ICCEM 2011,

7,S.di! Saglr, ZlfIq M Khan, Nadeeh lqbal, Asgbdi Maqsood, A companrrve

study on themol & dechdical cvalution of diverc fibes idpegnatcd polvme!

conDosiies, IBCAST, lslambad. (201l) (Onl Pcsnration)

8.Nd.cd hb.l && 8{.!, M.B. K!e, Alghd Mrqloo4 z.fht M. Kle, ACoEDGt ltivc Abhtior larsfuldd of Klvlr/NER Atilth! Co!'rodcr'tscAsT, Id|ln.bd (2013) (ord Pr!..dio!).

> BooloLLdhS{rt ,N.d..d&t L M.BXh.a tligh St ocfic.@9odir6l

$d.dr .!d !,GcLisl T..i!g of PdicL td Fih.r Rd&!dItisls&!||n cqodr! [.t d.lr hblidd iaYD],i, uK

h tlr€ Nnne dAllafi, tlvWcri-Ye,neirrrn &e

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AcknowledgmentsI 4n ydteful to thz folloving persog 4r.l orsqizatiw lot trcilitatins N with afective

gui.lelitus, Notagen nt, eqipwt s. tucssuie, h'dk& od ntat s/W'' to

@onplth ftis rese@ch wqk

+ Dr. Asshari Muqtoa.l. SI @entortow PtufesoL Ab Univqsitt PtF cokPkx

hlanabLd. Pakhtan)

4 D- tutanna.t Shahid (HoD, Md.nalt Etsi@.ri'& SCME NLST hlMobad

4 b Mohannatl Mrjqhid (PinciPal/Deoa \CME NUST lslMabad' Pakittan)

t Dr. Abttut Qtddos (cSO. AQ Khn Laboatdiet. Palhtan)

$ D,. N6ir Mehn@d (lswiote Ptul.M scw NUSI' ldoMbad Pakistn)

4 A AMit Habib (Asistant Ptul.sot SCME NUS| lsla@ba4 Pdtidn)

t Dr. fiitJlot E^stMGut (Asshtant Plofesot SCME NUS| tslfuabad' Pakistah)

$ Dt. AhttudN@a Kha"(Asi;tMt Ptuletw SCME, NUST klatubad Pakttan)

.. b. V'lLt M Khan On, NFa:OM klanM' Pohsld)

u Mt. MuhMd Mwofor (C6hi.t Moinqfice NUST lslatubod)

t Mt '!zh UIah (.|iststbtTccouttt Dbe.d HEc klanabad)

,. W sheitt Zonqft Ahned (MD, LonSdM i'I'lls Lahote Pokittan)

q Dt.Mohannad Tm|e er ( scME, NUSn btanabd.l Pali$an)

q & Mohtnnsdtghad A6hit (PhD s.hob scME NUST hlanoba<! Paiisrn)

" D.. Ali Eahait (;CW NUST, hlonabod, PatniM)

, MB. Sofa Alab(PhD srholo, SCME NUgl tslfiabad. Pakhtan)

* Mt- ltob lrran (PhD sthot@, SCME NU9I lsldabat P"ldst@)

4 Mt sata Bi Bi (Liba" ofreiq Longrnan Milh, Lahote, Pokittan

$ Pak&ton Railvdy Cotiage Factory, hlawbad

t lU gafofl'h', Lib@t, and Adni\ N@k of scME NUST hlanoba't

$,1d Specia, lo Htghq EdBatidc@nision (EEC) tslatubdd hr providins

tuficient f@.ial supPot to luAI the PhD reench votk

(qfg uotru\H) it ot t4 Dtltou tn*(paaqsoY4n-PqY) $Dl u! nqtot t I *

(n8og our11 Puo

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4.rfw.4+.fttttds

Abstract

The dissrrliion rcpotu thc cfficio.y of th€ mofilleE lo altc'ute lh@al

insulation. t\ernal desitio!, th..nal sr.bilily, &d m4hdicd chdetc.islis of $e

elbtonqic nanocomposit$. Twnty ciSh1 divete ele*onedc svstcds have been used

with tuncriomlircd nultj*€I c{bon nanotubs (lMwcNTsynanokrcliniG (FNK) dd

eldtom.ric mlriccs includins elhyld. Pbpyl6. mmnd Nbb€l (EPDM)' srttftbuadien rubber (SBR), sili@n tubbq (SR), lc.vtontuile butadi.i. rubb.r (NBR) ro

lab'icale polyms l)lll{){dpcitcs suibblc for Euldple applic{tions @rdirs lo lhe

$mo-n*heicd chmler. I1lc mo-in@tpoBtio6 wrc turdionlliad usins 3'

minoplopyl irinelhoxy silfle lo inPov. lhct disp.Eibilily sd coDpadbility wilh the

Acrivdted @lay with av.lagc p.nick size 3!D w6 syo$sized adopting novel

{ononical md 6y nethodology. vdbB concdrados of activated mo-

Finforc.m.nu hav. b@r idptgflcd ii the clasrondic naltices at sp€ilic tine_

&mped@ 4d olling velcily @ndniN Eblomedc mnpGit sFcincns in patticurar

mold s@n.iics v€E cured on th. hol istiric FEs !r speciic l€hpedtle &d presft

Fmclionalianior dd cryslallogophic sludy of &e in@rporat€d t&ofill.r wcrc ex6uied

usins on Fouiici hsfor@lion infrarcd sp4ltoscopy (FIIR) a.d X-nv dilliacton (XRD)

techniques. The labri€t€d cooposite specinds weF pul into tcsl for themal

conductivity/inpcduce. scuins.Lcuon mifts@pic, ditre@ntial scanning cdbnmet.ic.

$emd d€comlosilioq diff€turial thm.l ti.iysis, ShoE A hardnds od unidial leBile

r€stl !o elucidare th€ €ff4t of tuDctiol,liad @ofilleu on $e lEmal and n(b$ical

ch@ctedslics of e polyner sMpotilcs.TlFmo-m*h&i@l propenies h.v. b@ Emkablv if,flu.nc€d wnh iio€6i.8

rhe funcionslidd ndoclay/ndolubes con@nl!.tion in the host elstondic nalti€s High

themol sr.bilily, heat qlenching caPability, low tbemal @nduclivitv hiSh nechmical

shgth. dd emcied einfo@mdt-roLix adh$ioo m iddtifi.d 6 the mos! pon'n€nl

fdro6 for 6bec.d lhemal idulatioi P.do|llr.G ofelastom€nc n4oconposnes The

lean valrc of lhem.l @nd*tivily (0.009Wn K), dtnosl thmd impedmce

(5. t2m.K./v). and hi8t61ulfnur. tc$ib dEn$h (8-45Mra) l{@ $rulinizd fot l()s{Z

FNK impFelat.d NBR @ocompositc. The uppemost fimal srabililv lo*esi glsrrmsition dd crystalliation tempetaturcs wec obseded fot lMo/o FMWCNTS

iMrDo6ted SR @mposiic. In riew ofov.6ll pedonme, FMWCNTS a.d .sokaolinile

inpegn t€d NBR &d EPDM ehsbn.dc @o.onposil€s 4e dsno.$ral€d beter

@moarEd !o otho fabricd.d @nposite slstens Egdding all pqlormed theino_

The nov€ltv of this reserch wo* 6ides in iabncsdon md $emo-nechmic.l

study of rew eldloDqic conposil€ fodul.tioN sing nedion li4d @oliu.s. Itdtulr.?.spon snrdy &d diffeEnrial rhemal ddysis of$c tabdcalcd polync. nmdomposiles

e also added values to the presqt ei.ntiic liteiat@ o. elatomeric nancomposiles.

'IrE hislEst dt.mal iNularion clEfurd B ob*ryed for dE FNK/NBR systcns

ompadd to lhe contenpoEry availabL data or th€ elr$ondic nddomposiles.

The dsigier cu sl.cr a $ilabl. mmbinlion of eldtomenc ie@onposite for

$e snuion ar hed uiig $c th€m.l ranspoll/$abiliry/|nsnion lenpehl@s, spe.ilic

enthalpies ad hcchmical invesligalion dala prcvided in consolidatd fod ar th€ end of

Ihe disseflalion. Fan &d @nomjcil oure to snth.siz€d functiondizd Mokslin with

d ed8. pdn( le sr€ ks Lh& 5nm is also inrodled novelr'.

Contenls

ASTM: sllndld T6r Mdh.d tr Thmrr Condudt'ty of Solids try Mor oflfieG!.nld- Compdivologindiol Hc.t Frow T€hriqk

ASTM: sbdltd T.lt Mdnod fd Them.l Tdnsnision Pep.nies olThin nem.llyConductiv. Solid Eletrial Insuhtion Madirls

Section # I Introductioo rDd Literature Survey

Chrpter I lDtroductioo

L Tfimal lMhtd

6

t25

Bl

I

2

2

2

1

Il

5

5

9

l0

L l- 1. Clo(hing iMl.1io6

LI.2. Buildi.g imlationr

LL3. Mehoic.l sFtetn irsulstioB

I - |.4. sp*€rn iNLlids

L1.5.Au|onoiveinsul ioi

L2. D6igrins p{dc.6 of . th.Ml iNllrim

LL Chdderinica of thoml i$ubions

1.1. H.rr tr,rfo rhoud na€rids

|.4.l. Mod6 of lEr E!$Lr

L4,1 ,1, Corductiot

r.4.l.2.CoN.qid

I.4.l.l.R dhrion

l.t,Tn m.l @dudivity of i.cral3

l.t-l Mch.nim3 of har @ducion

1.5 2. H4l @ndlction thrcud mellh

l.t.l. H.rt tdEis ceMrcs

1.5.4- Thd.l @ndL.rioo lhD!8h polyn G

L6. F.dors .fcling on tb.ml @dsdviry

L6. L Hql C4eny

1,6.2, n ckrc$ oflhe insuhiion Drterialt

L6.4. M.r.nrl dEL6.5. M&ri.l sluon4

L6.6. Elcltic.l hnductiv ily

L7. Typ6 ofF&ri{rl tl.nnrl i6uUlioB

l.?.1. C.mic ineldioB

l.?.2. Poltmqic insDlotions

l1

t2

tllltl

Itl5

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l7

l3

22

22

22

21

23

2l

u

25

25

77

21

27

L?.2- L F-MWCNT/SR syscos

1,72.2. F-MWCNT/EPDM ryslen!

L?.2,3. F-MWCNT/SBR sr$etns

1.7.2.4. F-MWCNTABR sy$ems

L7.2,5, EPDM/Fu.ctjon lizd Nb@hy (FNK)

20

20

2l

Sectiotr # 2 Mrtcrirls.nd Chrracterization

Chrpler2 Mrterirb2. Polymcdc m!fi62.l.Silionobha

2,1,t, us2.2. Etnyhn. Pr.pylene Da4c Monm.r (EPDI!' rubb.t

2.2.1. Us2.1. srye buu{ti* dhb.r (SBR)

2,3.1,Us

2.4. Acrylonilrile buLdiem obber (NBR)

2.4.1. Us.s

2.5. P@ing lils2.5.l.Coslinkq

Chapler3

Chapier4

2.5.1.2. Dicunyl p.sri&2.t.2. P.ina.y @b66r2.5.1. s$&.y @l.Ela2.5.4. P@ir8 hbn{nts

2.5.7. silirc oupliry igol

2.6.1. Multiwall.d cdbon osorub.s

D€velopment of Thermil Conductivity,iLnpedance

Me8surenent Apprratug

Ll Then.l l'anrpon nudy

Char!cteri"rtior Tecbtriqms

a.l. Checlc.iation L.hniq64. L l. 'Incmo8nvifr.tic .nd Dift Mtill Th@al An,lyz.r

4.1r. Difr.mri!l S{.ming Cilodm.try

4. LL Meh.nic.l T6tin8

a.l a *un'nCEl.crcn v(Mopj And Ener$ Di>pedle

4.I 5. Fouri.r Trdsfom lnfided (mR) Speotsosoopy

4.1 6. x"R!y Diffdction T.chniquc

4.I 7. Atomic Force Micoeopy

27

21

l3z3

29

29

l0l0

ll

32

35

l5l5

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l6

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J7

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S.ctiotr # 3 Results and Discussioos

Chapter # 5 Relults ond Discursion

5. L surf.e nodifimlion ol EinfoMcDb

5.l.l.Synrh.lisod rlc modificdion of Kslinn€

5.1.2. surf@ modifio on olMwCNTs

5.2. F.bndion of nlmoBposii6

5l Fomuhrjon ot polync dno@pdites

5 a. F MWCNT/SR .mposit ryn.m

5.a,1. Disp€FionotF.MwcNTs in sR

5.4.2. Th.m.l condwtivity od th.m.l inp.ddc .tults3

5,4,3, Thcmolntim.riddiffdlid th.mal NDssJ.4.,1. DIt ..mi.l snin! 6l@mdd (Dsc) Dtlris5.4.5. Mehsi€l c|ldcrcdalion

5.t. F.MWCNT/EPDM.hrion.nqt.@omP4tLs

5.t,l. Di!p.6id of F-MWCNTS in EPDM cldoBcr

t.t.2. Thm.lcondEtivivanFdo€e.lysst.5.1. Thmll dsnp@tid &d h..r flow b.h.vior

t,5.4- DSC altsG5,5.t, M6h.riol pbFris

t.6. F-MWCNT/SBR .bsmcdc Meomt6it 3

5.6.1. Dig.Eion of F.MWCNTS in SBR

5.6.2. Th.m.l @ndEtvi.t.d tlFnll imF d.E b.hlvior

5.5.3. TlEm.l lbbility ond han flow cp.B

t.6.5, M4hdiol poFrks

5.7. FMWCNI/NBR dane.nc NMnpGit65.7. L Disp.6ir of F-M\YCNTt in NBR

5.7.2.Th.m|@nducivity/inp.d!@.nrlyet

5.7.1. fi.molnvim.rric lld diff@ri.l dm.l .Mly$s

5,7.{, D6C study

t.7-5. M6hsb.lFoFnn of F.MWCNTABR @pdilcJ.8. Fundim.liEd Nuok&linit /E DM .lqbm.ric n.n@mt6ics

5.E- |. DhF6i@ ofFudi{holizcd n.mrslinie (FNK)

in EPDM .l.slom.r

5.E.2. Thmd lnp.d.lc?MdstivityoduEmcnLt.8.1. Thdnll d.gndlrion !d h{l flw bchtvior

t.8,,1. l$thmd b.lnvior

t.8.t. Ultinlr. tlBilc atllglh xd h.dr6s

5.9.Fucti@li4d N{o*lliniltsBRclarom.ricnu@mpcilcr

t9,1. DilpcRid ofNolDlinic in SBR

t.9,2, Th.ml .ddativity ed lh.m.l iir.&ne dbs5.9,r. ft.mrl d..ldtolnion .nd Diltaoti.l Th.m.l .Mllsis

5.9.4. Dilt Mli.l sni.g crlodn.uic nudt

t.9.t. Menei.tl p6Fni6

5l

53

5t

t8

t3

t8

669

72

30

32

a2

33

84

86

ol

5.10r@lb.&.dlbdrhiillB.L6.aI'@I!"c510.1. Dicdodrdbn! hl|BrsJO.r.ftid.lcdrdYbnbdliEFi@dlls5.lOJ.lb!.al|vildlc rd di&rdl tEt l @lF

5.10r. txrc d4J.lOt i&drio.l &r.tLdc

IlD

tttot0a

105

108

t0!

lt5

S.ctiol # {Chry!.r 6 Codutlo.

Colcloio! & FrtIrG Pro{..tivc

List ofFigures

Chrpter I

Chapter 2

Chapter3

Chapter 5

tnlroductior

Fisw l: Q@tit tirc dcsdption ol Fouicrs law

Figur 2: Converive hdl rlsfd fon $lid suf@ rc Doving luid

Figure 3: Rldialion hell tesfd bcts@ a sufle .nd iB

FieBe 4: codbioation ofcoiduciior! coNection, ed .adiatron heat

Figwe 5: TmFslw d.p€dde oflh€dal coodtcivny for *v@l.€mic mderisls

Mrterialg

Figue 1: Cheni@l sfrcluc of sR monomer

Fi8ure 2: Chenial sduclur. oi EPDM monomer

Figurc l: Chdisl structuc of SBR motdmer

FiguE 4: Chemi@l $reilE of NAR torcms

rirlE 5: Sinsle *sllcd ..rhon @tubes wnh dill.Enl coobinarions

D€velopnent of Thernrl Conductivity/Impedrnce

Measurement Applr8tu3

Fisut 1.: $h.maric of MFElive-guatded]osiidind nd now svsten

lccdding 10 rhe asTM 1225

fisua 2: Th.m!' 6ducrivnylnp€d.M D4cmot

Relults lnd Discussior

1

2t

2l

74

25

30

lll3

Fi8urc I : Flo*hd of sudie modificltion md svnth.sh oi Mnokr'linne 40

liigurc20: FTIR spech olunnodifi.dmddifFn kaolinne

Firurc zbi xRD paftems of umoditr.d/modilied krolinit.

Fig!rc r: Surfae dogholosy of unmodinen (a), .nd modif'cd (b, c) cliy arong

yirh is compositioMl edYris (d)

FiguE 4: surfae loposnDhy oimodifi.d m&l.vFigure 5: Flotchd ol surf@ modifiorion of PIMWCNT!

Figurc 6: FrtR sp€cna for P*MwcNTs dnd F_MwcNTr

Fig@ 7: xDR p*ren fd PeMwCNTs !d F_MWCNT

FisuE 8: SEM micrc8nrtu ol PiMWCNTS .d F MwcNTs

50

FigGg: sEM grrphdEDsdlysi!ofPsMwcNTs (.)ond F MwcNTsib) 47

Fig@ I0: schemdic of fd $? f.b.icsted polvms nuoronpo,its 18

Figure I I sEM micorEphs of F MwCNTs reinlorced polvm'r nanocomPosrc ar

FisE l2: Thmal condslivity conlouts widr incE6in8 lemP.dturc (.) lnd

the .fet of F-MWCNTS on rhmd c@duclivitv of SR naneomposire

(b) 5l

Figurc t3: Tfie etrar of F-MWCNTS mEdions d lhcmll im!.dtnce of the

sR nm@mpoli6 in th. tcmpcntuF tu8€ oal2l_512K 52

FiBure I a: SEM nicrogoptu of F* thmal tuspon &s&d nmommposir

sp.cim?ns sRC I (.), SRC2 (b), SRC3 (o)' SRca (dl SRCs G), and the

conpdsiriondlatult3i5oflhel$4%loadedF MwCNTsinSR(D 53

Figd. l5: Thcmal oxid.rion hohdior ot SR @domposites in lhc lqmpemiure

ds. 25-8000C it an dvnonment

Figm 16: tlat qu*li.g clPability of SR n@posncs in th.

lcmp€rd|a 48. (2t.80t'C) in ai. dvimnm.nt

Fi8u. I7: DSC pofilc dhPhyi.g TB , Tc , Tm of SR tonsfiporir.s 56

FiBure | 3e Efe.t of@bd nuotub.s l@diDgs on llrimd. !.isil. sN€rh ald

peMil elonglrion el bMk in lhe SR 51

FiguE 18h llre eil€i of @bon noo$bes loadings on hddne$ in rhe sR 57

Figurc l9: Th. disribulio. of F-MWCNTS within de potm.t mtrix er vlnanl

mgriliarioN (!, b), @Dositiodl s.lvsG of EPDM coBFsit (c)

!d i|i. enb.dd.d t-MwcNTs (d)

FiB!E 2{r Themrl qdGriviry !t difr.d F MWCNTS Menf8tons

dd bp.nd6Figu. 2l: Thmal imp.dsc. ofd v&idt lodingt ol F_MWCNTS

@nccntarids cnd lcmF alurcs

Ficue22: sEMnicbgEphsof posld.mdhnspon&sled nmocomPo e

spsimensECI (a), EC2 ib), EC3 (c) Ec4 (d) EC5 G) tnd $e

comgisiriot.l !n.ly!h of $.lwgo l@d.d F MWCNTS in EPDM

FiAr. 2l: Thcmsl d@m!*nion dltsis of F MWCNT/EPDM

FisE 2,t: Ditr@ti.l lhmrl Dtlysis of F NIWCNT/EPDM speincis 62

Fig@ 25: DSC mlouE ofdr f.bd6r.d F-MVCNT/EPDM @mposibs 63

f_isG 26:Effd ofditr@ doDinaclr|Fdions of F-MWCNT on xEstuinP€dmocc of EPDM M6omp6i16 64

Figur.2?: Efreolofdif.E doping@ncmtrarionsof F-MWCNTonulrinate

tensile nFngth md peent eloqrtion at bEak of EPDM

Mossposirca 65

Fiaure 23, Etrer ordiaf@r doping trc.nlrllions of F.MWCN] oi shore A

hdfts of EPDM @@mposiB 65

Fi8@ 29: SEM inaa6 of F-MWCNT/SBR cmp6ia !'d th. @pditjonal

malyris of! Nnotubc anl ve/6 Motubs load.d $6im.nFig@ l0: Etrect ofl.mp.druE on themd @ndrctiyity (a) md th.dll

@nductivity atdiveBctcnpebturs(b) olF-MWCNT/SBR specimens

323-523( 67

FiBr.3I: Etra.toflh.Drl imp.din oflhc F MWCNT/SBR niNcompo$les

in th. &nD.rrur tugc l2l-523K

Fisu. 32: SEM inag6 ofpos lnsnll @'nucdvity/imp.dee idcnndMmpcit. spcinds scl (.I sc2 (b), sc](c), sc4 (d), sc5

rnd EDS mlys! of SC5 @posib speim.n (r)

Fisu. l3: Edecl ol F.MwNTs ongrations on tne $emal dqmdation oiF-MWCNT/SBR Ep€cinens

Endo/exothcmic b.hqvis of F-MWCNT/SBR specioe$

DSC conioud ol F.MWCNT/SBR speim.ns

ElTecl of F-MWCNTS coentElions on thc UTS .nd DcMrt

c|oncrrid { hsl ol F-MWCIT/SBR @({dp6n s 7J

Etrd of F-MWCNT! Mdids o rhc .len.ric hlrdn* of F-

MWCNT/SaR sFcim.ns 1J

Figurc l3: Micrc*opic vifl of F-MWCNTS dhp. ion in rh. NBR at diftercnr

EeidDs (a, b), compositionll andlysis of$. comporit! (c), ed rhe

spol €lcmcnlr | lmlysis of rhe nootube (d) 14

Figre 39: nemal cod@tiviry s.lour widr lhe lemp.druF Btrs. 321-523 K or

rheNBRamp.6iicsp€inens 75

FisuE a0: Efrer of Motuts qentltios o ihe rh.m.l @ndctitit orNBR

stsincN r diltmr EnFntlc 16

Fkm 4l : Inemal ih!€de6 t!fi16 of dF composie staimG *llh

T.sD.mtu /F-MWCNTS ooncantdion ancnuition 71

rigurc.2 Tnedal &gtub on Bpon* of$e comFiiG sp.c'n'i\ 'n

3r

artn6Dhdt !t diltdnr nlld con6t tjds within lhc cmp.mtuB

Fi!@ 4l: Diffirdd dc@l dtiysis ofde @mp6ic aPeidcb al v&iat fills

@nendim wilhh th. lcmp€rerrc tug. 25'1000"C 74

Figuc 44: DifreEnlid MninS oloiD.lric sludv of rh. rubbs nan@onposits

within rhe top.r.turc lpd -74 -45tc te

Figuc4sr Ef.ctofF-MwcNTscorcenhdoGon uhimrt t dile stPnah and

p€ld el$glrid |r b€I ofNBR d,MdPdncs

FiSw 46: Efrea orF-MwCNT! co@nFatios d htdnc$ of NaR @mp.6ir.

sleinasFigDE 17: Filler dis!ftibility Dd @mposiiional mlvsis of EPDM/FNK

specimens hy ft. applicdion ol SEIV,/EDS a2

Figure 4s: Efreol ofFNK @ncenL.lioo, on lhe themrl imP.dan@ of EPDM

Figr .t9: Elfd ofdilf.Mt tN( corenhtiN o thmll condutue of lh.

73

3l

36

b.e mmpciE fomukrio

Fig@ 50: Etrat ofFNK lo.iinss @ th. sutfle ddpholory ofth. ihmal

oosFd l6an EPDM n.ltsmpdiE spein.nr

FiguF 5l: Efel of dilldcnt FNK con@nnrtions on lhemd de@bposilion

en!'mmdt oltu6omporires

FigK 52: Efr6r ordifi.Enl FNK loldinss on rhe .nddcxoth.mic hehavie ol

M(mp6it.Fig!rc 53: Efr6tofditr cni@@ntalio6of FNK ondiffr ialsnning

€bnmdric dulb ol EPDM Mposit s *hhin lhc leop.dure mge -

74-450"C hlir.nviMmdl 87

Ficu. 54: Efieot ofdiffeMr oMttltions ofFN( on lhc strcsnain b.h.vior

39

Fig@ 55: Effcd ofdifr.rnt v&idt conqftri@ ofFNK o t Dlinde bnsil'

snsrn md .hogrrin tt ltsk ofE DM $ein.6Fi8uE t6: Etu ofdifld! lodingt of FNK d rh. .16!omdic h'rdnes of

EPDM speim.ns

Figh 57: SEM nicognphs ofnmok&linir€ di+€6ion d vaimr magnilimlions

(r, b, c) dd @dpositio@l d.lysis ofde l0 wlo/' lMded SBR polyirer

FisuE 58: Efd orFNK to SBR dlio o dmd co'iucliviry snhin rmp€6@mg. r23-t23K (a) od ils willion ot dE divcue Emp€duEs (b) 92

Fisure 59: Er*| or FNK conc.ntrarions on tnc rh.nal imp.dane of SBR

spsimcN wil|lin thpeEnE span 123-521K 92

Fisu. 60: sEM mi@8r+hi ofdE po6r $em.t @rldudiviry Es.d S( I (a), SKz

(b), sKl (c) S(4 (d) FNTJSBR sFcideo ud compGniond aDrlysis

ofth. l0*1% loaded Mposire sp€eimen 9lFislE 6 | | EtrFt ofdif@t FNK on@nrrioB o. rhe d'cmlt d.gd&rion i[ on

cnvnoa. of SER @p6ics sFcimeB in ih. renp€mruc tin25-85fC

Figure 62r Etr6r ofdifeEnr FN( t@dings on rhe rhhll lbsdb.nc ceibilnyol saR amp@ir. sp€cim.ns sirhin rhe LmFEirE ,&Ee 25{50rc i.

95

Fi$re 6lr Efcct olveid FN( concenralioN on rhe DSC a@tysisofSBR

sperme6 ir b.n@n.74-450cc 96Figure 64: Efrer of FNK/SaR mdo on drc 5rlsqrlin conio0^ or ssR

nusompGirs 97FiSue65: Influ.ne ofditr Enrconce GtioDs orFNK on rhc ulrihar. r.isile

sienr!',elmg.li@alb.qL,..dnodutu, I06rZ ct.niciryorlh.fobri*Ld SBR @mpdic sF.ine

Fi8ure 66: Efd of vdiur FNK toodings on tn. e|sbhe.ic hdn6 or sBR

$€.ineBFigm 67r SEM Dicbsr.pls ofFNKdbFdod vana tus,'i€tions

(a, b, c) and oDpoiiriond mrtysis orthe l0 s19{ toaded

Fisu. 68: Etrer or FNK @nqtrrio6 o dE rheo,t onductiviry (r2t,52r Klof potroer iuocofr polit6

FiguE 69: Efiecr ofFNK concenlrdjons on rc rh.mit inFdanc.(r2r.5zrK)orNBR amposia speimcns

F,gurc 70(a, b. c, d): SEM nicrcgnphs ofdE pod d.mst i6spd leddFNK-NBR enporil€

FiSe?l: Ef€ci of FN( @MnlirbF o. tt UFdl &8nA!id ofNBR

lpeiD.B r.sed eirhin rho &nporw linil25.700Pc

Fisw 72: Efr.c oftNK h.diqs o! dE hat rborbing dFbility olNaR

sp€cimc6 t6tod wittin th. tofrp€r.turo li6ii25-1WC

Fbw 7l: EF*t of FNK loadings on thc difedndol snning crlodmedic

@iM of NBI ?qina, laEd wi{in di. tcmFmE

l0l

t0l

linit -744t0qc 104

FisE 7a: Etrd of FNK lodings d d. $twtmin @tos of dE NBR

Fisre75:Efl..roIFNKlodidgsoth.bsit slHgrh.ndelolr.riodbqkofd€NBR@p@n speimos

Fbe 76i Efrer of FNK lo.dings d rh. €trlric modutu .r 100 dd 2OO%

.ldg.tion .r NBR conFlir! s?..ir.6Fisw 77: Etror of FNK lo.di.g3 d ihe €ltsiMqic h.rdB ot NBR emrsiL

List ofTables

Chapt€r I Introd uclioD

TABLD l: Thmal pbpeni€ of $n. mebllic marsilh l0

TABLE 2: Thmal pnFni.s of $n populd ce@i. hatdials 12

TABLE 3r TheD.| PrcD€rti.s oftolymcric mde ols IlCh.pter2 Mrteri.l3

TABLE I I Moib Md d.ncriLe ofde .l6l,omeric nat riak 26

Chrpter5 Results !d Discussion

TABLE I I sljtlin8 composilc of fabriBLd eldlomeric n.reomposilc

sF.in.n 49

TABLE 2: Densitiosollhef6b dt.d clrndmericcomposir.sconEinins

mdihm rinfMqn loding ldcl 50

TABLE I I Efrec! of F-MWCNT, on rhc gt.$ lmnsilion. cryna|jarion, and

ons/pal n.lri.g phe r.nFntuG SR cmposic speinens 56

TABLE 4: Efecr ofv&iadconcenr ions ofF,MWCNTs on the specific

drh.lpies (T!, T., T.r, & Td) of sR nommposnes

TABLE J EEe.r of vtridr @n@Fations ofF-MWCNTs on lhe gtr$ ltusnion,

crysnllidio, .rd fir/sond nehing phe rmp€aruH of EPDM

n$momp.sil6 6jTABLE 6: Efe. of veid co.mdtions of F-MWCNTt on the sF.ir,c

enlh6lpies(Tr,T.,T.,,&T.tofEPDMn.nocohposires 64

TABLE 7: Efi€cr ol F-M\VCNTS on rh. sls hnsiriol! crysr.ltianon. uoons.tp.lk nelt itrg Dhss r.np€drws ol S B R nanocom pos irs 72

TABLE 8: Efect of@idl @nsllrrioN ofF,MWCNTs on lhe sp..ific

.nlholpi.s (r, T". T"r, & T!:) dr SBR nonaomFsirer 72

TABLE 9: E tel of F-MWCNTS @nsrstions on de glas ttrsirior!crysbllianio, dd on*/p.!k nehirg ptE6 r.mFmcs or dE

NBR specimens g0

TABLE I0: Etr6r of vdior Mi..tioN ot F-MWCNTS on lhc spcificendralpiB (T,, T", T^,, & Tr, ofNBR noneomposires 30

TABLE ll: Efrdof FNK lodina Mr.lios o dr glN rN$itioG

crysrallianon,!d on*tpcaknchinsph.es reopfrarlFsih6r were

m4urld fiqn DSC @nl@ of EPDM m@sic sFinens 33

TABLE 12 Efetof FNKloldins@nmtltionsorlh.sDsifio.nth pi.sdma!

ph.$ uunim rnp€6tu8 (r, T., T." & Td) lhd lre m6uEd

liom DSc orconbuofEPDM !p.cime6

Fw DSc or @trroE or SSR spEimens

lim DSC of @nM of NaR spcin.ns

33

TABLE I lr DSer ofFNK lddi.8 onqrlrbns on ih. gtas n rsnioD,

cirr.lliz.tion, .nd on*vpa* mrltinS pnees top€r.ruEs rhat r.EnsuEdftomDSCdromofSBR@npositespeimds 95

TABLE l4r Etret of FNK lording conhbarions on d. sDeific .nthrtpi$ dala !tPha rtuitio |mD€mluB (T. Tr, T.', & Td) dd w.F m@ur.d

TABLE l5: Efrecl of FNK lodins con@nhlions on die stss iamnion,

crFt llialion, od 6ne/p.!l @lritrs phls rmpedrurs fid w.EDecuEd lioD DSC @trlouts ofNBR snposite sDecimcns 105

TABLE l6: Ef6r of FNK lading corcmhriois on th. speiic .nrhalpi.s dlb .tphac rmNitjon cmpelruds or, T!, T6,. & Tto)lhar vere 6c6uEd

Chipter 6 coDcluliotr ![d proposrd future work

TABLE I Overll lheDcncchmical pslomane of F-MWCNTS atrd FNKimpEgnlr.d elEromsic MMposik widr rh. ndinrumeinf@.menr loading ld.l 4

Abbreviations

AcN Acrrlonlrlle

ASTM Aneic^S,adordlsT.sni94tdu.MwntsAES1V Alt4lire Eorrh l'li.qt. tf@l

^ Atohlc Force Micturcop!

ASW 'llMi"vh Slieate Vonl

BD Butdd|tu

CMCS Cdahh Mat & Cokponks

CNIS Cdbon NMtub.s

CVD Chenlcal Yapor DepNltion

DCP Dicrnt Petuti.le

DOP Dioctyl Phathakne

DSC Difercntial S.@ang Cal@inaq

DTA DifeQnnal Tlc@l llaalrsis

FMWCNTS Fun.tlondlhe.lMultiwalhdcubonNMtubes

F-nmkeli,nilc F@dohalized Nwtaoli"ite(F|rI()EB Bonsanon aI Break

EDS Energ) Dispersite X-Ra! Spe.rrctcopt

EPDM BIv'LE Ptoprlw Di.re MoMqI'IBS C)aloh.ol Be@tk@l StWMid.IITIW Hish-Tedryotwelnsrlationvool

MBTS 2, 2 MertaptobeEothhtole DbuAid.

MMCS Me,al Marit Cobpotit tMMT Mortnqillqite

}{RR Acrrlonitile Bdadlew Rubb.r

NK Nawtnolhlite

Nc NMlarNACA Nationdl A.lvisory Cohhi ee|oA.rohdttics

PMc, P0IW lleE Corpo.t&r

PNC! Polrw N@WttbtPCW Polt'etedlbv@IP&MVNT ?tbt/,,l^MvdLdcebo6l{'/totub.tSBR Srathd,,,t'.&dbfSCA Stlat Cotglrg As.dscME S.rNl4Ch.*d & lMt &qr,,.,'bsSEM &adqBldantAaoqtSR $ltoor.ltdt /TG/IITA Ih.rtugarh.Ft/D{aatld llenl l,t llEet

TBC TMWCdfutTGA 1hqtuewtutu,/,rdj6itTMID r&awtuDn&ltTC nsndooieiritlTt n'.l|'olnq.btrUTM Ut@T6/agtddrEUtl Vdl,"d.T.rdt ets,qh

Ch.pler # I

Introductionl. Thermsl Insuletiotr

Tlr€mal iBulalion r.fc^ to Educiion of hot rmfer(the tdpon ot th.thal

eft€y b€tld objects of ditrcF. !.dpennE) b.w@ objdK in thmd o.t cr or

udd the inlluence ofndiatile slM. ftcmal irluladon can be e.sin€et€d with special

n€rhods o' pnesses 6 wll a wirb suilable obj€s sh.p€ ald maredals 0l.

Heal flow h m inevi$ble cosequence of contact betweeo obj4k of difoins

tflp€nlB. Iiiemai nauhlion prcvides a Fgion of iroulalion in qhich lhemal

@nduction n Fdu.d or thmal hdiadon is Fflsl€d arher thm aberb€d by rhe lo$rF

fte insulaling capability of a ml.rial is n6ed enh thedal conduciivity G) is

the capability of a tuteisl to @nducr h.ar energy as a r$ulr of tenperaturc diffsense

bet@n rm poinr l@a1ed on the mtedal rnw themal oductiviry is equiv.lcd ro nieh

insuldin8 capabilily (R-value). In demgl ergin.trinS, othd ihpondr popenies ot

i$ulalins natoials @ mtcrialdeNny (p) dd sp4ific heAl @pacir/ (c, 13.4 I.

To chmse lhe tenpeBtG of a! obj€cr edcBy is Equird ii lhe fom of bear

generaion to increde tenp.ratw, or heat extro.tion to rduce tempeBture. Obe the heat

gdeation or hear cxtraction is &minar.d a EvN flow of heat oeuB ro Even the

lmp€raore bek ro mbie . To @inlain a giv€n renp€nlu€ a confin@us encray ttusfer

k rcquied. lnsulalion qill rcduce $is enercr loss Heat lransf6 rhroush insuhtion

narerial occu by n€fls of @nduclioi, while hcal los lo or hol gain tion altnosphce

occus by neds ofconvstion and odialion [5,6 ]

The wod "Elarded is iopotl&t b65ue no manet how nuch iNulation h

applied. $e ievcs. now of hat ro mbicnt cd never be slopped [?1. nF pdmdy eensfor insulation de mey md vaied, lhe nain ones bcinel

. To rcduce heat los or gair

. To naint3in a temp@lm conditiot

. To nainlsinthe etretile ope€tion ofcquipme or chemicd e&tion

. To asbt in rDinlaining ! prcdud a1 a conslant lqnpenl@

, To plev€nl @ndensalion

. To c.eaE a conforlable envircmenlal @ndidon

I l.l . Clolhi.8 insuldtiotu

Clorhins @ help b ortbl dr hllM body tcmpentr liom $e atiDosph€ric

sgth€r cheg.s. Thict dorhiag i.sulstion is quncd lo comb wilh low mbient

t€nperatues. Veious ryp.s oI polyEcnc coatings have been €nployed o. Itre clolhing

sElaes to anoule their fifrul, nehoical. ard lie eh.d&l ch@clerislics.

Polyureths€, polr@ilitr , polyelcctlolyt , chitose, polym€$yl nethrcryl e,

polysiloxdne. poltainyl slcobouac{.tate, .lc ud thei! conposne costings e employed on

the nalul ed synthedc fiber fabnca b ehiev€ the equiEd/desied ser of propedies 18-

I ll-

1.1.2. Iuildines insulations

A ldee ponion of globdl e@.gy consmptioo can be saved by consruclinS well

iruulalcd buildings $at dininiz. enctgy lN o! rain fom the swundinss A w.ll

isulaled buildine is erdgy+fficidl, thls $viry the oMcr noney srd povides ooF6itbm renperannes thrcushout the spa€ n2l. Thft is le$ tempehtuie g6die.t borh

vedically {b€tw€en fl@r md @iliog) dd hdrcntally fton one wall lo lhe orber. x

Fovid€s r doE @nfonrble @lparr dviremoi whcn ourside rnFEnres a'c roo

cold or hot. Il hd ninimal rcmilg cxp€tue. Unlilc hdtire ed c@lins equipme ,

insulation nal{ial is cheaper md requie lifle to nainlcnmce cost 0 31.

May fms of thctul iruulalion als nduc. misad vibration. viz @nin8

ftom ouGide or otber r@m icid€ a building that poduces ! quicr€' envitunnenr

wiodow i.sulatio. fild can be appli€d in w@then2dion applicario.s ro reduee i.comins

lhmal ddiation in swD.r &d los in w'nllr I l4].

ln induslry, o.rgy hs ro be exp.nded to €is, lokr, or mainrain rhc tenp€nlw

of obj€ts or pmes fluirb. If th.e e noi idulslcd, lhis inc@s lhe energy

fquii€hmti ofa ptuess, thar evcntually imp&t rhe @st and €dibMe.ld issues.

L1.3. Meh.nical systcD i6ulaiioB

Sp4e hqtilg md c@ling syst€ns distribure heal througholt buildii8s b, hems

of pipe or derwo lnsulatitrg th* piFs rcdu6 enerSj/ los md

pevents @ndcrualion i'on oeunine on @ld &d chilled pipewo*. Pip. insularion is also

ued on wter supply pip€M* lo help d.l!y pip€ f@in8 for d aceflabl. tne hnerh

tl5l.

L1.4, Spocenft irsulations

Renty of s!@ vehicle ihrcugh rhc arnospherc genedls ulhnigh tenpe6l@due to conpr€ssio ftiction of the ai. at high speeds. Insdsffs must n.ct denandine

physiql prcp€rtiG beyoad $el lhmat rasfer ct rdet pbpcni$i e.g.

rcinforc.dcdbon{arbon conposit @s @@ ed silica fibq rit* sere .mployed ro

potccr sp@ shuile 06, l7l. DiffeMl t}?es of abtaii!€ lilcs hare b..n desisned,

hbncared, dd aligded on lh. E Gsrruclws for the succestut complelion of space

mi$ioN. Hid puity (99.4%) doryhou sitica fibcE, @boi.€bon @nposirs.aludina borcsilicab fiber. silicon cdbidc, ed poous silica bsed ablative riles have been

ued $mstully s themul Plol*tion sy$em for spa.c shuntB [ts]_ phenolh esins,

erhylene prcpyloe dicne nonomer rubber (EPDMI ntuite buradien€ rubbq (NBR). mdsili@ne tubber wilh nea€rbo@io6, nreilic{, ne@lays, high &npedh@ synth€ic

fibes (glds, c&bon, @rmiq .tc) d€ aho employed for ituularion of inrerconrioental

bauislic misil* (lcBM) rnd solid M*ct noro6 (SRM) [ 15,19 ,20 ].

Inteoal @nbuslioa sgin6 prod@ a tot of he{ duins th.ir combuslion cycle

This car hale a negative.ffe.r who it t achs veiou bot-snsitive compoients such ssmoB, bat ries od $!n€r nolos. As a 6ulr, theonat insuliirion js n*ssy to prcvcnr

lne hat fron the cngine @chins ttEs. conponenF. High p€lfomdce ks onen use

rh€ntul iBulario. s a meds ro imprev€ sgire perfolrlne I2l I.

1.2. D6E ing ptm.t n of.Iamd lulbdo!TIE d6ign of isqlation syslem is gov€m.d by fi€ naubl€d op€radng !al@,

qhich the pl&r rquiis affcr insrallation,

. TlFmal colditioN - He3l los/H€al gain

. Plirc lmFEtuF d@p o. ri*

. Condoetion pcY€trlion

. Pebomel prorection lenp.iatN

. Opiinal @nomic @ndii'oB

' Themnl onductivity of ir$lalion MLriol

1.3, Cbrncl.riliica of tb..Erl iullrtion!

A lot of fetors infl@ isulstio! pe.fotlma of ar insulating mterial

.mployed ovd dy rr?e of subsrari Sone oflltm ,!r as ud€r! Themal coiductivily ('r" hlu€)t surii@ missiviry ('t" v.lue)

. Tllennal heal quenching cllalility

It is impone( to no'e $ar $c lacroF inn@cing p.doMce tuy vary ovtr rimc 6mderial ases or envircnnenl{l condilion! cl@se [22 ].

1.4, fiea tr.nrLr tbrcugb Mrt€rir&

Ihemal pmp€ny of a @rrial ncds lhe rcaponsc of lhe mt€rial ag.insr the

.ppliation of h€r. A $lid aberbslh.dsl mergy in rhe fom of h€a! Ils r.npenr@

ds dd its dinmioB exp6nd. rhe.ftrgy my b. tusponed |o c@l€r regions of lhe

sp*imen if Emperaturc gradienls exi$ ed ultimat€ly, the sp.cinen nav n€I l23l

Thmll isulalion is b&rad on h€sl tDsfcr pheoome@. In clNidl th€modynmies, hcal

is defin€d s an enagy that flows de to temFBtw diffcdce. ll now in a ditection

noD hider lo lowa tcnF.llun sd..c md thk o6gy s neilh€r be obsened nor be

| .4. | . Mods of hel lr.nsfer

The pro@ss of heal lr@fei lates plee by th@ distinct modes:

Th. mehdis of hqt tiesf€r de !o i.mp€6ru'! gndie in starionary medim($lid md liquid) is called mnducdod. Hear @nduclion is know! as hear diffusion, it is lhe

diet nicrospic exchmge of kjnelic .nergy of panicles trough the boundary b€rs€en

vhd m objct is ar a difieEnl rcmp€aturc fiDn arorhs body or irs swudings;heal lrmfes tbrcueh @llisioddifflsion, fron the body al higher tcmpe$lure lo lhe body

al lowr lonpcEtu€ stans. TLis p!@s of han Fansfer comes io cnd *hq borh sufac€s

de ii thedal equilibriun. DE law which d$c.ibs thc de of heal hansrer rhroush

condwtio. i5 lnoM d Fouicfs tsv. A@rditre ro rh. bq 6le of heat @nduclion

$rcugh $e plane layd is di@tly proponioul ro lhe tempeErurc ditrs.nce dcoss rhe

byer md thc heat lrdsfr acr, dd inwely proponionat ro dr thictness of dB taJtr

1251.

Rale of h.ar,o0dqrion o (aRx!.mpeDfiE drlTee.e)// fiictnessl (r)

Ifr, a in FisuE I in a mediun rhrcueh which

Thus according to touiels law

tEr u coGider a rDpcrar* dirltibution

he.t is being @nduclcd alo.g x, dire.tion,

(!)

whee Qeb Or,) is dE alc of helt flow per oit ea nomal io th. diEaion of heal

nos. The ninus sign in eqoalion (2) indica€s thai heal flos i. rhe dir€cdon of deceasing

lenp.r.tw. l. th€ preseit €e dtd is negldve ed he$ nows h th. posilive ditdion. r(v/n-K) is $e poponiondiry @Nrrrt and is lnoM 6 thermal @nductivily of the

matcdal drcleh rhich hclt is beins €onducted.

FisR | : QmibLi w d$cdpt,on or Fouiefs hs [25]

Convection is lhe $@nd mode of {€.gy rresfer berween sotid surfee md an

adjqnl liquid or 8!.s th.t is in motion s shoM ir Fise 2.

A@o.ding !o the NeMons hw of @ling, rhe lare of conv*tior heal rester is

proponion l to the tempdrure diflem@ dd hclr tr.6f.. a@

Rate of het snvet@ o (dm) (r.Dp€nlurc diff.Ence) (l )

Let us consider the flow of cold fluid al a temperalute L ovc! a he.red sufaca at a

t€Dp.dture I,. -11'6 hcll tr nsfeft€d ftom lhe su'tue !o the flowing 0uid due ro $econvectio.. According io rhe NeMon\ law of coolins is given as [261

a-.**= tA G, - r-)

wh.E 9."@ Ov) h thc Ete of h@t tader by onvecdon,,r(o') is the hd rffit€r@a, /I=f L - ru, is th. difTeren@ b€lw@ lhe suface t€np€rature ed nowing fluid

lenpcntuc. I 0r7rl-X) is rlE .v.Bee conv.cliv. hear tesf€r c@mciht oE lbe ea ,4.

6mp.du'.r,

FigE 2: Conveiiv. hel L.nsfq fom $lid su.fe lo moving fluid 126l

Th.y mi( Ediation ar loM rat. rh& 6rt of idel body. fhe@forc, $e Ere of cmisjon ofradjal e.erg/ froh a real body is qinen I

Rale ofddi&rhe fler8y = d. Arr (6)

wh@,1 (m'1) is the suf@ ar.a, I(K) G lle aEFnnre of ihc surfsce fron,hich rh.€nqgy

^ b€ing radiard md r is lhe S!.fe-Bollznm @6ranr (WmrK4) !iz.ind.p.ndenr of sulfd, n.diM, ard t np€mtorG, Th€ . js tnoM 4 enissivity viz equal

Thc find n.jor mode of hc{ rzrofr is by ndiatio4 qhich @y oNu rhrtugh a

velh or ene lrsparcnl Fcdib (elid or !uid). Any s!bsLr@ ,r a fnite lemp€flture

enils energy i.1h€ fom of€leclromagndic wves in att di@ions @d ar all waveleryths.

nlis €@sl, tesfd t@ogl photoN k loom 6 rh.mal ndiaior Th€ dounr oflhemal radiation emitled by a surfrce depe.ds upon irs absotule tenpeBrure ed rhe

nar@ of |ne sufac. 121.

Aeording b lhe Sie&n-Bottdtu t.w, the ar of r.disr energy cmitied fton $csurf&e ofe ideal Ediator is also krom 6 bldck body

's

giee. by

Rore of adtur hear en.r&/ = dAf 6)

lo th. Erio ofFle ofdision ton I! l bodv lo 6d A@ tt. id.al bodv bolt b.i!8 tl lh.

s.rc raFdlt I 'fte ddi.tid bdt rnnlfd bctr€.! . tu.b.! .ad iB surounding is

FIg$c 4 shos dl thr!. hods of h.{i r.n!fc!. In lhls car th. heqt conducild

thDW! lh. pld. is t!futld toe t!. pl.t. stre.c by r coi,.irdon of @vccrion aldrddiation. An cner$' t.larE o! tb. pbr. i3

Figw l: Rldiatd h.a! tra$ftr b€tl{q ,'rh.€ .nd iE ,unoudiner [2?]

Coldu.lid .1..5' - C@vlctiu 6E| + Xditlid cr.rgy

-u*= -M(r,-r) + c.AQ! -r!) (7)

6qndFi8@ 4: Coobi!.tioD of@ld[dio4 c$vectio4 ad Ediaiion heit $.I|!fd 1221

1.5, Tldrndl conductivity of nrleirlg

Thcmai co.dNtjon is the ph€nomcnon by which her is t sponed lion high 10

low-tenpsature legio.s oI a substaicc, The prcpeny that cheaclerizes the ability of a

nEledal io trdier h.at is th. tiemal cond@tivily, Il is ben denned in ims ofeq@lion

2 wh@ P ddores the het 1lux, or hat flow' Fr unit lime per unit area {@ bei.s lalcn

6 o'at p.rpeodicul& ro th€ flow direiion). r is thc $mal conductvny, md dTdr is thc

rmFralue sEdi€ $rcleh lhc codetine m€diu [28]. Ilp uits of q md t e wnr(Bitnlh) ed wn-K (Btu/fi-h-F). €sp.ctilely. Equtio. 2 is vatid onty for steady-sllre

hd ltoq that is, for sit!.lions in *nich lhe h.at flu dB nor chdge wirh rine. Ale, rhe

ninus sign jn lhe expression indi€tes thot lhe dnediotr ofheat flow is fron hot lo cold, or

dong rhe lenpenrur gEdiat. For fic$ €xpBsio6, r is ,nalogos lo rhe dimsion

coefficienr D, ad the redpmrlE gndiqt paallek lhe concenrralion gndieo! /a7d I29,

301

1.5.1 Mechaisms of H€ar Conduction

Hcat is Fdsponed a! eud @i.rials by bod tatdce vibElion @ves (phonont and

fEe eledlons illl. A tbeual condwrility h Nscialed wirh eeh ot rnee nechanisds,

&d Ihe iolrl @nderiviry is rhc sm of rhc two @niriburion$ or (x = rr + &) whcB & ddr, Fprcse.t the lattice vibalion ed el@tron rhemal conducrivites, Espectivetyi usullyone or ihe other pEdomimt*. Themal .nergy No.iat€d with phorcos or latlice saves is

lmspon€d in the direcdon of fteir morion. Thc & cotuibulion csllls fron a oet

moveneot of phonons tom higl lo low-tenpsarur€ r€giols ofa body rcrc$ which a

tempeduc gEdi.nl exi$s. Frc€ or @ndEting cL.rrcff Fnicipare in ctctronic lhe@at

conduction Kinetic ene4y is imparted io rhe f@ €l€clrons in the hot r€gion of the

speimcn I25l- I1l.y lhen ni8rare to @l&r a!4, vheE som. of 0!i3 tinedc enersy is

rtusfered to the atohs rhenselves ls ribndonal €nerey) 6 d consqu.nc. of collisions

wirh pho.ons or oiher inpe.f.clio6 in th€ cryst l. Th. Elarive @nribltion of t lo lhe

lotal $emal @odkdvity incEA6 wirh inftasine li@ €lecron concendalioni sincc

no@ elecmtr re availaue lo porticipatc in $is hcar rrmfeEne pme$ 132,33 I.

L5.2. neai @nduction through m€Dls

In higtlpuity ner.sls, lnc elc.ton ndhdis of hat tr&spon is nucn moE

emci€nr th{ rh€ phomn co.tribulior b.csuse electrons e nol s esily scaltered as

phonoN ud hav. hieho velocilies. Funhcrhoq n€tds @ extemely s@d conducloB ol

hqt bease Elsrively lee€ nMbss of fc elelrons enst lhd panicipak in $emal

conduction []41. Thmal conducdvnies of sevml of rhe connon nemls are sileo in

Table I &d thci vales genddly tuge betwen 20 to 400 V/n'K. Since lrce eleltons

sn Gpo.sible lor borh .leidcal and thcmal cordslon h purc mclrls, thcoElical

trealhents suSgest thar the 1wo conduciivilies should be Elared @ordinS ro the

L-W'l (8)

whqe I is thc .lectdcal condetivity, I is th€ dbslutc lemp.rsturc, ed , is a cosiant

bou s rrEM nmber.'Ih€ lh@rcticat vslue ofr, 2.,r4x10-8 o -wlK)r. shourd be

i.d.pendenr of remFratur dd rh€ erl. for all me|!b if ths hed en rC/ is u-nsponed

entirely by fee el€crro$. Included in Table I e rhe expeihcnhl , valucs for tescs.veol net l$ note $at th. ag@ndi betwo ed th. th@r€licd vdlu. is quile

caenabl€ (well w'lhin . fmror of2) []51.

Alloying metah with impuilies Esult in a teduclion in the themal conducrilily,

for $e @c rcen rh6r fi. €l@tricd @ndeliviry is didinishcd: nmely, lhe impuiry

alohs. esFci.lly if in elid elution, a.l d $anering enleB lowering lhe emciency of

TABLE l ftemalpropenl.r ofsone ncGltk Mcrials 1.251

C. (Jlig-X) (rc' 0121.6 2.24

336 t70 t98 2.25

l2a t4.2 I5 .1.50

|l.3 271

:032]5 428 .1. tl133 r78 J.t0

1.5.1. Heat trmf€r elmicsNon'ne$Uic naiedals ae theml imularos in a mucb as lhey lack lase nunbeF

offre .l@106 (371- Th6 ti. phonos sc pri@ily 6po6iblc ld lhemal onduction:

r" is much snallcr the 4 The DhomB @ not 6 effeeivc as fEe el.ckns in rhc

rdpon of hsr enetg s a result of $e very cfficieni phonon scattering by le(ice

inpe{€.tioff. Th.nn l cond$iiliry Eles for a nmber ot emj. dal€nab aF

labulat d in Tabl€ 2r Mn.tenperatu€ rhemal @nduclivilies tdge appoximately 2-50

v/n-K. GIN &d olher doryhou cffics ha!. low @rducrivities $6 dysr2lliie

cemic5 since ft. phonon scaneine is nrch noG.lTe.tivc whcn rhe atomic srrucluE h

highly disodeBd ed ireguld[38]. Ilrc saftdins due to laiice libnioN baons nore

pDnounc€d wirh rising lemlEonft: hence, rh€ rh.dn ] co.drcdviry of nosr eEnicmatedals domally diminish.s *ith i.sr.si.g €hpenrne, a! lea51 at rehiively low

r@poatuEs 6 een in Fis@ 5 [39].

I5z

d

d

T€.rpEdure eC)

Figw 5: TenpeEture depeo.L.e of ihmal @rductiviry for ev€'sl @mic nare als

Figu€ 5 indicates ihc @ndwtivity b€giN to incre4e .l higbq tenpera|ues, which

is dE o ndiei hst Fesf6: signifiMr qudtis of i.fBred ndiel hal n.y be

tmponed 0!oud a tNpeni emic naierhl [40]. 'Il. et]]chrcy oi lhis ptoces

inc@* wilh temp@rw, Porosity in ctuic malcdals my have a dmatic in0kn€on themal conductiviry; incBing rbe poE volu. will, undei host cilcudstances, resulr

in a cduction of thcmal condNtivity. Ii fac! Dey ct@i* th.t e uscd for $emsl

isulalion @ porous. Het rrdsfe. acoss poFs b ordiMily slow ed inefficient. lnremal

poEs iomally @nr.io still air, r,trich h6 d €xlr€Dely low dr@al condEtility of

appbxinatcly 0.02 v/m-K. fun[@or€, gasus co.v.ction wirhh the pors is sle@oletilely ine,Ldive [41].

TABLE 2: TlEdal prcperti€s of sone poputd ce€mic maleriah [42]

(J/kg-K) (K110-)

1_6

)7.7

1.7

350 l.l

l5.4. Thmal Co.duclion 0hush Polyft^As no[.d in Table 3, th.mai snduclivirie! for nost polyneB de on the ordd of

0.1 w/n-K- Fo. rhcs mt riab, oer8)t rtusft is e@dplish.d by de yibnlion ddoration of lhe chain holecul.s [43]. The maeritud. ot the themal cordudility dcpcnds

odt!.tlcSrofcrysrdlirityi!pollner*irhabighlycrtstallin.ndordeed$rucor.will

have a gGarer co.duclivity the de equival€ dorlhous mar€nal, This is due ro the

nor eftecive coordimkd libhdo. of $e Eol@uls chaios fo! rhe crysralline srate.

Poly@u m otun ilied s fiemlt iNrlalos b.cau* of th.n bw lhcmalcond@tiviries [44i 4s]. A3 wifi erdics, thei. imulative popenies hay b3 runber

enhoc.d by the inuoducrion ot sDAll poc, f,trich @ odiMily inrodued by foamiry

duiog polyrerianion. Fod.d pollstycne (Styrofom) is comdonly Ned for dri.kingclps dd instnaing ch6ls [46,47 ].

1 ABLI 3: ftemd Prcpenies of Polymeft Materiils[zs.4 8 ]

(J&c-K)

t350 106t98 0.4@.50

t925 l4ll30 0t2ll70 0. tl

t2G2t6 0.t5

c = dQ/dT

1,6. F .(on sfietitrg otr theroil colductivity

A solid narenal, whe. heated, .xpqien@s e inc(ts in tenpcdrre si8nifyihe

rhal sone energy ha ben abelbed. speific heai @pacny is a Fopeny $ar is indicalive

ofa mar.rial s ability to absrb he.r filn rhe surmundings, It Fprcsenk rhe anounl ofenergy rcqli€d io produ@ a unn lenp.dlw n$ in a uit D8s of lhe material [49]. tn

naihen iol lms, |he hdl €p@iry C is exp6*d c lollowr:

(o)

qhft dQ is rhc m..&/ r.quircd b p.od@ r dT rempeniure cbsge. OdiMily, her.apaciry is sp.cified !s dole of o.tcrial (c.g., J/nolK, or callmol,K). Spccific hed (often

dcnolcd by a lowrcde c) is sonerimes ued: rhis rcpreenrs $e he capaciry per unir

h6s ad hc vdious uirs (J&s-K or cil,7g.K or Btu4bm-F) [251.

The!€ de lcally lwo ways in which hqr capaciry d.y b€ measued, @ordi.8 to

the €tviromenlal condidons accompanyine iic iran.fer of h6t. Oft is lhe h€l €paciry

(Cr) while nainuining the sp.cimen volme @N|m! tbe oth{ b for cotutht exr€mal

p6sue, *hich is dcnoted C,. Thc mgniude ofc! is dlsys gEarer rhs C, howcv.r. this

diffftnce is very sDall for mon $lid n dials at rcon tcdpmrure lnd below &dhoseler lh€ t'vo cm be considc€d equal for solids.

I 6.2 Thickn€ss of insllaion haterials

E fed@*s ofm iEulalor is idi€l€d by i$ Eshtane valuc (R-value) which is

R=d( {10)

wh@ d is the thickrc$ of isulating lay* dd ( is the themal conductility of insuladn8

@t dal [25]. Hiehq the R-El@. rto low wirh the eMgy lr"sfeE 0'rcueh iBulaling

layd. So, dte R-value is di!.clly popodional lo the insulator lhicknss ed iole6ely

poponional b rhc lh.md onducliviry.

The effes of lmp€ratue on rhmal condlcfvny h di0erenr for merah sdnomeuls. In meEls, themrl @ductivity h primily due 10 fe eleclbns ed in

noMerals is miily due 10 lanie vibraionr (p[onont ta4]. FouowinS Wiededum-Fl@

lawof themal @nduclility for met ls is alprcximrcly pbporioml ro &e absolute

lehFEnr. (in Kelvin) rircs €lericrl condNtivity. h pE meids rhe elecui€l

coDduclivitt decleases wilh inca6inS tcdpedlure od Ous the producr of rhe rwo, the

lnemal condwdvity slays appmxirarcly @Eran. Itr atloys th. chege in .teclric.t

conductivity h usually snaller srd rh$ rhmal condudivity inclles wi6 r€mpelaluel

onen poporion'l lo lenpedrurc. On ih. orhd h@4 rhmd @ndedviq/ in lonmerals is

nainly du. lo laftice vibnrion, (phonons). Exepr for hieh qurliry cryslats low

l.mpetuwi Ihe phonotr Dw lie pdh is ircrcsd sienifi@lly .t tow rcnperahfts.

Thu the ficdnrl condeivity of nomcrals is .pproximarely con$mt at low r€mp.6lures,

So, below Dcbyerempdatu€ (he rmperalue ihal @ b. achided due ro a singte .ornalvibFtio.), rbemal @nductiviry dccltls [42,50 ].

Wien a natcii.l udetgcs a phse chag. fon solid b liquid or fron liquid toga, the@l @nductivity nay .le ch..ge. Ar Mple of 0ris Noutd be $e chase in

thcnnal cond@lility thal o@w eh€! ice (in€@rl .onductiviry of 2. 18 W(n.K) at 0 "c)helts i.io liquid warcr (rhemal @nducriviry of0.56 w(6.K) at o "C) []21.

PecrynalliEsubcrrl6 @ .xlibil ditle@t rhcnnal condudiviies along

dilfere.l crystal dcs, due lo difernces in phono. @upling atong a given cryslal

dis. SapphiE is a nobble ewple of vdiable ihcmal or'ducivit bed on onentatio. ar

sne lenpddturc (100K) wilh 35 W(m.K) along the c-dis &d 12 W(D K) alons tbe a.

dis 151,52I.

L6.6. El*lrjcrl conduclivily

In melals, (hmal conducriviry lppoximaiely lracls eleEical condudivny

according lo the Wie.lemm-Fru Law, os tely moving lalence electons tnnsfe! not

onlt el€clric cftnl bul al$ hal encrSy. However, the genedl conelaioi betweei

eldrical and lhmal coidrct ne do€s not hold fo. otlEr noo-mct ls, due ro the inc@dinpono@ ofphononcdis for h€ar in non-ncrah. Highly elechicauy co.ducive

silvr is le$ thcmally @nduclile 1h6 dimond, which is s eletdcal iGulald 142,51 l

!.?, Typer ol Prrtical Inermll llsuhiione. Celmic insdatoB

. Polymeric imulatioos

1.7.1. Cemh lnsuladons

Ce@ic i6da1io6 e oE of the @jor lt?e of Ihmd iroulation. Ce@icinsulatio.s have high heat cdpaciiy dd low th.@l @ndulion that mable rhcn ro be

uFd in a wide leiely of applicalioG. C.ruic isulalioG cs be used .s spdk-plug

iNulating bodies, efilcto.y biicks, emic *ml, high l@pcnore wool dd e'utthcmal bmid coaliogs Gombonion liG, ti6t{ra8. blad*) [54].

Ccrmic insulatiohs dc $bicred 10 tulfill1h€ fouowins prcFniesl

. HiSh n.ltilg poi

. No phas tusfomation bdw€en Mm |enFrature &d op@tion redpenlure

. Low themal cooducdvity

. Chcnical inenn$s

r Themal expesio. mtch wirh the netallic slbsrare

. Low sinterilg Erc of lhe pooE mi€roslructw

Alrq, Tioz, nuUire, CaO,{rgUZt.>,, 2i'l,on ed r^zzhoj e frcqEnrly usd

cermic insulalions as lhcrhal bdid coatins [5s, 56]. Alk{line Eanh Silicare vool,polycr'sdlinc wd &d Aluminm Silioie Wool rc u.d 61heml imulation w@l J25,

L?-2. Polyffiic insllarioN

The *cood major clN of lhmal insulalioD is the polyn€ic themal insulalions.

Polymeric themal iNdarios have be@ne otr of th€ nost pronisine rcsdch @6 inlhe neE of polym( $iftc ad t@hnolo8t. In view of sy p@.$ing, low deNiry, odlo{ cost, they de widely used in sJery appdh, aerospee th€mal prorection systens,

aeo j.ts, aubnobil6. buildings, eletricd $d €leuonic alpli&es, etc. 0 5, 2ll. Usudly

polr!rcthde, ethylen€ propyl.oe diene nononer, and expmdable polystyene tous aE

ued s themal insuldioB. Dif€r€nl typ€s ofela$oneric rubbe^ sd lheir conposircs in

de fom of@adngs or shers aF.ppli.i ro th€@dly iBdde lh. buildings, ,uonobiles,

gloves, elc. NdorcinfocnncLs hav. ctlciently enlEn@d the lhemal insulation chde&rof virsin polyno sysrtu- Ahons rhe eoebfoEem.nls, wbon @oiub.s (CNT' ednmoclays ccupy lhe princ posnioi. Us of CNTtclay in th€noplGtics likc

polypmpylene. md polystyrcne, er. aF widely studied. Rec€ndy CNTVclay rubb*

M@omposnd hav. also Eeived sp..ial afl€nion. Fillei Eirforcemenl is morpronounced *nh non c$lal-lising syn$etic rubbeN tre silicone. NBR and SBR

onp@d lo EPDM vhich udcees crystalliation on $retchi.8. In rubber

einlbrcchenl, the most imponer cheadensdc of rhc reinforci.g filler is its snall sia, so

llat ibe panicl€s hale a ldgc surf@ aree ro interacr wilh polyDeric chains of rubbe!. tn

addnion b p6rlicl. sia dd $rlcluEs also inflEoe ils BilfoEing efficimcy. B*aue oflhese excellent propeni€s, CNTs/clay cd b. used ss ideal rcinfoEing Illler for bish

p€rfollMe polymd onposiles. Ajryd el al. [5?] dponed the fi61 polyher

nuocomposnes using CNT5 d nlbr. The nmbq of anicks md paEnB h polymer

cohposires conbining CNTS is incBiis ev€ry y€ar [58]. variou polymq mahicB de

us.d fo. .onposins, includin8 themopla$hs [59-61], $mNuins Esitu [62, 6]1, tiquid

crystalline lolynen [64, 65], eleFslubl€ polymqs [66], conjugatcd pol)he6 []1,

do.8 otheu. fte p.oFni.s ofpolynd nd@mposites lhat s b€ inpmled due to $e

prcence ofcNTvclay iocludc rosil€ sf.nsdt 167,68 l. rdsile modul$[69, 70], roughies

1711, ph!$ trflsition tenp.Bre [?1, 72]. therm.l condudilny [73, 74]. dd rhemal

ln the pre@nr dissenalion. we have i.vesdsoted $e prcpenics viz, rhcmal

raspon, th€ml dcSmd.rion, h@I aberbing calabiliry, difercnlial sni.8 dlorjmcric

dd nehmical propeni.s of elasrmcric M@Fposi&s bas€d on muhiplc tuofiue^

.einforced ii vdious polynciic darices.

Thc following eldtomeric nairix md @ofilk. syslem hale ben f.bdeted,

ch@Gri4d, and dieus.d in this eelrch m* [22, 2]1.

l) silicon.l6lon€r (SR).fuctionaliad mulimu.d cebon mdubs (F-MWCNT'

2) ElhylcGpbpylenedicn m@n6 clElomd (EPDM)- F MWCNTS srst 'n

3) Sirrcn buradime elasroner (sBR)- F-MwcNTs sysren

4) Acrylonilrik buladio. elaslon€! (NBR)- I-MWCNTS sysien

5) Erhylm pmpyl4 diene nomrcr elaeonq (EPDM). Fuc(onaliad ndftlay(FM) sFtem

6' Avylonikile bukdhi. e|8ronq (NBRI F\X Brsro..

7) stFne buladie@ .la|(lnq (sBR! FNK slst h

I 7.21. F-MWCNT/S8 tltten

Sili@ie ElaroDq (SR) bas shou good flexibility, thcmal slabiliry,

el*Fi.!l tsist nce ed di.lectic strsgh dre !o the high cns-linkinS d€ruily.s wll 6dcgree of polyndiation. SR conposit s aE used for a wide rdg. of lpplicaio.s from

s.n$r tech.ology to ndd ab$rbilg mat@.b. An int@sling l@iw of fic SR

conposiles is ils Etenrion chrfflqistic ehploy€d ovet thc bDad lemFmw @gc,100

to 3 looc and due to this unique specl thcse composiLs de ued in door and wiidow €als

of rp@ vehicles that M.in 0€nbb ai low temp@t6 enlert jnet .t upper temp.rruE,

or ud in ov€n door sb $,tich must ritb$rnd ln8]t tenpcoturs. At nod.Et€

tehp€ratures, SR @opositcs denotuhate ur imiled life. SR composites have also sood

n(hflicd strEnsLll eilioce. !d elongarotr dt bEaI [75,.

c&bo. nuotub., a homoe*ou b€@re suucrw of ca6on atons th2t tmthenslves i.to a ruh. in lhe preencc of a suihble calalyst and uds specinc

pEsudtenp.Etw @dnioro, is a mekabl€ i.ventio! by llima in 199l[?6]. Trlis

cdbon ph6e ba oFned rcw hoda6 ol study in .lnosl all fields or cse.Rh &d

dev€lopnent. Cdbon ndoub€s (cNTt h6v€ a flomine.t inaee mons tbe nanofilles

fmily due io lheir outlsndiog f.alws, Th. elNlic Dodds &d t€nsile slrcogrh of the

Motubes ft equ.l lo fiar of di@ond, i.e, I T€E PNd dd 200 Gi8! PNal.

Esp.crivcly. Calbon molube (CNTs) al! b.li.t!d !o b. rcmdtable filld for PolFcr

mar'ies de !o irs high spccl r.iio (!P b l0'), $.nMl ,talilily, €l€.tii@l poFrti.s

sDecific sude. sla (l3l5m?8) std low d.nsny ( I 38/mr)

C).rTs hclp in a$,ncii8lhc thcmtl, nechmicd !d .lccuomtgn.tic Fop.nics ol

polrn* conposir.s. Thc incoDordion olCNTt in a polymq hat is.hdlcnSing task

drc to irs hydrephobic Flue lnd van dd rub i lddon Mong de nm$b.s thrl

aggloncdt ! $cm sld podu.c difficulty lo disFrs.lhltn unifomlv in th. polvmd [77].

Thi3 prblcm is r6olv.d by th. modific.tion ot lh. MVCNT! Eing dirednt

tuetioMliatio|r ir.di{ion, snd polyM codinS t .lDiqu6 thd cnhde $. molub€s

conradbihy wilh thc polynE hllrix 178,79 I.

F MwcNTs wd u$d to fsbdclt F-MvcNT/sR polvmd naroconPositca lo

cxeute dic cfrer of t|etub.'s loadirg on ih. th.ln l @ndutivitv, $em3l imFd&cc

|hcnll sbbility, cndott\.mic clp$ility. snd ph!s. ttsitio! tenFdtw of th€

!.7.2.2. F-MWCN EPDM tts.nErhyl.rc ptlpyl.n di.rc mrcmr doe.mt (EPDM) i3 . rvpc of $|!nl.d

synthclic clstorlcric polymd. fts Pcrfomrne in lighl, o(y8.n, hei. ed paniclldlv

oDn. .lmoahd! is sigif@t. Th. lcy pr.lrnetd of EPDM are Fladvc @nl4c of

cthyl* in thc polync chlins 8d lhc alL.Mron in thc conommr comPosilion of

div@ chris 1241. EPM ed EPDM .la$ond wilh .$ylcrc conlcnls ssr€r thd 60

nol% @ ircBingly c.ysttllinc rnd e bush EPM 6 bc vulcanized ddicauv uins

D.oridc @$lint E. Th. eri$.ncc of d td di€ft rcnomq in EPDM .pPrrcs

@nrcntional subhur wlc5nizdion .nd oth6 vuldistion sy$cni lilc rcsins at lhc

D.nddt sit6 of uNnldion. v$ious nlls lit csttd bl&k, silica, chys. clc cintrods.d blo th. EPDM polyM to a.quiE thc dd'tld hehdicd, rhcmal, $d

.lcticd Fop.nics [2 ] l.

Ircr8anidoryldc nonn.ls (iDDds, imubcs lDd mnofibc6) hlvc bco u*d

lo fabriclc n.r|Mmp6itcs for speific lPPlic.lioDt Thc* @Ndc Gintoffi.nlt

dhm. lh.mal, .lccrrical, rEgn.ijc. tnd ndhdicd pmFni6 ot lhc hosr datri@s due

io rh.i 1.r8. speific rutfe. arla .!d MGcd. i d.tion wilh th. ciPicnl Polvhcr

nsMompcirls (PNct G b.ins u!.d in . vsicry of ficlds swh a &$pac.

1a

Eutomobile, medic61, ed c.Gtrution. PNCS uslallv hrve low de.sity wilh hiSh slrength

b w.ielrt mtio 6 @npoFd to melal and cc@ic oat'ir @nposit s. Multiwlled ca6on

.dolubcs d€ used d Einfor.iog ntld i. PNC5 due to iis ou6andinB slreoslh' lhemal

stability. el4trotu8ne1ic eff€cls, ud fir rcteddt caPabilirv lEol Five diff.F t F

MwCNTs @nce raio6 v@ i roduc.d inlo EPDM el4lomer ro fairic.te polynei

composites for llFno-n€chmical invesiSrtion

1.7.2.3. F-MVCNTEBR srn n

StyEne bu1adi6. elstone. (sBR) is prcduc€d wins cnulsion or sollton

polyme.iadon. SBR onpGit€s e Nd in iiE teads, conv'vor bell €ov€s! gskels

nds, sh@ el6, ctc due to ils er@ltcnt nnpict stEnSth, 8@d r€siliffi' t€6ile src'$h'

ablasion Eshlsce, net llic adhesioq l€ar @sisiance, acid resisrdcc' water resislance ed

Mintaic flexibility a1 low rhFratasSBR is ! th.mopla*ic el6toft., c6unred with lhe addiion of a csdinkn i e

sulphu, pdoxid.! ot odistion cmslinli'8, etc' Crcsslinled els$oderic natrcas have

b.rq fimd stabilig, n@harical $i.ngll! agins resbt'ne' abdion Esisknce' weaiher

fsisrrne ed ld sftngn compard b 0r Fistitrc Polvmet @Eix t2ll

Dif€.ent filt€s (ndoolavs, nanocebon. 'dosilic4 cdbon nanotubs' gnphenq

silicon ca$ide, tlurina elc) have b€d used to hilor the th€nnrl mehoicsl' adhaion'

abrasioq etc prcFrtis of SBR [81] Duing lhe v'hiclc operalion' hdt poduc€d due ro

lhe fiiclion oI tirc surfs. wilh @d thar Mv degrade $e nNhanical dJensth of the

€b$odd. So in ods !o sus:t in lhe hahlnictl sE ngth of riF $cmal € |me of $e

.ldoner should be conpatblc F-MWCNTS eMklblv influenc€ thcnal characrctrn'cs

!iz. rhemsl skbility, mdoth.mic capabililv, T& T", T'L' dd Tin as well d m*neical

p€rfol)@e of SBR ctdorc. Five difcc't F MwCNTs concenmdo6 wR inuoduced

inlo SBR elasbmc. 10 fabiotc Polld* conPosites for ihqnGDeh&ical iivesrigarroi

1.7.2. 1. F-MWCNT/N BR ststen

Acrylonilrile buladi.nc rubb€r (NBR) with suD'rb $6nal/mdhdisl prcpenies'

oiL4iol u ageine, and sselli.g cai5Ln@ hlve b€'n cxt€tuivelv u*d in altomobilc ed oil

indsltles l23l selelion ald deiigninS of E @DPosile for t speific apPli@rion

neessit tes ilg themel idispott/dduanc d.ta

Du. to th. exceptioMi ch@crer of th. I]mlub€s, Its€4he6 aoud $' wotld

hav. inpegmtcd them in NBR matrix sing wios pro'sing c'hniq@s lo dcvelop

mo@rposit€s for e4ineeriig apPlicaliois, ie., spons indusq, aulonobil€ induslrv'

ensSy $onge, o.dbme lecbDloeJ, e6pe induslrv 'nd

ltmy nor'

HonoseMult d'sp.Fcd mtub.s develop ! n.t*oA m ' Dobftr Mrix Utsr

rcsiricls the thmal dobility ol polyn€ds chai6 in $e hqt ahosPhqe So' sEau

qunliry of ndofiUcB 6 atutablv inpow fie phFicd ed chemicat chdcle'isrics of

the hosr nairix [22].Iirc difi.Mt F-MWCNTS @nccntalioN wrE itrodN€d inlo NBR

€lasiomer to frbticale polymtr conposites fo! th€no'm€chatucal irvestigat'on

17.25. EPDWFNK sttted

An exc€lleni dbpesion of fild l€lullilg in good adhesion al rhe polvmer/nll

inrerfec is thc bsF Equcn€nl for &hieving. o mh E nlocmcnt ed lo$ h) $eresis

in clsion6. Ndoclays swh s s4onitc, hdene, kaoliniie dd montuonllonn€ @

*idclv sed a! t€inforcii8 fillo fot .lasiome' ed diffeE polvDe6 ll'eelbe

nd@lays hav€ a $41 pordtial for cbslF einfocmts due ro their abudml

arrilabr|q. incxFNn€ dd nalural odmne chdscldis'ir Kelinit€ n d lluminG

silrcale mme-al clav haL ints la) eRd sdcru. u*d rn parns medrcin's rubbea ( osmarici

ctc. Ndokelinit (FNKJ is c.tud€rd s d eflicient 3ub6dnLion for sitica ad dbon

blek which havc o be nixed ar hieh loadings in odd ro slrdin th' se perfomsne sih

low concenrdrion otNK Addniodallj.l obrrued $ar helps he elsromenc cornposire

|o mai ain t modou 64hdjcal pbp.ni* evo '8q

the 'xp6re

of rhemal ed

ch.mical envionne.ts [821

EdrJlene pop)lene diene nonomq elslomer (EPDM) is m eldLoneic pobner

p|lpa.ed bt sluliotr or dulsion polvftrization EPDM hN €rellcnt mechdical o@ne

Bi${r od lherul rsi$are ch{a.i€tislics Efr*r of th' vui&l FNK conmldl'oG on

thc $enntl lrdJport dEmalskbilitv 'ndothmic

capabilU dd Fecndical pmpenies

of EPDM @mDcite sp€cincn is eportd h'rc'

I 7.2 6. NBFJFNK srtten

l2y.Ed silidre nincd clat

polym€r @tric.s (ePora, dsroh@c

kelinile (AlrSilOdoHI) i3 .xrdlvelv sd 'n

m.tri6, Dolyvinvl cholorid.. polvfinvl al@ho!'

erc) b tailot rhen cheoical, mah&icst, thcmsl, .de.plioD dd biod.sddablc PoFnies

Isll. Neol@olin enDttably i.tlud6 the physical md chmic.l ch@tcrislics of the

base polynq nalrix. nmal sllbilily, adolhmic or exothemic ctplbihv' lhemal

eoduclivily, lhemal inp€dflce dd phse tidsilion Pmp€dis hav€ tI. k.v mpodance

lo detn. the unable l€np€Blw .an8. of the pollner nmocomposiie lor vdietv of

applications, To enlzc lhe thenal €nduancc md dinitish the demal llesfer thtough

the rolymr Darrix, @o clays (taolinitc, hallcile, montlodllonir€. b'ntonic etc) have

b.d incorDoE|.d in the host n rrn [84l Efiel of lhe vdidl FNK conenlratioN on

$e temal ir.6!o.! ftmal srlbilitv, .ndothcmic epal nv' ad mcchtnical ploP€nid

ofNBR @DDosit€ 3p.cin€n is Epon d bet-

I 7.2 7. SB&/FNK systen

Montmorillonit€. t&linile, bsto.it , erc were ued in polvmer nduic's to enbdce

rheir rhemal, physical, dechmical &d ftc rcittdst cb{acterblics Thc clavs study hG

b€@D. a ponincd ropic of [E p'!s.nt cl! du€ ro fi€n 4v ed sbundd availabililv,

low .o{ and .nvnoMent fn ndly Et!E. The clsvs have DdlidisiPlimry rypli@lions

includins @nstNction, polFq, n dicirc, c.miq 3nd nel,l pl@sins indutrics I85l

Paniclc sid of clav is 4 inDotlti pa@dd thal inlluences th' lncno_

n4hsical cheeter o Lne bde Dolvner Neclavs ha\e evdl sd\anL28es o\er micro'

size clays due ro thei! l{ee s(frce e4 nano$ale i.terelion *irh lhe polvmsic chains

Modified mokmlidk-/polym.r composiles have excellol tn€ml srabililv

$mal rcsislac drd n4hanic.l iteiSlh ll nms il*lf i o dif.Fnt ph'ss udr $e

preCrisively inc@ing hearing ovi|omor bul cD,i! in siliql€ fom up lo high

remle.arw F 1600"c) [87]. Nookaolinic (FNK) wiih low deditv ln8h 6p€'1 nio.

loge su ace se dd sn miun hs dlimcd lhe premisi4 einforcins effecls if

oifomly disptrd in $e elsromqic mslix Gtlme buadie.e rubbeo t8El

So, the INK inpoves themsl enduance, thmal rsi$ance and necboical

slr.dsth, of tne SBR n&@onPosiles 10 p.rfom b.nsr duing irs usge [89] E||*t of tbe

vdiet FNK conenlnlioc on thc rhcmal t"nslo4 li€dal slability, cndo&emic

€Dlbility, tud mshei@l poFnid of SBR conposit sFcin4 is Epon'it h'd

2t

Chrpter 2

Materials2. Polymeric malric€g

Polyftr o.rri6 of viz EPDM dastorcr, NBR SBR, ud SR wec €nptoy€d in

the ple*nl siudy !o tabricale @hpsi& sp@imeN for invcstigarine &ernEl rmspon,phde rmition, tedbnl degndatioq ed nehanicat pbperics.

Silicon €ldtom€r (SR) h a sp€cificalty synth.siad polym* of dincthyhitoxuenonoDer. Th€ polymeriado! pt@s of SR is @n[oll€d lo acquiE lin@ polyneric

chai.s or scvenl lhousand nonomer unns of siticon.o\ygcn wirh rwo nelhyl ndicalshaving moleuld *tigllts ofl[e ordd of t00,000[90]. th€ sR potymd is in de toft ofagm rbft is rcinforced with de suit ble iao.seic nlb, b gile b.ner $.mo-physicalpropcnjes. The bonding eidgy of Si-O bond is L5 limcs eeaEr rhe rhe C{ bond. It cdb€ cwd by dicmyl rmxide o. dib€@ylFonde J751. U3ulty, sili@ is usd to hilorre rubbs hddnes of$e silicon cldioner Tbe merits dd demqirs ofsilicone etdtoner

e ltutcd in lable t . The ch€eical sEuclu€ of SR bonoDer is porrrayed in Fis@ L

Silicone el.eomer is enptoyed for mdufeiuring thc foltowins:

. Adospae lndustry

. Automorive Indurry

. El€cuical & elsmdcs appliNdr Biom.dical mrcials

In r,'tc p6enr rcs.\ Silion dsloma (sN-?280) ws rceived f,or JiesyinHuaqieS R!bb6 & Pl6ti.s Co., Lld. China

.-1,-"1{,-'}i-Fisue lr Chemicil $ructue orSR nononer t78l

2.2. Etiylem propyL.e dh& ooDo.r (EPDM) elutoE.rEPDM is d elaslomqic uEaluar€d fom of ethyl€ne and popyhie wi$ an

addnioDl no.&njugat d third nonmq die@. trs @mposir.s Frfom excclldr in to$. dwell a high lenp@tur envircmrs J9l, 921. It shows ttul€ c.ystaltiaion oD

clongation dd takes the app@pdare tlosc ofl€inforci!8 iilteB to improve rhe thetul and

he.haical proFrti6 of the rubbcr [93, 94]. Sutphu or p.bntbs qdmizio. ,yshsd€ Ned 10 coslinl the polyher. The chenielsFucture of EPDM h givcn below [],91,93,95,981.

-f';1,;l;;1,; " "-"'.. r,, F-r,;i,-

Hc--c_.--:.||\ H"/

fi;--\."I

Fi8@ 2r chehicil sltucir ofUE EPDM nonoDq t99l

2,2.1. Uss

EPDM is wd in rhc fotlowile applicarioa:

. Electic cable insuldrion

. sp€irl houlded aniclB

. BridCe colstrlclior to alsolb dmping energy

. Ma.ine applicadons

. 'nEnDl insulatioE

In lh€ preseor study, EPDM .tasronr (KELTAN 433tA) ucd as a @t ix in rhe pres.tinv4tigdion vs slpplied by Tshricd Rubber Ptoduds, ChiM.

t.3. styr.le bulidie.e eLrloDer (SBR)

SBR k . tudon @polynq of stlm. md blt di€n€. This is a rclatilcly bish

hyslercsis dbbcr, In the l9l0 s, th. f6l cdulsion polytuird SBR knoM 6 Buna S wprcparcd by L C. Fdb€n indust ics in Celrmy, 'nE U. S. Govem.nt in 1940 eioblished

the Rubber Re*rye Conpmy to sl.n a $ockpilc ot nal0al tubbei ed a sF$eric obber

precm. nEs Foglfu w.F qp€nded d rhe Unied Sr es enrBd wodd wd ll.The syalhetic rubber etrons mE inirially fou€d on a hor polymri4d (41"C) E-SBR.

Prcducioi ofa 23.5% sgrcne dd 76.5% buladien copolymd b€se in 1942 [86, lO0,

1051. Thc chemi€al sauctw of lhe SBR n@Dq is displatd in Fig@ L

",(\f, l-t-.-c\$--e.-,.,rf ), af +".-\,,,,ro(.,, .\'' I

,,lr_.-J",,t--._!,, t_,.,:1' _t^

Enulsified styme butadicrc tubbe (lNDOpOl 1502) used in rhis study ws su!,plie<l by

EvergGn Globol Pte, SingEpoc.

Figre 3: chchi@l souctuF of th. SBR nolon* t2li

'nE SBR is u*d in rhe followirg indEri6:

. Autonobile indusry (conveyor b.lls. V.belh, eftuded sskets. carrks, auronobit€

. Houehold Soodr (\l@ nrb, bt5. she rote, h.els, dd sitary producrs)

. Food g@rls Ghewins gm. food @nrainc. stels, sponge anictes, rood

. Biomedical mldials (Ph&n@utcal ed sugicil)

2.{. Acrylonilile but diele .ldoober (NBR)

NBR is pbduccd in e mulsioa polyD.rizarion syslem [9?]. Acrylonildle ( CN)

drd butldie.e (BD) nlios @ vdied for sD€cific oil and flel resislare bd loq

temp@lue rquiements [l0cl08]. sp4ial NBR polyneu whhh conBin a thidnononq (e.e. divinyl beltzft, me64rylic acid) @ ale off@d. Aqylonjdle co eni

@g6 fton 15-51%. They @n de withaqide @yof endsifie sysrem, coasutmts,

slabilircs, nolecdd w€ight dodi66, dd chenical composilions. Thitd moiones are

added ro $e polymd backbode ro povidc €ild@d p€rrodocc. Erch v&iation provides

a specinc fuctior Cold pdrDs e polyndizd al ! rempqatue @se t.r5oc. rr

depends on the baldce of linedro-btuched nol€cul& chain connsuDrion desired.

Tltc lowr polymeriaion r€np@lws yictd morctinear potyme, chains.

R@tioB m @ndwt€d in pdess uilrs.ity knoM s @dfinuos, $mi_continuou

4d baich polymedation Il ll. Tle ch.micat st ucrue of NBR is ildica1in8 $e lhree

possible isneic structues for rh. buladifle &ghcnts. The chenicsl sEucruE of th€

NBR monoDe. is displayed in Fige 4.

Ijgu€ 4: Chenical slrucnuc oflh. NBR nonon€r

!--'.ft../'-il

I22l

. GloEs n&ufacturins

. Autooobile industry (oil sts, gstcts, auronoiive raBmission bclls)

. Synthelic halhs indusrry

Nitrile bua<tiene €lsloncr (Kblo KXB 35L) ued in thh s|udy ws omha€d amn

ABF Inlematio&l CorD@Uon linired. I(o@

I ^Bl

L l: Menrs and demeriB olelemcnc n.tenals 15.20.78.oo.l09l

Silicone Elastomer (SREx€ll..I heat Gisldce dd lowlempeEture r$st lcei excellent

Bsislece ro wathenng, ageing ddModeiare nechdical p6peni€s; nodelatEsisLne to oil; *nsidv€ lo hol Mlet dd

G@<l el.ctridl insnlaling pbFrtiesiconstaot valu€s of nechdiel

pD!.nies over ! wid. reDpcdt@

Ph'siolosically unobiectiomblc

EPDM ElastomerExcellent lbsion Esisrane, lflsitc,flennx dd reltnce ch@teristics Modqare adhesion to fabdca and doals

wide mge ofoFains l€DFdiur6:@n1inuo6 l25"c Gp*iak 175"C)

'nlcm nt €xpow to 200 C, toelehperature llexibilily h g@d at -?0"C

&d elairo 60% reBile stEngrh rrI00"c

M6l be einlorc€d wilh Cdbon black orspNial while filleE

wide @gc ol lomuladons suirau. fotinjecdon moldin8i exhibiring bish edlow hysler$is lor qcr$, absrption

&d Esili.nce BDecuvel

VeD pooroilud h)dM&bon rcaislance

ousbnarng esrsbne ro superhsledstcah. acidr ed b@s &cepr. painB,

mne sd *eaderine. hot watcr

Try 6isl!n@ not a good rs NBR blnsinilar 10 SBR

Acrylonitirle Butadiene Elastomer (NBR

Ability lo re@rer affer dpplieddefomado4 very good FsiU.@ ednshanicalpopenies(temilesEengrb.

elunsdiotr abEron Bs|5n()

P@r Bisi'ne lo tronad.s and polestvents.andoil

B.uerheal EsisGnce $e SBR, tow Fan w.odEring resistece; I annabl. withlomalion ol bric flue s6es

V.ry C@d Esisldce rooit hd frEtsiood comptsson set prorenier

Styrene Butadiene Elastomer (SBRBctld ab@ion csislance aid ageing

res$tale rhan NBRFlamabl.. Failpoor rcsish( rooit\.

Wnhsbndr for shon penods oili,i;hasher t€nD.dtues lnd NBR

Lf,s, rererc{h r€si$ee thtr NBR

Poc€sin8 lids for d rubh.r

plNticily, polymenc chain mobilily,

d rhos hatenah viz employed fot crosslinkinS,

cuiDS r5le, od to goveo ene o$er spects in lhc

The chenical croslinki!8 b€twe.n the pobme.ic chai$ or macbnolecul€s t ke

pl@ in polrircriation or b flb'jcti.g eticl6, Nlring i! polynd with ie o

stuctuca. The reactio. which @cN duing fabicaiion of eldomes is knoM Nvul@i2ltiotr in rubber indlsty, and cuils d hardoing in rhe pl.sIi. indGtry. Ccslinlsin rubb.r @ foin€d by the r€&tior wirh a suitlbl€ lul@izing agen! lsully sulphur.

Owing to lh. gE ler E$riction on the mbiliiy of rhe s.crcmoleculu chains d a resulr ofooslnrinc, thc modulB .nd elN tdBition teDpe'arw inc@s in borh hsdened

6ins ed sdphur coslintcd rubb.r. sllphu ii !5€d for wlc&iation for EPDM, NBR.

sBR exepl silion rubb.! [82]. Sulphu is slpplicd by McElq ccmdy_

2.5. L2. Dicuntl penti<lc

Oledic peloxid* seh as dicMyl p@xid€ {DCp) o. benayl peroxide de used ro

cosdint lo&lly eruarcd clasron u. Upon h6rin8 lh. FoxidB, fie GO bond breaks,

gendai.S fr€e radicsls which ext@l a H.atoe fion rie pol)eq blckbo.e. tE e&rionpceeds by a ndicnl m*h{th &d rh. rubber hs C{ coslints It l0l. r1B Dcp u*dio vulcani@ silicon tubbs i! ihc p6ent Es€lrch ws supplied by Jiangsu ywydsPhrmccutic€l Co., Ld. Chi@.

2.s.2. P.imary acccledror (MBTS)

The sulphu clNlintirg b iniriai.d, 64l€d€d, ad @mple|!d in de pEecc ofsome orSa.ic i.sEdients $at are call€d udearos, The 2, 2 Mercaprobenzorhi@le

Disulfid. (MBTS) is u$d a a pdha.y .4leoror fm EPDM rubbea NBR. &d SBR I I I I .

ll2l. In thh worl l-3v1% MBTS w6 sd in the rubber forhulations. MBTS *us

supplied by Dalia Richon Cnenical Co. Ltd, China.

2.5.1. S€cod.ry @ele6!or

Cyclohexyl beMlhrzyl sutph€mid€ (HBs) is delaycd actio. sulPhenmide

sondary accel@ror. Ir plodu$ ! wtmizatio! syst n wnhin the rubb.r

mmtumol€cule! lh.t hs betnr he.bmic.l sd ageing popenies conparcd lo lhi@k

dcelcnloB [031. HBS wi$ 2-3tn% B ued d lhe *condary a@eledror for EPDM

md SBR lo fabdcare polyns nmoonposires, HBS ss supplicd by Dalis Richon

Chemical Co. Ld, China.

TelEnelhyhhiw Disulnde GMTD) is ced d s@ndaty accelentor for NBR in

rhe pcsc.t E$@h lo fabd€l€ rubbd bas.d compdilcs. ft is vcry active, non'dieolodng

ed sulphw b@ing.celeEtor 0031. TMTD is on4 us.d lo &lilatc rhi@k or

s'nfooamide curc systens. IMTD qw prchNd froF Dalim Richon Chenical Co. Ltd,

china ed 2-3 Mo/o ws ls€d in the NBR @oposnion $hcms.

2.5.4,ProcNing lubn c&t9

Rubber prccesinS oils ore wd d[ine fic cobpoudinS of rubbq conposires lo

enh&ce th€ dbbq tlo\ pl6tici9, filLi alerptioa dd difiuion duins the rubber

conpoundins n031. Aomtic oil(10 !r%) wes used for EPDM a.d sBR. Anorher

p@$ing oil diociyl phathrlar (DOP) (10 *1%) m ls€d s pee$ing oil for NSR.

Borh pGssing oils wd€ puchsed fion ldenarional Frocbehicah (p\a) Ltd, palisre

Apan fiDn p!l){sing, tbjs |€s€dh h,s ur.iled fares rh dc beneficial to

wa.s @ lons chain hydr@rboro wi$ low mekins poinc_ pMrnn {,s is aper.olcum ddived Pllduct sed io tre Nbber indusq ro plasdcia and €dlce rhe rubber

vissny duitre @mpouding. tt als inpbv6 fi. €i oE.ment diftsioo in ihe rubbq

narix [l]1. Pdamn w used in $e pesmr study w6 pEhded fron r emalional

peteh€nicals (P!,t) Lld, Potind.

Aclivdlou @ the mlerisls ued in rubber conpoudin8 which eljvate lhe sutphur

qoslinking pt1Bs duing thc rd@iz on of $e polynqic ch!i6. Zinc oxide and

steanc acid @ popular rubber actilatore ued in lhe Flym€r industry Stearic lcid also

..}&as lhe pollmer-Finfo@ndr i raction by inc@ling wi$ bolh filler atrd m.uix

ud plovidB acrivo siks ro inrend wnh @h olhq [ 04]. Zim oxide s'd nernc acid tresuppli.d by BDH.

Surfera se conpoun.ls lhal lowr th. surfe. tesion (or i el|eial rc.sion)

beisc.n two liquids or bets@ a liquid dd a elid. Sufadanl! de uully org&ic dd@philic @npoe4 n nec tbar rhey h6w both hydrophobic ed hydDphilic 8nup. 'Ihis

is lhc '€sn

ihn d€y e soluble in *aLr s BeU 6 oil [15]. Some of su'facr$ls have

cationic dd $m€ oltm have diodc nane. h rhe prcsnr Gs.arct! calionic su.f&terviz. cent inonim blonid€ (CTAB) is N€d. h n widely Md i. the s)nthcsis ofndopqlticlcs, CTAB sas povided by Mfttq C€mdy.

2.5.7.Silee eoupling a Scnr

A sile coupliag agcni h6 th. clprbiliiy io dev€lop s stro4 bonding b€Mcen &epolyn.ric marrix dd rhc i@rgeic/orgsiic reiDto@nent, The p€s.n@ of silee coupli.g

aeent in the rubber fomdation imprevB rhe @ofiller dispeEion wiihin the nr&ix ddfo@ a dMble fiUelmainx bond rhal impbre fi€ O€@l md meheisal chaoclcfistics

of rhe fsbriqrd ndocompGic ll05l. (t-Ani@pbpyD Ejm€doxysilde E nsed in lhe

preenl reedch to fomulatc conposites wirh efljci.n $.mal and heheicalcb@cdsdcs. Silde @upling .go1 w ruppli.d by Sig@-Alddch, UsA.

Naofills like mocdbon (N330) od nanosilica (while kbon) wqeinsrpomcd inb Ihe rubbq 6arix io €nlE@ rh@al i$ul.rion dd nehlnielperfom&e of th. fabdcard nsno@nposns 18,E8 .100 ,l l4 -l2 r I.

carbon (C)is e elen€ntwirh abmic nMber 6 in rhc Friodic |able. rr is

nooncrallic in .ar!r. Crbon exisls in ti@ difercnr isoropic foms fld several

allottopic foms like gBphr€, dim@4 ald dorphoB ca.bon. N&odbon (N330) wprovided by Zaozh@g Xin]le ch€nical induslrx Co., Ltd.

Ndsilia (SiO, is lbe oxide of sili@i. silia ir narudly foud in th€ rom ofsd ed quafiz md syhthesis of silia including fNd quarlz, crysr.l, Ius.d silica, silica

2,6. L Muhiwalled cebon n@iub.s (MWCNT'

Cdbon tuotubes (CNTo ft cylindrical ndostr@tw allotrcp€s of carbon. cNTs

have laluoble posirion in rh€ fidd of mor.chloloey dd ndy o$d fi€lds oi naredal

sjenes CNTS govm ihcn hiSI themal @nducdvny, supenor mecheical ad €lecrlical

prcpenica ulll, They ee calegoned s single, double, riple or nulriwalled cdbo.ndotubei The sfieturc of a SWNT @ b€ udeBl@d by wEppine a onraloE-thick

layer of 86phiL i o a F@les cyliider. fu way a enphene sheel is wlapped is

'.pesrdl by a pan of indiccs (,,rn) wheE imeg€u , snd z denote rh. nmb.r or unir

vccto* alo.g two djrcrions i! the honeyconb cryslat latd.e of Smphcne. Sii8lc,wa|ed

cdbon ndotub.s (SWCNT9 e $bdivi.led inlo four diIIeF conbi.adons of uilvmlo$ likc mchzn (n=n), chiml (n+!), zigag (lr m=0), sd gnphenc ribbo. 6 shown

Nano odsil wile Carton Black r@e Silica wilh pudly 99.8% \6 suppli€d by

t€Denin (ShoCIai) indslry Co., Lld.

IF desiged fabdcated nanocohposites werc b$ed on two fiIlet!, one h

multiwlled tubon @otubes (MWCNT' dd rh. orbd is loolinnc (AhSirOr(OH!).

ZiszaS(n,m-O) GrapheneshectFi gue 5 | Si ngle walled c albon hanotubes with d ilTeEnr combin.rioff o I unil leclos

Muld-wued cdbon neorubes (MWCNTg @nsisl oi huhipte olted talers ofeEphen shel [76]. thec @ rwo mod.ts l) Ru$id dott Dodet ,nd 2) pmhned model

lnal @ be ued lo describe the slrucruFs of MWCNT9. In Rusiao dol model. sbeers of

chir€l (m, n)

sraphile de meged in co&enric cylindos md in fie Pmhnenl model, a sinsle she€t of

sBphite is blled i! around itsclf, like a olld of n*spdpd !22,123 I.

In this rce@h, mchat (n#n) MWCNTS Mle used 10 labdcate $e composire

speima. MWCNTS lE fabnc{ed dreugl CVD Felnod u$nlg F€ a et lysl. They hay€

purily > 95%, dimerer 20-30nm. lengrh 50-70ltd, sd avedge 6pei Edo 2400: I ). CNTS

wc purcbad ton N@Fn Co. Ld. Chim ad \r@ us.d a @.ive4

Kaolinile is a white lays.d clay min@l having chenical @mposition

(AlrSi!O(OH).. Il is de tnou a chiE clay. Kelinite ha low @p&iry !o srrll, shinlq

ud ation .xch6ge. Kloliaile ud€rgod a snes of phas ransilion upon rhemal

plocsins in lir alnGphdic pre$s@ 1241.

Fi6t endolhemic dehydrdion begins at 550.600"C lo produce metataolini&

(Alrsizor. Thn ptl$s b ob*rcd u! io 900oc[ t 5].

2 AltrSilO(OH)i r 2 AhSirO? + 2 HrOUpon rurth€. h.dne 925-95fC ir @nvcru ftom n€Dlaolinile to aluninuh,

sila@nc (sirAlloD) wi$ silica(SiOr.

2 AlrSiO, - SirALO,, + SiO,

Alter thlI alminM.silicon€ (SirAl4Or) nucleacs strn crlci.aton ccu6 ar

1050"C &d trlrifom to mulite 3 Alrq . 2 SiOj

I SirAlrOD - 2 Si:Al6Otr + 5 SiO:,

'Ite ldSc$ Be ofk@linit€ is h plFr indunty. Ir h ale u.d 6 emi rci.foicins

ageni i. rubbcr for enhddng Ue Oem.t ptup€dies offsbiica&d @nposit*. Kaolinne hsupplicd by MeEk, Gcr)@y.

ChapterJ

Development of Thermal

Conductivity/Impedance lVleasurement

Apparatus3.1, Tiermd tnnsportltudy

Themsl conducdvity (r) of the fabdcatcd elaromdic co.rposne speimeG $deceied oul ecording to ASTM E1225-99- Th. t€st ne$od dcscribes a stqdy slatc

rechnique for rhc d€leminadon of $e $emD1 conduclivity (k) of homogeneou-opaque

elids. ftis lest nedrod is fo. m.re.ials wilh onductiviLi€s in rhe approxinab ranse 0.2 <

K < 200 w/, K orer the approximab t€np@turc @ge 90-1300 K. h c& be ued ourside

thee reges {i$ decaa$d a..@y. I}e csr€d specimea hr linch: sru and lonthic*nss. Coppd M used 6 a €tativisric nateri.l for x neaswmenr of Il ].

A rest specims k inened uda lo6d berwen rwo simjl& sDecinens ofa mariatof known themal prcpenies. A r€npedrr€ gladieni is esrablished in rhe resl sllct md

h€t los dc mininiad by E of a longi$dinal guld havilg appbximalety the efr.temleralure g6dien1, Al equilibriun condilioG, rhe tiemll co.duclivity h derived frcnthe ns.rued |.np.raturc €ndiqts in rhe cspeive speinetu ad $e fiemar@nducririry of$e relerene naerial) s shoq rn figG I

Schmtic repe ation of mmp@livc guard€d tongiMinal heat flo*, sysFm inFjgu€ 2 depicts the possible l@ados of lemperau€ slnes, hqrins source. warer heltsml, lmpeEluE data loggd ed a lapop. Timelmpdalu€ conro!6 of all

thcno@uples lolaled ,t sp€cific posiiiod wee nonilord oo ihc laptop $reen rhrcugh

Cmt OQ6l0 6 Cb@l Thm@olplc l.pu1 Dala Loggei x of rhe NBR ndcodposirespeimetu lm De6md sing Eq@ri)on t sp.t ASTM Et225-99 .

Themal cofttucivity of sp€cimen= x -(0;4) -l&-

&)

Hd flo* a' toe br =a; = ##

(t)

Figue 2: Tltemlconductivilylhp€danceoesureDot

Hd now ar boron bd =0; = l##k = Themal condBtiviry ofrh. copper mcrer b&

hql flow syskfl according (ongirudinrl

| ,.ll

schematc of a conpantive-gusrd€dlo

lleASTMl225

"I

€8 | :! t.

l\,T2,\,Ta,T5 and't6 e fhc tdFdtws ^d Zt,Zz,z3,z.,Zsdn4z6 I tJa

corespondins posilions of the six lhm@uples uscd fo! $etnal Sradient measuremenr'

Themsl inFdde (/t) of a narenal is ils lbility to 6isr rhmal,tempentut.

lluctutions in a vdiable hearing envircMe . n M n suod according to ASTM

D547G01. This Lst helhod n.offi .tedy-srrl. h€1 nq tbrclgh s flal sp€inen.

Calculations @ nade s if ihe specincB @E honogen oE ed non-honoseneous.

TfEmal impedlN tesi data @ innMced by @nlacl prsur€s, sFciDetr surface

checteristics. ed the dist€nc€ of alFmare mths for bcat trmnision which de nor

lhoucl thc srecincn. To evalEte i of odtositc speimd! fou thcmocouples havc

b€co Ned.t w6 calctdared @orditrg !o tlE Equdon 2.

nremsl ihp.dee (m'? K/(.,) = R = (Ir - I, (3) \2)

He^ Ftow to = votrase (v)x c!ftent(t)Temp.Eorc ofrpp.r n.i hd sda! ii enbd wirt rh. !p..ina(/o : tr = T, - (?l

T.npeduE of lder nd6 hsr !u.f*. in bbd wirh rb. 3p..ims(ro = 7, = Tr - (73

Ir (,()= UpFr teop.€tw of upp€r md.r bd

?, (I() = lowd ternpenlw of uppd mder be11(D= UpF t€np.Bnrc of loE !El.r be

Ir(I()= Lower tenperanft of loB het4 bd

d. (n)= Disrar@ bcrren T, !o T2

d| (n) = Dht nce bdqeen T, io s supl.d. (D)= Distance ber@ Tr ro Ta

dd (m) = Dhtance belwen Smple 10 Tj

l,i

_rni

Chapler4

Characterization Techniques

4,1. Chr.a.lerlAllon Te.hniqoe

4. LL nEmognvim.t ic ed DiffeM1i61 Thedral Analya!'IlEmoc6vim€Lic dalysis (TOA) @ll@rs infomation eSarding rc ch&8cs io

a marerial s . ielio. of t mp.Etc (o. tim€) uldq a @nloll.d .tnospbeF. Ir p@vidcs

inlomarion leg&ding the malerial's th.msl sLbility. filler conrent ii polyneq mohrure/

sollent @!lenrs, ed the pe@nl @mposirion of @nponents in a conpoud. Diiftrential

themal alalysis (DTA) rrcvides infomalior/d.ta rcglditg thc hat absrption/exhausl

crpability ofa halcdal wdn 16r.

Perkin Elmq Dimond 100 TG/DTA, Japan a ued ro aElya |he themal

deStEdarion md dndod.mic/qothemic epo.F of the polyna nanoconpositcs wilhin

the tenpedturc span 25,1000"C ai ! helt intgBle viz, l0qc/hin in mbienl ahosphee ar

4. L2. Dif€E ial Scming Cdorineuy

Difrerential sc&nilg calorinciry (DSC) ne6ures t€npeEtEs ad heat tlows

s$ciglel wirh $eftal rmsirioD (T., T! T") in a Mtelial. C.bemlly, $e leftp€ratue

Ptuglu for ! DSC .nolysis is dsigncd such thal the sple holder temp€BnB incr6es

lin@ly d a tuncdon of time The b6sic principle of thh lhcmo-eaMc.l lechniqk is

bsed on the dir.rcnce in the dout of hd equircd lo incE6e 0E tcope6tu6 of a

snple md a relere.c€ which is neasued d ! fitrlion oi tenpehlw. Both the smple

ud the referco@ de mainlained at n@ly rhe sme tenFlane tuoughout rhe

exp€rimenl. Orly a fcw niligris oftulerid @ qdcd io M the &alysis.

Perth Elm.r Di@ond DSC, J.p@ m us€d !o .xeine lne phyrical phatrnsitions (clas, cryslgllidioll. od oa.t/psk beltind and their speific enrhrlpi$ of

th€ fabricaled smples with he.ring late (10'c/ninute) in th. lmperatule rdgc.75 lo

4.1.3, M.chaictl Tdting

Univ@l rd$ile tgrins @hjF (UT|\O is u*d b m4E $e ullimar€

tc6ild@npEsive sLe.8t ed elongstion at bre.k of oalerials The basic opeodon of

U'lM is by hydraulic taMi$ion of load foF tcst speinen to a separat'lv hou*d load

indicdor. The hydhulic sysrcn is ided thiough tev€s md knife edges' which ee pNne to

wed &d danage dE b the shock on ruplue of t€$ specimm. Main cvlinder of th€

podulun dynmond.r syslen is hols.d i! th€ colttol p&El Thc cylind€r ol the

dvnmomdter k a1e of slf lubric$ing d6ign- The load is tresincd !o lh' cvlindtr ol

$e dyndond{ is FaGGred lhrcugh a FndulmTcNilc lsring of the @(){@posit speircG B 6ied out on univesl tensile

iesling machinc (AG'2oKNXD uu, Shioadzu) a@dirs 10 ASTM ttandad Drl2'984

10 elalulie ullinate tensile strds1h, .longation al beaL elastic dodulus aid plNlicitv of

the polyme! conposite speine.s al SCME, NUST,lsloEbad

Hardn*s h the pnp€rty of a ma!.rial tlsl eMbl6 il to r€sist plestic d€fodadon,

lslally by pen.lntion. ltowryer, the &rn hald!€s mv .lso rfa lo rcsi$arc' ro betrding

edching. abEion or culting. nE principL us.d to mdm ShoE hsdBss is bt*d on

nduring lne sislrn@ foM of the pc*L.lio! of a pi! into tne tesl ittcrial untler a

knom spdng l@d. The @dt ofp.rctdiion is onvett€d lo hddn€ss eading on a sc'le

silh l0O Sho€ A mils. ShoE A hddr$s of6e rubber conposrtes was 'm'neo

on

To6ee, Tokyo tsting nachine to sinulalc thc elfeci of th€ vdiant Einfotcemeols s'd

dren bading co.@nllatio.s on lhe fabdclttd .lsloneric aFciieo hadn'ss in the presnl

4. | .4. Scmilg Elslrq Micrc$Py .nd En ryv Dis?ebire SPeao$opv

SEI4EDS povid.s ropognPhical ald elemenral infodaion al Ntu!

mas.ilications of lox to loo000x, with vinu.llv unlinited depth of licld A finelv

focL*d el.cuon b.m s@ed (rcss rhe suta.e or rhe smde Senedl'! \econdal

elecmN, back$atleled el6hons. md chdeleristic Xiavs These signals &e collecled bv

detc.loB lo fom i@sd ofthe smpl. displty.d on a cathode rav Nbe sc@i Fealues

*en in SEM inag. my $6 b. inn dirltly altlvzed foi do€ al @nPosilio' urng

EDS. S.@ndary eleron iMsing shows thc ropoenphv of su'f@ lotuts a re*

hmoddd acos. Bdk*neld electton inagingshows th€ sPaiial disributio' of

elsnenls or conpouds sithin lhe top Ficon of the @pl€.

Sdning €l€cuon mi@spv (SEM' JSM 69404 '@1,

J!!&) along enh the

€tr4sy dtP.6ive spdto3.opy wa u.d to altbz rhe sdtc' morpholoev or

modific.lmoditjed MwNTt4@tinn.. Utifom disrribution $ifomi9 of

nmorcinforcnelts in lhe polynd naLix, ind suf6@ terlue of $e po$ lhmal

condudn,ty tested spe(bm. elem.nBl aral)sis oi Ure Morube and n4oomposirr wre

als deduc..! frem SEM/EDS .natvsh. The comPosie s!@im.c *'c b'oken in liquid

niuosen &d @r.d *ilh goftl (30m) to har€ ln.m mdEijve for SEM dalvsis Ale

$eir cos-slio@l a@ vs amlvred lo ob6erve the FMWNTS disP'sion in $e

elaioDedc mLix. All qp@nents @ p€rfom.d 6ine S.dins Elccttun Micbspv

coupl€d wilh Ene.8y DisPesive SFcdos@py al SCME, NUST' hlmtbad

4.l 5. Fouier Tmsfom Intared (FTIR) sp€ctro$opv

Fouriet T@fod InAaEd (F IlR) SFcttosPv ir us.d to p€rlom qualilaile md

qudtariE edysis of oqrnic cmpo$ds ltd lo detemi'e th€ chmicsl sr c$re or

IMy inolgdic @npodds Bs6. ch.6icd bodls alelb iniied {lR) ei6sv ar

sFcific li.qwncies (wavelensrhs), th. b&sic sttuct@ of @mpolnds 6 be deFDined bv

$e sDedral localiols of lheh IR absotptions fte plol of a conpoud's IR lrmsdissioo

vssu f.cqrcncy is ils "fingeip.int," Phich who @mpaFd to Eference sPedra idenlifies

the material, Photonetdca maintai6 one of th€ l&gesl corhercid IR_spetM libtuies

and oIf€B . spdFal sqarch sryie to its industial cli.ds dd o$er labotatori* ibr

idenliting |he m.lcti.ls in fie spet! obt in d

TIc inlised specira for iMrPo6Ld @ofiUe6 sw ohlined uiog Perkin Elner

Fourier ttusfomaton inli@d (ITIR) sFct omclet at the pre'r shool KBr wd used

as a rcf.rencc malelal for IR sludy. Thc experimed w6 petfomed in $e rmge of 400'

40o0cd L with a sanple ed rcsoludon of I cm r'

4.1 .6. X-Ray Difrdliotr Tebniqw

x-Ray diffraction pGD) is . po$rtul dd nonidtnrcliv' tcluique u*d to

chrtrrcria crynalline mtft of mal.dds Th. rypic.l Fdv difiieiomcrer @6i"8 of a

$urce of sdiation, a nondttonalot b ch@* the wavelse1n' slils to tdjusl the shape of

rhc bean, a sple ed a d.tetoi Xays f@6ed on ! trple fixed o. 6e a\h of the

sp*fomerer e dir@lcd by the smpl., TIF chtu8.s in fie difnctcd x-ny inlensilies

ae mesuqi, remrded dd ploltd agaitut lhe otation mgles of tlE smple. Thc Esult is

Eienql lo $ thc X{ay diltlction pan€m ot lhe splq Conput€r sndFn of$e peak

posifions md immsities dsial€d with this pattld .mbls 4wtitative Nalysis.lar.iae

@nstaor dereminarion md/o! s1r€s delcmiMlion ol the smple. Qta,nihtiw analys\s

nsy be ondrcted on ihe besis or FlI heidt or Fd a@ Ihe peal< o916 od pofiles

nay be ued ro detedine panicle diu€t F.nd deg@ ofcr'sLlliation, and arc usetul in

co.ducling p@ise X-ny sulctudl ealysis.

'nE crynalline sirucllE ed d4re of crystallinity of the wodifiedmodjfied

sdpl€s llft chdacte.iad by XRD. XRD pattem wcrc E@rded fton I 0'80' (2d) silh a

s@ing slep of O02oA. The cryslallinily of the sdplds is delemired by Cu-Ka radiarion

having a wvel.nglh equals 1o th€ supplied volag€ ad cudt ro th€ Mchine e 40KV

and lsmA r€sp€diyely 0.1540m- XRD ponm ofrhc iflofill€rs srG obrained wilh lhe

20 rmge viz. 04-80! at a *m 6r. 0.050/min. x-Rdy Diftacrion (XRD) expc menl ws

t rloned oD x-ay ditr!&tomdq (STOE, Cmtuy).

4 L7. Aronic Force Micosp/ (AIM)

Atodic foEe mim$opy (AIM) is a vEry hish-@lulion lype of edning probe

hicb$opy with d.mostded eeludon on rh€ ordcr of fr?ctions of a n&omcr{, moe

lbe 1000 limes bert€r ths the opthal dilh&iioi limn. The AFM consis$ of a

turilder with a shatp lip (pbb€).t tu cnd fi.t is us.d |o s@ ihe lpecimen surface. The

cmlilever 's

lypically silicon. or silicon nihide having a dp ndius of cudalure on rhe

order of @onete$. WlEn 1he tp is brougbl inlo conract with the sdple surface foEe

b€lwo 0!c tip &d th€ sple le.ds ro . defletion of th€ @tilev* dording to Hook s

law. D€p€.ding on tE situatior! fo@s th.t @ e€urcd in AFM inchde nechmi€l

@nhct folca, vm dq weh. capilley foGn chehiel bonding, magnelic forces. elc.

Along wiih force, lddnionll qMtili6 may sinulta@uly be n*ured thnugh the us ofsP€cialiad rt?€s of p.ob.s. TrTic.lly, the deflccrion is mruucd uinS a las! spot

enected flom the top sulace ofcdtileler inlo e ad.y of phorodiodes.

5200 Jol Aromic force nic!\Mpy, Jap6n w6 usd lo eMine rhc surlace

topogEphy of the 6ncio@li*d mdlay a1 rhe hosr i6tirur€.

Chrpt r #5

Results and Discussion

5.1. Surfrce nodificatioD of reiBforcerDents

Ndorcinforcemdts hold rh. proDilc of Foviding ousledine mullifi@lioml

ch@cloistics, Wilh $e ercwj.g i.tercsl in applying trdotller i! so Dey difTeE neus

of irrercsts h6 hd lo @ntinue<l .iIons to develop disp€sion dd functionaliarion

r4hniqu6. To mploy nmfills s cflativ. rinfo|mdt in polyncr m@npcftes.pbper dispeBion ed apprepriale ificrf&id adhsion bet@n lhe MonUer ad polyner

trDrrir have lo b€ sllamle€d- Mdy Escdh.fons h.ve b.e! diEcl.d rowards pDducins

nmorcinforc.menvpolynq compositB lor fiDctio@l and st'ucrml applhations 005,

1261. Howaei, den affd . decade of rseh, lhe tull polential of enploying

idoreinforc.menls ha beeo severcly limited bsause oIlhe diflicuhi$ ssciat€d wilh

dispesion duing prcessing od Door inie.facial int€@lion t€t*€en nflofiller odpolymq mddx. 'nE @ne of disp.Bion pDbln for lfufillr is Ethd difftnt fren

olhd @nvdtioirl (micGize) fillcr\ sh s sphqical p6nicles ad carton fibes. Ir

hippen€d b.cats Mofins fike Dulri*rllcd cebon nmtub€ (MWCNT, havine wlldiuele ad hign dFd Fljo e cha.acteriad by extrencly largc surlee dea. In

,ddiiion, the physical nat@ ed cheEical smcture ofpanicles als play an imporlol role

in uifom dispebion of monlld into polyher mafix 027, 1281. lb olds ro enndce

filhr/fiber to polyner inteactiorvcompatibilily, the Einfo4 o€n$ hale lo be

n4ctu@liadl nodified-

5. L L Sy.$esh and surfa.e nodificadon of Nel@linilcA 3ilme @lplins aeenl (SCA) lminopopyl'trinethoxysile. (APIMS) along

wi$ ceilihoniun bronid€ (CTAB) rc ued fo! the sufae nodification of layeEd

silicatc ninml clay (kaolinile). 'Ihc $hematic flow chatt lor su ace modincation is

depicled in Fiew l. A sFcific mou| of th. wodified clay wa added in ulr'a puE

w|.r in a Etio l0:lo0 ed thc nixt@ ws $ni@t d in ulFa-eni€lion ba$ al ?0'C dd40 ldlz trcqwrcy for 30nin. Aia lh.l, ll1% CTAB *6 pfi in fic pr*| mitufoUo*.d by tunhd $nicrion udd limib condilio6 for Ga 30min. SubsqEnlly, 5

volme% SCA wa added i! the nixtua ed tudls enica€d for rhc ho!$. Tien,

ll|gi.dc niding folloxrcd d 100{tFr for t't hou vilb 9dC lr'$ F fonncd. rbrqiclted lolutio! r!! dilutcd fv. lid!! .nd \{uD.d tur io fiE liln€3 io rllrnlliD its pH

Coiritug. (C@nrioo Sci.difc C2 !di.3) .! 44()0rro for 30Ei!dr. eu op.6t d to

Ecovcr tt dD lhmi*dlicri. chy. TL FL-liDit! (FNK) sph. elF dticd ovff

niSh d S0rC !o r.dov. DoioG. rb folosilg t.cn!i$s viz t!!|!a @ ohrimd toE

lb. FTIR, )RD, |nd SEU r4 Fforod lo co!fitn dE firdiotdiztlioo noictv

.nrcbtFl, crr$rl 3tucntq DdPholorv, .!d coriF.ilid of tvtlh..iz.d INK

FigG l: nowctlrl ofrricc dodific$o dd t}!dsi! ofotloL4linia

tigwe 2a shows 1be FnR speha ofumodifi€.vnodifi€d li&linit. The peaks al

2g22.gl.zt{lg.l4- ed l4$25cm 'indentif v lhe presN of timethoxv tilde noittv 'tthe suriace of moclay. Exp.liDot l csdls rcveal th6t APTMS PlaF dethod

sueGsnnly attach.s silde moi.ly !o Motlolinitc pqnicles [ 129]-

fII

T

Fis@ 2a: FTIR speto ol unodifiednodifi€d klolinie

Figut 2b elu.idates lhe XRD plttdts bet$Gn t-8oo 20 for both $c umodified

dd nodifi.d kaolinit sp4im.ns Th. dilbaclion pcals of umodifted clav enplcs de

n@w and int6e, @nF{d ro the nodifi'd e!tPl's' indicatirs that $' raw k@linite

sleimen hrs a wll odercd snucnr' Thc @mpmliv€ dalvsis of both XRD pdlens

dieloes th.t the ultlsonjcation po'es in the Plesen@ of the sufsidt dd silue

coupliq agot @us ! prc8Fs.ive and gcnc'al t'duciion of the Dedt i'rcdnv ol au

EfleclDN located b.t{een 4_80". F Fdco e1allllol 'lso 'ndos6

thc above X&D

erllanarion in bs anicte Drtrdcnoo ptn'tu of the modilieduffiodriled specimen 'ho

clucdate ihc tDctinic slruc$t r.d@don for th€ synlhcsiad FNK'

The a\erace psnicle st. obs'd in frgw la s'lFm ror L\c nodrlled rdol'n'le

rne svnthcsis anl modification pltrcs has slestullv tld*ed lhe P'nicle sia of rbe

clay up ro l00O dnes The av.nge padicl' siz€ nod@d in FiguF 3(b' c) fot nodified

k olinilc is l5m Amlhs itt€t€sling lring in lh' moryhological analvsis of $e nan@lav

is ftal all psniclF have lp9toxiMrElv simils sphFcal slate dd sid Anothq dvdage

of lhis oute is thsl toil i!. MFFniclc s]alheiis !d mdificdid hlvc

sFcltm@usly. 'Ihc EDS sElysir i! FilnE 34 i[Bt Ls tt pt*@of Al

(32.86), .nd o (46.(B) Ft cat io iool6liri!. (A[Sip{oH!) &!r 6e."5

umDdlicLsmi tin ltcn diSiltl ooPociti.o ('broditrd cLy).

2l|raFiSue 2b: nD Fd.t!, ofuDodifcdnodifi.d raohic

Fisrt 3(4 b, c) $oe5 th! nicmgtqb of umodificd tdd nodifi.d cl.y d Ei.!tDlg.iftiti@.ldg wilh l}G oEp..ilidl rn ly.i! oftta lDlilit i! FisuE 3d.

(2r.05), si

tdl

Fi8@ 3: sufla. motpholo$/ of uModincd (a) &d modilid (b, c) clay along witl ils

@mpositional dtalysis (d)

Ultrasonication at 40kHz 7trC cmpcdre &d orgEtic stidng at boilins

@nditioB pbvid€ sumcicnr mryy b erfolia& the lay€Ed sili@le k@linite inio armosr

single layer shet slructur., Undd the abovemenlioned prcce$ @.dirioG and in the

pEsnce or CTAB dd AmMS, nicF krolia @nven d ino very fine noditicd

noopotrdq. AFM inEges clw rhc p€nicte si2€ tuens (l-5m) ofFNK i, Fig@ 4G.

b). The approximte sv@gc panicb sia ob€fled ii AFM snd SEM inases is less than

I0@. The neduEd aveqc panicle siz of$c f.bic$.d FKN is eud 5nm uins SEM

soliqe. IE no.lhology of thc aldhesiad FNK i! spherical. TIE ITIR, XRD. SEM,

ed AFM dalyses revealthe suc@stultu cdonaliation otlGolioire, which nquicheasydnd aomDic.lly viable p@s for sall s.alc s EIt s trge $ate producion of $eFNK wilh very firc D.nicle ria.

Fisue 4: surf&e ropogFphy of modifed n@ctay

5. I 2. Surrace modification of MVCNTg

A sile couplins asen (sCA), teinopmpyfrdmcthoxysilde (APTMS) alongwifi elliDoniun bDnidc (CTAB) ws ur.d for lhe s!{ae modindion of rhe

hllriwalled carbon nmotubes (MWCNTO. The s.h@iic flow chan for surface treatDenr

is d€pided in Fig@ 5. To bodiry rhe su.fas ofpdnine multiwalted ca6on neotubes(PSMWCNT', f6i puilicrlior qEj F omed d 4000C with he3liry ntc viz too(rninfor 12 bous lollowed by their rearnent with hydrcchloic &id to rcnole imporities viz.m€l.l tas, dorPnou c&ton ard 0$€t impuiri€s frlm h.!r ucalcd MWCNTS. In rh€

scord stcF. purificd VW(iNIs {cre iNne&d in lolucDc at roon lempcnl\trc thcn,

M\l(r\'lrrolucne sohdon Nas $nicatod in trhnsonicaror ba$ ar 'r0 lH2. 90"C jor

-lonrinurcs All.r lhal. l\1ol. CTAI} $s rdded h the pre*r mi\l[B folLo$cd b tunlrrllncanonolT0 Nnh40kHzlorncxt5onrintodc-aggloneL ctheMWCNls.

@

H..ed ow€r th. niaht.t4oo.c wlttr |o-clm inutes

s€nlotlon tor4o|\rtnut.., at 9o-c, 4okHz

n.rr so Mtnut.s ar 70.c.40kH2

add 3ml tra (3 amiho-propvlt amethory5tlan€)

sohietfon fof4 hours..t s,(Fc. AtokHz

M.an.tic st.,,lh.-a,IiF-t;fi a,i-ffi ;-

w..h thc sotn-i;r artab;i-.;:;i;;;i

9.ntrlfua.for4s Mtnut..

riguE 5 lrlorchan ol surtaccmodlltcaridrot t,$NlWCN|\

SubsequenUy, 5 lolllme% SCA wa added in the nixtw &d snicated ar 40kHz

for n.n fou hou at 90'C to stt in sildc noicties. Ncn. nagrcric sririDg folloeld at

l000rpn for two bo6 at I20"C *s dFddld flr $ni€Ld elution sls rh@ diluled

nve iids dd sashed six iines to @ilrain its pH levcl al 7, Cmtriluge ar l200OAm fot

lomiNle ws u$d to rlcoq the MWCNTS. Th. ndoob.s sole B dncd for

ovemighr al 100'C lo r€hov€ Doi$w fion the sp€.incn, The foUowiig csulrs eobbined lion Frl& >.RD, dd SEM ch@lsiadon ro confiD of surfae modificarioo

Fisue 6 reprcsens mR sp@tn of P$MWCNT5 &d F-MWCNTS. rR peak ar

t463.32.2900, & l03l.3J @Nsponds !o silan. n@iry arlrchrn€nr 6 a E$lr of rh€

surfa.e trdrmflr [?E,] 3 t l.crysqlline natd of F-MVCNT9 is als confim€d belren 1G80. (2d) XRD sd

$in a s':mitrg scp of 0.05"/nin. liguF ? shos $e dif.adio! pcd6 $ 26.?1. dd44.91'cor.sponding lo glphire $rudure deiived fmm MWCNTS. Fu.lhc@ore, the

inr€sity of (002) ed (100) pcaks of F-M\VCNTS aG much ctosr ro psMwCNTs

provid* $e evidme fo. th. fel rhar the rrdl|!.nr d6 not.lanag. th€ gnphdc layer

IEa?tF

Figle 6: FnR sFdn for PS-MWCNTS ed !-MWCNTS

a.T

ficw 7: >(DR patrch for PS-MWCNTS and F-MWCNTS

SEM couplel witb EDS w$ p.rfom€d ro invesligars the

norpholog/conposilion l rdyrh ofPeMWCNTs and F-MWCNT3, CNTS wE @aled

with gold 1o malc rhcE mr cqdEtire for SEM &atlsis_ t|€ SEM @epsativctuulris ofPslvIWCNTs rnd F-MVCNTS norphology waB ceied our s shoM in Figure

8(a b) Dic!@opic Dal}lis @lflfu F-MWCNTS d..g8t@o6don s. Esulr of surf@.

lr€one ol prisliic @orube. The nlrtiolalizrion ed dqsclmor.tion of tuolub*€n!e6 lhe fillq lo polym* conp6ribiliiy and dkFbibitiry widin te etdroh{icmtlix. Sihi. @icty edG @rdion wirt h potyEi. ch.i$ io dercloD @!rt@tinte.action. Thie ph.nobeno! lcad! ro imprcvc rhedal stabitiry as wll as n{hsicalsEdgo ofihc el6roDdic aysten.

FigE E: SEM dicosnphE ofrsMwcNTs (.) .d F-MwcNTs (b)

Fjsue 9r SEM sophlEDs alalysis ofpsMWCNTs (a) md F.MVCNT9 (b)

Compositionat d.lysis (EDS) for borh uFar€d&tlred MWCNTS cl6 tePesqc. of elemenG orher lhen ceboD viz. Si, O & N. These .lenenrs confin rhe

pt€*nc€ ofsile @icry on rhe surf@. ofndorub€s. EDs &rtysis endos.s FTIR s!.crB

5.2. f.bdqtior of ..trNnp6it6Modified @ofi[6 viz F-MlvCNTs $d FNK wn in@DoFled inro th. rubbo

matix usine dhpesion rneadd al llo"C fo. thiny einulcs to evenly dkp.e md diillse$c .aF filleu in !!c !6t Flym.r Mt ix oth.r vilh rcinforcd€nls viz @Gdbon or

@osilic4 ed proesinS sidr !iz, pla{icte$ !!d rctiv.toE Et. inorpont.d ido $ecladom.ric marir.. IIE posl hixine oft\e neofilreB polyner bl.ndetl .ubbef in leasue

wirh dic sddiion of cmslinl@ and seteBtoB B canied our on re .oltcr mirine mi s

at 60"C &d 40.Fn rcUer speed for r*€niy njnuies- prc-curd eldomeric conposire shedrwitn fou or fiv. div.M @nenlrarions of the nslofiUs w€r€ cullivated. The comDosir€

sp.ciDm wnh dimc6ios 25 x 25 x I mr fd lhcmEl r..6pon eatysis $d teosile

lesnle spec'm.ns @ording ro ASTM D 412-98?1 wre curd on hor isstalic pf$ at

130'C ond l500psi for 30 mi!ut!s. The oomplcc ehdnatic of fabication of

t|.t]@npcic i! &picrd h figc lO

Figre l0:scheE ic for fabiat d pob!|cr DlllMbDoliE

53. rodl|ldou of potrle Doo.potib.Tltc F6dr FsMh wo* !les! ! thc f.b.icarion of s€rcn ditrerenr r}!d of

polyG irD@ntosire sys&E Fu ditre ct stou.ric nrtric viz siiione ubbcr(sR), ethylme propyl€n diqe monodcr rubbcr (EPDM), acrytonibile buladicnc rubb.r(NBR), drd st)ftF botadi.E rubbcr (SBR) w! u*d (, f.bric.te oioposit spcciDeswith sutfd.e modifi.d tEmdle. like F-MWCNT! &d Motrotinire.

T.ble I illsid.tc rt b.si cl.lroddic @npo€iie fornot.tioos fo, rhc foucbsioioedc nEtrL6 &d 0*106 !q&d ndoffU.s viz I-MVCNTJ dd FNK. Tl|corlpo$G sFdn.os s.l! loDi.d€d !! Ect, sRct, scl,.ad Ncl fo! 0yr96 F-

M\VCNTS/S& EPDM, NBR, SBR) c.oposirio! !.hef, Bpccrivety. F-M\VCNTe u@imprc€n t d wirh fou.livce @Mtuio! ilro th€ h6t.tsrondic m.tix (SR. EpDM.

SBR NBR) a 0.2 $196 (SR2, EC2, NC4 SC2), 0.4 *1% (sRl, ECt, NC3. sc3), 0.6 wi%(SR4, EC4, NC4, SC4) and I wlo (S5, ECt, NCs, SC5) in rhe b$ic fonnuralion.

Ndokaolinne wE iopres@1ed wiIh fou diffcEr @nHlratioN inlo lne hosl

polymo mairix (EPDM, NBR SBR) B l0 M0l. (EI(2, NK2, SK2),20 fi% (8K1, NK3,

sK3), ed 30 $d/. (EK4, NK4, SK4) ir th€ basic fmulation (EKl, NKl, SKI).

NdoEinfo@Dcnts viz Na@dbor and @osilica, cossliiler Gulphut,

activaro^ (tn€ oxide & src&i€ eid), ac@l€ntos Dicmyl p€oxidc (DCp),

M€qprob.nzthiele Disulplidc (MBTS), Cycloh.xyl Boatlirzyl Sltphe@idc(HBS), ed Teadedyllhiu@ Disulfde (-IMTD) md pl4ticias Di@rylph.ral e

(DOP), @madc oil, w) wft als u.d in lhc €lasbd€dc fomulalion orhcr thu the

rubber narrix dd ihe &tivsted narotileB.

TABLE I : Sratring mmposire ol fabd@ied elstomdic nllDcomlositc sD€cinen

ECI

2.5

MBTS

TMTD

The densilies ol the fabisted ndocomposires wilh hdjhm GintoMtucnrcomc.F.tions in lhe h6r narricg e p*nr.d in Trble 2. The lcd detririF aeob$ned for F MWCNTS inpEgnated SR polymr @@onposile.

TABLE 2: De$iies of1h. fabdclt d €l63omqic coDlositls @.i.inin8 lwimm

,3

NARNBR

sx5EPDM l32l

5.4, f -MIVCNT/SR cobpo.ll. ry.teEr

5.4.l. DsFtsior of F-MVCNT' i. SR

Iigue ll elwidli€s ihe SEM micresnphs of SRC5 0.0 slo/0 F-M!|/CNT/SR

@nposir.) .l veiN r.slifc{id.olffritr8 rh. l|dfoE dtuFBion of CNTS in th€ host

polyme. nailix. The uifm disp€Eion of F-MWCNT! in SR naltix shongly influenoes

th. diol@tic, elebic.l, srrunlrl .!d lb6ql poFni6 of d|e polyd{ d@ b lh.uifom dispenion ed sEong interhcial inEractiotr betE n the polyDer chaihs dd rhe

@otubes sufie[?El. Swfhc. oodificri@ of nmtute .frectiEty .olElces rhe filtq iomtiix i eoction dd ihpdns e inlonet rol. ro ddggtanoqte MVCNT'

FiSw I l: SEM mi@gophr of f-MWCNTS Eir&G€d Flyru. M@bposrc ar woBmgrilicatiotu

50

5.4.2. Thennal conductivily &d thcmd iDpeddce aDly*s'l hemal conductivily contoB of |be tubbo @@nposircs n6ur€d uirhir

lempenlure iage 323 to 523K e illBtrated in Fige l2a. At lower lenpcraturcs,

thcnml @nd@tion th@ud the Drocohposit s is high. I is ai.ibrtcd to the loq€r

tcnpenNre difierencc (AT) belwcer the two {alls oflhc conposire specimen. Ac@lding

ro demd onductivity n6uing equrion (eq t, ch, l), lowr lenFrarw direllnce

@ntibutes b hi8he. thernal t dlpon thrcud $e Mre'ial. A d6ic decline is obrlvedin lhe x valu6 of the conposne in rhe Empedl@ mge l2l-371K due to ncctilny in

temlmlue differcne b.t{en Tr dd T6 yiz. lne topenlws of te lowcr ed upper

spsincn levels. Afte! th6r *ch rubber .eoconposile has eshblished a sepdale level of x

in the pe€€di.g tenp€Erue mse O.ncat find of x onlouN is ob*ryed rowddsthermla tnnspon decrcbe with in@$i.B rmorubes @ncenr.rion in SR nar x.

5

I6RCq

TsrFdur€ (n(l)

Fisu€ 12; Ihe thcmal conduclivit/ €ontouc wirh inc@$ins t npdtue (a) od rhe

er.d of F.M\VCNTS on themll onductiviry of SR na.@Dposik (b)

SRCS @Mmposne hiving | $i./o F-MWCNTS hs Oe tow twel ot K dur loenormous heal quenching ap.bilily of$e neciiomlizc heoruh.s s in Figurc t2b. The

uilonly diqEerl F MWCNTS hav€ ddelopcd a .elw in Ihe polyner morix $ar€olrap llE phonotu witbin rhe ndwork dd i€sist rbe rhemal ndsrorr thbugh lhe

55

9o!7

50

@

50

51

n@ocomposjr. [?9]. As a Esulr, lest b.ckfe rcdpmluts is en$d al rhe back wa olItE tcsling ohposile spocind with ircBing Molubes @@nhtioo in de siti@ne

rubber natrix. Secondly, lhe F.MVCNTS @ morc €ndothmic rban fie psMVCNTs

dE io rhe pl€se@ of trim€rhory sit&e hoieiy on rhc surfe of the I,MWCNTS lhltevdlDnls on hetng a wt* molecules md Cq rhal evenlullv rcdles lhemal

@nducliviiy of the ehslomedc .onposiis.'Irtemal impedmce E) h m importarl checi*isic of a FtyDer conposite

rt'ich elrfui th. €pabiliry of a mtedrl to Bhr rh€dnal vdiations qcoDrer durins a

sp{ific @mposit€ appli€io.. Fig@ ll indi.ales the cfed of F-MWCNTS on rhe

tEmal impcdae of t\e '.lrMnposiie

speimec 6 a tuncrion of tcmpeDtuc ofmeasmenr An impovement ii R valu* up to 500K is obsercd in lhe shph. Aier rhar

Eduction is Gn is lempcatw inc!€s.d due io rhe Ed!.tiotr in l.mFnrure bel*en TA

&d Tb.l1 atdburd b $nming ad ihe sran ofrh€ lh@st d.composirion ofthe potyh{

3

6.

F

Figur. 13: Th. erdl of F-MWCNTS conc€dations o! rhemal inp.dmce ofrhe SR

luMonposils ir thc tebpdlue tuge 323-532K

Nflocompositc SRC5 h4 rhe frdinm abiliD' lo resisi incoding heat 0u Nirhin

fie complere ksled lcmpen$r€ @gc dE lo Minu CNTS inorpoFlio. ino the

polymer nalrix. F-MWCNTS n€rwo& wilhh th€ potyna Mbix enlEss the lhcmal

5o:(a

I2620

1.0

Tsrpsdur! (n

stabilily .d thffid Bisl!* of the faldQled 4no.onposiI6 by c.9turi4 lhe phonoN.

Fisr 14 (4 b, c, d, ed €) 3hos the surfa& norPhologicsl &ttlysis dd thc Fiew l4r

confim th€ EDS $dtsis ot lhe p6l tbedal @ndudivity t sied @o@mposile

sp@in ns h lbe lcmFbiE Enge 323 io 52JK A lagc nubq of nim voids eobsed€d in sRC I while ih. si4 ed qwtity offi€s. pores have Fmekably

'educed with

iMins F-MwcNTs @tHt'lio in rhe rubb.l @lrix. The F-MwcNTs dnnanhh

fimal dcconposirion of thc m@mpolitd dw lo U.ir €xc.ll.nl thcmd slability ,nd

uifom dismion in SR @lrix.

Fieu. l4r SEM nicroeBpbi ofposr rhefrul tEn3pon rded .mconposic sFcihetusRcl (a), SRcz (t), sRcl (c), SRc4 (d), SRc5 G), and fi€ @mpositionalddysir of rhel*19l. ldded F-MwcNTs in sR (0

5.4.3.Th.mo gnvinetjc/dif.rcnlial thcmrl elylith FigG 15. tb€ Oamos|l@ d.nrc $c Gff@y of Ftdr ie@al of F-

MWCNTS in SR polF€r matrix. TL 6on tur th.mal stability improv€nent is du. ro

slrong co!.ldt irt etio! ol F.MVCNTS with rolymdic chaim ofde horl @ttix. The

rh@d d@bposition beblvio! of F-M\VCNT9 iFqFDt d polyma @mposir€ is tulcdd SRC5<SRC4<SRC3<SRC2<SRC I .s is so in niew l5.ln conclwion. lhmogdms

lqd @nfm tal F-MIVCNT/PDMS @bpcit6 alibn mE thertul shbilily te

prisrine SR dn€ !o ihe heat

$mosmsl2], lll-ll7l.qu€nchio! ability of F-MWCNTS s obviou in DTA

siclsna2

s8c3$cr

sc6

TqrFdrE(oct

Figrc I 5: tlemal oxidalion behlvior of SR l|lljMnpcites in Oe rnFalre ange 2j-800t i! air envibuenl

In DTA cwcs, it is cl@ rhal F.MWCNT/SR M@nposiles aberb norc inpur

he'l rhm pristine SR dw lo bond cl@vage ofcolale ly anached moieties on rhe surface

of F-MwCNl s. Thc DTA behavior of borh potyDer matrix aDd @mposires is conple&lyendo$emic but the polyner ab$rbed additioMl heat dre b ihe presnce ofF,MWCNTs.Figw 16 illustrates lhe upwdd shift in lhemogms which illusmres lhar F,MWCNTS

hsve cnhded the dEmDt sralility ofihe hd polyner,

5.4.4 Diffcrcndal scminS calo.iman (DSC) malysis

Figw l? elaboril€s thc DSC p@fite of SCR nu@onposjle specin€n. The

smples wele rested wirbin rhe hpcratur rdee viz, I6SJ(]O0C ed tenperarulc

incEaing Ete all DSC qp.rinetrls B 100c. Crysrallizlio. i.mp.hr@ (Tr) eradulrydellss with i@ing of F-MWCNTi It is anribut€d io ihe rcdrction of spherutite

siles io th€ polyneric composile. The s€ behavior is rcvealed in $e netdng rnFraturc(T., 'l;, Fspo@ of lle comFsir. sFcim@. The gls Fdsirion lcmpedrm (Tr) ot F_

MWCNT/SR @dposnes d@ees wj0r rhe p€ee enhdenenl of F-MWCNTS in the

540

-1CO

TJnpadl{.(oq

Fi8ue l6r Hedl q@nching epabiliry of SR ndoconposiles in the rcnperatw ra.ge 25-

E00r in air dviromml

The reduction of Tc, TC &d .ntdcenot of Tm @ m rhe pmijciocy of.donib.s due to the inrennotsuts inr@don belween the silicone ,ubbo nol@uldchlins ad F-MwcNTs.Tablc I giv6 rhe T", Tr dd T. vdB for @h sF.imcn_

Tl'e ausmot don in the o$er &d peat neldis points of lne ,olyne, conposiicss due lo esislance olfered by the F.MWCNTS to slow doM lhe rhmd chain nobilily ofih. polyhd nabix in rhe hering cdviromd!. T.bl. 4 disphrs an eIf€dive Educrion inspsific othalpis of gls$ Fa$nion/crysbltiarion sd inFovene io sp.cificenthalpies of rhe onser fld peak meldng pha!.s. Ir atuibur€s to high lhemat nability,Fsist:@. ro polyme.ic cb'in nobility, ed hdr absotbidg copabihy of rhe in@rpoFled F.MWCNTS[78].

host polymcr nalrix owing !o i e@rion betwen polyne.ic ch.us @d Motubes $rough

trincthoxy-sila noicties. The @o EinfoMnent ihprovcs Ihe dlclildrubbery beluvio.

of ihe roltdd marix up 10 - l3oc tl36l.

5.4.5. M.cheicsl chahcldiarion

M*haic.l prcpeni4 inctudire rcisile skqgrh, elongrion at bFil, mdelbtomeric hardnBs de iuustnled in Figw t8 (a b). The l% addjtion of F,MwcNTs in

52i!

E

tt

lhe S& nalrix ha elevarcd the r.nsilc strenglh up ro 100/c ud elonSation at breal

pronoled 10 : 60% d ompa4d to the pristine polyner malix. This hspF6 due to the

extaordi.ory mechdi€l prcp.nies tud w€ll dhpe6ion of F-MWCNTS in $e host darix.

:6

,6

fI

Ir-p.a6Oq

FigN I ?; DSc pofiles dis?layjng T! , T. , Tn oflh. SR n neomposites

TABLE 3: Ellet oi F-MWCNTS conc€nidtions on $e gta$ atunion, oysralliation. trdo.set/peal oclring phes lenFdruEs SR composit spdoens

ID

TABLE 4: E ler of vdidr @noir.tiotu of F-M\VCNTS on rhe sIeific enrhdpies (T,,T., T.r, & Td) of SR na!@omDosiles

--Lllltrd. T.ndL Stsllh-.-€crddr i bra(

FiguG l8a.E(Ier ofrbon moruh.s tordirss on ultimr. r.Nile rtrcnSdr and %

erdgarion ar bllat in ilE SR

I!I

5t!

5E!6.I5iE

=

tod

t

0 out oa o! i.0Crbon lwub6 M%)

oI c&bor lmtubes loadin$ on hdrdn$s in th. SR

C.bon ib|oluDc (x,t 0

5.5,F-MWCNT/EPDM el.rloEericnooconpdito5.5.l Dispersion ofF-M\VCNIS in EPDM elstone

Thc dispesion of morub.s in EPDM dbbe. MLix is @tydd by SEM

niclosnlhs a1 ditrdnl mrgdficrioG i.e. depict d in Fis@ 19 (a b). nle coblositioMl

a$lysis of polyme. Deoanpositc (Fi8r l9C) dabomtes the presence of the Zinc.

Cdbon, Sulphu. OiyS€l! Niho8ctr, Mg e1c, th.r co.fifrs rh. composir. fomutaion$h.me. FiSE l9d dnosi.des fie EDS &dysis of inpFsEt6d Motubes qirhin $eeldlomric @lfix. The obld&d tslt! show rhc Pls.@ of 100% oofining th.ooorub€s €xisleDce wilhin th€ etstoneric MocoEDosite,

rise le: The d'sbiburiotr orr-MwcNT3 wnhin |j. potytur d.;r d v&iermagnifidiotu (., b), compositioul a&lysis of EPDM conposne (c), and &eembedded [-MwCNTs (d)

5.5.2. ThotuI @nducliviry/inpedsse edrs'Il'emal condudiviiy ed $mrl impe/ace of F_MWCNT/EPDM

nmocomposile *!F n sGd id renp€nnE reSc j23.5t2K ud.r sready $are heor

@odnioN and th. &chutalcd d.|. e p|snlcd in Figc 20 dd Fig@ 21. Thc th.malordrctiviiy of Ihe n.|t@nposiL sFcimc6 r.duq wilh itu@ing filler lo mtix n1io.'nte mai6h EduciioD is obeFed, i_e.,95% at 373K fo. EC5 ,llalivc 10 bas composire

53

fomnlarion, ECI- The I Mol. F-MWCNTs in@rponlld tubb.r nooonposirc hs 29%

(at 3?3K)impNved therMl ihpedec€ compar.d to the ECl fomulalion due ro de hdtqueochinS ihough phonon enrapping by rhe incorponled nmotub.s, 11h qlso ariribuled

lo uifom disFnion of F-MVCNTS wirhin the hGr narix. tt @y .tso afibur. to heat

ab$rplion by sil&e moieg plffir oo thr surfec of the mo b€s. Rctarilely lo$tn.nnal o.duclivity of F-MTXCNTS @Dpaed b de cdbon btacls als ihDdls o'nponet

role to nininiu lh.mal traspon $mugh the fabdcsrd conposite specincns

ll32l. ! n.mal conduclivily of EPDM conposites is Fdued wirh incresjns enllonme.rrempenl@ due to the acrivalion of plt)csing aids evaponrion, polymq plaolrsis, mdendodcmic ph@n€na eirii! $e polymrndmhposic 1791.

o3

07

06

Y

35

Fd

5

05

o3

02

Tetv..df!(q

FigE 20: Theoal onduciiviry al diff4nr F_MWCNIS concenFatiotu &d lemp€Etures

Ficw 22(a, b. c, d) rp@sqts thc suface morlhotogy of the cohposile specinens(ECI-EC5, rcsp€dively) wirh divee F-M\VCNTS co@entrations after lhemsl responlcsdIg, Tbs p€enred llg@ show rh *nn inccding tlE F_MWCNTS loading h therubber m!trix, G!.i@red @Eposit s6laiEbitity e.h&cca in $e aDlosous O6hion. Tteincorponled F.MWCNTS hav€ lugn€ord lhmal $bility od diminished suaaceddamage in heddog envircMe due to rhen hi8hs thmd eoourance, surrace area. and

strcng .ntargleoenr wi$ lbe @trix polyneric chains The lnifom disrnbudoo andsurf&e nodili@rion of rhe impFgrEred Motub.s also ,npa e tnFnm ole to

59

develop dE F MWCNTS fttrr witlin th€ tubbq mrix thar cnhrncB its rherul

$abi[y/6ist G. TIE Mjor elcmd$ C, S, Si, A, O, Mg &d Ca s€E foud i! llF EDS

onalysi! or EC5 due 10 pBence of dbon blek. F-MWCNTS, ZnO a aclivalor, sulphur

6 a cbslint r, MgO dd SiO2 '@ tne impuirics in the incoryohtcd lillc|s ddplt){sinc .ids i-e. dcpided in Figre 22t

ItE!F;

!

TnFft.!(iqFigw 2l: fte@al inp€dane of lsidl F- MWCNTS @cntrdion! & renp€dlB

Fige 22: SEM nicoglphs ofposr ilcmit Farspcr l.ned m@mDosileICIG). EC2(tr, EC3 tcr, tC4rdj. LC5(e),&d rhe@mposiiionalrhel $f/o lolded F-MVCNTS in EPDM rubbc. (O

oso

5.5.3. Thmal de@orcsition md heal flow behavior

TleftogBvineric amlysb of the tuGoiposires i. rmp€Iatw tue. 25-750oC

is pllsled tu Fiew 23 shos . ie slep llE@l degtulalion. The prinEry lhmdd@mposition is ob*tued ia ihe i.bpeatft rdge 200-450oC due io rhe ev.poralion ofmnatic oil, w dd orher Foc*sing i.grdienB. The sconddy thdmat oxidatioi is

sen in the rdptunr mgc 450-520oc du€ ro rh€ EPDM pt@tysis, 'fte ituoduc on ofF-MWCNT ilio rhe rubtd mEix has cnhaMt th€ th.mat siabifty of $e hhi@redM@onp0er6 dE !o hiel ihm.l adurd@ rnd ieo$ate inlereiion ot the neotubes

thar lesuicb the themal notio. of noleculai polyme! chains in herting envircuenl

ll42l. Thcmal srabiliry inpoven nr up lo 4% ar 6o0oc @ ob6efled wi$ th. peak

iMqDErbn off-MWCNTs inro rhe bos marix.

T'rFdlE(oc)

f igu 2l: IEnn l de.omposirior eElysis of F-MVCNT/EpDM monDosn€s

Difl.dtial ih€mal ealysis of dE eocoDposil. sFcincns is <tisplayed inFigw 24 that elrci.lals c1Iatve egn€nlliion in bqr aberbitrg capabitiry wilbihceBins rhe neotubes loadiDg in EPDM hatrix. Heal quenching capabilily is ahomptuved with incmine the .dotubes co cnts in the host naFix The peat helringleDF6r@ is nowd lowards th. hishd l.mF6rw witn iftEsins tE co.ceoralion oa

ITJ

61

F-MWCNTS in lhc pdFq n.nixde @@nposites s provcd fron

qhch G evidene of thdal

IID

E

:IE

I

rnp€'i'r.eq

Fisue 24: DifeEntid $mal analysis otF-MWCNT/EPDM sD€cinens

Figue 25 ellcidais th. di'r€Mnat emirS catoinetic srudy to udeBund lheinflueice oI F-MWCNTS on the class rdsirioi (e), crysraltialion (I"), md onsr nelrine(/., & p€al nelring rcnpenlut€ (Id) leDF6tuics of the composite specimens. Tte.cquicd dala of $e$ ph& ch,nging lenpeorGs N prsted in Tabte 5 arem rh€ DSCco.bw. ?i of th€ @mposite spcinds has b€n Educed with re in@rpoEtion ofndotubes in the potynd mrix. IrE r€les Fspotue is obsfled tor I.. Il arkibuted lo F-MWCNT nelwork io the polymer matix lnalconsrrainl the phase ch&ges by inreractinSwith tc polyndic chains at nde$.tc and br@d.ns rubbery ph.s. of rhe fabdcakdpolrDcr Momnposica, C.ruelu€trtty, ECj @@Dposile d b€ op.ared jn noEncgatilc IeDperatre @npdt d b olld oDs up !o _2OoC [143]. I"/ an.t ?"2 Esp€ctilely,arc enleced up ro 58.28 and ll.2toc, sp@tjvely beque .eotubes have o|feIld mucbr$islanc€ lo rhe @hix hol@uld chlin dobitny by.nrzppire phonons wirhh rh. flkrshctm*. Anolne mjor t@on oa lle meldnS rcnpenlw .nlnc.nfl is rh€ hisherlbemal st2liliiy of in@eonl.d F_MWCNTS conpar.d ro cdbon blak I 1251.

TABLE 5; EIIect of !&iml concentrlioosctr$alliaiion ad rEl/!@.dnmocomPosnes

Cl6s trqsirion ed crystauizrion d €xoth.mic ph€iomeD but melting ot $cporyher comDosirc is m erdolhemic phenomcnoi [r44] which msns thar the nanotubes

impFsmion in rhe c&boa tlled EPDM cobpGire.nlmes O. eMorhc@ic behavior oft'€ composile speim€tu_

Figw 25: DSC @niou6 ofte fabricared F-M\VCN-VEPDM @nposircs

Sp€ciftc enrhalpi* of the M@omposite specinw @ depiccd in Table 6. Il isobserved |hal sp.citc .nfi5lpies of glds rmsitio! md crysialiadon phasd chdges are

ennanc.d wirh incmi.g rdotubc b Datrix hrio. ,tE spsifi€ orhltpi$ ofon*t odpe.* DelinS phas a el€wred d@ ro cnhdMor ij endolh.mic n ruc and tmal.nduee ol $e .ooconposite vi|h inci€Ging 0D dopinS @rcentrsrion of nootubE inthe rubbd naltjx. Irris phenonsoi is ,tso endoGed by rhe DTA themogms

ofF.MWCNTS on the slds tunio!,neldrg phe temperaiues of EPDM

I8€

'Ee

;

T

rfnpddrb(oc)

TABLE 6: EfI6t ofvei&t.okqrratioB ofF-MwCNTsonth. sF.ific e h.lpies (T!.Ts TDr, & Td) oIEPDM @nDosircs

ECI EC!

5.5.5. M@hanical popenies

Sb6s rF.in @mours ofthc Dno.omposiles ft disptaycd ijd auSno|,ion in tnsile srlngth s.hit elol8ation b@t suff6addilion ofcsbon motlbs ih dr. EPDM rubber mrrix.

FaTa

!"isM 26; E[€ct ofdifr'€nl dopins con€ftrdions of F_MWCNT o! srcs{rainperrodee of EPDM MMhpoiics

Figw 2? shoqs tut ll1% inco,pontion of F_MWCNTS in the rubb€r darixelevares tne tetuile strtiglh ed elstic nodutus up to 4l ed lll%, rspc.rilcly. Ir isaftibuled lo .v.n disFBion of @otubes in ilE polym€r ndrrix, snorg MWCNT-polyft!inr@don,ad suFrioi meh&i..t sr.enet of r\. @bon @orubes t I a3l.

$dn (Yd

F gw 2?: Efdl of difremr dopiog co!@ldtio6 of F-MWCNT on ullimt GNile

std8fi rd pdent cl@galio! at b@k of EPDM nwonposiles

@OE.ot

.ioiegiso

?:,EIEd:

t

?E

6!I

FiSN28:Efierof difcrc doping mnentlli@ or F-MWCNT on $@ A hardnes of

EPDM nrt)@mFsile

A ptosrE$ in Shot€ A hard!$s of the composne specitne6 is obs ed in Figrc

28 with inc@ing lillq @nlenls i! th. n$ber naldx. T!. .ddition ofI-MwCNTs in the

ton pdym mlfix .uSncrrs tbc rutlbd h.dtB dE to 3t!rg inteEction or nmtube

lo polyndi€ chaitu of dE EPDM [45]. Anouq !!e. !o .nhdcc €laslom€tic httdnes

i5 Blelion of ch.itr oobilily wih im&sing F-MWCNTS conc'nhrio! id tne nosl

5J. r-MWCNT/SBR.lrtaor.rt r.!..orPoril65.6.l. DspcBion of F-MVCNTS itr Sryrc!. bdrdi@ ctaslomq

Fi8ur. 29 (4, b, c) €lwidates the Nn dhP.sion of motubts 'n

the SBR @tix at

difreMt magnificaiioB. It neG fiat sutu€ modific'tion of MWCNTS inPtoves 'ts

disp.uion .lffcicncy wilhin the Polynlcr E|mx bv intetudng with lhe polloenc

Nl@ubr chritrs d mogL. FiSrc 29d f.roEvt ooposdoEl drlrk of r-MwCNTs

itr@rpoded @mpotle !p@iB.a *nich !!v€.ls lt Fec of lh' *ton !|@tub6

tl42l.

Fige 29: SEM imgcs of F MVCNT/SBR .@posic tnd tbc otnposirio'al a$lvsis ofr nanotub. h lwr % lo€dcd s@it@

5.6.2. Thcmal colductivig ed Ocfrd ihpcdece behavior

Themal @nduchvitv @nlou! of 1h. n n@nposile sp.cimcG in lenpe€lw

tug.323-523K @ dlplaltd in Figua 30r At low tenpq'ru* fron 323.148K ltcmd

codE{ivity of .ll @6positd €ob&cct tvlchEmusly' bln lh' 'l'vadon

of SCI

obpo3ic sp.cimr k almod ls|f @mp8!d io tLc oi!.. .lBFbn 3?!521K dbbq .lnc@posit sFciltB @intain ' speciflc l*l or x

dd rc ftih.r big ups !d dom @ obwcd in t valEs with ircwirg rcnpdrtw

sc5 M@onp$ite sttl$ ilelf al a lowdi l.vel of t anq l48J23K due to ihe umosl

level of F-M\VCNTS loading io ln. polynq mstnx

osl0 5oioo5l0.,r01

o35lo30lo,5J0,..lo{0.101

o6lool

s

3

qioII

5I!!T

TtrT.rdt {{

Fiele 30: Efr*t of t mledur. on tumlcondldivitv (!) lid thmal @nd@tivnvd divcN temFdl@ (b) of f-MWCNTISBR sp€.ircns i. $el€mFEtm tutgc 123-523K

cNTs phrsically dd ch.micdly i dact wio thc moleular chais of the polvmer

!t thc tuosd. ad Blricl thc lhmd mtio! of $c Polvm€ric chli.s in h€aing

dvireMe lla6l. F-MWCNTS in SBR rot ix . rdt photutu strich Edue $eoul

@dNtjon ed mdimiz. lnc thdmd stabiltty of the n nMmposi!. speircs. FiguE

lob illulta&r a do*nfstl in fielrnal @ndu.livity valEs ,t 173' 421' 473 dd 5?lK

simultan@bly wi$ incGing mtube! @nent ation in dl rubber mirias tesl€d 'IlF

ndinm v{lu6 of emal@ndwtivit} in Wh-K e oberyed for SCIie. 0.091 0 063'

0.053. md 0.M? !t bcfoF Dertioncd ldnD.rat@q conespondinglv. Tlt minimm levds

of ( in wo-K e noliced for l $tol. l@dcd @mposite sp.cimen i e 0 034, 0.029 0 021.

&d 0.012 Mording io fou mcntion.d tcmp.Btuies SCS has 63. 54, 5? sd 74vo less

thenal conduciivily conpNd to SCI al th. sPecific t mpetaiws displ.ved in FiguE

Themal impedane (R) is th.lo1.l h.at rclisbrc. offcred bv o @tcliol aeainsl lh€

heal flos dd is medued ac@tding ro ASTM 54?043 in the &dp.ralue range 321 ro

52lK lrgw ll illusudcs d inctsa D R valle wi$ incrctsirg upper copper bd

t mpeduc up to 473K for all rubber neoconposi|es and rhen a decEase is ob$tved lbr

SCI ro sc3 @npositcs [50].

25

2a

e

8

I;

510

Trrp.&t (4

rigN I I : EJlecr ol thcml impedece ofth€ F MWCNT/SBR olno@nposires in tc

rnpeFtur€ @ge 321523K

SCI conposite scupiB the lowcsl R lev€l a1 52:l( while SC5 minains e

apptuiim.tc equilibri@ ai.r 4?3K dd n ha ds lh€ mdimm R lalue in tll lhe

f.bricaEd specifrens SC5 hs 3|r0l' exca$ lhmal €si$dce conpded to $e SCI al

47lK rlk ro tbe ituolpodion of F MWCNTS i! |he polvn'r lBtrix $it etn"c' the

insuladon capability ofte ndooonposite fte @nbimtion ofF-MwCNTs &d SBR hd

didinish.d rh€ dneinal Dobililv of phorcN stich Pregces themal impedme ol lne

poly6er .eoomFsites. SEM inlges ofrhc post $@al conductililv/inp'dde t€$ed

@Bposite sp€cimeN se dhplavcd in ligu'e 32 (a' b' c d' md ')Thc SCI @nPo$t aPpeab b hav€ hiShct poMny @np'r'd ro tle o$er

nmo@mposites bascd on Fisue 32 vhich meds thar the conp$ile sudace danage n

highd ii 0E her.unosph@ in @otrst wilh lhe othd on* The prosressile addition ol

ruofubes in the polvher mblfix h6 augme ed the $emal stabilii] and surfacc laler

prctecion of th€ comPosiF sp6iD.6 C, S, Zn dd O de $e elenents delected in EDs

&dlysis of S5 dd poriBve<l in Figw 32t TIF incoryoBrion ol lhc Motubes r'ro the

bae composile fonnulation cnh!@s th. suif@ preL.tion of ihe composite sFcine! 'n

lh. srqdy dale h..l ahspn r! osing ro tlE bigh lhdml stabilitt.

FigN 32: SEM ina8.sofpontlemal co lwlivitv/inF{t!@ tdcd najMnFosit'

sp.cim.N scl (a), Sc2 (b), sc3(c), sc4 (d), Scs (e) sd EDs @lvsis of sc5

@mpGiL s!6incn (D

5.5.3. them.l ltibilitv and h.!t flow dpone

Thmogdvidelric u.l'sis of lh. bba nd$cobpciLs in rc6Pentut 25 lo

800"C is deprcl.d ,o Fisc ll ro 4q.n!in eff*r of F-MwCr'Ts loadinss on thmal

$ability of sBR tnatix. I1t lQelo wishi lo$s b obs*ed in $e GmP€tantre r&ge 200_

{odc dG !o pmcsirg oil iraaic aid aid w GvtPontion Ttu traimun lhemal

d.grad.rion u notied in thc advflc. Ioooc dB o rlE polyn'r maui\ Pvrolvsis

IrEignifi@t wigltt lN is obed€d up to 6O{fC and thc maxinM tlemat desFd'rion of

thc compGite spcciM i3 noliad in li' Fo@'diig 2afc F7l'

Figre l4 clucidltd th. helt flo{ rcspo$e ofilnc polvder nano@mposites and the

nAinM vqidion in hat flow is obw'd in dE rsnp@ff! tuge in which the

mdim@ fiemd degEddion h4 h'GD mticcd in ih'tuogrwinEEic etlvsis Th'

compo$re maldials l.nd lowdds the endodemic Rlpons wirh lhe progFsi\e

incorpoBtio. of F-MVCNTS in the host naiix SC5 hd ab$tbed t\e naximum input

heal onparcd lo o$er ones.

8*!"

rcrpc*n0Q

Fig@ ll: EIIel ot F-MvNTs @'mt!|roN on lh. thhtul d.g!.Llion oI

F-MWCNT/SBR speioens

5.6.4. DSC aiudy

In older b aDly4 the c|Iet of F-MWCNTS conentdiod on gl6s 1r'6irion

lenF6tN (Tr, cryslallizion t mp.stuE (Tq) ud nddns Lmpedute (T.) includine

$ei. speific olhalpis, diftrcnl'al scannins calorimeiric (DsC) wd oFdted in rhe

lemp@tne m8e -?4450"C FigG 35 4d datr i. l abl. 7 illuirac that Ts tdues up lo

6.15"C. T" rcdncd up 10 4.91"C. T.1 sd T" ioctease 1 44 ud I 300C. @sp€cdvelv snh

ht% addnion of F-MWCNTS in th. SCI composition, The dects. in the T! inpmvs

the rubb€ry behavior of scs 6d .n.blcs th. polymoic chlin nobililv posibl€ ev€n in

noe nesalive tedpentu@ [ 136].

'nE rducdon in T" wi$ iodeding neoubes conceDration in ihe tubber natrix

i.di6t$ that p*en1 crylhUinity ol the nanocomposile irc'€se wilh inceasing fi€ 6ller

The slielt incEase i. onsel &d te* m.lliog Poinb of rhe polvmer cohposnes is

.lu€ b resistance oiTeed by F-MWCNT9 lo slow dom th.@61 chdin nobihv of the

polyner nauix in heatids envnoM.nl.

td9o

E

II

Fis@ 34: Endo/Exolh.mic bch.lior of F-MWCNT/SBR spccimns

Fisw 35: Dsc @n!o6 of F-MWCNT/ SBR speidctu

T.ble E dhphys d cil4dve rdudion in speifi. .nthalpics or Slds

r&sitior/crysLlliation ed imprcv.tuit in sp€.ific cnthrlpics of on5.1 ud p€* mclting

ph66 w'1h progEsilc in@Dor.tion of ih. mtlb.s in SBR du. lo higl thmd

sllbilily, rlsi$ee lo polym.nc ch.n nobiliiy, 4d h.ll .b$tbing caplbililv of the

in6rDo6t d F-M1vcNTs,

Idtfi3II

TABLE ?: Effecl of F.MWCNTS @n@nraiioN o! the sla$ tlosiion, c.vslallialio.. ..donse/peak nelling phdB t€tnp€niu€s of SBR MocomPosiles

sc3

TABLE 8: Erect ot vdier concenlrstio$ of F MwcNTs on tne spdific e'thalpies (Ts,

T., T.,, & Td) of sBR Moconpsites

5,6.5. Meb.nic.l pro[..n6

Udvcbal tc6ile tcsln8 rchine wd us€d ro ex4ute lhe str'stain b'havior of

ihe fab.icated nanocomposites Figuf 36 illuFltes fiat wi$ incF6ing frller

concenlralion in the rubbr maEx, stess b.sing calabilitv of $' ndoconposres rs

rmpbr€d bur elongation Al bRal suff.ted ll is obs'd rhd uhrMt' tmsile suenelh

(IITM) is Eisd uP lo 47% ond elon9tion al btaL dininish€d !P rc 48% wilh $e I *1%

in@eodtion of the o&oubes isto Uc bas @mpdile fomuladon showing s@llenl

sechanical siangih, strcng nlleFmarix bo.ding and uifom dispc6ion ol F MwcNTs

Fig@ 37 illustrat s thd eflsl of F MWCNTS concentration on the rubber hddne$

of lhe M@ompciLs The plogBiv. F MWCNTS impngMlion b fie Nbber mtix

h.s lueFdicd rhe rubbd bEnns of SCt up !o 5? Shorc A elativ' to lh' bN @6posne

romdatiotr (SC) ) i.e. 40 ShoE A, @ulctPln

"8o8,o!of;

FE

!6

.!

I5

Figw 16: Efl6l of F-M\VCNTS co!@tnlids on UTS a.d Ftc clong.tion at b@t

of F-MWCNT/SBR sDccin a

This inplovmcnl h lh€ Nbbcr h[da.ss of lhc Potvler @@nFosil€s is du. lo

nm*lte iDcn tion *ith lhc polyftr ch.iff, .r'd dc uifom dispc6io! or ca.bon

motub.s in fte rubtd duEix. h i! .le .tEibln.d to th. mtubee turwotk winin |he

polyftr Mlrix th.t tsttict! thc Polytudc chlin mobilitv .nd evdtunUv cnldes

deslon dc hardFss ofrhc @mpcii. sp.cincn.

Figue l?: EiIed of F-MWCNTS cotudtr$ons on clstoDeric httdrcs of F-

MWCNT/SBR sp.cim.ns

3

E!t

5.?.r-MWCNVNER.luloDqi.nm@npo.tld

5.?.l. DispeEion ot F-MWCMS i! Nittil. Buirdi€le Ela$om€r

Ev.n dirD.Rion ofF-MVCNTs h th. NBR Ertix 6 h' $rutili2€d in lhe sEM

ni@gnphs, di+l.yed id Figw 3S (a b) rtoo€ with EDS in Fi8@ 3E (c' d) The cvd

di$.6ion ofF-MwCNTs i!lbebot Drlir DdG.|t'I|@bpotiL trroc clloenr und'r

thmal or incch{ic.l lodd. Th. cotnp..it spoci@ EDS (FiguE 38c) cotrfims tr'

addinvs Dresenc. sttilc lhe EDS pEscn&d in FigrF 3Ed @nfitln3 th' exisiqe of $e

@ot$€s wi6in th. hosl Polym bittix

Fieue 38: Micro!.opic viw ofF_MWCNTs di!p.si@ i! th' NBR maFix at dif€rcnl

Esion! (., b), @ryosilidd cdvsi! of 0F om@tosiL (c)' and the sDor

clcmlt|ld rlrlFis ofdt onolulc (d)

5.7-2. Th€mal condu.livity/int€daac. .Idvsis

Thmal condulivity m€Gwncnts of lhe rubbs Mocomp6il6 in &npqolr'

@ge 323-523K e ponny€d in Frglrc 39t 'Il!e eldati@ 6f rtmal @ldqdion al slln

7'

of expgin nl for NCI is low tban olh( tutt@nposn6. r falls dou wilh inctaing

upper @pFr bd tmPdaluE uP lo 173K. tnd thd rypmxihaely 6 @Nt l*el of k fo.

rll conposir€s is cstlblislFd itr the Fo@cding tenpennE tugq NC5 senles ibelf at the

lowest Dosibl€ level of t mong the otho @oconposi€s due lo the matinum

incorDoralion of f-MwCNTs in lhe polynd mas'x [u8]. t d€cleaes wilb incEasinS

CNT5 6l]m$alio. h rh. ho$ nanir d ,hom in FisE 40 NC5 ls 42, l?.5 ed 50/0

l6s ( @parcd lo NCt at 3?1, 423, .nd 473K dpelivclv Thmal @nducliritv of thc

polymer conposilB d@@& upotr th. chenicd coNtiucnr' nolecule dcosiiy

disi butioq bond shength, rcinforcenent lype/loading, Focessiig conditions and

Acording !o popo* lhdbal @nilucrivitv nodel of Y A!! i eral tl46l, thmal

@ldetivity of the polymd cmpc'&s uith hrSI 6lla volunc @.r s h dininish'd

wilh nsnE tmp€61w. ln mc polyncric srslems uifomly inpregmled f-MwCNTs

in the polym€r mattix d.v.lop a .mtlb.$polymq chai.s nelworl lha1 rcsisls te phono!

tsporr tftugh th. nanocomposir* owitg ro ll€ Phonos oltspping wilhin the nctwotk

So. lhe ln.d8l @nduchvity of lhe conpcire sFcines is tduced wilh incFdins

nerut6 b maldx ra$o,

T€.rpidr'€(9

Figu€ 39: Th.drl condknvity onto!6 in thc tenp€onE rmge 123-523K ofde

NBR composit ryeon$

tz

t6tI

0s:0.601o55l0 5010.45,1

o.0,j051030{o25l0.rolo15.j

0.6,|0@t405'l-

Themal imped6c€ (R) @ oN of dE conpositc sp€dneN i. rhe sctenpqarde rege de depicted io Fig@ 41, R.l.vdtes up $ 503K lbr.1l lsoconposiks

but th. bte of R elwarion is augnoled wirh dE prcgFsiv. in@rpodion of MwcNTs in

tz

,6!I

0.@

02 o3

5.7-3. The@osnvimeuic dd di{IcMtial lh@d dalv$

Theml degraddtron of fie labri*led @olonPosils

@ to00"c i! displaycd in Frgw 42. Tnis show $al

tuCilo|t lbotu!6 (wt9q

p)

ligue 40: Efi4l of mo1ub6 concdfiatioN on the rh'dMl conductivitv ofNgR

spFin E al di|Icrcnl |.mpcdues

NC5 ofcu mdimu lh.dil Fsi$ue to inp hat in conplet' tmp€raiue

@ge due lo F_MWCNTS neiwork in NBR nailix tbat clprws Phonod ed 6h$ lhe

Uolnl mouhy of tre polvmeric chais A r€duction in R is ob€€fled 'Its

a specilic

tenpedu€ but the decrcasing rate ofR is obsqved nininun for $e Fal f_'MwCNTs

in@!po6c<l nso@nposiLs dc to tu etrdive @olub€sDolvmer chains nelsolk

withi. tho conposile At hrgl rcDp@urcs e475K)' lhemal Fobilitv oite polvmeic

chac $.1esulrs i! bond $ision of thc mol'culd chai6 and co'*qu€ndv' th'nMl

impe.le@ olihe ndoconPositca is €du€d affet a sFcific tenp'nture el€valion [149'

r501.

25

-.- 373K-4,-423K--*-473K

Meomposnes inc@ei Pith imBitrg F MWCNTS

This bapp..s due to higl fiennal stability ed the

polyn€tic chai! nobililY.

concdltalron in $. rubb€r Mtrix.

lbility of F-MWCNTS lo 6nt

3

E

5Bc;a

2.0

1.6

05

Fis@ 4l: ThedEl imFdlne prcfi16 ofut @olosite speim'6 wi0t

cDp€fi w/cNTs @Imulton atr€truliot

T1l€ $emal decomposilion up lo zoplo is okeryed in $e Enperalue rdge 200 lo

400"c dB !o lhe evapoFrion of l!. plGssing oil, sl6nc sid ald *q i e i'cluded itr $e

b6e fomulatiot ofrhc Moconposiles Msinu rhemel dcgradslion h obsefled in lhe

p@eeding loot inctm.nl due 10 the polynB datix Pvolvsh The olerall ninidum

md mdinM thffil d€86dation e obsryed for NC5 &d NC1' €speclilelv At500'C'

lhe lmass% F-MWCNTi iFpFstr tion in thc rubb€r Mtrix ha eilurced tbe fimal

sllbilily of rhe Mocomposii6 up lo 3 4% Flalive lo the bde odposne fonulalion

(NCl).

FiSw 4l illNrdtes difeEntial thcmat analvsb of the @o@nposics in the se

tenpdalue @ge An .xolhe@c Gponse is obw'd @ud 400'C due o @mlic oil

exhau$ and then all mooonposit€s absotb e'omous h41 Hqt quenchiiS capabihv of

the conposite specineN.on&@s with ih€ Motrbes inpcgdtion in the NBR narir ts

CNTS hlve rh€ epabilily |o entq phono6 4d awhcn| rhe@al srabihy of the rubber

@4ohPosite

15

0 2@ 4@ 300

Tclpdfltseq

Figw 42: IlFlmal desndadon @spo!s. in .t ltnosPhcr d difieMl fill6

@nc€nltalioN {iihin the l€ip€ntw dge 25_ l000oc

02@4@@TdrPd{,!09

FiSw 4l: DifI@nrial themal aralvsis of the conposite spedinds at vsimt fille!

concdtraliotu withi! lhe tenp€tatw 6nge 25'l000oC

59bIg!t

5.7.4. DSC srudy

Difeedial *min8 calodmeric sudy in FiSuG 44 sho{s rh€ ell4t of F_

MwCNTs o. fie glss l@sition (r), dyslalliation (I"), dd meltine (r^r & I.,tenpdlws of the robber M@omposiles. The calculat€d data ollhe$ Phas choeing

tempeFlws ae labulared in Table 9 fon th. Dsc cootous. 7s of the .docomposile

speciDos has bee. tduc€d wilh the incoiponlion ofneolub€s in lhe polrher marix md

$e sme r$ponse is oberved lbr I..

E8IiD

!I

T{fFel!0c,Figw :r4: Difre@tial sc!.ning calorinetiic study of the robbd m@omp6nes wilhin

rhe lempenlue spa! -?4- 450'C

ft is anribured ro CNT\ rctrcrk in the rubber natrix viz resisls the phas chfl8es

by ider&tine with thc polyneric chain al lhe mossle ed brcadeos tbe rubh€ry dnge. ll

nes lhat NC5 neo@nposit€ tr be openled ih nore negaliv. temperature odpded io

ottEr ones up 10 7.17"C. TIE ons.t ed peal delting rcnpe6tures viz. lal ed I-lEsperively ee enl@d up io 12,13 &d 2,ll"c, Esp@tivcly b€suse nanotubes

corotain tho @Erx noleculd chain nobility by entraPPing phonos witli! the filleas

ner*o*. Spsinc. h.lpi.s of thc Moconpositc spe.im.6 @ dePicted in Table l0

Il is ob6@ed thd sD..ific enthdpics of the 8ls mnion ed cr'sLlliation

phe chdges e dininished with incrtsing till4 ro naEn Blio. But rhe sPecific

crthrlpias of oNd .Dd Flt mclting phls rr. .l.vn d dG !o lhc cnhasm.nl in

cndoth.mic 6tw &d thcml .ndl||!F of t|| nrnoconPcir. wilh imBiry de

doping conccitr.don of 6e nd'otub.s in thc NBR rulrix. TIus phenomcmn k .le$pFn.d by dE DTA thmortlB a shoM i! Fi8@ 43.

TABLE 9: Ef.cl ofF-MwCNTs c.!tc$t ioB o dE ghss t$!idon, cryqdliadon. adonscuFrr mddlg plE!6 t FFntur.3 ofdE NBR sPeircN

IDr,(o r. cc) tr fQ

t{clNCt

NC!

TABLE l0: Efl€c! of vader @Enflliotrs off-MWCNTs on thc speific .nth.lpics (T'T., Tir, & Td) ofNBR Ma.npodtd

NC'

5.7.5. Mehrnicd Fop.ni.s of F-MVCNT/NBR omPosic

T.Nile @$rng of Mncompo6ir. splcs B wi.d out ro cvd!4e th. ul$hat

tNil. srcnglh dd p.dnt cloqdion !r bdk Maxinm srcn8ih of thc ndftomposild

irc@scd vhile thc clonsrtion.r bial d.uled wi0r 6c sr% in rlMt of F-MWCNTS

@nr.n!e in lhc NBR h.ttrx s dcDictcd in Figun 45. Thc mcomPosir. with I $,1%

loa<lin8 l.v.l of F-MWCNT3 hs 23% b€r.r tc$ilc strln8rh' NCI b's. compos't'

fomulllion. A 13% tlduction in clonsalon .t b|!r|( is.ls ob6.ry.d in th. hdhsictl

prcpenics d.t for NC5 s @mpcd lo NCI conPdit duc to th. Glsnic mlG ot th'

30

7.

E

20t9

15pID

F3

a.It5

t

?

b!tI

Figw 45r Efiect of F-MVCNT3 on ultit t t Gil€ str'ngh 'nd P€tcent elongrdon at

t@k of NBR sPeineN

Figure 46: Efle.t of F-MWCNTS oo hedness of NBR conposne sDecinens

'Iis @6 dE to lhc @o*ale nlory intcdtion of $c inpcenat.d nootuDes

wilh dE poltd€ric chans of the polvmd nano@sPosite

Crbon rf.dD. M95)

50.

crldt l5snit- ({90

A! incrcdins tend of Shor! A h!rih.$ with ircle6ing filler conlents iD the

rubbd maldx is obsrcd i! FiSrE 46. Ib. | $t'^ inpr.glalio! of F-MWCNT! in the

NBRn trix has.D!r@l l! ebtq h{dn $ of tbc F-MWCNT/NBR lt'll@opositcs up

to l9a d@ !o tle b.inle Drtur., cvcn di!p.t!ior! and t.lt p€sl tug. .la3lic mo<luue of

t inorp@&d 'letu!6.

5.& locf...lied N.loLrolllt /EPDM.L.aordi..ilxFbpclit65.8. | . Di3pdsi@ of t|ek@liliL (FNK) i! EPDM d$bnd

I1F dos-s.cli6 of th. t65itc frrctund MkaoliniL/EPDM rubber

mo@mposir€s sFcin@ wls okclved in SEM 10 onlm 6ifon disFBion of

n&okrclinire in tle hdl rubb€r mat ix a! in FigN 47.

Fi8@ 47r ril€r disleGibility and comp$ition l odylk of EPDTTTNK sp.cincn bv lhc

aDolicalior of SEM/EDS

tdl

iri

:I

I

:!I

3Z

5.8.2. Tbflnal lrnp€d6ce/@ndFtivity n tsurcmot

Themal imlfddce E) is the lolll Esiirn@ ofrer€d bv a matcial against tbe

rhemul \rbating enriomoL R ol th. rubbd Mdomposite specine$ Ms measuEd

dd the @eivcd dan 5re conpiled iD Figw 4E

It i5 obs4.d ltor the R of fie @npo6it spocinm is inc@d with irccaing

tcmFErue md filld @otents in tlE rubbd tllrnx T!€ bighBl iftorpoBlion of FNK into

$e polyD{ nai x has augm€ ed R up to 64% al 49lK s conp&ed lo the bs€

conposit fomulalion (EKl ) 11 is dhibuted to excelle bet lbsorbing capabilitt' warcr

evalomdon sd ev€n disp€$ior of th. tr4oclsv in lhe hosl nslrix R of lhe composne

slein 6 i5 elcvaEd eith incBinS |€rnpcdtue up ro 473K duc !o the edomoN hcal

lbGotunon in ht$e vibndos of fie polvmic nol*de chajns sd 16r photun

5o

za

e

!II!I

FigE 48: Efled of FNK @@nFations on thc lbennal impedecc of EPDM composile

'Itemal conduclivily (x) of thc omposilc sFcid$ wls @ndudld according 1o

ASIM E1225-99. Ficw 49 €luciddes th€ ( elhdemcnt with incFding 'npul

t€np€nt@ which ac@lelates tbe atonic libnlio6 donS the molecul$ polvder char's

@.1 4 a 6ult the b&kf@ leoFotN of the re$€d nalenal dso enndced thot reduced

tlE roF.alw diI1irc@ b€rw€d lhe ts fa..s [149]

33

1.5

Trrpi nrt!(lg

06

o@

Figure 49r EfI*i ofdifeent FNK

conp$il€ fomuratun

TmFtl|8(n

conc.ntations on the ihemal @ndu.hnce of lhe b6e

h b ob$ry€<t thar K of th. Dolvmd n n@Dposil6 is diminishcd wilh lhe

pree€ssivc addition of FNK in lhc rubtd Flrrit owing ro De ficmal tllbilitv hcat

qucnchiog cap$ility, ald evcn disPcsion of6c nm6ll$ in lh' host maLix SEM imqes

ofth€ oosr lhcnnal r&sport l€sted @mDolit spe.in N e displav€d in Figut' 50 lt n

oodced tha! nico.Dorcs @ gene8t d io the low fitler concotrsbd rubbtr conposites

compded 10 $e highly lold€d sp4im.$ due to the excelled lhmal endursce aro even

disrribution oflhc @@lay in the EPDM malnx

5.E.3. Thcmal d€Sradatjon and hdt flow b.hvior

Thcml slabilitv of rhc dbbq n@npo€ites vd qsul€d in the rcnF dtue

dgc 25 !o 850!c in air.nvimmnt a.d rh. @lldted dara @ @nPiled in FiBUF 5l-

lnsignificul wigltt lN is ob*rycd for ihc fabd@Ld @nposile speimfts up !o 300'C

Atur dar @ud 23% themal degrtdation h sctuini4d due 10 the arcn ic oil 4d wq

dapodion in th€ PMeding I Oo'C h.st now dung the dmogravinelic analvsis'

Polymet d.clad.tion dd polym.ric ch!i! sision re ootic'd in lh' lenpcraluE

rsge 4?O-540oC. TheEEl enduec€ of the polvnr ndocomposncs tt orve$

emD.6rG is progrEs€d wirh it665ing FNK otmlalid in th' b$' conpG'le

5a.

c

6

!

fomulatio.. I hrppens du€ 10 th€ q@ll€nl thmal sltbihy od evfl dispe$ion of lbe

qfolialed la'€Fd siliotc m@lay i! EPDM.

Fi8e 50: E|f€ct of FNK loadings on th. sufa@ norphology of rhe the@al raispod

lded EPDM nan@nposirc spccimN

Dire@tial th.ml analysis of thc FNK in@ryont d rubbd compGiles w@

cdied our in ft tedp.lal@ @8. 25 io 900t h d. cnvimMent. Figue 52 elucidates

$!l lh. mmporitc speimens aberb hai up 10 100'C, Tlis mrey Nd to ov.rcone rhe

covd€trt boldiry amry th. mMers md to cvapoEc lh. pbticizirs aids included in

thc cmp6it6. Aftd dDl h€at exllult in the pFcdirg 2OO"C owi!8 to lh. rclatile

pbducts dd g6es (CO2, co, sO, a0 .spirg duing chding of L\c cbslinled

FNK iEpcgnd.d @Dposii. speim@ lac dsorbcd .notma hc5 in the foE

@ning lodc GDp.drc sF!. It i! lnribut d dw lo .ndoth@ic debydmxyldion ofthe

inco+onred tuo.t.y in 1!. renFrsur! r.ds. 50G600"C which udsfom kelinite inlo

g"loIE4t

'I15

0

TdP.tnf!egFig@ 5l : Erel ofdifl.|lir FNK ondlr.lio6 on thc ti.dal &@mposnion in an

evilonhcnl of neocohpositcs

5.8.4. lelh€mrl behdior

Difcrcdial $@ins cllodn.ttic a.alysis of rh. FNy./EPDM composires $6cond@Ed in lh. cmp.nrue 68c 744J0t i. ai..vibm.nl &td th€ reived d!t! mconjuSat d &d pEsc edinFig@53.

figue 52: Erd of di|Iccnl FNK lo.dinSs on rhc .ndc,/.xothcmic behavior or

t6

?II

20x!,{q)nD807@ADS

36

582E,eloI

TfrFdr6ecl

Fis@53: Etr€d of dilf.Fnl @@ r.tios ofFNK on the difcEntial scdnins

calorinelric resllts ofEPDM codposites wi$io rhe temp@tw dnge -74-

450"C in air enviomoi

5.E.5, Ullimale lelsil€ strength dd hardness

Tosile tesling of the FNK incorporaled rubbd mo@mposires w6 ex{uled

lc.ordine lo ASTM E1225-'9 ad oblained Bulls @ displayed in FiSm 54. h is

Cl6s !@iirior reDFaie (TJ, crrsrallizatiotr tcDpeotw (I.), osa mellios

phae lenp@iw (T.r), md pal melting phae tenp.rature (T., along wilh thei!

specifrc €nlbdpies werc m€6u.d fron ihc DSC @nlos. The collecled dala ae depicFd

in Tabl. lldd 12. It is obsePed rhst TledT. e dihinish€d up !o 5 dd 2'C,

Gpelively with ircGains th€ FNK loldiis in the rubbci matrix de to thc soR Dt@ of

lhe ne@lay which exrends the tubbery nnge.

The @l€blc inclt* of 3? ed lo'C in the T.rod Td. Espatively are

eruiniz€d in tbe presenr.d dala wilh thc mdin@ impEgnation of FNK in the EPDM

ba* codposite fonuldion, Il is atttibur.d to rhe.ell.nr themal srabihy, endothmic

capability, md den dispeuion ofthe ndoclay in EPDM matrix. SFcific enthalpi*oflhe

fi'sl two trsilion lehpcEnE @ rcdued while the Delritrg rraitioo sp.cilic qthalphs

@ ausmenled wilh irct6ing FNK cont nts in the baic rubbcr fomuladon.

ob*Frd thlt bolh str6s and sdlin ate .fel€d prcellsiv€ly eith ircrding n&alay

contenls in the rubb€r Dalix.

TABLE i I : ElIeci of FNK loading @.@riralions on rhe gl6s l'dsnion, cry$alliation,&d oBcvpek melling ph6B temp€nt6 lhal wcrc n4lrql fton DSC

@nroN of EPDM @msii. s6in@

TABLE | 2: Efecr of FNK loading @Ncn|!"tim on tle sF.ificlraffirion r.mp@tG (T! T., lnr, & Td) |har EGcontour of EPDM speimeds

tx3 EK4spalfi c En.b.lpy orcl!$ Trrriiior

Sr..lfi. E b.lpy otcrr!|llhrdo!

stdinc Eo.n.rp, of Frd M.rdo3

Spcmc Edh.lpy Sdtrd M.ri!8

IrF INK imFeenalion ha md. thc rubb€r @@oEposile lougher with e.haffed

plaslic rcgio!. Figua t5 €leidaas dEi ultimte IqBile sLdgth sd elonsadoo at brcat of

|n. f.bnded @mposite speirca e.nhdc.d up to 92vo dd 100v0 wirh 0E l0 $r'lc

incorpoddon of the .doclay. Thtu is du€ ro sfory filler to natrix inr€rdlion and.v.n

dispeaion oflhc NK in rhe host rulrix I l r 2,152 I.

Shore A rubbs hddnes of the rubber conposile specimcns w6 delemined aDd is

disrlayed in Figw 56. It is ob*d.d th.i rubbq hddrBs incca*d wilh inc@ing FNK

l@ding in lhc b6. @mposiE fmllation. thc Iwinm impEgnalion of lne @@lar in

dre rubbq nalnx h.s auemdted thc hatdres up to l//". It is Enribuled ro th€ Esist nc€

orered by th€ ihprcsnated fillei agaiisr the polynaic chain flow uds the dyMmic

torce. unilom dishibldon of the nsoclay in rhe hosr nairix due !o the elleclile sufaoe

modifistio. ol th. Melay also imp€tts m impo,tali rele lo .nn3ne lhe m*beical

ltrdgih ed elasbm.nc badlB ofth. labddcd @mposiie sFcimm 0 531.

33

z

65

5.0

1.5

o5

6 i 1do 1b 2io ?ao {D 350.0 4so 5m 550 dosdn 00

Figw 54: Eff.clofdifrere FNK conc.nlniioB the strestrad beh.vior oielstomoic

;m-ra.t ibellsh

Figre 55: EIfet of vuidl FNK @I@l!llio6 on rhe ullimarc t€Nl' strn$h dd

clongltion at b@t of EPDM compcile sp@imm

F

!tPlg

T3

!6!t

5

tSot-llnlb ({tvq

A

15

10

?66p

I

rigue t6: EiTst of diffemt loadinss of FNK on the elaeoneric hddms oi EPDM

5.9.Fu!qtio!rli!cd Nrolt oli.itdsBR EhtaoD.tic ru@Dpo'il6

5.9.l. DisFNior of llmk@ti.ite b SlvEnc butrdienc dsbn6FiSu 5? {a, b, c) explidte6 th. €rcn dispesioD of trokmlinit' in lhe SBR

elsloneric Mtnx al div@ etrldg.mcntt ll sig.in* Oat $e surfde modification of rhe

nmoclay hD inPrcved ils dhpeBion effcacv withi! the polvner matrix bv i edct'ng

wi$ tbe polymeric mol@ule chais Figu. 54d elucidates the conpGidonal an'lvsh of

th. marimu loaded moclay monposit sp@'meq which co'iims the cxistnce oi

$e C, O, Mg, Al, si, ZlL S, md Ca in rhc fabdcdcd obbs foodlion [E2' I 54]

5.o.2, Ihrnal C.trdutivily dd rbcnul lmP.dee aElvsis

ftemd @nduciivity (t) 6ntout3 of thc .ubbd le@mFsit6 in th' t'mPc'?o€

r&g€ 123 ro 52lK e illBrated in Fi8G 58d lririallv.lhmal @bduction thbugh the

SKI composile is nininu conpat d to ihe clav @donposires A d'asiic de'line is

obse ed in lhe { valnes of 1h. @mpcit in thc lenpet'nE rmge (TR) 133-3?lK After

that ea.h Nbbd nd@omp6ite hN d.blbh€d a epdralc level of k in 1hc prcc*din! TR'

fte SK4 n6o@nFsile h.ving l0 *t% FNK h61h. least level of tdu' !o l&g'r hcar

q*rching abeth.d by m@lay dui4 in phlsc cha46 ald wt{ evtpontion

90

riSuE 5?: SEM ni@gnph! of '@t&linit!

dilp.nion al vqi4l n'slificdiom (4 b' c)

dd @rysitioBl onlbli3 of 6. 30 s l@tl€d sBR Polvler

t|ltrocmposit6(d)

Ttr vdialio! ofxsilh.*pccr to thc fNK ilclui@ is disPhv'd in FiSBe 58b It

.lucidails ti.t r is diDi.ited wilh i!. FDgnsliv. &ldilio! of FNK i! thc tubbcr trailix'

'Ih. high.sl FNK l@ded Mocmpo€i& foddation hs 41,22, ed 4l% l4t ( comFred

|o 0 $t% @nc€ntal€d SKI @mposit tP.cim.n at 373,423, and 473K' respelivclv ll is

attribuLd 1o th€ hieh sufee $c4 €rell.nt h.3t abEotling capability, dd ndosale

int tunon ofNK *ith th. polyinlt mti,( [l ]8'l 551.

Iigw 59 sho{s tF.fi€.t ofINK on t tbc@tl inD€d'fte offte mocotnposiL

sGin€c A! cl4.li@ i! lbmd inP.d&ce (R) vdl6 l4 to 493K is ob6tdcd in dE

gnph.d lh@ t r.dEli@ is ot$nEd.t higld t DF!tue dE lo tldPi6lio l @lug

.F.ol ssocid.d wilrr dagonion of s$ntlic oil *itbi! ihe ltMtotitc sPc'rtncs

Th. m@onpsite SK4 hrs tle n xinun .bilitv lo 6 i@ning he|t 0llx wifiin $'

t.st d tlEDdalw rdee dw 10 th. mlnhum namctsy in@lporation into thc polymt

mahix 038,1561.

020

:

5

=3E6!E

Tin6d'!0q

Figw 58: Eff@t of FNK !o SBR 6rio drdnal conducriviry wifiir th€ lemFartrcmee 123-523K (a) od wi$ vdiatior at 1hre€ dives. lenpedu* (b)

.'lrE2 5.1

il1ol

Io5lool

tgT

T

;

T

rcrpr&r.0Q

Figue 59: Eflal ol FNK on rh€i'llt impcddce of Ihe SAR nmMmposires wilhi. lhe

rcmpsalm sp0i 323-523K

Figue 60 (r, b, c, ed d) sho*s the sufrce morphotosical on lysis of lh€ posr

lhemal conducrivity t€sled ndo@nposnc spejdds in te lempemlue mee 123-521K.

A lsge nwb.r ornim voids d! ob$ntd in SKl. Th.5z dd q@tiry ofihs po6

e r€ndksbly rduced wilh inl)@ing FNK @ncosation in the rubbq maldx. It neaff

th.t M@hy impE8naEd rubbs i,IrlrcmposiLs h6 lcss sufa4e d.tDge in the he.ting

envimmc @np€rei io &e be pol'ra- lt is anribuled to the q@Ue lhemal

siability ed heat absoibing capabiny of inc tunclionalird nodlay. Fisw 6le

elabdllB lhe @nposilional ulysis of the 30 ef,6 loadcd rubbd conposn€- fteercmenrs c (59.99%), Al (5.69%), Si (r2.55./o), O 04.52%), S (1.10%). Ca (l 96%), Ms

(2.5E7.) ed Na {1.6270) @ foud i! thc.nqey disp.Rive spellosph Mlysis

6nnm in8 0'e labricded M@DposiE dgrgncd fomuhxon.

Fig@ 60r SEM micbsnphs offi. pcr rhcmol condrctiviry i6tcd sK I (a), SK2 O),SK3 {c), SK4 (d), FNVSBR speincn and composilionat analysis of loMyo

looded obF€ic sp€cimo

s.9,].Th€ntul dc composido! a!!d dif€Enri.t rh.mDt rndyss

Thmd edlme of tnc Nbb€r Mocomposits \l@ ar'lyed in aii arnospheE

froD oon tchp.mture to 850'C ad potualed in rigN 61. An iGignificer weigh to$is ob*nrd up 10 425!C. Afrd rhd rhe tuidm rh@ai degEddion is s@linied in th€

prcceedin8 l00qc due !o potyner prrolysis md polynenc doleculff ch6i,s bcakage.

Fbh 550 !o 85dC, l[G is no signilidt chege in wigh( 16 is obsry.d for rhe

@o@npodte spoinens du€ io lhe llmitrirS cabo! chd ed dc neo inclusion, A

93

monentous .nneceDdt in demal odudce is noiiced at .ll lemPenlures with the

in@.sing @ncenugdon ofnodificd NK in tr SBR mtrix[871.

Fiew 62 d€mostdt€s lhe led qutuhing poiotial of thc FNISSBR

naoconposile. Tlt composir. specim€rs absorb enonou h@t up ro 100"C rd lhe

upward plal..u ec obw.d up ro 60dC dE lo rhe qhaul ofvolarile prcdErs included

in the rubb€r @omp$iles. The h€at abedine capability of th. noo@nposites h

augmented wilh thc ptugressiv€ iacorponrion of FNK in fie n$ber tnarix. I is affibued

to th..xell.nl thcmEl sr.bility, hid sutf!@ d.a, dd strong n.mc.le intchction of$enooclay widr polyneric noleculd chai.s tl57l.

5.9.4. Ditrcrcntial s.minS c€lodn€tric audy

Figu@ 63 illusrdrcs rh. DSC datysis of th€ rubber nanoconposilcs in rhe

teop.Fnrft MBe -74 io 45dC lo ealyz rh. €fld of l]'@tay @nenralion on rhe

phae tmsition lemp€ralur€s and tut sFcific €nthalpi€s. cls trdiiion temperaue

(T!), crlsrallizilior renp€nnr€ O,), o6el @trinc lcmpe6r@ (T.r). ad p.ar mettinB

tenperatG (T.:) wnh $el 6pectiv. spsific e tatpies of rh. FNX,/SBR

nMocompoJne) ar compiled In fable 13 fld laresp(li\e

Tarlcdreec)

Figue 61: Etler ofditrercnt FNK @rccm€rions onlt thmal d€snd.rioi in an

envmmenr of sBR @mposn€ specimcns ir lnc tEnpemlw timir 25_85oec

I3I{

6{6-sE-l-oEl{ot

rs'Fd|!eq

Figw 62: EfI€.1ofdifreE FNK loadings o ihmat aberbane caplbihy ofSBR te@mposite specimeN wjlhin thc lempdllule mlce 25-850t in at envirome.t

The Ts of $e poly@. M@nposiI€s is edu@d wilh iDcBing ler

corcenlration in lh. hosr datix dd a lo"C Ts Fducdon is noticcd with rhe lO rfloiroDotuion of FNK in fie dbber @rrix. It nlfu Oa1 thc mGincluion harn&rauy cnldFd $e rubb€ry phe of SBR noMmposire by inl@ring wilh tbe

polttnedc ml*ular chaim at thc nmscate, Edcing the @$linting density of th. bsepolyma, a<l dE lo ihc $n diG of rhe filts. Cryslalialion l€DD.6r@ of SK4

@@onposile is les &e thd SKI @npo$it du. !o exc*s FNK loadiog in $esnbeq@t fomulaion [ 100.136 ,156 ].

TABLE I3: Etied of I:NK toading @nentradons on t. elss r!6irion, cryslauiation.ed oD.tp€rt oeliir8 phr$s tenp.Eturs rhal w€ detsured &om DSC

I6EIiI

r.rFau!eqFigre 63: Efd of vdidl FNx coMnralioB on DSC o4tysis of sp..in€N in berwn

-74 10 450.C

T,{BLE 14: EfT{t of FNK l@din8 .oncslralions on the spe.ific enrhalpies data al phasetrus(Dn |.nFdw' (r!, T., Tnr, & Td) lha1 *.rc Dc.slied fbn DSC ofcontour ofSBR sD€cimetr

fte poglc$ire addnioo or rhe m@tay ba Educcd rbe T! of rhc €onDosne

spe'm.6 d@ ro th. crysrdti& Ehft of rh. FNK. Thc .ffer of lhe nllq onenlration on

the melting chdacterisics of thc tubber @ocompdiie is opposite to Tr md T! nre

nexing |mpcEtures Tnr .nd Td wss iEporcd dd tbe lrron qfl. concenrdion ofFNK devars Td up to 19"C. tl rs.tribuLd to high lheBal sLbilily, he$ absorbing

capabiliry, suface aca ald even dislebion of rhe @oclay in rhe hosr polyne. nafix[]39j. Tbe speinc olhdpi.s of gt4 rEsirion t€dp.hr@ dd crysb izriohlenp€raturc phtres ee dininbhed whilc a signifiqi cnndcameor is noti@d in lhe fisrmd s$nd delriIg ph2$ resitiom. tl B atrributod to th€ surPlB hcat absoding

9C

a<t

l?l

cap&ny ol $e FNK. The SK4 M@nposie has 74 J/g noE spsinc.nlhalpy conpedro the SK I lomllario. due lo high.r onftntralion of fie rcidoni4 filld in SK4.

5.9.5. Mechmical popenies

Ihe srcss stlin conros of lhc polyms m@odpcnca e djsprayed in Fi8@64. \nich shows . Matable inpDvmor in loughnN of the @nposie spccinens witir

incrsine fiUcr in@.poraion inlo lhe rubbq tutrix. IlF erlecr ofFNK loadins on $elcnsile sftnglh, elongalion ar brcalq and nodutw ar lo0l. ela3ricity ofrbe fablicared

composn€ fonulalions t conpilc{t in Figft 55.

3g

3220t,5

20 { & e i@l 1@

Srdn 0q

Fieue 64: Effer of FNK/SBR lalio on lhc srEssuain onlom of SBR ne@mpositcs

The uhidul€ rcGile sreng$ is iocrascd from 2.7E_5,lOMpa, clohSation at bcaln in@ased froh 137-l6l7q od nodutB of etdricity al l0o9,o .toegarion is incrcs€dfrom 2.04-3.40Mpa artributed ro 0E 30 sdlo nmoclay dddilion ib 1he polyh€r marrix.High surface aca lay€red strude, even dLp6ion, dd moscate inlcocrion of rhe

tuftdoElied n@ntld eileliv.ty dns@ lne ne.tMiql chedsisrics of composne

Shoe A elaslomeric hardoN @np&ien of rhc rubbo .eoconposnes isdisplaycd in Fi8re 66. Shod 4 hrdr* is augn€ .d with iic@ing tunctioiali-dneok olinite in lhe SBR bas fomltdjon (SKt mo@mposne). The inco4oEled

t&

Einforcenent Educ$ the flo*-ability oflhc polymd natiix lhal wentu.llv augmcnr lbe

rubbd hdrdn6s of thc fabncdcd tu@mDosi& [891

FigN65: Influen@ ofditrercnt @.centr.do$ olthe FNK oo the ultimale lensile

stEDgt, €lonealion .t b@L, ed rodrlB !t | 0f4 elGticily of fabricared SBR

@nposr€ spffm€ns

Itrt?

e F€tt93 t".€r r"FI t:!. ltF P5PH t=

t=

5

::

a.

E!!.

5'.2.

50

f;oA&

!205

risue 66: Effect ofvdiet FNK ladinSs on Ur darom{ic hdon.ss ofsaR sp.cimens

62

&50

42

tb|ddlnlb (e190

5.10.N..oLroun it /nitrll. buLdi.!. .hraon r n.looDp@itd

5.10.l. Dispdsiotr of MoleliniL in dtrilc butadi€!. ela$omd

Figw 57 (a b, c) clucidr6 ilc uifo@ djrFBioa of lrnoholinic in th. NBR

mtix al dir@i magnificstioG- It trHtrs t'l lhG sufee aclivtlion of i!. nlnocl.v

imprcvG ils dbp€sion efiici.ncy qilhin thc poly@ hatir resulied de 10 the danosale

ituEdo! wilh lhc polytrcric @le.uld cltils t84l riSu€ 6?d eluidaGs ihe

c@pcidotul .Mtlsis of th. hic!6t dtochy iMryond .mP6iL sFcin n, which

Fveals the flAdce of rh. c. o, Mg, Al, si zl! s, sod ca in lh. f.bdcaled rubh€r

Fig@ 67: SEM niftSraphs ofFM disp.nion at vdi6t maelificalioN (a, b, c)

dd @hposiiodt &dysis of th. l0 s1'l. load.d sFciDers (d)

5. 10.2. Th.mal conducnvitylhsnal ieFd.ne ealrtisThcrtul @ndEtivity mnloN of itE rubbcr M6onp6il.s in the coniinuously

iftBiog tanpdan& atmahse e d.picl€d i! Figu! 68. Irrc m*inu vdi.tion in

t"lr

ii

the themql cooduclivily of lhe rubb€! M@omposiles b observed in lhe tenpelalure

ruge 123-3?5K, in shich NKI shoNs the hst lhemal conduction 6 comp@d to lhe

@clay loadcd composite sFcinens. This happ€s due io the pho.ons &tilatio! @ong

rhe @oklolinir c.rstals oopaed o ihc b& @mposil€ [] 55,I 5E I

a 15

t 10

I!05I

5mTrlpinrs (19

FigE 68: EiI@t of FNK co@.nr..tions on |he rh.mal cond@tilily of (l2l-521K) of

polymer noo@nponles

Affq 373K, n&@nposiI.s ldatt apprcxima&ly a sp.cific @niot level of

th€nal ondu.livity up ro uhosl rchp.6tw. NK4 ha slbM rhc loksr level d@ ro $e

pEence of Mimm FNK @nr€nrs in rh€ NBR hatix. Thc presrcsive addnion of FNK

in the rubber mrrix effectively educca rhe themal @ducrivity. lr h allributed ro lhe

.do level iiieraction of the nuer panicle with the hosi mallix, ligh surface dea, good

themal stabilily, &d excelle heai absorbing .apdbiliiy ofFNK, The e(Iedofclay layes

hd ben ruE cxplained s supqior iaulali@ ed b6s ltuspon bmier aSrinsl thc

gd€aftd during th€ d@nposnion of polymr unds 0r.@.1 condilioN volaile

conFuds in $e polyneric @oconposites.

Thcmal inpedance ofthe @nposile sp€cinens is depict.d in Fige 69 which

snoss ihar th€rmal imDed@ce ilcqses wirh incEdiog tenp.ralule up to 498K tbr all

rubbe. lomulaiions due to endoihmic phenomem viz. tdspin onal cooliog efecl due

ro th. cvapoEtion of ematic oil, hat ab$bed by nanosili@ du. lo ils hiSlt h€l

capacily, lars€ surf&e ea ed mo$de inletulion wilh the polym nauix[ 159].

x0

1.5

o5

Midnm themal inDedae fall is obsened for NK4 owing lo the excellcnl

rbeBd cndufuce en.lothmic ca!6bili9 ed bonogemB disr€6io. of FNK in NBR

maEix [39, l4U. NK4 comFsire ha ]6% exc6s lb.mal inp€d&e @np&cd lo NKI

rubbe! cohposile due ro lh€ mdinu incor?oplioo ol th. moclay inlo lhe NBR ddrix

vhich cnlEn6 tbe odothemic caplbility md Edues the baclt f&e tenp.€tue of lhe

fabncaEd polyftr .omposne 1149,157 I.

e

!

Figue 69: Effs1 of FNK concenrtaiioB on the themal impedtuce of (323-521K) of NBR

@npcite sFdns

S!.fme malysis of rhe p6r thmal lraspon l6cd rubb€r @@omposiFs was

exccuLd sine SEM md Oe nicbgnphr @ dbplayed in Fig@ 70 (a, b, c, d). Ileootpholosical snldy shos rbal tte tr,rel.y ibprcellltion hrs efficiolly diminished rhe

nico-voids genmtion ed suf&e damage duing th€ conlinuous heat flow h sanribu.d to $e excellcnt theml slsbilily ond €ven disp€sion of rhe FNK i. the bde

T.npr{re(|9

5.10.3- fte1Nlr"viftEic.nddiff@nti.i thcmrl tnly3is

TrFdtal degndalio! of tl|€ polFd nam.ompotias opcBLd in air 6vibm61

within tenpe|alw dnge 2t700'C h dkPlavcd in Figure 7l flF @hposile spsneB

show approxin.lely do wcisl lo$ qPtc' 4ldc Mdimu *idl lo$ b ob6efled in lhe

poceding I lOoC d@ to thc be polyffi prrolysis md mole@ld bond bt€akage NK4

rubbd @composite hls lhe suPl€ne th.mal stlbilily in th€ tesied lemF!.t$ mge

mors the lou fabdcaEd compositio lr is annbukd !o tie ulno$ nuodtv

impcemtion in the NBR dlmx which ho! rcmdklbl. thmal slabilitv up to hieh

Figlr 70(a b, c, d)r SEM tniciogr.pt$ ofth. posl thcmrl irmpon E$ed FNKNBR

@Dposit€s

Diffe@tial fiemal ealysk in Figue ?2 d@idalcs the heli absorbinc/d€eding

€palility of 0E rubbei o4o@mposiles. fte cndolhmic abiliiy of the polvno

Moonpodte is lugmlDld wih in$.lsitg nanoL@liniic corr€nts in ihe polvrer Mt.ix

which ab$rb nor thcm.l 4rgy dqiry $c phe chhg6 6cMir8 *ilhin the @oclav

sith ircBing ahosphqic l€np@lu!! [l 00,106 I.

15

TsrFtu eq

FisuE 7l: Efrer of FNK @n@!!rid @ $c l[@d d'sndstion of NBR sleimo

tncd wirhin lh. lcdPdaturc linit 25 to ?odc

2A

II

4iDI;

f

Tdp...luBeq

Figw ?2: E[.ct of FNK @c. Etiotr on $e har aberbing cqabilnv ofNBR speimen

Rsted wirhin (he tenP'EL@ linit 2t b 700'C

5.10.4. DSC snldy

DitrercDlial emirg calorinctic aralyss of the polt@ looeonposiles in lhe

tcmpcmte ase -7445dC @ dhplaycd h Fiew 73 io qploE lhe eflel of de

Mofill.r or the pha lr.6itio! r.mpdalNs ad ih. Mialed speifc @ihrlpi$. Glds

rEsirion, crysrrllizirion, nEl rchin& ald s@nd rclling plD* lempcntuEs weE

n6Nd Aom the DSC @n1om tlut @ labul.l€d in Table 15. TIE aducdon of slasrransilion rdp.ratu. up to -2roc is obFded in rhe prcsent€d data due to th€ l0 wr%

@ok&linile inpEgnation in lhc rubbo maldx, nr crystallizarion tempeBtuG of rhe

rubbq ne@onposiles is dininish.d wilh incrdinS nuer cont€nls in lhe lolymc. matrix

ed th€ mininw is obwed for NK4, i.c., 79.?'C I l60.l6l ].

Fis@ 7l: Ef41 of FNK concentrarion oi the difeMial st)ming calorimerft comous

of NBR so*iDes lesicd wilhin 0F cmD@lue liDit -?4 ro 450'C

Iis drcp ii ( h!pF6 dk b th. dd'!e in of $e coslin|<ins dmity ol ihc bde

polynd naui,!.'fte @clay ituotDo.adon 'n

lhc hosl @lrix qtends lhc rubbcry ds.ad rcdE6 the dy$allidion pobr. The phe traGiiion t npeElws oflhe fict and

wond m€ltins poi s of 0E onposirc sF.incN 1|@ inpDrcd wirh ii@4ing FNK

.on dEalion in rhe rub&r drrix. h is snribured b rhe hici h€r quenching.apabiliry,

even disp€nio4 good the@l st bility, ed @o-sale inrehclion of the FNK wirh $e

tEaE

I

TABLE l5: Effer of FNK lolding @n@nrados o. $edd onsevp€ak neliing Phases t np@luesco!{od ofNBR composiG sFcines

gl6s rtusilion, cry$alliztio..$at {erc ndured liod DSC

(r.'c)

Efi@l of FNK loodiiS oGntratioN on thc sleific 6$alpies data ar Pha*-

i*.i'ti"" r.*..t'i fr" r., r.r, & Tnt thar werc moGurcd rlom Dsc of

@nbu ofNBR sler.dIABLE 16:

ID (J/c) (r/o iJ/r)NKI

IIK'

Th. Pl6ented dal! in Table 16 also elucidat* that fie sp@ific e halPies of glss

tnEition ed cry$ltia[on te6Fatrr6 s* dininished *hile li6ts@nd mcltne

phlst tempeiatwt sP€ciiic € halpies *E inplovcd with i'cFasids rNK in the NBR

duEix. ll slbstd l!.l $e incoqoraled fUq renstt'blv inlllenced th' phe tNnon

tmperatues md their 6s@iat€d spsilic othalpies

5,lO 5. M€chsical chaE ledsl'cs

The su€ssulin @ntou6 of the pol'@r nsoconposites @ displaved in Figw

?4, which shos a reMkablc aolurion in toughfts of fte onDositc sPdimetu *ilh

irc@ing iilld incorpotadon inlo lle Nbbq rut'ix FiSue ?5 shoss the efect of lh€

inpEgnatd ll@kelidte on fic G.silc sE ngln tnd €lonsation prcpcni6 of rh' ba$

polynd nailix Tensile slrength of the rubbet Moconposits is austnented up to 143%

dd.lodgalion al bctk is elev.t':d up to 63% ei6 rbe ndimu itcorpo6tion of the

Fn@lly io$ tbe bsse comPosiie romulaiion (NKl) I w bappened o{ing to the

uifon dbp€sion, hirh surf&e @4 .N]d'l sLong inteactio' with lbe polvnflc

105

hol(uld chaiG, low hardes (2-2.5 Mohs s2le), ad fie fllemallix compalibihy of

$n(E

Figue 74: Efi*i of FNK loadirgs od i!. $r6s_strain codos NBR 'onpos't

spec'dens

FiSue 75: Ef@i of FNK loadings o! rhc Ensile srrength dd elongation ar bMl ofth€

NBR codposite sPccinos

Th. Dodul6 of.lslicitv at l0O od 200% clongltlos s* Ddlred lom the

strBs-slrain contous ofthe fabricaled comPosile sFcinens ed are dcpicied in FiSut 76

h is ob*Ned thal the inrod@lio! of th. @ctay into th€ polvner nalrix eiliciedrv

.nhees thc lO0 ed 200% Young\ mo<luls ofNK4 rubbd @nposite !p to 8l dd

9CF/0, respectilely telodve to the base conposik fornulalion (NKl)' FNK incoQodion

ino NBR ha Gdarkblv cnh@ced ultimt€ teNile slr€dgd dd 'longalio'

at bleat

F3td

J3

connmi.g thc @bpdratively b.trer r€inforcing efl:cl 4 compE€d to Ndoqlbon od

Fisure 76: Elfecl or FNK loadihSs on 1he elastic modulus st l0o md 200% elonsation of

NBR @nPo$te sF.rneN

Figuc ?? iustlda rh. efT6t of th! fill4 co@Dhtio' on lhe shoE A rubber

hddnes of lhe polynr rdo@mposites md il is obseryed lhat Oe ndokelinite

iocoao€tion reMlobly enhdccd $e rubb€r hddncs ol the conposne specinels due to

th. eduction of flowabilitv of thc host D tix *irh th€ nan@lav'PolvDdic nolccnle

chain linkg. development

i

I

ic

t

e6!

Figw ?7: Etfet of FNK loadings on fie .lstoneric hardncs of NBR conpcrc

Chaptcr 6

Conclusion and Future Prospective

6.1. Conclwiotr

T@ty eight div.e elaJtonqic sysc6 h,t bco used oith fucdomliad

@qrcinfocm@ls (MWCNTS ed n notaolidre) &d bat'ies Gtvkne poprlene

mononer Nbbo, $trene buhdien rubbet, silicon rubber, niilile butadiene rubbeo to

iabncat polyno nmocomposilet for tlrmal isdadon svslec nte ndo-ircorpodions

srE popcdy nDdiondizcd to e.hde thcir disleisbilirv ed @mplibilirv *nn the

hosl eldomeric narrix. Fumio@li4d .eok@linik wnh dvenee panicl' sia less tlrd

lom ws syndresircd uins s €sy, fasr' dd econonicauv viabl€ prcces lhe

sy h€siad fbcdoDliad ndokelitr 4d MVCNTS w@ pur Inlo rest 'or

firctionalianion cryslallogdphic dalysis md micosPic analvsis lsins Fn& XRD

SEM, and AFM t€chniques

IF mofilleG we inpr.gEtcd in the .l6tom€nc maltic€s Bing inlemal

dislesion kn@der fld lrc_rcld mixing mill Ior a sp€.inc d@tion. t'6pe6tuF dd

pllinS velocily conditio.s, Et61on€tic compeit€ sp@idetr wft cutsd on lhe hot

ie$ad. FEss 6t a speilic lenFrate dd pt€sG The fabric*€d conPos'le spec'bens

q€F pul inro ren for rlFmal @nductivilv/imped,Ee sc@ine elsft! nicosopic

dalysis, diffcE ial $a.ning calodieilic amlvsis th'nnal desdPosilion analvsis

diferedial thernal dlysis; Shorc A hardness md tehsile tsts io €lucidale he effect ol'

mciocorPoialioB on dF themal dd m.chdical checreonics oi rhe €lstomerk

Tho qulily of a $emal insulation h best een i' tclns of the thermal conduclililv

md te temal inp€ddc€ uddet vdid $eadv $de tenpemte anenuliohs The

sysromtic $udy helps b deat lh. polddal oflbe fmcliontlizd ndo-cinlb@m€ns to

adjust $c themal tespon, lhmal it nsitio'. theldal degEtlatior sd n*h&ical

chdde srics of difrecnt Polvft! sysleEs The following pmgiaphs conclude thc

.dofiU€h iI l@ne on lhe fimqm.chdical poFnid of cdh fabricatcd

@aonPosile ehemc

r03

> FWCM| inwes'atetl silico? tubbet (3R) stste^

The 0,?5 s,t% @nc. tadon in th. SR nairix has .nn@ed th. themal impcddce

up ro 28% s.hile the thdml @ndwlvity hG ben Gdu.€d tp ro E0p/o fl 50dci the

th.nEl $ability h6 augrncntcd up 10 310/0 ai 8000C; Slss tasiion aod crtdalliaiior

tempedfts diminish at 13 6ttd 9oC. csp€clivelv whil€ mellng €npdalue in€eaes uP

to 6!C Eldir. lo th. SR mlrix duine d. Phe lrsnsiti@ studt of th. m@nposne

Thc !-MwCNTs !.rsork wi$in lhe polymE mEix hs efe.livelv niluc€d lhe sttd@

dmge duling the themal tmsporl study IlF pe! F MwcNTS in@rPoration inlo |he

SR marix hs rcmad{ibly implovcd lh. m@hdicll ch.hct rislics of lh€ fabdcoted

> F-MtvCNfs inPresnoted edyten Yoprlene dietu nononel (EPDtt, 'tastonetic

'DF proSrcsive incoryonlion of molubes inlo $' polvner hatrix hd renalkablv

.nhoced dE th€@al otd declEicd p€rfomdce of the mocomPosiles Themal

uNpon $udy ev€ls thal dE iMrpordion of MVCI'IT' inlo rhe EPDM Mltix hG

cftccliely enheced the $e.nalresisirnce oftbe fabricst€d @nposiie speciids up to

95%. Ihmd st biliry ud endotbemh capsbilitv of the fabricaled cobPosit's e

impovqi Endkably tith E @otubd int,ldErion into rne rubbd mlFix DSC $udv

illusilates $e F-MWCNTS incorpootiotr inlo $e bas' coDpositc fomlldlion hs

succcsfinty incr€sed the m.ltidg t\dp.tatN sd tdu€d the gl6s trasitio' €npedlure

of the dev.loFd onposilcs Ulinale LBite $tngrh lnd ShoE A rubb'r hddt's ad

elonealion at bqk of the dbba moconFosites hale bcn inPrcved with i'd'siog

fiuer to natix hlio du. to ihe 4en disp€Bion, du6bl' fill€r lo rnailix bonding' ud

cGllmt nehencal stogtlt of F_MWC'UTS

> F-W,4CNT| in'F.?kate.t acrylonfuile butadiene fubbq (NBR) etutonin

F-MWCNTS re .vcnlv dis!€tsd ih fie NBR Mtrix lo fsbd@re dbber

.mo@6posites foi themal dslyes SEM iroges and the compositioMl dnalves oflhe

tmil. taclut€tl cobposiL mples €lsid.te th. d6 dr+eBion of lhe incoryorated

@oubes inlo 0r hosr PolyF 6anix Therml @nducriYitv of lhe polvmer

.anocomDotites is rc.luc€d by 5ry" ehlc themal iinpedec' 'lheed bv 9?% *ilb

inctesing th€ Motubes onenltadon in the Polvnd madx h mees lhat $e iNulllion

chsad.risris of the Nbbd @hposiies s. imFo*d' Iltdal $abilitv dd €ndorhem'c

capability of the tcsted sp€cinens have beo remdkably improled wi$ increasing

t@tioralizsl CNTS in 1h. hosl matnx DSC sodv thows thal glss ttdnion dd

crystalliaton tmpcalurcs are diminishcd uP to 7 'nd

6'C' rcsp'cliv€lv whe@ of,ser

dd p€at neldng phase lemp€ntu€s e .lcv.ted up lo 22 ed 2t' coftsPordinglv wilh

ircEing the F-M\VCNTS imtrEtrdion in tlle rubbd ndtir dd a simild b€havior is

obkned for spa'Uc enJEtpi.s of ph6e bdnions (cM'd wi xn $e 'omposne

specimens. The P.tI n@lubca lddidon in the nbb'r D'trix hs inprcv'd fie rensil€

srEngdr elsdc modulus dd hsdms ofthe f$riqtcd moconposil€s up lo 21 2? dd

> F-MWCNTS impregnated sqtetu b adiete tubbet (sBx) etastonqn s,stens

f.MvcNTs sft dispc6.d in rh€ SBR ndlix poFlv SEM dicogla9hs h've

elucidatd ihe 4e. dislibution offfnotuh.s in the rubbd natax A rcdarkable edudron

(up lo ?9%) al 523K is ob€€rcd in lhe themal @nducliliiv of th€ polvms

m@nPosiles {ilh irc@in8 litler @G!F?tti@ in dE hdt trlvnq natix Th'ml

inp.ddcc of the composit€ specimeE h6 been augne ed up to 3911p/" 61 523K resulted

owing lo lwto, F-MWCNTS ircotPo6rion i! rhe rubbd lEtrix Themtl stlbilitv dd heat

absofti.8 capabiliiy ofthe nan@onPosil.s have b€en €lelated with incrcdirg liller lo

naldx drio, Tc dd 1. oflh. Polvnr conposiEs nlvc bM d4t€ded On $e other hand

wbite T.' 4d Tn inctsscd wilh in Easing Motube @ne rarion in th€ polvmf

nalrix. The lvt% addidon ofF MWCNTS in the SBR Mtix has elf€clivelv incEsed lbe

spe(ilic cn$alpy of ndnng of $e daMmFse bt 4q' @dpded o thc bls comPosne

fomuldion suf.cc moqhologv dalvsis ofthe poet rhgmd uzlspon iesl€d sp4rmcns

eveals $a1 rubbd mdonposit6 with Mddm loadins of f_MwCNTs a less spoil

> F-turokaollnite inlegnated EPDM elastonqic t],lte s

LayeEd sihc.k min.dl. @okelioe *6 inpegEud in the FPDM rubber

marrix b flbtide rubb€r M@mpo6i1ca ro €valulg $en lhemophvs'dl ch@clens|'cs

'nFml o.duclivity m Edlced up io 40 % utite lh€nal imped,ne of thc co.nposilc

sp@imem M inprcled up to 64% at 493K witb itrftsine @oclay cont€n$ in the

Dolyner narrix. A renEkabl€ erlurc.nent in th€ thenal stabililv ed heal qucnching

capabilily w6 notied for the FNKTEPDM with lhe posBsiv. additio. of ndokaolii in

$e hosi narrix. Dsc 6ults slDw fin the hiShd incorpoBlion of the n&@lay into lhe

rubb€r matdx n6 dininished T! ald Tr doM 10 !2'C, rcsFcnvelv Al$ Tnt ond TtupSdd.d to l/c ,nd 1dc, dT€rircly, Elotirc to rhe baF onpGire fomulation (E20)

ullin.le LNile susgl! elongBriotr sr brcd( atrd obttr h&de$ N6 imprctd to 92 100

md l?vc, Estetively with lnc !0s1'/o t&o.lay inFnion in the polvner satiN The

ex!.rim.nlal resulrs eveal thal lhe uifotnly di$etscd @k@linite @ aller lhc t'emo'

nehdical prcpenies of the rubbd matricd due 10 ns excellenl $emd 3tabilitv.

fmctionaliarion etiviry od n€ch&ical streng$

> F-mnkaolinite ihlegnate.l NBR elastonqic slste^

The pre$d nv€$iSarion Epoils th. ctfcct of vdidt @nc{l$tiotu of modilied

Mclay on l[€ Frfomdce of lhe NBR m@mposites The'ml conduc vnv md

thcmd imped.ne of rhe Flyn r nlll@mpocira wrc evsluled uing th. dome$icallv

desi$cd &d !@ugatued aPp@tus accotditrs to fi€ ASTM 8lid€lines. lt wa obsrycd

$at $e thmal @nducliritv qs rduc.d bv 560l" d 2500C; therul impeda'e ws

clevaied by 120% d 250"Ci th€mal deEldation m tedrces bv lop/o at 650"C; Glass

ransition and cryshlliz.tion lenpdalurcs wet dininished bv 6 ud 5'C respecivelv

whil. the fist md sond neltirg phre t€tnpe6tres lr@ auem€nkd bv 42 and EC,

r.sp€criv.ly; l€Nile st€neth, .lonSation al b@l! 100%. &d 200% modulus qeE

incltsd by l4l, 63, 8l,.nd 9l%, rarP.cliv€ly; ed l!€ sh@ A hudncs of lh. Polyner

nMomDorites w€E dgm.nled !p to 227c wnn th. l0 wg. iMrpoEdon of rh. n&@lav

in tc bs polyner @nposile fomubtioi (NKl )

> F-wnokaolinite inprcg\oted SBR elNtonetic ststem

Plo@sed mokelinite. a lavered silic e nin€dl is flenlv disp.sed in $e

sl\rcne buudiene rubber mauix Th.msl condlcr\irv of $e rubber mnsomPosires b

Fduced by 4l%; lhmral imp€dmc€ h ircrcsed bv lo 4l%; lhelml slabilitv h ptonoted

ut (o 5%; gl6s trNilio! ard drsLlli4lioo L6pdttu6 re diminish€d up lo l0'C and

It1

l"C, especiively; fiBl .!d se.ond melting phae t€mpedtws e i.oeased up to l 5"C

aid 19./C, @mpondilgly; ulid.t lcNilc sftn$lr rubbd hddnc$, elongaton ar

brcal, dd nodulus of elasticily al loel ebngation @ auSrhenled up !o 2l7MPa, 10

Shorc A. 2470, drd L3Mla, tliD€ctirely wilh l0 fi'lc @lay inPGendlion in $e bae

comDosik fomulstion. Hd1 .bsrbing caFbilitv ed toughle$ of rhe polvner

ndconlosites * te@tably €tlrncad willl the progrsive incorpodtion of the

@ofiud in the hosi SBR dltrix SEM tuDlvsit of th€ Pon th'ml rtdpod tcsld

spsim€ns rcveals tbe micro voidt size and qwlilv reducdon Mth incredilc nllq lo

mlrir 6lio due lo |h€ exellor lLdnul nabihv dd slreng eirforcenst-polvner

interetion developed owing 10 lhe surfacc Dodificalon ofthe inpEgdted mclsv

Tablc I ffiad6 th. @nplct rt*arch *o*- nE msimm lo'ding ef*l or

ihe .do-Finfor@ments on th€ theml and n*h&ical p€rfommce of $e fabdcated

polym.r M@npcl16 is dmoDsral€d in this dnPahtive an'lysis Tlt' Ptes €d rabF

helFs lhe dcaiper to Flect $e appoptiat mooonpositc fomllaton suilable io! a

3p€cifi( applsLion .c@ding @ the desircd *t of Em't dd h'chucal chmcreistic'

Among $e F-MWCNTS 'nolpodlcd

ela$odetic Mcomposir€s lhe mdinm

rbemal stabilny al 600"C, l€st gLs udsilion (T.) /clvsiauizarion (Tc) lenpdaturc md

suprcBe Sh@ A hadncs.fr€cr N mtcld fo! fic I $rvo F-MWCNTS inpeenaled SR

composite, The minimm hemal condwlivitv, naxinm lhcmal inPeda'@' ullrnat€

kcite $r.nsth and speific 4lhatpi6 of T./td 4 oh*ryed for the molubes

ircorpootd NBR nmo@nposie: rhe urno$ netrin8 r'mpedues Oir &d Td' sp'cinc

enlhalpy ofTd dd .longation al bEak aE edtinized tor I $f/o F_MWCNTS Einforced

EPDM M@dposit.; ard thc lEinm 3peific 'n$alpv

of crvstallidion tenpealw

is oose^ed lo' lud"0 F_M\i C\ ls doped SBR MoconPo'n'

Amongsl llt *ds of ll@l@liniL inpEgFted polvner ndeompostt" me

Mi6d themal inped@€. lowest ihcmal @nduclivitv' highesl temd stabihy al

600"c. higtEsl sp€citic drhalpiB ofT" sd Ttrl?. I€6t c.y$alliatio. (Tr) t€npentuE

hishst shoF A hardn6s effd tnd thc hiehd ullimate cdik stren$n e nolrced $e

mininM Tr ed nqimm sP.ciic enth'lPv Tnr de obwcd for the l*r% doped sBR

tu@mDosilei dd lhe peat nehbg t BpdanB (T'r lid Td)' sleific endElpv of T!

dd cloosdioo * brt.L s! t!d.d fir I etx F-MlrrcNTt bc"?oftLd EPDM

h vi.w of oml F dre, f'X[rcNTt rd trditil ioFlsled NBR

ed EPDM .LltoD6tc n4@Dotit . .t! d@ooitd'd to b' h'tt'( @Dporcd lo

!o@po.uy b.@ldc. rltrttrr tlrn l cdddYtryfA'da"' lLdrl tdlioo

rrdFrd!!+ lLd.l a.HliF, adtuic c!0.!llbv' ed !'d&i0'l atDoc!'

TABLE I : Ot.dll D€rfdlMc of F-MWCNTS ad Mo*.olin't inorDor.r.d .ldonm< n.lrMnporic wirh mu imum lodins le!.|

'Th.mal Dqndaftn (Ms ris %)

qck6s TB6ilion Tdp€dE

lcrystltlizrion Tenp.aru@

rond naths rcmpaature

rPdk M.lli.g T.mpe0nN

ruhinar Tensile Srangrh

6.2. RecoDnend€d Protpecaivc Rse.rch Work

li lu1w, we shsll 1ry lo pog€s lhis 6eeh ptuFc1 on lhe basis of the following steps to

cinmce th. themal. iderf.cisl, md m.chanical Popenies oI the polvtrt

> Firc d:rddi ch.racrerislics ofth. hbriercd elsbnenc 'e@npodtes

will be

.ddt$ed in tun!€ uinS @D. caloinet r, UL-94 16! elc lo enldg' th€ dea or

aPpli@tio.s of thc polvm{ @@npotles

> The n€chdi..l pop€rties of el.nom.ric compciGs at a sensiive fu'cdon of $e

sllai! 6tc that my i.flucne tbe coDpliece of L\e polvEer ne4onposit's in

p@del us. ft is thcFforc Mm€nded that favoroblc eldlom€nc

n&omnPosit€s mv be subjeted to d)4mic d'chdical demal darv$s ro

ob*ne thc efi@l of lhe l@ble tmFatlrc sd op€fling freqEncies on dE

shee nodulls, stoBge nodulus, lo$ nodulus' c@p Fsisttnce' rensile stensrh'

.lonealjo. at bE*, sd elatic nodlls

> Inle acial shidv ofL'te Einforcesent-polymermsirix bohding to inplole tr filler

|o @trn id€@lon fo. b.nd dsp'6iol! rh'm'l snd mdhoical aP'crs

> The @ge of $mo_set lDtrices €nPloved b fabricate ihe polvmenc

nd@nP6ites @Eposilcs Mv bc exrdcd ro includ€ ladder silicore polvmert

HNBR, ePon6. elc lor a t&ielv ol neoliller @dbiMtions

> Fabdsriot th@t l, fld nechsical invcstieation of Polvnet nsomnposres

$ing vsiou n|noclavs. @o_hvdrcFds' @o-oxides' etc with vdianr dopine

@renirdioG in $e host Mtnx

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Il53l R. Al-Sary. R AtMahaidi, c. p. SinonJ. Habsudr. cntur Buitd Matq 28 (Je.20t2) 169-118.

t1541 M. salehi.lil. R,zgli-KshdiJ Appl Polyn Sci 126Q0t2)253-259.

ll55l L. W. Mu, Y. J. Shi, X. F€ry,I. H. ZhqX. H. Lu, TtiboL Int. 53(Apr'2012)4t

1156l H. Yq L. L. Li, T. Ki.lo, G N. X, G. C. XlrF. G!4 , ApPl PolyE S.' 12{ (ocr.

20|L)669-671.

ll57l Z. CibulkoE, A. Ccnq ?- Sinon, r. t]ltu, K Ko!ar,P. L.h@ky, J Th.m Anal

Cdoiin. 105 (201l) 607{13.

0581 w. Xie. z Gro, w. P. Pln, D. Hbt r, A. Si!s!.R. V.ia ChenisLy of Mai.dds

t3 (200D 2979-290.

[]591 M. A. R!2, A. V. K. W€stv@4 C. Sftling.N. Hondoq Conpos. Pt. A-Appl. Sci.

Meut 42(2011) l135-1343.

tl60l Y. GuA L. X. Ztrds, L. Q. Z!og,Y. L. L't Polyh Dcsnd Slabil 96 (201 D 808-

817_

{l6U M. A. M&sill4 L. Sih, w SdSEno, A. L M,@!ca"{. somoza, J Appl Polyn

Sci 125 (2012)99'999.

$[1 oeienruon: e rzs-o

l.l Inir rd ftrhod.L$dbes r daly 6oc @loh@ tr

)ms.Kusop'4e slids (c NG I 'nd

2). Tfis t iarhod ir ror mrdirL: *irh etr div. .@dudivniq itr rh.)proxi are nng. 0.2 < [ < 2m wz'K ovs $c eprorinac

'nplhrE tuge b.rwen m

'nd ll0o K. lr es b€ used

!6id. rhe mg$ *irh d.cEr.d ulruy.NoEl-ful'|rEldfudi4e.ly4mRe@'

bymEtb154'fu,@ib5qt.arcsft$rynm@ni4

)@lrlbykfu:J4

iiidl'!ryfl d*nlrrLerytudd nf'drb+M.Fn.d,4Fi.d!fu

t.l mir auturn dNr nd purqn b a.ddns oI 4 L\2ol.a wt*, tt tt, Bsid.a wnh iE e. h it ttt$pffiiuti, oJ

'h. B.t qtu 3@M

vilk !4?t! drd r.atk retia .a!t d2khnn h. qtia.'ili, d 4utata1Inlbtt^ ptiot b rv

C r77 Td Mdhod ror Sbdyr@ Xd Flor M6@En6 d Tl'mr Tmsmision ProFnia by Ms ofU. Curdd-HolPld. Appdd'?

uqiY yotwhn wc

C lo45 Prctic. for Crlcullting

standsrd Teat Melhod lorThermal Conductivlty of Solld3 by Mean3 ol lhe-Gu.ded'Comparallve-Longlludinal Heat Florv Technlqua'

Protaries Und.r Scldy'SbE cmdiriom:D 4351 T6r M.thod fe M.Nnlg fic Thml c.DdE

dviryofPrsriebtuEEvlpo6dm4 siMicM.$ctE 220 Td Mdlod I' crlibErid of Tn.'l1Ntrpld by

E 230 T.mpeatw.Elebmorive AJBo (EMF) labl.s ror

Sbdardizd T[.rnocoupL*'f431 Pncrca ld Erdu.nng Tocmrl Condldivny or

3,1 D6.rip'iffi a, r.m ard srnd' sptitc to rhij

3 | l.l tumt c.rtudivity, ),4j,e tiuidq@dyddirioDr,'mushunire,p.runntmp.nrudsrdi.d iD {E dierid p.iFndicuLr ro rh. @:

3.1.r.1 rrqErt thtnot conlrctwt-or h.d h6tu .hu$ ! mei,l @ F.&d ii lddirioi ro.ondEtion, m. dula of $r ftsdn.is p.lfomqr e.od.itr& ro rhis br mdod wjll EpreFd rh

rhdm3r cood*riviry td rhe nardid brcd.

= d.mlcondEtuiry oI ftrd brr (cf*nc.md.rills) a a fuodioD or r.m!.dm, (w

= rh.mll conddtiviry of lpaih.n 61cu1a.cdby isno ns hea exchrng. .ms'ior, (w

\lI) = d*mrl @'i@dvny ot iitubrion 6 i fuictid ot r6!.tfu, (wrn Xt

rhcmal condudlviry ol rop nebr bar (v/

rh.ml @dudivi.t of bonom mas blr

rhrtul cuddjYirr oI sp.c,ftn ofu.dtd h.ar .rddg. wift iesry, (rv/

lfilr E 1225

psirioi u\ msurcd fmm $e uplq eid of

hd now pd uii( d@,|M" 1,

I

suird cyrildtr inr6 FdiB, (n),3Md bm!.ftluc $ r tnncrioi ot p.dirioi,

sunnrry ol T6t M€rhod

4.1 A E$ qEdnH L ins.n d uder tod b.r*ei $oDila sp.cin.tr of r md.d.l 0f ltuwn rhm{l proFni6. Amp.hn'E Brulkir n $ublishrd in d. re! rhk aid h.dis.s lrc mii'h'z.d by u$ or ! lonsirudinot gurd huviosIrux'mE'y'h.s@thFdrgfujj,dnnn\. ,hr rh.rut cmdudiyny is d.rrx! fom rh. Mn.d tempemruE smdi.ns in rhd Espectiv. rplcimdi snd

'e|hchld.o dElivilyollheaf.d.end.ndl

12 Cd(nt fdrE olT.n Mdh.d:4.2 I ',fte g.n.nl fetues or rh. s!'d.d tongirudiilt h.d

t. A sp..itun or ultftownEnMi d,'dEtvi9. rj b!. h.viis m dritur.d rhmD,tri'ludmeof^j4'k'nNnlcdb.|@Dtyom*bnsofnown rhcmd sndudiviry. I", of d.mikr 'nm .dducur.rj I!,?!. a mE 6det4 br

iri4 oa' disk h.&h sid. b.r*.d h.ds

nd hur Nir. AppronmAcly oic.hlll of rhe powlr voutd rhcnu, hmrgh 4h irc.imd w&i fi. m.i b.n ad sp.crr.n n neh'{irurr .ylind.6 ol qu,l diJftc ft. kh'qud

r d4cnh.d 's

$c c*br nerhod vhd rh. cs!4lonrl dimq'ior. N lfed rhs $e rij.tn6s ir i'4ab<i r rrE ir slrb .ompcnnv. ndhdt. EsDr.Iy myhrF {!n b. und a lory d rh,. mF bG aid sri@r hir4.?.2 A r@c n rrpti.i b d. otum b truE 3odorrer dlEn $aiftis. TlE lbt n slsid.n 6v b

nuhrionni.nrlol r.mrl 6iddivirn \ | The rn:ullrtons crdod r r gu"d shelt wirh ! ndiu4 r,, h.td 4 d.emectuE, t, rr a cnp.dm s'dnd n 6p6.d on

'trlru'ni by mdnrmitrg rh. rop d r bnpc6rw, r r dd rh.{ron d reopcilruE I} 7;/J is uNurly a liftii Fmp.ruruGladfm mroh'n3 8laarituEly rh. sDdtN sbtjshal inh. ki sbk fi@rE, rn i&rh.tut sua'd widr ri 1z) .q!:t

imen mry {te b. ued.\i un8!rd.d rtnem n noL dodncnd.d duo ro dE pociri.ja-y laB. hsr lM, pJnicutsty .r .te€rqr htsducl).' Ar \c!dy n&. ft. rmF{ur gidi.nb rrou rh.

i@rioN ic ulcul!@d lrun medtr.d EmFrula ltons bc

rmftdcd rd h.'r shtrditrs) crtr rh.n b. ddmn; u;iDh. lnllosiis.qunjoi *h.ft rh. iorlrion is rhown in Fis l:

.le

tlh E

, (2. zrrr"L'r, n [r), r"-"r]^ tlr,-t'LE-4-l'f E-A) "'

'Ihis is a hishly ideiiz.n snuaioi, howlv.t in* irrm6 no hed.xchaiec b.r*6 $e c

rspaimei inredE. Tn. emn ctumpriois vary qidcly sd N dh0u$.d ii S!4on 10.

Due of rhcs rrc.fls, E.ri.tions mud b. pled oi thi3

i ne$od ir lne d.siEd scutuy i: b bs r.hnvd

1225

imtrorcd p@du6. tlecv.( Fw or irFlved rehoiqEsmur b. rhou3hly r.:cd $d t quic@nb Id qlllityitrg airppMui e ourlincd in Serior 10.

6.1 Md.t Bat R.t are Mak |L6.1 I R.tcEn@ na.nrfu or ttugls \oid!'d! *ir]' kmsD

rh.mll .ond$ririri.s mue b. usdl ror rhe meEr baa. Sii.crh. miiinum N$ucm.nt.ror ol lhc n.rhod is dE rrer0iiry ir I f ir b p€f.lrbL ro u* n.ndioml $^dddr ldomrory Orher Elercne m.Enlrs 3aovdl0bb he.dus ium.rcN nsduEnrns of rL h!v. benm.& dd 3o@nl ecpbe oa h. vtlTlbl. I lkb ri. cwnrly !v!il.bl. @giized cfereremddds iicludiig $e oYlilrbL rDmSondlrdi sd Tchiologt Fis 2 shows $? tppnxmdevdirtion of r, wirh EmFnec.

6.1.2 TibL l b nor .*hrs.i!c and ousd 6 atdc6. Tn nf.c@ nddi'l dd rht $w ot I-vdB ihdl b. Mr.d h rlr Epd.

6.1.3 TIE 'qlidd6 tor 0Y Ermdtbiliry oM &c rmp.dM tugl ot*nh o$4 ryltn .mpoEnl! 'Miblt 6l .a or rheF

il4dpL rEhmir, !d an c.1rulv kmwn rh.nnir !uddjviry. SiG h.! shuuitrg mB rdr !A,rri6 frch uiit, (l) thc 6Lffir b lr.hoh b. uGl for th. @r b!6

6.1 4 lf .mpL hat!r,bd*en rvd. Er.d€ *i6 rh. high.r ,!, shoiol unFdtrE drop rldt h ormi

o.2.1 A h4. vri.ry or povdd !6rcuhu 'rd fib.rdHtL .rd fc

'td*'ns bdh

'rdi'l h4r flor in rk

.dw SU.td onulu tnd rurunds sd &.r shn ing tus6. dlMi s.\.ril fc'B mu{ b. c

hi of rt Mr !pp'!p.r!E iMuhtrotrubl. oq

'h. 4riciPdcd EmPcdur

.d h.6y ro hodl. l.0ddirion rlr. iNuldiotr shuurd ior@tumiie sy$m @pon.no s@h a m. tmpcdruE snsr. I nu* h!r. lo* djcirv, tnd ir ihodd nor oidudoledciry h s.n.nl. Do*.LB md Pdrh.y gocr Erdily, H@.v4. lo* d.n:itv llbs blmkeb ch ars

6.2.2 S.tu.aidida& idulariols d! liltd ii T$le 2

6.! Tnp.tutrn Satott:6,3 1 Th.r. thdl bc a minimum ol rwo

on re[ Nrd bs oid rwo oi rhe 3pcdmr wh.Eterp.sibb, mt md{ baf lnd sP.cinde si$B. The .xta lcNoB ftlii.siry of rcmp.mruE Esus dishna dmg trE

'orumn d

iidi.otiry ai.tor du. @ o remperatu

6.3 2 Th. ryp. or i.hp.mrurc &ntor 'ri4, rnp.nrur &., lnd de sFk

mll.d by fi. 'nsl.ioi m.krb! s

t. rvsrm. enr *ou Fsse"ns d.qude scur*v mv Eu*d rar orp.dua mNEd. (2) dd bc rcd in lr+'

lo" 9cnurbaton bJ s. tmp'nrlEkM^ *ould b. r.srsibl. Tt m

:50ia0E

5trot:

200 ro @ ra !.o troIs e^tlJlftQ

F|d2ADd|nfub|uio?bhm|co.d6[ydb!;rPodbrr FrmB fr'r.! tu [d.i

5.1 The tompuatr( m.Lhod of mduEmd of rh.mrl

Eludiie cmics. polymds, meuh I!$ons, rnd aophiEs inddin8 ombindioN

'nd o$or 00m'

5.2 Ptuptr design ol ! sud.d-lonsirtrdiial svsh ir dini-urr and n k id pruli.ar in r m.ihod or dts rvp. b u] osdbljsh deuih or constudotr 4d pc.dun. ro oEr dllontrn-!.n s L[a' m,gh' off( d'6.ulu\hil rrcqr.dg. oRnrg dory orhar nor' cmp.n_ft m6mmi6.,trd gtmnlbrins pRdet sbtu'a_ii or rhi kr mrh.d i: nd iit nd.d ro

atn* 6 m$.& or

*)- ------r'-'--

(Jlr E r22s

ii rhc ncirl. when r slErdi.n $.tuupl. d r rhermo

@pl. *irh bdh rh.mLdib iimltu is De4 0* rl'lmdpl. d@lmdt s\o*n in Fit.

lhdld b. $mrlry @iercd ro l'.$ibbl. gle d nish bmp.n[c epc.du6 shovn ii Ft. I lhourd iE$. $ u6, "iE

lmp* in i$$.mrl ai?\, Oemal wi'tg'outrds on the gurd, q a combindlon or 3ll rhre (s)

6.1.6 sinc. metuinty in @mpeuurc fis Lodion kudlb lrs. emn, rp..ial .e nui h. bt n ro dtumiB rh.cdar ditu b.rrei eN$ lnd ro cdcul& the po6siblr

cmr @ldns ton ry !nm y.

6.4 R.d'.tit of cN@t R.'i'rM.:6,4.l nis rd Eudt r.qliG u fmkillsrdorrh.

tua b.r b spcitrtr inE K: wh.Es rh. Enp.dudris 4 virhin

' disl'@ qull b

'^ ftud 'i iitrtf.

(6).

Ini qnircGnt l@$iuB r unifm mtr6 rcsiatutsffi rh. djoining eG or ncB bN lnd sp.cinens. This is

nmilD lruiial by E ofun lpl)licd orial lod in .oijuidioirirh s.onduding d.dium !r rhe imo

v*uum k rcq 'd rd pddior Dlaops.6.4.2 For de Eldixly rhh rydftns nomrrl li€d ror

mGil|3 hviDs a ld fidnd oidudirny $. bm!€Ernrc$s mNr h€ lmied cla ro rh. slrre ,nd in cuns.qEc tn difmjry or M@ E5isrre i5 njricrl li str.h

c6, ! Ery rhin larrr of! ooplriblc [i3r'ly midod,€ [uid.p$lc Fn mdd foil. or i.nci shrll b. ii!.drd d rh.

6 4 3 Mrds shsll be povidd Id inmd .oisb lold sloDs rh. Nlunn lirh rhe PriEq pripo$or mi'imizins ituifehl aisbfte\ d merer bunp.ciloii& @. Siic rh. IoM .ppli.d ro $. @l!mn osally all(s

nploy.d. TrEi $rl .i4 dd rh. * oI.tklftit @

6.1.3 wn n lh.'lMdpks s .nploy.d rlry lhNld bc

dkic{od fom wid which e 0.1 m

oNuN r.mp.nture ftterenc. shlLl al*old jundions nris Ef.de .!i b. in ice{ld ddy (3), ,ombn( Emp.6oe 6i. bor, o n d(tmic ic poielcrcn* All $nNudc! .lull b. Ii.bd.ltn ns .nnadibntd rh.Ilflnupl. *iE (r) or rDm€nili.n by dr $pplh b b. *ithin th. limit ot .@p..ilicd ir Tsble I oI SEnitud E 2lO6.3.{ In.trl]lIdple dbttu h impotut b rhir @n-iqo. ddg b eNG ma cliabl. tnp.rdua l@@ciB !E mrd. ! speifc poii!, Tn vri6s cdriqB err'B'nrd itr Fis. 3. Itr'inrt jurtimicbk xi'l rlloys by weldins indjvidudurr&* (Fis 3r) Bu( of bed w.ld.d rheIlrffiupls jum-iois on b. risldly droh.d by tening, ..rcndns, d *eldin8n li'E sruves or smirl hol$ (Flg. 3b, 3q b'r 3d)6I5 I'i FiB. lb. rhe th.m@upl. bide ii a ndkl slo!

nd ii l--is. 3c rhe Itmuplc h plllal rhntren 3 adi, holc

llJl, E 1225

hfuje.deM{,1fu€hfutFhfdm&ied!

.Nc a Gn .d@ d'NEftnr pE irioi or 10.01 K ad0 inohe.tu |6s rhln :o5 *

6,6.2 INrru mdbrion for thh rehniq u. $tra be dql !!b hnrjnbin rhc rc{uiEd hp.durc corrrut rnd m6rE

'llp.nind orgur volbgg *irh audy omftNBb wir[ lrsytu.lp.!irir, Aidbugh mtrbr @n b. turd3 rehniqu.ufthis g.mdl d.$dprion .!i b. aubmrrd $ rhd | .onpuEr

rmc.joN. ..qulrcs a p.niicd,Dib8s. $d.ltcute dc fi.mr md!.dyny o).7, Sdllln3 $d cmditldhe T.d Sprb.E

7l Lrrlp?d'.rr Tnh B turhod i5 tror Blnq.{ k !pdrure 36m.ry. c.nel pmri.e n o !F.yllnlrhal or4urc ct!*srim. TIE condu.tion mEf.Er smphs mN b. rh. ffi b wirhii I 9a (w N* 3)ud my di&cn.. ir @ .bll be rzlculcllalins ot e ffi'rh Ff rh. cylindrlcr L conhsuorion, rh.ndii of rhc lp.cimen and nEtd bm mur asE ro virhitr: I 4 dd d* rpciftn ndius, r,, rui b. sn.h tur r ,/r,nb.rh. 2.0 od 3.5. Ei.h nd sure of rh. speitui .ndEflcm. mud b. nd wirh !

'u,{@ rinish.qnrt ro or bdbr

rtun 32- sd $. iomd ro d.h endshrllbc l)eollcl$irh rherpciM di3 ro wirhin r I0 nii.

srffi ft! :erq5 nbh e h4 .m3l.M|dngbsfu.rytrqf@b@l$uicnftFnllqd

r. otrkr Btue, n tr &siBbh nd n fre b. vdi,r{.,.nsr rlr Ir dcs !d change rh l@ vuiadoi. n siu .ri bd rppl'ed cid.r picunlri.olty, [y(lletic{l]n bypnng eror or by puring r d@d wighr on rhe column. Tlebovc rod roh,.t6 h.E ri. dvoe!? ot rDining

ci mlghr b. s row rhdE lppLicd foc Dun b. limibd b thc d.d w.ighr ot rh.pFr md( b!. ln rhis cu, lpejrl @ mur b. Erq b Dmirtu cad by qu .dd by j'ricio6 po6i.imine ot,nFEuE snlm,*0y rbm ay r'.!r fl@ psrldlim d

6.5.r 'nr {Ejnd.mb br otunvnhin a 8n:nr bb. or piF mnnilty oI nshl cimlI syift-ry. Tnk gued cyrj(hl co b. eirhn als insidc ndiur shourd b! su.h rhlr rl. dio ,,/r" 11 beEr*d 2.0 6d 3.5 (l). Tiir gDd cyliid.r stEll oibin dd om hak r( mhlling d'. &np.dft pont..lds

6.5 2 ',In. 8ua'n sha b. conrturd rnd opcmred so rhd rh.cnp.durc otrh. gtrfd$ re is eirh6 irodsdtsd.qu'l

nlcBnry hr!. u arltqituLty tiftr pmrilc *id tna bpfd horlim .ndr or $. 3ur.d mdch.tl b .mspoiditrs)o3

'ons rlois rhe colunn In .eh ci!., ar tdr b€

.mpcned stuon sh,ll b. @h.d ro rh. gurd d tnoMbiriotr b msua dc rnp.6rE prcril.66sJi$ldffin@id:6.6 I Th. cohbiDrioi of Empenr4 !.isr a.d rh. iNh-

ncft Nd ru nesunrs $. s.i5r ourpd rha be ld.qnsb b

lllD E

flp!!ln!'iiMLlkd uaur liadri.y d. b L* tud s7.2 saryl4 aai Clnlitixia-Unl* rpdr0.rlly e

v. .!ei@i shrll b..'lFd frcm r'e smpr. 8d m e@idirioidg i$ ro h.

Cdibrdio rnd vdioat o.3.1 l]iea e ndy siodids $n crll ln.quipm @:fm oFnriom on unkN*n n iats.an 6. e.csfuly$mplish&j. Thee includc rhe rollovj'rgR.1.1

^tu' iiirirl eqnirmci @ds@rion.

s rhm ol tr 3r&rrhmil .odEhE

3 r .r wh.n rhe 3p€jmli shsp. n .omptcx or rh. .p..ind

3.1.{ rvh.n.huc6 h.$ b..n md. ii rhc sysbm B-m-

3.r.5 whenhdstuoriNUl iotr m{r.ri'tofi?r rhrn L'lN

ha h6tr b r hjsh .tuushidFnrurc b cbge $. ptupsr6 of I .mpodd rEh a

32 nc* !{s shrll b. rui by .odp{ins d tqn rrcif.de mrdiil. in r lo owins DiEr:

rh. clEc ri&nn londariviry ro dr 6.itur.l rherol .ddEriviry or rhcnkiowi slmptr shoutd b. mehii.n ecording b 6.1, lid

1.2.2 The dcmd @ideirny I or rhc $€imn t$ric,r.dm r rcrcde mend dln dd b

'lxs,nd s d6cnb.d

I sdjon 0 siig ftEr blb frlric&d fFn rmlhd EfReh&nal which I'a rhe closr I ro rhlr of rhc sp..itutr. Forrunple. rechnlqur dsn hishi b€ mlll. by msudng onl.@ 9606 usins Drq bffi fabdcn d fDo sRM 7rtbitrlcs sbl. ll d. ma!rtd rh.mt Mdtrdjvny of ll:r*mfl LlilrrE.s *i6 fi. lJr rmm Tibl. |

'na zpptlirs

E(or!!onr fo,l'.d *ch!ns.. dirionr .froi h Equ'Ed

9.r wh*. posibk od rturicd, $l.d rhe E ercfr. spoi-rrds (meEr brt $c[ rhd rh. rrmd 6)drbe i{ ot rheam order or mgniod. s rhd dp€rqr rd ft. br ,!eind.\fi.r inrrutu iry .nd idrllins rtE FlF i@ brs. d.p..inm shoutd b. insrurcmcd sioibny x snorkt itEn b.is.ned no tc c$ s@l such rhd ir is 0r olignrd b.r"cn rh.

h rp..in.n su,re inonk' Nrh rh. 3djcd ftk be

'nd $ft roit or dnd

Dnedne @djum, if rny, usd ro rdoc n $. syd.n mD$ b! lt!@.cd IDn ondlior dldngh. ci or it op.'lrion quie ! pdico .oihl r,, rh. syn.n snoukl b. pump.d ud p'nred, lid uE,p.dtr.e 3a :dd F*ur 6bblish.d. Ttt p|rd.Emi'.d

:iil Esisbn.c sholld be apDlidro rh.lord.olumn,92 Heden d enh.r cid ol $e olum rhtuld be eEtiz.d

1224

(s Ne a) a'd adjrtl undr fi. tnp.rar@ dilLrcMb.rKn poirtoN z, dd 4. zr dn 2,. nr 25 el la ttb.rwen 2m dfts th. inpa0nio of rh. At ft6tr.fti6dd mK. and rhe s9.rinci n d rlre rvdagc cmDcruuEddicd td rh. n*strnr. Ald@gh rh..xd cmp*!!c9oiiL,]o4 6c ssrd n d inpotur rs r,/.i > r. rlE po*do rt. glld h66 tu"ld b. rdjd{.d 0isr rh. cmp.nrucpmfrle

'rotrg 'r'c gnd, ri tr, n ms

ro wlrhin 10,1 K ed eirlEr9.2.1 Alslrinsdy lin4 o rbd 7, l:/ oii.id6 wirh rh.

hFtu lrou dE spl. cdumplG i*l'jdii! rh. bmprdur. ! rhc rop s.isr dr rh. rop

92 ? C@br wi$ 6Fcr ro : b qirhil :J K 'dr ih .$ lp..im.t

hndb'sdftdjs,bhft@e

Fmd e iori n.. '!o

hlrn r ad

93 An . UE sysbm ta Esh.d s@dt iic (rdrin <o35&h), rduE rh. ourpd ot 0ll bnp.arurc knss

t0.r AppnnM. speci*n rh.mt Cnducti y.10.1.1 Tn. odps aiom $. bnp.tuurc sei$u shill be

@vd ro kdperutoE ad ue appq 4. h rh. r@ b.6 sh.ll b. slobd usins rie

4.-xN _6_i

q,- \ 4-.li @cn ot $.e €qudons, De Ix vrlu. (G Nor t ro b.

iEded dElr b. obh!'f,d f6n ft. iDl(xmdoi or 6 I for ft.N6l. drci br r'p.duE. Arrhoqi r[ee rwo v us. 4'rond 4 . snould ige

"irh .mh orh.

vhen hsr .rchss. *lh do iislrlrion ir smilt. sql a!r.ndr k d ! $ficid!.oidiron GMditio) fn lo* h.a $umiry .d.

10.1.2 A vdE 16 dr ip.citrH rhcmrl @dudiyr) arGmpenErc (4 + t /2, qs li@ftd.d for h.d exchuw *idrri. insLidion co $d bl crlcurr&d usi'lg rh. rollovilg:

Crlcul& /f" (ri - rrlr i), r,,aj. and upply ! cod.dloi lnrdllll]ds hor lrow s dcsibcd ii 102 b idjus r' ro r&.r.d ,ll dul6 rordins ro serim I l.

O e rzrd|!bi'd[l@'i'!ImhfuM

lo.z Cotuitulot Etu@M Hd flow:102.1 C.lclldio of dt .teiM lt.mll dd*tiviry byimpL conFio of thpcle gnditu h dE

'|@ hdr

rhd in th. r@imn h 14 ydid wlEtr rh. r..iM a 'fu*. d bdh, h.E low rhsml @dlctvitid Elni€ b rhd of! icuhrjo. Trr .rF e ihdld b. d6ill.d b midnil.* mn od ir{adid d |ni.ls hctr.mh..d ! ojmi rh. d.vilitr ft6 uiilm hd nd b$ bd

r=.A €)drE f. n . tudid oa q$str ditlsis, .nl fr ir .mMof r]r' [^.na [rrll rh. r, Em h5 0 vdE bac!!d I fr tu mio ol surd ddrui b olrm diupcit.dr |hi. sy&h. ft. /.^ h ir Ao*n in F4. ,l 6 . tudjd oll, ra v$e v.lc ot rrA , fd ! liH lEd Ar hi8ni6 oI

^ !& rn r/I, ddjG slH d b. @ery

@ Ur &Ftu fM id..l hd [@ vNld h. n Fo(uda dE prldB of tr .ri a! wllil b. l!5 or 0.10

0 *) aor.ll tltalllmits wh.E I !/I, r"d rv,r, w 3'r&!i lo lr rrr v'l* or F r/Fr u b b. Lrt b.loq I0 9', dt!6

^"/1, 'nd r,/ll,

'Er b. d ni th.

102.2 MecrE o Mi.L *lEE dE nn6 of lr^,'d

ljl\, do id t:ll {irhin $e bondli6 dru b. ac@tri.d sirh .@tiod fa.rhd lrl nd. Ire *diN etr b. ddmii.d i! . followitri dd ditdt

10.2.2 | Ue ol mlyricd t@hii46 $ ddoib.d bt

10.2.2.1 UiiE.dc!ld@ lm nriEdtr.'@ d iiric.1d hd .o.dErid cod.., {10.2.2,1 D.@ii.d doqim ll, by 6in! s6l ar.tsE ddh& a riBf6 nodld. of dt@r fiaol s!fu s wild. TIE ItstdlE N b. !r.d cditrllY

n5

los

!0 lo l@ l.@

Flo.fulgllh&Mtt....h|ir|.rb\J|,h..nrwdcv\

sii€ dl sEn ipainM $ould h8. dF sm 5i4 a rh?

srciM *ith d uilrwn th.f,d oiddidy ud hrv. rh.

l l.l llr qon otttp n nrd6 qU i6lud. lll. tollo*_

tl.l.l Cdda ,0eici i&{ri6did imluditg .hrp.

ll,t.? Cmpka n..tifiorioi of iMul.rid od se oI l,v.lq 3|t. xd gD F4t

ll.l.3 St.@nB of tlE'l|EoPI. rY

Il.lt cdlold. lidhr ol lll gMicd ditrfuio6 orfi.3y@ i'rludin! 'r.

., lpeiM h.i$L fts bt h.isht!d dilllE bq€i lnF{uc e.s

ll.l.6 Me b! ,|eirl rd ffi oI v vdG ildh.r

rl,l.? R.lmbri.cof rhn@r llr'.td of dE Fqr.ac ridi.i oI 0E q'djncdtondl6 $od t tu vdu. 6ot .rnel., in.lDl oddiv_

y dll! m Py|uff 966 unry SRM ?35 l@ b.^ f.Ed nn ras ol d. ..c.r..d YdG fa PY|!..d og o.hps@ tu8! Im 210 o 90 X,'

rr.r.3 wied, ilsr fM $n 6 mdDd lrd0lBebh.Fpoi.dsh.Yin!hddo5..jn db,thLdlh.4th6dl

'.{ui'g|d p(sib.d b rhir dhod :hdl b. d rvh.d

uh odiridr ft d.r.r rlE rlle All cqui,.Mu or$h dnod h.€ h*i d *irh $. seFifl of .' call b.idLd rn . @pl* lid oa dE .sprhB ircl'd.d:

I |,1,9 Mdt d vtlB oa GnF{uE .nd 5peitri td_

l2.l Da.nne Em6-7tu d,'nift ffi of q I n:

l$l-l\1.l!3:!l.| 1!j3 |

ut,-t,) rt!-r,,qzr-z') rtr. - tn. E_.za'--E=zF- - tz:=zat|f.- r,$1zr - 4l

t?'- 2)'c

.'ft,'-u"llr tlF iar no*! rnd lirFduE sM 6p.itrE e

sridlr dE m ir d. mu b.E e tlut c .rtrodh6 .

12,2 Eun* 6 De^itu Effi12,2.1 A$hDti@ td ! ry$m *h.c bdh nG D.r od

dE .Fcimtr dof .qud Llt b dnr th. &mnpciiSt e

t!t.,"d,4-4-'4- z,'1-4= ttnn'r:- t, -ti -4- rt- r,- r0{l

.44- z)' uL - 4 - r\2. - 4 - n2 ffi.@

llli E

t(r1- tj) - qtr - rJ -.(.i - t') . de.12.2.2 rn.nwinumvdEorqa-zndc.ws.F'lui

Fbd by i$uminc ar lndrjn(y or t !, (*itr dimd*) d

.dd oI *h su n 0? m4 rhc uididy in dEr rq t{r: - 7,) .r.

os.lkuldr€d b{$d oi dE $iw ib$lu@ eoncyri ui@ib.y h r'r

l?.31 ft.f e !r lce{ $ac o1h6 mn r[d cm .oriL. b dd sys@m .mr alll fis E (l) nm{nifomrdf-i,r 6kl2F. (2) h6r .(hr€c bd*a 0* 6t'mrd $. suid, anl (l) hed shlmirs rlwugh rlE inshdoo

1225

dDun '|l.6lum.T1e

tn& ms nrr h. miiimiz.d or

{pr.trie 6d;N +plied to rh

12.3.2 Tla contiblriotu fM rh. l$t rvo d6 co h.d.bmii.d !99Dnddy siDg sllts r'm .!p,qrid! .ip.riMs @icd or:r ditrftor Lv?k orsrrd tnp.6ruE roNtcirun .@t tmp.6NE our of bdad.

12.4 opar-An iocMiod, i .nabo bryhuidtubii(e) ha lhown rhl r

p€;id of c6.3 * @ b. dbitud ova th. r?mpadE di.3m b 600 K. Ahhough rc d.6 a bis.ould be eobliNh.ddF& @ iodidim rllrl rh. valudr rloF rhr dc otrdncd bt.bolu! dnodi Tr s p.F nor rL ar ASTM c ! El@h Fpon,

|u|i.Tftnm*''.hw r. e ,. *do r. &iM todq4 crydii li rc Btr , fir r, r0 r'r @.1r) lD6).

lMbkdr@nErid'-jdy|97dF|l|{'

(6) Fr.d E. ?&d codkdi4 w ,.

oMq4M,r.dtB(o A.,fttu|6.re'.Dc..d.Pkilhfus.NY'NYl93]F4s

(l) F@ D. *, .tu Cedldliy ofrhr z*tu e/c.d, 94ii tutr€dr !x nid(r{dtu,1 c,fr,R P mdsnih,s.6

19']fu.l.D'v.d.naaA6HilLrdlri, tu6 br r. e rfl. r$)

fufu9.1*6bead@bMfi|dbned'fud$r|d4Fdtlc6${fubfu

?YdPa9ryq&!tp

tte.lgMrlon: D 5rl1' - 0l

St ndard T.3t Method lorThermal Transmbslon Propcrtles ot Thln ThermallyConductlve Solld Elact.lcai Ingulation Mat€rlalsr

didr4ro<.{e*drqa es

rh.rur idpd.M of djo.lcrdc.l io$l.tio iei.ltcomposic rh.mrlly dd(riv. slEr tuEriol hngiry fion

o@hd nu dmnghr rd ipdiftn. Crkllnio8 @ nrd. s ifrh. sF.illx6 14

sft6El|'ndbo@sen.oN, bd r[. Ndmpriq der @r d.@r f6n rlE s.tul

I4 In. Em \nma] .od!.!vny' lppli$ only ro horev. ebcuicd jaDldiig

Mdrls e &rlly i.mgdds siB rh.y rypjdry in-clud. nll.6, biidas. €infm.mna sch a ira hb.r 16l!or i l.y( ot polyffiic 6lm. To woid coifo.iotr, lhn 6rtrErbod uscs dppenr ihrmd .onmei6 ol borh lbnosoo$ lid nm homgcrour narnlls

15 A limitunon ot diig d; Es ndhod b cdcuhc.pFmr lh.1nl ondxrivirt i5 rlr pd6ld ol elfulyddminiit rr'. sFcimn d'icrrd. To and rh. .mftridptrdce or n.lNdng rhi.li.$ s naurmrudt dhfi Ulim.bunng rricknss

'n an dsmbly, rhickm$ k d.emin.d

*id !,Grhod c of Tei Mdho& D 174.1.6 Tn nDd in9.ir@ B d'6 c iniuaEd by d@i

p6!@, lF.jmn $de rhMjs s, dd rh..risEEof arremab zurhs ror hed trln$i$io whi.h e d lhfl8hrhc spe.iNtr Thir E* m.rhod ddmifts rh{mr @idoiionpmFnies rrdq I spdin. $r of condirions (idudln€ r 50.caaEs. 6r ldFnk) vhi.h nly d,ge.rrdy virh rhcondirids itr r :ppridton. A! , cDlL rlE d.sc ol

dy pdjdk rlrli,

rt Thit io .d dar Nt Nrpa,1 tu o E$ o1t of Lt

'tdt @e@ [ ,q. aski .d iErpANbitir oJ tk et ol thi: aonlod b

^tahtkh oppn.

pnok :teD nnn h.alk p@iM tud deMt^c th. aprt@-bili' aJ t suldtal Linibtkns rfir h Be.

D 174 T6r Mchod! ra lr'ick6 0f solid Eler.iol ris!.

E 691 P'Erie In Cddlcrin3 0 Inrc rhddurr Srudy rdD.tmin. rh. ft..i.ior of. T4r Merhodl

dndi!(y orSdLjdr byM.s of rh. cl6d.d-compmriv.

2.2 Mititart src.itcdim:MILI-49156 ltuul{io. SlrL Eldncd. S ierc Rubb.r,

TrEmllly Condtrcrive. Fib.Bh$ Reiirocd.

t.t D.htitio8 oI r.m sp{ilt b 11,n shadod:\ | | a|.q. t@t.tut tol a u.Ju.), "- tt r*3.1.2 .dporr,, rr mftnil m!d. up of di$iid p(6

w[ich oibibur., eirir Flpo idr]ly or synssi{isll}, ro rhepnpsdq or 6. Mbdeon.

l l.r td-r.n.M d,zd. n+ roBi.l in *hich at-.mr prcp.nid e nd ! fumriotr at r r.dirid virhii dE

{S o rzo3,1.1 th.dul conoivid l)t,Ft\. rine dE ot id flow,

. pd unir Empdat€3ddi6t itr th. diErid p..Fndi.ule ro E 'et.1.s th.mt inp.da^.. ts),4- tj"drt @o6irid rhd @ss.nbry (mEfilr, miEnd inrerfet pEro6 to rh. tl@ oI

i.1.6 fi.ndl hr4t4ia1 iq..luc. lM dsi.@),tr-rh. rmp.dc dif.@.

'quicd ro FldG r unir ol

h.or fltrk d.lF okr pld6 b.lrEn ih. spein.i $des

un&r rd. rn. symbol In 6d caisllE h rrt.t.1 k nut n*riyiD, n-tll. @i9

dEriviry Undr n..dy4[r. mrdiriois, rhc 6p.duE sn-dicd, in lne dtdrion peQ.ndiuutlr ro e isorhenut surte

3.7 Stibok:Sybdt uad in rti' 94rd4d,3 2.1 I = L\m,i m'nucdviry, *atr p{ m@,K,I 2.2 I I = GmFote of hot 3une. in @trkr widr e

l.?.1 7 r = lnp.durc oI hd sud@ oI I jr€ilr K3.2.1 I. = !hp.F & of cold surle. of a $cimn, X3.2 5 T,= r.npe*rlE of cotd sud8. id .onod wirh a

3?.6 ^ =mof . rpcitu\ m'.

3 2.7 x = rhickft$ of .pei@. nI1.3 I = rime h@ ot her io*, w or rs.3.2.9 4 = h.d iux, d rim. 6r ot i.d now F ui. aa3I r0 0 = ft.nd ,mFd'R Emp.]r@ drf.Ene p.r

{, suM.y otT.n M..r.d4.1 h .nir En medod (. nodilisrion or T4r M.rtDd

E 122t, I sFcin.i i3 Md*i.hed b.rwd rwo mut MsiomFr!.4 lnd suppli.d *irh a lroUd Mon or rE!.nc':I ar .qoiribrium. rmp.@B e tlE!,sl {d a.hdhrr imp.n!ru is .!hulsr.d. rh rh.tut inp.daic andftiornes @ 0*n b compub lpplrd rh.mrt codudiviry

5l Li! E{ 'ndnod

mmurcs rh. rtemlt hmnissionpropcrdA o, rov modurus (dcfdtubtc) dieteuh mrEi,ls,TlEi llreil]s c us.d (o rid h.d hBr.r:o rrcric,t,nt

id.nddu nkddt r

5 2 lln 16r mdnod n dpeflrtty us.tut for s.@,trgriii o h. firbd wrh

s. rnn 6{ dcdod @y,void p..hr.m oI

'lr6uEftd dE ro idunifih

'.*lG,b acnbt.detuic

5 3 ln .trdr. rhis br mdhod sumr rhd speimn r'yssl* .rd rh.r th* k no Gtreri€ in&d-id Eitubd*ci br.6. Tn. dor. or rl; pld oI rlmrr imr.dd

8glinn muldiv. ih'ckn* Fmibrimd @idlcrjlny wirhour ESud b $.md int r.i&l

5.4 lnis 16r dd.d n Atiov.d rtr r by rt D.p:nn.rior Detqe, od k indud.d in Milibry Sp.ciricorion MIL-I

TESI METITOD

rr cErcBr r@i @ $ovi h Frs. I r Fig. 2. TrE!ppa@ .llM in Fis. I lg ! Etfte. cdqidkr b&Emim m. tu of her flow rhEu3h rh. speitun. option-illy onir $e cfffi.. carorireror (Fig. ?). The fuG of r(no* in U.spaim.n is ddmiid lrcm $c d!tuic, porcrrrpltd b rhc har sMhly liii$ all m4ring su o.5 row hil 04 ln b

'p!ruxin* r tu plarc for $. me bon in

.oid. wiri rh. sp..im.n surl*..

.1.+l

@@@

T1

r4

& o srro

6,2 In. haE mn (a bldt) i. .dc or coooa d dlshiihry6'ns E tr{6rl. odririn3 on id& d inilt ricw'i lsEE h tr ,!.rr.d I6m i tlEunri| F.td hsby . l.ya oa rh.dl iehid dFin (.porv FRr arimild) 5 m di*. TIE tltd hds i. rlo i4ld..t t6 tEr dd.@c $1.|| rElutd dsly i @rfdndl b

6.1 Mft bs c .Whd.d fm hio{ltdttd dtd8-vny mda lNiU Fdld *dlin8 .udE A li!!L

Nldrl or orhcjd k I Nd-prity rflb rlMile6.4 Ti.Efgt@.rldi,|ei. duu.d fM r !&iil

shi.h hc . t|oM rlmt dddirity oq 0t nllt of BhFnrud b b. s.d A dnEi.d ld'irl i. sRM'ra62 rlcnt {rirke.4l. Td dioa E 1225lii dlErcfllhrbi.liot.dfutu!.

6.J T1E aliog uiir ir I cd Uer oLd h, ilid{rdi.n r,m | 6Mr &trrF@ b.th tEn ! u.rnp.doE n n$iidd !trirod t *irhi. :02 K

6'6 Tn 'E

i' c4.hL of mnili.l th..p.!ifi!d tdero rlE Br ii@ rhMth r fcllodirt 4tcfrl d uh'd. b Frd olts lodr &d w6 pls s dt B

67 lialdid rtudha d. lIeim cr, 8.4 it r6bM {Fd idldint bldlq le 3 31

7.1 Fe Itu'tu1 Itr&'.c-rt*. E lpoctfti rM 'Di@ of d. 6 l|@ij. dr l@ @ {L4th od vidh) 6iL dai! h.r, ud*

'raiuly kDwtr .'n p.ior b

dEd ii6 th. |6bU '|sE . rhjdB oI rh.

ie itr stt@ enn Ta Mdn d c o, Ta M.lldl

1,2 Fo awfl h.nd turtictnr Mb.r oi rrdi!ft b 9t.'irb UE Gqui'ld numb.t or

7.t l*.ldr cdr'nlorhr-unld dlE i$ ,F.ii{d.d dE @idd i! fi. &div.d .e R.tur 0, dad ndn die std.ry oeiEdd hY r aiebL m-r*ti.i .ld r.i.. 6 ein& 10 cMua ilE EmYor or.kdiU &l6ta e $iLhh dryiit F.adu6 ttu mv

3,1 Ar dm cmFfu. ,l*'s rlE lrcimn drrffih r.dd.F *ith id udnod c of Td Mdnodt D 374.

3,2 C.G tlF tFcidi b.rcr |n. rm fttE b8s3 ldd dr ;fm..16ie, iI ei,. b.rEn tlE

low |l* h{ dd dE .elilg ujr'3.,1 Ec d. enbLd @ ck itu r. p.63.5 u/irh rlr

'|a, lptly I fm D E rEl Mh

'h{ r'0

: o,l.MA 'EuE

! .p9li.d b th. rFcimn Mrtrbitr tn!gladE 6 rb. t&t ta rr* ljldid ot rh. 6tk ,_r'xedrra!'dq*b|r& brdriri*

egdbd|br&h.eb''ncdgnq&ia

3.6 ord& @litrt nud i.d .ttlv Po*r D rh. hdin!.krd. M.irb! rlE !u!td h* mFduE b ridii =o2

&7 Sie ||, F;!a mt ilr:'* dutirt ld!P. Mid.ld {js dr 4rli.d lm in E

'|B b dnkd' uE

inoar.d olt.@ o uE ttditrtr ds b l|lmr .rp.rid3.3 co.det t[. Bd'a uda odjtiod dd pac d

.8n3. sFciM qrFiuc ot 5(rC For i.daNnB!d. r hF@.boE m ( n i. @{qty ro rPPrY r6broE tlFd lrdrhr bLit r lo6.tv d.d E cddim_

39 nEdn 0F Gtr$dec of uE ie ba $d rrE

EIffi oldima r.quilib.iuF h m..h{oE of !rf.t@ crldi|le. @d th. 6lu3! dd .@d rppli.il ro

d. lEe, Ihltb|iun ir roi!.d *ho 2 !|lc6iv. *B ofroFrr c.diur e bt ! n l5_mii iiEdk .|n ftditr;d bcEtr rh. N d k 5 d0 :02 K

3.10 C&!|l! dE trd .Peirtr EnFtuE d hdsDl nned.r tth.l th. oidl.d {'.dl inFarcr* dE .iDil?lrF.F4iM s dE rh.dliqrdr* ol

3.il D.hn* uE do"'l im!.d!e ol nunjpl. blt6M'nbi. rh. l|d r..@rta of in huxiDllhv.ttd $c!'|B drhh :2 X oI rh. alrk lryd.pciNi mFntuc bv

Ed!.ln! r|l. ld nu s . .unbq ol lrv6 it id@d.

FOFCEJ Jtzr 69S'

^\v (y L!,

T1

f2

T3

T4

d$f o totoe.t.t H4 Ft!' uiinq R.tude cdo,r@..-crrcut b

rrdnlc .'rodeb @diiss a

e=L#'r', ',r

a= 6@d @idEdvny or rh. EI@ .itdin

rJ- 16 = hpaduc dirftm. b.@r dxtrrdopr.sor lne rct Eie c.lodneri K. ad/ = d;hn€ bdwetr dmeouplcs itr rhc atd.

e | 2 E.d rbw trh4n Nor uti's R.f.n^.r catotinrEpc .!l!b rh. hai how rDn rlc !ppti.{ d{&ic,t pors as

o=rrt c)

v = .r4rdcrr por.nrirt {pri.d ro rh. h.de( v aid/ = ereb.d cuMr flo' in dc hqbr A.9.2 Dsiv. ri. hp.duE of rt, upr.. ffi btr &lfE in

sfl&r !'$ ur.sp€imn frcd rh. fondin8:

i\- r, itt,_r)

T. = rnp.tuE or L\e upp.r m.@ br $ni.. ii

=disbn.cbclwdbmFhl@&ns.o''hd= dirurc flm tu lefr gMr o d.loEludc

9.3 D6lvc rh. bmpcftrr ol L\.low( h.@ ba su ,e itr.okd lnh !h. qdimtr tM r]l. followirt:

rD=\+ ic,',) (4)

I,r = Gmlqdun of $c lower mdc b& srlc ii M@Ir = upp.r bFiruc of rhc lor- ftrE be, (,tr : la*.r rmp.nruc ot $. row< nda b€r, K..1. = diskn( belwel EmFEUE sNoB, m, ondr', = dhbne rod d. uppd ei$r b rh. uppcr ru col

rh. towr ftra br, m.0.4 crrcur& $e rh.mit inp.dd@ Irom

r_cA r;\ta!d dpn$ irin irs or (X mrYg/:

riviry 6on ! ptor otdErharinp. ie lor riisl. odhua9trigdEEspa{E'FcinH'hicr6

0n rhe is dd $pcimn rhcm

95 r Tt c@ h r eth lii. {h@ doF ii rh.nddirir, t'. iiEr!.pr

!i alo dlckisi k the th.mal iiblfsirl imp.dmce, tl,,.?ci6c b dr splc, clintt'ig f@ !*i, a.d rhc dmpns

91.2 A3 a pftf.ftd rlcndive, ompua lhe stop. sd rlr

'n@rr 6ng r4r ntm !q0@

l0.l R.poi $o tollo*jrg iif(mionl0.l.l S9eift i id.nritf, ltmil0.r.r.r N@ orrhc moul*rm,r0.r.r.l B'Eh or ror numb.(10.1.1.3 Gnlc d.signdio,,lor.r.a Nmad $itci ddlor r.5 Any orl'tr inromlrid p.n n.nr ro ri. id.d|icl

10.r.2 Nunb.. or bltB $.d il dr bL10.1.3 Avdea hp.duE or d* sp.cidi, if dhs rhm

lo r.4 P6$c us.d duing brins, if orrer dm 3.0 Mprror.t Tn.|mr tusisidn ItDFnns:l0.l 5.r Appm.nrft.md.!nduqivn),.10.1.5,2 I4h, inp.drie r6n 9.4. adI0.r.5.r n'.@l inda&iat imp.d@ tM 9.J.1.

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A fevc! Composles Par 010l

Thermo.mechanlca Inlest salion of Nanoreinlorcerenl3 Doped Ela5lorn€ric Mnocomp6ite Thema

'nsulallons Abslraci The di$enaton repons the efticacv of the nanofller5 to altenuai€ the lhermal

insulation, rherna! lra.silion. lhe.nlal st bility, and rechani@l characleistiG of the dastore c

na.oconposires. T!€nly €ighl dive.* olastoreic aystenE have been used silh tunctionali4d iiJlli\'\6ll

€rbon nanotubes (FM!1/CNTS) and nanokaolinite (FNK) and elaslodE c matric6 includlng elhyl6.€

propylen6 monorerrubbef (EPDM), slyr€ne butadiene rubberISBR), sili@n rubber (sR) acryloiitlebutadiehe rubber (NBR) to labi@ie polyner nanoconposites suilable for nunrple applielions. The nano_

incoDo.ationsEre tuhctionausd usino 3-aninopropyl tirethory silane lo improve |hen dispensabrlily

and conpatibilrty lifl the hosr elaslomgic mlix Ihe nanoieinlofcements ha!€ be€n inpregnated in the

elastoreic rotric€s us ng internaldispersion kneadd andlsD{olsrdnng mlllfor a specilic duralior

rempeGtufe and rolling velocty endiions. Elaston€ric @nposire spedrenswre cured 0n the hol

isostaric rress at a specifc lerperallr€ and pressur6. The fabrieted @r'posite specirens Ere pui into

lest lo. lhemal @nductiety/irpedanc€, scanninq €l€ctron rtcroscopic analysis, ditlerenlial s6nnrn9calor mstric analysis, lhsrmal decompGilion analysi3, differcnlial th€rnal analysis, shore A hardness and

uniarallensile tesls lo elucidale lhe effecl oftunctionalized nanelncorporalions on lhe thermlandrech.nic€l cnaract ristics ol lhe elastoreric nano@mposites. The lhermal and r€chan@l properles ollhe $ynth€si2ed nanocodrposilas have been posilively influenc€d $ilh infieasing lh6 @n@ntralion otihetunci onali2ed nanoclay/nanotubes ih lh€ host elastomerc @tric€s. High lhermalslab lly, hel qlenching

capab lily, low lherhal @.duct vL9, high mechanicalslrenglh, and rema.kable reintofcemenl-mstrix

adhesion are idenliied as lhe rnosl proninent 1ac!o61or enhanced {remalinsulalon pedonEnce ofelastodBic nanoconposiles. The leasr value of therml @nduolivily (0.009w/m,K), ut rcsl lhermlimpedance (5.12m.1(W, aid highe3r uhimare rensil6 slr€ngrh (8.45MPa) refesc.uri.iEd for 30sr.l FNK

imp.egnared NBR nanocomposte. Ths upp€rmosl lherrml stabiliry, lov€st qlass rransirion and

of/slallizallon iemper.tures!€re obs€ ed lor lt!to/6 FMICNIS incorporaled SR composrte hvewofoverall p€dom.ce, FMI /CNTS and nanokaolinib irpeonated NBR and EPOM elaslorericnanocomposites are demonslralsd ben6rcompared lo oher fabdcal.d composit6 syslems rega.ding

iherml conduclivilylmpedan@, lherml transition t€mp€ratures, lherml stab lily, endothemic capability,

and mechanl€l asDecls The novehv of this rese.rch rcrk resides in lhe rabri€tion ornewelastom6rlccomposite tormlalions using tunclionaliad nanotlleB. Thercl tansport study and difiorential lhermlanalysis oflhe tabdcated polyr€r nanocomposit€s af€ also add value to the pres€nl scienljfc lter.llre on

elastomeic nanocompos les The highest themal insulalion charactgr @s obseo6d for the FNKNBR

syslems compar6d lo lhe cont6mporary availabl6$la Thedesiq.e.can sglect lh€ suilable combnalion

oi elastorenc nanoconoosite for ihe sitlation al hand using rhe therml iransporv3lability,'lransilion

tedEeatures speofc e nlhalpie s and nEchanical inv6sngaton data p.ovided in consolidated rormtoMrds

the end ol the thesis, Chapter # 1 Inlroduclion I Thorml Insul3lDn

4Thernr|l iGulation lr th€ rsduction ol ho't trtGr'r (ih' ranspon or the rml

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