qualification test for a/c panel adhesives · federal aviation 5 administration adhesive...

Presented to: International Aircraft Materials FireTest Working Group, Atlantic City

By: Rich Lyon, AJP-6320

Date: October 21, 2009

Federal AviationAdministration

QUALIFICATION TEST FOR A/C

PANEL ADHESIVES

International Materials Fire Test Working Group

October 21, 20092Federal Aviation

Administration

Establish Establish similaritysimilarity of bonded details.of bonded details.

OBJECTIVEOBJECTIVEOBJECTIVE

PURPOSEPURPOSEPURPOSE

Develop a qualification testDevelop a qualification test for flammabilityfor flammabilityof adhesives used in bonded details.of adhesives used in bonded details.

APPLICATIONSAPPLICATIONSAPPLICATIONS

Certification of New PartsCertification of New Parts



Administration

ADHESIVES TASK GROUPADHESIVES TASK GROUPADHESIVES TASK GROUP

3M3MAmerican AirlinesAmerican AirlinesBoeingBoeingBombardierBombardierBostikBostikC&D AerospaceC&D AerospaceDassaultDassaultFAAFAAHenkelHenkel



Administration

INDUSTRY-PROPOSED METHODS OF COMPLIANCE FOR CERTIFICATION OF INTERIOR MATERIALS

INDUSTRYINDUSTRY--PROPOSED METHODS OF COMPLIANCE PROPOSED METHODS OF COMPLIANCE FOR CERTIFICATION OF INTERIOR MATERIALSFOR CERTIFICATION OF INTERIOR MATERIALS

BONDED BONDED DETAILSDETAILS2828

25.853(a)25.853(a)

Bunsen Burner Bunsen Burner SimilaritySimilarity

25.853(d)25.853(d)

Heat and Smoke Heat and Smoke SimilaritySimilarity

Testing detail Testing detail without without adhesive*adhesive* to Appendix to Appendix

F substantiates the F substantiates the bonded configurationbonded configuration

Test requiredTest required if: A > 2 ftif: A > 2 ft22

Possible Test if: 1 < A < 2 ftPossible Test if: 1 < A < 2 ft22

No test required* if: ANo test required* if: A < 1 ft< 1 ft22

Ref.Ref.No.No.

Feature / Feature / ConstructionConstruction

Part 2: Methods That Will Require Supporting Data

*For FAA Qualified Adhesives? *For*For FAA Qualified Adhesives? FAA Qualified Adhesives?



Administration

ADHESIVE QUALIFICATION TEST ISSUESADHESIVE QUALIFICATION TEST ISSUESADHESIVE QUALIFICATION TEST ISSUES

FAR 25 versusFAR 25 versus Other Measurement MethodOther Measurement Method

Sample FormSample Form

Effect of Effect of AdherendsAdherends

Effect of Thickness: Effect of Thickness: Does thinner Does thinner substantiatesubstantiate thicker?thicker?



Administration

-10

0

10

20

30

40

50

60

70

-10

0

10

20

30

40

50

60

70

Thickness, inches

Pea

k H

eat R

elea

se R

ate,

kW

/m2 T

otal Heat R

elease, kW-m

in/m2

Peak HRR

Total Heat ReleaseTotal Heat Release

0 .040 .080 0.12 0.16 0.20 0.24 0.28

EUROPLEX PPSU Clear

Example: Thermoplastic Thickness RangesExample: Thermoplastic Thickness RangesExample: Thermoplastic Thickness Ranges

OSU Peak HRR of 0.040″ does not substantiate .080″- 0.16″OSU OSU Peak Peak HRR HRR of 0.040of 0.040″″ doesdoes notnot substantiate .080substantiate .080″″-- 0.160.16″″

Proposed range



Administration

Combustor

Pyrolyzer

Mixing Section

Sample Cup

Scrubber

Flow Meter

O2 Sensor

Exhaust

Purge Gas Inlet

Sample Post & Thermocouple

Oxygen Inlet

Standard Test Method for Measuring Flammability Properties of Plastics and Other Solid Materials Using Microscale Combustion Calorimetry, ASTM

D 7309

Standard Test Method for Measuring Flammability Properties of PlStandard Test Method for Measuring Flammability Properties of Plastics astics and Other Solid Materials Using Microscale Combustion Calorimetrand Other Solid Materials Using Microscale Combustion Calorimetry, ASTM y, ASTM

D 7309D 7309



Administration

250 300 350 400 450 500 550

0

100

200

300

400

500 ηc

hc

Tp

Hea

t R

elea

se R

ate

(J/g

-K)

Temperature (°C)

μ Noncombustible Fraction (g/g)

800 850

THERMAL COMBUSTION PROPERTIES FROM MCC

THERMAL COMBUSTION PROPERTIES THERMAL COMBUSTION PROPERTIES FROM FROM MCCMCC

Peak Heat Release Rate =Heat Release Capacity (J/g-K)

Total Heat Release (J/g)

≈ Burning Temperature



Administration

PP PE

PS

PET

ABSPMMA

Epoxy

POM

NYLON 66

PC

PPOPUPAR

PPSU

PPS PES

PEI LCP

PAI

PEKPEEK

0.1 1 10 100

Materials Cost* ($/lb)

Phenolic

KAPTON

1000

10

100PVF

Heat Heat Resistant Resistant PlasticsPlastics

PSU

PVC (rigid)

Commodity Commodity PlasticsPlastics

*Truckload Prices, 2001

Engineering Plastics

Hea

t R

elea

se C

apac

ity

(ηc)

, J/g

-K

TYPICALLY PASS FAAHRR TEST

TYPICALLY TYPICALLY PASS FAAPASS FAAHRR HRR TESTTEST

HEAT RELEASE CAPACITY VERSUS COST OF PLASTICS

HEAT RELEASE CAPACITY VERSUS HEAT RELEASE CAPACITY VERSUS COST OFCOST OF PLASTICSPLASTICS



Administration

Pro

bab

ility

of

Pas

sin

g V

BB

, p

Heat Release Capacity ηc, J/g-K

η*= 448 J/g-Kn = 4.46R = 0.97

η*= 448 J/g-Kn = 4.46R = 0.97

ASTMASTMD 3801D 3801

VERTICAL BUNSEN BURNER TEST (114 plastics)VERTICAL BUNSEN BURNER TEST (114 plastics)VERTICAL BUNSEN BURNER TEST (114 plastics)Probability of Passing the UL 94 V-0 Requirement

0

0.2

0.4

0.6

0.8

1

0 200 400 600 800 1000 1200

p =1

1+ηc

η *

⎡

⎣ ⎢

⎤

⎦ ⎥

n



Administration

HAND LAY-UP OF ADHESIVE / RESIN OSU SAMPLESHAND LAYHAND LAY--UP OF ADHESIVE / RESIN UP OF ADHESIVE / RESIN OSU OSU SAMPLESSAMPLES

• Fiberglass-reinforced adhesive samples are made by hand lay-up.• Samples cured between two Teflon-coated aluminum plates in heated press.

• Cured samples trimmed to 6″ x 6″ for OSU HRR testing.• Resulting samples ~ 40% resin by weight.



Administration

OSU TESTING OF ADHESIVE RESINSOSU OSU TESTING OF ADHESIVE RESINSTESTING OF ADHESIVE RESINS

BPA Epoxy

BPC Cyanate Ester

BPA Cyanate Ester

BPA Epoxy & MDA

BPC Epoxy

50 kW/m2

Silicone Resin

Time (minutes)

2-min HR

(kW-min/m2)

Peak HRR

(kW/m2)Resin

44111BPA Epoxy

2688BPAE + MDA

2872BPA CE

2848BPC Epoxy

1233Silicone Resin

1313BPC CE



Administration

0

50

100

150

200

0 100 200 300 400 500 600 700

(R = 0.8264) pHRR = 6.4 ηc

avg

⟨pH

RR

⟩, kW

/m2

⟨ηc⟩, J/g-K

OSU PHRR (binned data) 101 RESINS AND PLASTICS)OSU PHRR OSU PHRR (binned data) 101 RESINS AND PLASTICS)(binned data) 101 RESINS AND PLASTICS)

Maximum Heat Release Capacity from Curve Fit

ηcmax =

656.4

⎛ ⎝ ⎜

⎞ ⎠ ⎟

2

= 103 J / g −K



Administration

• HRR ≤ 65 kW/m2 = Pass = P

• HRR > 65 kW/m2 = Fail = F

pHRR19

101315222950

105108115120120121121127129136140141152153155156159173192196201203215215230235248261265276295298301316345349359

82559136631553054926149

1236052

109646569

1109030854572

10636327465

213150

97258

5544

188199

93211232166115207

90

127

174

254

355

36 9/10 = 0.90

6/10 = 0.60

3/10 = 0.30

4/10 = 0.40

0/10 = 0.00

ηcp = P/(P + F)⟨ηc⟩

Etc.

y

OSU Data for AIRCRAFT CABIN

MATERIALS

OSU OSU Data for Data for AIRCRAFT CABIN AIRCRAFT CABIN

MATERIALSMATERIALS

Transform Quantitative Data into Qualitative Data Using Pass/Fail�

Criterion

14 CFR 25.853

PPPPFPPPPFPPFPPFPPFFFPFPFFPPFPFFFFPPFFFFFFFFF



Administration

Pro

bab

ility

of

Pas

sin

g O

SU

pH

RR

, p

η*= 140 J/g-Kn = 2.4

R = 0.97

Heat Release Capacity (ηc), J/g-K

η*= 140 J/g-Kn = 2.4

R = 0.97

14 CFR 2514 CFR 25

OSU PHRR (101 RESINS AND PLASTICS)OSU PHRR OSU PHRR (101 RESINS AND PLASTICS)(101 RESINS AND PLASTICS)Probability that pHRR ≤ 65 kW/m2

0

0.2

0.4

0.6

0.8

1

0 100 200 300 400 500 600 700

p =1

1+ηc

η *

⎡

⎣ ⎢

⎤

⎦ ⎥

n

ηc

max = η * 10.683

−1⎛

⎝ ⎜

⎞

⎠ ⎟

12.4

= 102= 102 J/gJ/g--KK



Administration

AdhesiveAdhesive

PartPart

SubstrateSubstrate

ρρp p , , ηηpp

ρρa a , , ηηaa

ρρs s , , ηηss

ρρii = Areal Density of Layer = Areal Density of Layer ii, g/m, g/m22

ηηii = Heat Release Capacity of Layer in = Heat Release Capacity of Layer in MCC MCC ii, , J/gJ/g--KK

mmii = Mass Fraction of Layer = Mass Fraction of Layer ii = = ρρi i //ΣΣρρii

EFFECT OF ADHERENDS and THICKNESS (Additive Approach Using MCC Data)

EFFECT OF EFFECT OF ADHERENDS ADHERENDS and THICKNESS and THICKNESS (Additive Approach Using (Additive Approach Using MCC MCC Data)Data)

ηconstruction = mpηp + maηa + msηsηηconstructionconstruction = = mmppηηp p + m+ maaηηa a + m+ mssηηss



Administration

AdhesiveAdhesive

PartPart

SubstrateSubstrate

TTii, , ρρ , h, hcc, E, A, etc., E, A, etc.

TTi i = = Thickness of Layer Thickness of Layer ii, cm, cmρρii = Density of Layer = Density of Layer ii, g/m, g/m33

hhii = Heat Release of Layer= Heat Release of Layer, , J/gJ/gEEi i , A, Aii == Thermal Decomposition KineticThermal Decomposition Kinetic Parameters of Parameters of ii

EFFECT OF ADHERENDS and THICKNESS (ThermaKin Numerical Burning Model)

EFFECT OF EFFECT OF ADHERENDS ADHERENDS and THICKNESS and THICKNESS (ThermaKin Numerical Burning Model)(ThermaKin Numerical Burning Model)

TTii, , ρρ , h, E, A, etc., h, E, A, etc.

TTii, , ρρ , h, E, A, etc., h, E, A, etc.

Transient energy and mass balance calculationTransient energy and mass balance calculationTransient energy and mass balance calculation



Administration

OSU HRR OF BONDED CONSTRUCTION (ThermaKin Simulation)

OSU HRR OSU HRR OFOF BONDED CONSTRUCTION BONDED CONSTRUCTION (ThermaKin Simulation)(ThermaKin Simulation)

Heat Flux = 35 kW/m2

(OSU)

+

15 kW/m2

(Flame)

Heat Flux = Heat Flux = 35 kW/m35 kW/m22

((OSUOSU))

++

15 kW/m15 kW/m22

(Flame)(Flame)Adhesive Layer Adhesive Layer Thickness = Thickness = 0.2, 0.2,

0.5, 1 and 1.5 mm0.5, 1 and 1.5 mm

hhcc = 2X Substrate= 2X Substrate

Substrates =Substrates = 1/161/16″″ ((1.5 1.5 mm) Thick Charring mm) Thick Charring

Plastic Plastic (Polycarbonate)(Polycarbonate)



Administration

0

0.2

0.4

0.6

0.8

1

0

0.2

0.4

0.6

0.8

1

0 1 2 3 4 5

1.5 mm Adhesive Layer1.5 mm Adhesive Layer1.5 mm Adhesive Layer

0

0.2

0.4

0.6

0.8

1

0

0.2

0.4

0.6

0.8

1

0 1 2 3 4 5

1 mm Adhesive Layer

1 mm Adhesive 1 mm Adhesive LayerLayer

0

0.2

0.4

0.6

0.8

1

0

0.2

0.4

0.6

0.8

1

0 1 2 3 4 5


HR

R (

arbi

trar

y un

its)

HR

(arbitrary units)

Time, min

0

0.2

0.4

0.6

0.8

1

0

0.2

0.4

0.6

0.8

1

0 1 2 3 4 5


Time, min

Time, minTime, min

OSU HRRs of BONDED CONSTRUCTIONS (ThermaKin)OSU OSU HRRsHRRs of BONDED CONSTRUCTIONS (ThermaKin)of BONDED CONSTRUCTIONS (ThermaKin)

qualification test for a/c panel adhesives · federal aviation 5 administration adhesive...

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