evaluation of water vapour permeability of solventless epoxy – nano talc/montmorrilonite...

Evaluation of water vapour permeability ofsolventless epoxy – nano talc/montmorrilonite

amino-silane coupled coatingsNaveen Sharma, Vivek Singal and Dawid D’Melo

Advanced Materials and Processes Department, Crompton Greaves Global Research and Development Centre, Mumbai, India

AbstractPurpose – The purpose of this paper is to evaluate the water vapour permeability and mechanical properties of a solventless epoxy – nano-plateletnano-composite system compatibilised with an amino-silane.Design/methodology/approach – The performance of a nano-platelet reinforced coating composite was studied with reference to the water vapourpermeability and mechanical properties. The effect of addition of coupling agent on these properties was also studied.Findings – The addition of nano-platelets to the solventless epoxy system resulted in an increased water vapour permeability which was reduced onthe addition of coupling agent. The talc-based films showed a better performance as compared to the montmorillonite based coatings. The mechanicalproperties of the films increased though the addition of coupling agent showed a larger increase. The gloss of the coatings was compromised onaddition of nano-particles. Comparing coupling agents, the primary amine based silane showed better performance and lower tactoid formation ascompared to the secondary amino silane based coupling agent.Research limitations/implications – The addition of nano-particles to solventless and other eco-friendly coatings needs to be studied further.Various other coupling agents could be studied to further improve the performance of these coatings.Practical implications – The formulation developed could be used to reduce the water vapour permeability and performance of solventless epoxycoatings, which could be used as anti-corrosive coatings.Originality/value – The study of performance of nano-particles in solventless epoxy coatings and their effect on water vapour permeability couldincrease performance of these reduced VOC coatings.

Keywords Coatings technology, Permeability measurement, Vapours, Nanotechnology, Epoxy coatings, Nanocomposites, Solventless-epoxy,Epoxy coating

Paper type Research paper

Introduction

Epoxy resins are widely used in the formulation of anti-corrosivecoatings due to their excellent properties (Howarth, 1995;

Sakharova et al., 2005; Sørensen et al., 2009). In an effortto increase the performance of the resultant coatings

various compositions based on anti-corrosive pigments

(Kalendova et al., 2004; Pipko, 2001), hydrophobic moieties(Abd El-Ghaffar et al., 1996; Xu and Wang, 2009) and platelet

like particles (Bagherzadeh and Mahdavi, 2007; Ali et al., 2010)have been used. With the interest shown in nano-materials in

recent years nano-based coatings have been extensively studied(Alam et al., 2008; Sung et al., 2008; Pieter et al., 2009;

Zaarei et al., 2008).Due to environmental concerns the use of solvent based

coatings is being restricted and slowly being replaced by

alternate technologies, such as power coatings, water basedformulations, high solid and solventless systems. These are low

volatile organic content coating systems. Volatile organic

content of a coating arises from the use of solvents, whichduring the film formation stage are emitted into the atmosphere.

This increases the environmental impact of coating systems,

could create a possible fire hazard in poorly ventilated paint

areas among other negative effects. Recent specifications

relating to volatile organic content of coatings for anti-

corrosive paint is 250 g/L (Green Seal Standard GC-03,

1997). As is reported in literature the compatibility of nano-

materials with the polymer matrix is the main governing factor

in its dispersion and consequently in its performance

(Bikiaris et al., 2005; Chow et al., 2003; Garcıa-Lopez et al.,

2003). The effect of intercalating agents in the case of layered

silicates or the addition of functional groups in the case of other

nano-particles has been studied in conventional systems

(Lu et al., 2004). In cases where the compatibility of the nano-

particle with the polymer matrix needs to be improved,

the use of various coupling agents has also been studied

(Kusmono et al., 2010). The use of micro platelets as barriers

particles is a proven technology, with the use of talc, mica

and graphite, among other particles showing improvements

in barrier properties (Murthy et al., 2003). The use of

nanoplatelets has also shown similar improvements in barrier

properties at considerably lowerfiller concentrations (Kim et al.,

2005). Conventionally talc and MMT are used as fillers in

a number of applications. Apart from its use as a filler

modified MMT is also used as a thixotropic agent in coating

formulations.The current study will focus on the use of nano-sized talc and

montmorrilonite (MMT) and their effect on the barrier

properties of a solventless epoxy coating composition. The use

of a primary and secondary amino-silane coupling agent will

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Pigment & Resin Technology

42/1 (2013) 45–52

q Emerald Group Publishing Limited [ISSN 0369-9420]

[DOI 10.1108/03699421311288751]

45

also be studied for their effect on the water vapour permeabilityof the coating as well as the mechanical properties of the coating.

Experimental

Materials

The epoxy resin formulation was procured from M/s ShreeSurya Coating Ltd, Nasik, India and had an epoxy equivalent of180-190 mg KOH/gm resin, viscosity of 2,330 mPas (258C) anddiluted with 10 per cent (w/w) butanediol diglycidyl ether soldunder the trade name SuEpo Prime 535. The curing agent was apolyamide obtained from M/s Shree Surya Coating Ltd,Nasik with a total amine value of 365 mg KOH/gm resin. Themontmorrilonite (MMT) used was obtained from M/sVesta Organano Pvt. Ltd, Pune, India and was treated withstearyl amine hydrochloride, with a d value of 2.2 nm andspecific gravity of 1.87 and the nano-talc used was obtainedfrom Innovation Center for Applied Nanotechnology, Pune,India. The talc obtained had a d value of 3.14 nm and specificgravity of 1.62. The chemical structures of MMT wasMx(Al4-x Mgx)Si8O20(OH)4 and talc was Mg3Si4O12H2.Coupling agents A1100 and A1700 were obtained from M/sMomentive India Ltd, Mumbai, India. The coupling agentsused was amino-silanes where A1100 was a gamma-aminopropyl triethoxysilane and A1170 which was bis-(gamma-trimethoxysilylpropyl) amine. The coupling agentA1100 had a viscosity of 2 cSt (258C), refractive index of 1.42and boiling point of 2208C, while the coupling agent A1700 hada viscosity of 6 cSt (258C), refractive index of 1.04 and boilingpoint of 1528C. The structures of the coupling agents is shownin Figure 1 and their method of interaction with the polymerand the filler is shown in Figure 2. It could be observed that theparticles used have only hydroxyl or oxide functional groups, ofwhich the hydroxyl groups react with the silane through aetherification reaction and the amine portion of the couplingagent react with the epoxy resin.

Preparation of composites

The MMT and talc were dispersed in the epoxy resin undermechanical agitation, at an rpm of 1,500 ^ 100, while beingsubjected to sonication. The resin was taken in a reactionkettle fitted with a mechanical agitator and submerged in anultrasonic bath. The coupling agent was added in the required

quantity along with the resin and the nano-particles added

to the formulation under mechanical agitation and sonication

over a period of 10 min to achieve uniform dispersion

and prevent agglomeration. The addition of nano-material

and coupling agent was carried out on a parts per 100 g resin

based on the epoxy resin, i.e. 1 phr would refer to 1 g of nano-

material or coupling agent for 100 g resin. The agitation and

sonication of the dispersion was carried out for 4 h.

The temperature of the ultrasonic bath was maintained at

a temperature of 30 ^ 28C. The nomenclature used for the

naming of the epoxy nano-composites is as follows “EXY”,

where X is the nano-particle used (T for talc and M for

MMT) and Y refers to the concentration used. In the case of

coupling agents the nomenclature is further extended to

EXYAB, where A is the coupling agent used (A for 1100 and

B for 1170) and B is the concentration used, for example,

“ET1.0A2.0” refers to an epoxy composition with 1.0 phr

nano-talc and 2.0 phr A1100.After dispersion of the nano-material in the epoxy resin the

physical properties of the dispersion were analysed and the

hardener was added in the mix ratio of 1:2 (1 part by weight of

hardener for two parts by weight of resin). The mixture was then

stirred and films were cast on mercury and cured for 4 h at

60 ^ 18C. Post-curing was carried out for 1 h at 80 ^ 18C. The

films were then removed and stabilized at 258C for seven days

before testing. The coatings had a dry film thickness of

100mm ^ 10mm.

Test methodsPermeability testingThe films were tested for their water vapour permeability as per

ASTM D 1653, using the wet cup method, with a cup of

diameter 5 cm and placed in an air circulating oven maintained

at 50 ^ 18C. The weight loss was measured after 12 h and

the permeability of coating calculated using equation (1). The

results have been reported as the percentage weight loss per unit

area per unit thickness of the film, this would take into account

minor variations in the thickness of the film:

Permeability of coating

¼ loss of weight £ 100

Area of film £ film thickness £ initial weight

ð1Þ

Mechanical propertiesThe tensile properties of the films were also evaluated as per

ASTM D2370 at a crosshead speed to 10 mm/min.

Thermal propertiesThe glass transition temperature of the cured films was

evaluated using 7-13 mg of sample and were analysed on a

Mettler Toledo DSC822e machine with a heating rate of 108C/

min. The sample was cycled from 258C to 2508C and 2508C to

258C and the same repeated. The glass transition was evaluated

from the second run to eliminate thermal history from the

sample.

MicroscopyThe transmission electron microscopy (TEM) was carried on a

JEM-1010 machine (Jeol, Japan) the samples were prepared

using an ultra microtome cutter.

Figure 1 Structure of amino-silanes used

A1100 - gamma-amin opropyl triethoxysilane

Si

EtO

EtO

EtO

EtO

EtOOEt

OEt

OEt

H2C

H2

H2

H2H2H2

CC NH2

Si

OEt

C

H2C

C

HN

Si

H2C

CH2

C

A1170 -bis-(gamma-Trimethoxysilylpropyl) amine

Evaluation of water vapour permeability

Naveen Sharma, Vivek Singal and Dawid D’Melo


Volume 42 · Number 1 · 2013 · 45–52

46

Coating application and testing

The coating was applied onto mild steel panels with dimension

8 £ 15 cm, which were degreased, rinsed with water, dried andabraded with a 100 grade emery paper. The panel was then

cleaned to remove any adhering particles and coating applied

via the flow method. The dry film thickness was 50-75mm. Thegloss of the coating was evaluated at 608 using an Elcometer

406L statistical glossmeter as per ASTM D 523 and the

adhesion were evaluated as per ASTM D 4541 using a DeFelsko

Positest AT-Manual pull off adhesion tester.

Results and discussion

Physical properties of composites

The present study focuses on the effect of nano-platelets, i.e. talc

and MMT on the water vapour permeability of a solventless

epoxy coating. The effect of coupling agent has also beenstudied to increase the compatibility of the filler with the

polymer matrix. The coupling agents chosen for the study were

amino-silane coupling agents where the silane portion of

the molecule would bond with the hydroxyl groups present onthe surface of the filler particles and the amino group would be

available for reaction with the epoxy resin, via a standard epoxyamine reaction, as shown in Figure 1. The coupling agent A is

a primary amine and coupling agent B is a secondary amine.It is assumed that the reaction of the coupling agent has

occurred completely, i.e. a 100 per cent reaction, we wereunable to practically verify this. The formulations investigated

with reference to the epoxy – talc/MMT are shown in Table I.From Table I we see that as the concentration of filler increases

the viscosity of the resultant solution increases, this was alsoreported in other studies (Kuhlmann et al., 1965). Comparing

the viscosities of talc and MMT it was observed that thedispersions containing MMT showed a higher viscosity as

compared to talc. Further, the addition of coupling agentresulted in an increase in the viscosity of dispersion. Theobserved increase in the viscosity was due to the increased

interaction between the particle and the filler, this has been

Figure 2 Interaction with polymer and filler




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shown to be true for micro-fillers where the interaction between

the filler and polymer matrix increased and the same would hold

true for nano-fillers (Kusmono et al., 2010; Kuhlmann et al.,1965). The increase in the compatibility of the polymer matrix

and the filler should also be reflected in the mechanical and

barrier properties of the resultant composites.

Variation in Tg of coatings

It was seen that the glass transition temperature (Tg) of the

resultant composites showed a lower value than that of the

pure epoxy. A double layer theory has been proposed to explain

the reduction in the Tg observed with the addition of nano-

particles to polymer systems (Tsagaropoulos and Eisenberg,

1995; Singha and Tho, 2008). The addition of coupling agent

was seen to initially decrease the Tg of the epoxy composite and

then increase the Tg as the concentration of the coupling agent

was increased. The addition of a coupling agent increases the

interaction between the filler and the polymer phase through a

chemical reaction. The formation of a double layer with the first

layer being tightly bound onto the polymer surface and the

second loosely bound layer would still show a lower Tg due to

the second layer. As the concentration of the coupling agent

increases amount of polymer bonded to the particle surface in

the tightly bound layer also increases, this would explain the

increase in the Tg as the concentration of the coupling agent

increases. In the case of ET1.5 the Tg was seen to increase

nominally.

Variation in permeability of coatings

Figure 3 shows the effect of addition of nano-materials on

the water vapour permeability of the film. It was observed that

the addition of MMT or talc resulted in an increase in the

permeability of the coating, except in the case of ET0.5,

where there was a slight decrease. The effect of talc on the

reduction of the permeability as compared to MMT was more

pronounced at all concentration levels. The increase in the

water vapour permeability of the coatings at higher

concentrations could be attributed to the increase in the

capillaries formed at the interface of the polymer and nano-

particles. Since talc showed a lower water vapour permeability

at 0.5 phr as compared to MMT, the effect of addition of

amino-silane coupling agent on the permeability was studied.

It was observed that the addition of coupling agent reduced

the water vapour permeability of the film. The use of a

coupling agent increases the interaction between the polymer

matrix and the filler by chemically reacting with both the fillersurface and the polymer matrix, as shown in Figure 2. The

silane portion of the coupling agent reacts with the hydroxylgroups present on the filler, while the amino group reacts with

the epoxy groups of the resin. The increase in the polymer-filler interaction would lead to a decrease in the interfacial

voids between the polymer and filler, this has been found tobe true for a number of studies involving micro and nano-

fillers (Kusmono et al., 2010). It was expected that thedecrease in the interfacial voids, brought about by the increase

in the polymer-filler interaction would reduce the watervapour permeability through the film. This was expected since

the capillarity of the composition would reduce due to thedecrease in the interfacial voids. A decrease in the water

vapour permeability was observed using both amino-silanecoupling agents, with amino-silane A1100 showing a slightly

lower water vapour permeability as compared to A1170. Theincreased performance of A1100 coupling agent as compared

to A1170 coupling agent was due to the increased reactivity ofthe coupling agent with the epoxy resin due to the presence of

a primary amine group.

Variation in mechanical properties of coatings

The tensile strength of the epoxy nano-composites could beseen in Figure 4. From the results it could be seen that the tensile

strength of the epoxy-talc based composites showed greaterperformance as compared to epoxy-MMT at all concentrationlevels. This trend is similar to that reflected in the case of the

water vapour permeability. If the interaction between thepolymer and the nano-particle is weak then the tensile strength

would also be lower. This would explain the lower tensilestrength of MMT based compositions as compared to talc

based compositions. In order to enhance the compatibility ofthe polymer with the nano-fillers the effect of an amino-silane

coupling agent was studied. It was seen that the addition of thecoupling agent increased the performance of the composite with

respect to the tensile strength of the resultant composites.Comparing the properties of the coupling agent A and B show

that the tensile strength of composites based on coupling agentA show a greater increase at 0.5 per cent as compared to that

shown by coupling agent B. This could be due to the fact that theprimary amine of coupling agent A would result in a greater

compatibility as compared to the coupling agent B, due to theincreased functionality and reactivity of the coupling agent A. At

concentration levels greater than 1 per cent there was nonoticeable difference in the performance of the nano-

composites incorporating coupling agent A or B. In generalthe tensile and elongation at break properties are antagonistic in

nature, as seen in Figure 5. However, in this case it was observedthat the tensile and elongation at break showed similar trends.

The composites based on MMT showed a lower elongation atbreak as compared to talc, while the addition of silane couplingagent resulted in a further increase in the elongation at break

values. One of the areas for ultimate failure of a composite underthe application of stress is the initiation of a break from the

polymer-filler boundary (Wypych, 2000). The addition of acoupling agent, which increases the interaction of the polymer

and filler, could result in an increase in the stress whichthe composite can withstand before ultimate failure of

the composite (Alkadasi et al., 2004). This would explain theincrease in the elongation at break with the addition of the

coupling agent.

Table I Properties of epoxy – talc/MMT

Sample name Viscosity (mPas, 258C, 12 rpm) Tg (8C)

Epoxy 2,330 66.59

ET0.5 2,364 66.38

ET1.0 2,498 64.56

ET1.5 2,750 67.76

EM0.5 2,554 58.34

EM1.0 3,744 62.85

EM1.5 4,529 60.17

ET1.0A0.5 2,989 62.82

ET1.0A1.0 3,220 62.91

ET1.0A1.5 3,809 64.49

ET1.0B0.5 2,599 61.83

ET1.0B1.0 3,350 63.03

ET1.0B1.5 4,579 67.13




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Variation in gloss of coatings

The gloss of the coatings was evaluated and the results areshown in Figure 6. It could be seen that the addition of a fillerreduced the gloss as the concentration of the filler increased.The comparison between the two nano-particles showed thatthe MMTresulted in a coating with a lower gloss as compared totalc. At higher nano-particle concentrations the decrease ingloss could be attributed to two factors, the increased viscosityof the coating, which would result in reduced leveling of thecoating. Second, as the concentration of nano-particlesincreased their concentration at the surface of the coatingwould be higher, leading to irregularities in the coating surface.Both these phenomenon would have an adverse impact on thespecular gloss of the coatings.

Variation in adhesion of coatings

The adhesion of the coatings to the metal substrate was alsoevaluated and the results are shown in Figure 7. It could be seenthat the addition of talc and MMT resulted in a small increase

in the adhesion as compared to the pure epoxy coating up to0.5-1.0 per cent after which it decreased, though the adhesionof talc based coating was seen to be greater than that of the pureepoxy coating at all concentrations levels studied. The addition ofcoupling agent resulted in an increase in the adhesion ofthe coating to the substrate. The coupling agent will function atthe interface of the polymer and the substrate in a similar manneras that at the interface of the polymer and a filler particle. Thisresults in an increased interaction between the substrate and thepolymer, which is reflected in the increased adhesion of thecoating. This was observed in other studies involving the use ofsilanes as adhesion promoters (Plueddemann, 1983). Thecomparison of the two coupling agents showed that thecoupling agent B showed a greater adhesion as compared tocoupling agent A.

Microscopy of coatings

The TEM images of the coatings showing the lowest watervapour permeability were studied. From Figure 3 it was seen

Figure 4 Variation of tensile strength with concentration of nano-particles and coupling agent

60.00

50.00

40.00

30.00

Tesn

sile

Str

eng

th (

MP

a)

20.00

10.00

0.00

Epoxy-MMT Epoxy-Talc ET0.5A ET0.5B

Concentration (phr)

0 0.2 0.4 0.6 0.8 1 1.2 1.4 1.6

Figure 3 Variation of water vapour permeability with concentration of nano-particles and coupling agent

0.00

5.00

10.00

15.00

20.00

25.00

30.00

35.00

0 0.2 0.4 0.6 0.8 1 1.2 1.4 1.6Concentration (phr)

Wat

er p

erm

eab

ility

(%

wei

gh

t lo

ss/

squ

are

cm/m

icro

n)

x 10

–6





Volume 42 · Number 1 · 2013 · 45–52

49

Figure 6 Variation of gloss at 208 with concentration of nano-particles and coupling agent

Glo

ss (

@20

°)

50.00

55.00

65.00

60.00

75.00

70.00

85.00

80.00


Concentration (phr)

0 0.2 0.4 0.6 0.8 1 1.2 1.4 1.6

Figure 7 Variation of adhesion with concentration of nano-particles and coupling agent

Ad

hes

ion

(M

Pa)

1.80

1.60

1.40

1.20

1.00

0.80

0.60


Concentration (phr)

0 0.2 0.4 0.6 0.8 1 1.2 1.4 1.6

Figure 5 Variation of elongation at break with concentration of nano-particles and coupling agent

Elo

ng

atio

n a

t B

reak

(%

)

6.00

8.00

4.00

12.00

14.00

2.00

10.00

0.00


Concentration (phr)

0 0.2 0.4 0.6 0.8 1 1.2 1.4 1.6




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50

that ET0.5A0.5 and ET0.5B0.5 showed the lowest water

permeability. Figure 8 shows the dispersion of ET0.5A0.5and Figure 9 ET0.5B0.5. From the TEMs it could be seenthat ET0.5A0.5 showed a better dispersion as compared to

ET0.5B0.5, although the dispersion of ET0.5B0.5 was notpoor. Both TEMs show the presence of tactoids indicatingthat complete exfoliation did not occur, however, even withthe partial exfoliation of the nano-platelets the properties

showed an improvement.The study shows that the use of nano-platelets in a solventless

epoxy coating necessarily requires the use of a coupling agent.Further work could include the effectiveness of using plateletnano-particles in a pigmented composition, which would have alarger industrial impact. Another avenue of research would be to

further study the effectiveness of various coupling agents and itscompatibility with the epoxy matrix with respect to the increasein properties.

Conclusions

The addition of nano-platelets in the solventless epoxy coatingsystem resulted in a minor increase in the mechanical properties

of the coating, with a 45 per cent increase in tensile strength

as compared to pristine polymer based film at 0.5 per cent talc

coupled with the primary amine based silane coupling agent.

The water vapour permeability decreased, with the primary

amine based coupling agent showing a higher degree ofinteraction with the epoxy resin as compared to the secondary

amine based coupling agent, with a 70 per cent decrease in the

vapour permeability in the case of 0.5 per cent talc coupled withthe primary amine based silane agent. Nano-talc showed better

properties as compared to nano-MMT with a 10 per cent

increase shown by the nano-talc at 0.5 per cent as compared to a

6 per cent decrease with MMTat the same concentration and a14 per cent decrease in vapour permeability using talc as

compared to a 7 per cent increase in the permeability with

MMT. The primary amino-silane showed marginal betterperformance as compared to the secondary amino-silane based

coupling agent with a 70 per cent decrease as compared to

60 per cent decrease in water vapour permeability at 0.5 per centtalc and coupling agent concentration, which was found to be

the optimum value. The use of the coupling agent was found to

be essential for the optimal performance of the nano-platelet

reinforced epoxy films.

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Corresponding author

Dawid D’Melo can be contacted at: dawid.dmelo@cgglobal.

com




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