UNCLASSIFIED

NAVAL AIR WARFARE CENTER AIRCRAFT DIVISION

PATUXENT RIVER, MARYLAND

TECHNICAL REPORT

REPORT NO: NAWCADPAX-99-112-TR

HEAT DAMAGE ASSESSMENT

FOR NAVAL AIRCRAFT COMPOSITES

by

Henry McShane
El Sayed Arafat
Philip McLaughlin
Roland Cochran
Kevin Miller
Fred Arnold
Randall Cramer

7 September 1999
19991119 031
Aerospace Materials Division
Air Vehicle Department
Naval Air Warfare Center Aircraft Division
Patuxent River, Maryland

Approved for public release; distribution is unlimited.

DTIC QUALITY nWPBOTHD *

UNCLASSIFIED
 /
DEPARTMENT OF THE NAVY
NAVAL AIR WARFARE CENTER AIRCRAFT DIVISION
PATUXENT RIVER, MARYLAND

NAWCADPAX--99-112-TR
IS^emfcesr 1999

RELEASED BY:

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ROLAND COCHRAN / DATE
Head, Polymer Composites and Materials Branch

dJsA^ i/l/l*
DALE MOORE/DATE
Director, Materials Competency
Naval Air Warfare Center Aircraft Division

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Blank) 7 September 1999

4. TITLE AND SUBTITLE 5. FUNDING NUMBERS

Heat Damage Assessment for Naval Aircraft Composites

6. AUTHOR(S)

Henry McShane Roland Cochran Fred Arnold

El Sayed Arafat Kevin Miller Randall Cramer
Philip McLaughlin

7. PERFORMING ORGANIZATION NAMES(S) AND ADDRESS(ES) 8. PERFORMING ORGANIZATION

REPORT NUMBER
Naval Air Warfare Center Aircraft Division
22347 Cedar Point Road Unit #6 NAWCADPAX--99-112-TR
Patuxent River, Maryland 20670-1161

9. SPONSORING / MONITORING AGENCY NAME(S) AND ADDRESS(ES) 10. SPONSORING/MONITORING

AGENCY REPORT NUMBER
Office of Naval Research
800 N. Quincy Street
Arlington, Virginia 22217-5660

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Approved for public release; distribution is unlimited.

13. ABSTRACT (Maximum 200 words)

This report presents results of work funded by the Office of Naval Research to study heat damage in organic matrix composites. The
results presented in this report identify the mechanisms of heat damage, and the effects on physical and mechanical properties of
composites subjected to high temperatures. A model to describe the heat damage process is presented, and a methodology to determine
composite damage is supplied. In addition, specimens and data from this effort were supplied to government and private industry groups
developing nondestructive evaluation techniques for heat damage evaluation in naval aircraft.

14. SUBJECT TERMS 15. NUMBER OF PAGES

Heat Damage 190
Composite Materials
Thermal Exposure 16. PRICE CODE

17. SECURITY CLASSIFICATION 18. SECURITY CLASSIFICATION 19. SECURITY CLASSIFICATION 20. LIMITATION OF
OF REPORT OF THIS PAGE OF ABSTRACT ABSTRACT

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NSN 7540-01-280-5500 Standard Form 298 (Rev. 2-89)

Prescribed by ANSI Std. Z39-18
298-102
NAWCADPAX-99-112-TR

ABSTRACT

Polymer matrix composites are becoming more widely used for naval aircraft applications. An
inherent problem with all organic matrix resins used in advanced composites is their
susceptibility to thermal oxidative degradation following exposure to temperatures above their
recommended upper service temperature. In current applications, composite heat damage arises
from fire, engine exhaust impingement, equipment overheat, or a mishap during composite
repair. Composites subjected to these exposure conditions experience a decrease in the glass
transition temperature, which serves to effectively lower the upper use temperature, and matrix
mass loss, which reduces the mechanical properties of the composite. The composite structure
may or may not exhibit visual signs of damage, and this damage is difficult to measure by
conventional nondestructive evaluation (NDE) techniques. All naval aircraft that use composites
have the potential to succumb to composite heat damage, including the newly developed V-22
Osprey and the F/A-l 8 E/F.

This report presents results of work funded by the Office of Naval Research to study heat
damage in organic matrix composites. The results presented in this report identify the
mechanisms of heat damage, and the effects on physical and mechanical properties of
composites subjected to high temperatures. A model to describe the heat damage process is
presented, and a methodology to determine composite damage is supplied. In addition,
specimens and data from this effort were supplied to government and private industry groups
developing NDE techniques for heat damage evaluation in naval aircraft.

ACKNOWLEDGMENTS

This work was funded by the Office ofNaval Research Airborne Materials Technology Project
under the direction of James Kelly. Fellowship grants provided under the American Society of
Engineering Education (ASEE) were helpful in bringing Dr. McLaughlin and Dr. Arafat to
NA WCAD Patuxent River, Maryland, and their assistance is greatly appreciated

Many members of the Polymers and Composites Branch at NAWCAD Patuxent River were
instrumental in completing the testing presented in this report. They include Paul Mehrkam,
Eileen Armstrong-Carroll, Gary Neumeister, Stanley Ng, Andrew Guy, and Robert BoswelL
Nondestructive analysis was aided by members of the NDE group of the Metallies and
Ceramics Branch at NA WCAD Patuxent River. They include Paul Kulowich, Ignazio Perez,
and Rachel Santos.

n
NAWCADPAX-99-112-TR

CONTENTS

Page No.

ABSTRACT ii
ACKNOWLEDGMENTS ii

INTRODUCTION 1
1.1 BACKGROUND 1
1.2 SCOPE OF TESTING 2

MECHANISMS OF LAMINATION PLANE CRACKING 3

2.1 INTRODUCTION 3
2.2 MATERIALS 3
2.2.1 NEATRESING 3
2.2.2 COMPOSITE LAMINATES 3
2.3 EXPERIMENTAL PROCEDURE 4
2.3.1 ENVIRONMENTAL CONDITIONING 4
2.3.2 THERMAL EXPOSURE 4
2.3.3 SAMPLE NOMENCLATURE 4
2.3.4 THERMAL GRAVIMETRIC ANALYSIS 5
2.3.5 DIFFERENTIAL SCANNING CALORIMETRY 5
2.3.6 VISUAL INSPECTION 5
2.3.7 ULTRASONIC INSPECTION 5
2.3.8 THERMOGRAPHIC INSPECTION 5
2.3.9 FOUR-POINT FLEXURE TEST 6
2.4 RESULTS AND DISCUSSION 6
2.4.1 EXPERIMENTAL DESIGN 6
2.4.2 ENVIRONMENTAL CONDITIONING 6
2.4.3 THERMAL GRAVIMETRIC ANALYSIS 7
2.4.4 DIFFERENTIAL SCANNING CALORIMETRY 8
2.4.5 VISUAL RESULTS 8
2.4.6 ULTRASOUND AND THERMOGRAPHY INSPECTION 9
2.4.7 FOUR-POINT FLEXURE TEST 10
2.5 CONCLUSIONS 11

OUTGASSING OF EPOXIES 12
3.1 INTRODUCTION 12
3.2 EXPERIMENTAL , 12
3.2.1 MATERIALS 12
3.2.2 THERMAL EXPOSURE 12
3.2.3 SIMULTANEOUS THERMAL ANALYZER 12
3.2.4 FOURIER TRANSFORM INFRARED SPECTROSCOPY 13

in
NAWCADPAX-99-112-TR

Page No.

3.3 RESULTS AND DISCUSSION .13

3.4 CONCLUSIONS ZZ.U

STATIC AND FATIGUE MODEL OF UNIDIRECTIONAL COMPOSITES 16

4.1 INTRODUCTION 16
4.2 CUMULATIVE WEAKENING WITH THERMAL STRESSES 17
4.2.1 CUMULATIVE WEAKENING AND CHAIN-OF-BUNDLES 17
MODEL
4.2.2 CUMULATIVE WEAKENING WITH THERMAL STRESSES 18
4.2.3 ISOTHERMAL STATIC STRENGTH AND FATIGUE LIFE 20
4.3 HEAT DAMAGE IN UNIDIRECTIONAL GRAPHITE/EPOXY 21
COMPOSITES
4.3.1 MATERIAL-RELATED HEAT DAMAGE PROCESSES 21
4.3.2 THERMAL DAMAGE EFFECTS FOR A PARTICULAR 23
GRAPHITE/EPOXY SYSTEM
4.3.2.1 General 23
4.3.2.2 Time/Temperature Property Variations 23
4.3.2.3 At-Temperature Fiber/Matrix Interface Damage 25
4.3.2.4 Residual (Upon Cool Down) Fatigue Strength 25
Versus Cycles Curves
4.4 CONCLUSIONS 26

CONCLUSIONS 28

REFERENCES 31

APPENDICES
A. TABLES 33
B. FIGURES ZZZZZZZ.'.A9
C. THERMAL GRAVIMETRIC ANALYZER PLOTS 99

DISTRIBUTION 183

IV
NAWCADPAX--99-112-TR

SECTION 1
INTRODUCTION

1.1 BACKGROUND

Airframes, propulsion systems, and other structural components are exposed to extreme
temperatures from a variety of heat sources that are sufficient to cause damage to composite
parts. NAWCAD Patuxent River, Maryland, has defined these high temperature exposure
conditions for naval aircraft as fire, engine exhaust impingement, equipment overheat, or
mishaps that occur during repairs. The properties of structural composites subjected to high
temperature environments needs to be understood in order to intelligently use these materials.
This report presents the results of an effort to investigate the process of heat damage. Subtasks
in the program included identifying the temperatures and time-at-temperature conditions (within
the bounds of Navy heat damage scenarios) that result in structural damage, understanding the
effects of moisture on heat damage, and their relation to observed heat-induced property
changes. Several techniques were used to evaluate the chemical, physical, and mechanical
properties of composites exposed to high temperatures.

The behavior of composites exposed to high temperatures first became of interest for NAWCAD
Patuxent River in August of 1991, after a fire in a composite wing of an A-6 aircraft. Questions
arose regarding the flightworthiness of the aircraft and of the Navy's thermal damage assessment
capabilities for composite materials. Five evaluation methods were initially studied: ultrasonics,
Diffuse Reflectance Infrared Fourier Transform (DRIFT) spectroscopy, thermal mechanical
analysis, hardness, and thermography (reference 1). After 2 years, the aircraft was certified
flightworthy and returned to service. During this investigation, none of the nondestructive
evaluation (NDE) methods proved effective in determining the effects of high-temperature
exposure to the composite. The need for a method to evaluate composite heat damage led to
other programs either conducted or sponsored by NAWCAD Patuxent River. Techniques such
as dielectric spectroscopy, Raman spectroscopy, X-ray Photoelectron Spectroscopy (reference 2),
Fourier Transform Infrared (FTIR) spectroscopy, and Laser-Pumped Fluorescence (reference 3)
were studied. Their results, when correlated to mechanical property losses, showed that none of
these techniques could accurately, with repeatable results, define strength losses in a composite.
Ultrasonics, the standard depot-level technique, is effective at identifying damage when
delaminations are present; however, studies show that there are heat damage scenarios where
there is a loss in residual strength without crack formation or delaminations in the laminate
(reference 4). This effect, where there are strength reductions not detectable by current
nondestructive inspection (NDI) methods, is known as "incipient" heat damage. These
evaluations showed the effectiveness as well as the limitations of current heat damage
assessment techniques and the need for better, more accurate, nondestructive assessment
methods.

Graphite/epoxy composite structures can, in some cases, survive (with some damage) very brief
exposures to temperatures in excess of the decomposition temperature of the epoxy (reference 5).
Heat transfer limitations can offer some protection during short-time exposures, especially if a
porous char layer forms, or if blistering or delamination occurs, or if gas evolved from the outer
surface carries away sufficient heat to protect the inner plies (reference 6). To better understand
these observations and to investigate the mechanisms of heat damage, information on the
chemical mechanisms and kinetics of degradation is needed. Thermal analysis and spectroscopy

1
NAWCADPAX-99-112-TR

have been used to investigate decomposition of composites and matrix resins. Global
degradation kinetics are typically measured by thermal gravimetric analysis (reference 7). Two
Thermal Gravimetric Analyzer (TGA) methods were used by NAWCWD China Lake to measure
weight loss kinetics of epoxy resins; an isothermal method and a dynamic, or constant heating
rate method. Results were compared to give confidence to predictions based on the kinetic
parameters derived from TGA measurements. TGA studies need to be supplemented by
spectroscopic methods that can identify chemical changes and measure kinetics of the loss or
appearance of identifiable chemical functional groups. Infrared spectroscopy has been used to
examine the chemical changes accompanying thermal degradation in epoxies and other resins.
In particular, DRIFT has been used to investigate heat damage in epoxy resin composites
(references 1, 8, and 9).

1.2 SCOPE OF TESTING

As advanced composites are becoming more widely used in naval aircraft, the incidence of heat
damage will continue to increase. Many instances of heat damage have been documented in both
fleet and developmental aircraft. A significant amount of time and money are spent evaluating
the damaged structures. In addition, the large amount of aircraft downtime that results from
investigation and evaluation of heat damage affects fleet readiness. Understanding the
mechanisms of heat damage will allow for more efficient and timely assessment techniques than
are currently available.

This report presents results of work funded by the Office of Naval Research (ONR) to study heat
damage in organic matrix composites. The objective of this work was to evaluate the process of
heat damage, document effects on physical and mechanical properties, and develop a method to
determine composite heat damage.

There are three main efforts documented in this report. The first effort, MECHANISMS OF
LAMINATION PLANE CRACKING, is a study of IM6/977-3 epoxy matrix composites. The
results documented in this section describe the effects of temperatures near the onset of thermal
decomposition of the matrix in varying moisture conditions. This aids in determining the
mechanism that causes cracking and disbonds to occur in a composite exposed to high
temperatures. Thermal and mechanical results of the various exposure conditions are given.
Two nondestructive techniques for detecting heat damage are evaluated, and areas where
mechanical damage occurred but was not identified by nondestructive techniques (incipient heat
damage) are documented.

The second effort, OUTGASSING OF EPOXIES, builds upon the results of the first effort. In
this section, the outgassed products occurring in IM7/8552 epoxy matrix composites during
thermal damage are identified to better understand the thermal degradation process. Identifying
the temperature at which these products were generated led to identifying the mechanism of
incipient heat damage and a possible heat damage assessment technique.

The third effort, STATIC AND FATIGUE MODEL OF UNIDIRECTIONAL COMPOSITES,

presents an analysis of fiber/matrix interface debonding and matrix property degradation due to
high-temperature exposure. The model developed assesses the degree of tensile strength and
tension-tension fatigue life that are lost due to such damage.
NAWCADPAX-99-112-TR

SECTION 2
MECHANISMS OF LAMINATION PLANE CRACKING

2.1 INTRODUCTION

Previous heat damage programs at NAWCAD Patuxent River have shown cracking to occur
between the plies of a composite laminate after high-temperature exposure (reference 4). These
disbonds run parallel to the plane of the laminate. The candidate mechanisms of lamination-
plane cracking have been theorized to be 1) material thermoelastic property (TEP) mismatch, 2)
high thermal gradients, 3) thermomechanical interlaminar stresses, and 4) internal pressure
buildup due to outgassing of volatiles and/or water. One goal of the heat damage effort is to
determine the primary mechanism(s) of lamination-plane cracking. A set of experiments were
performed on neat resin and composite samples to evaluate each of these mechanisms.

Thermal effects on polymer composites show that there are heat damage scenarios where there is
a loss in residual strength without crack formation or delaminations occurring in the laminate.
This type of damage is extremely difficult to detect. In fact, heat damage resulting in a loss of
mechanical strength that has not been accurately detected by any nondestructive technique has
been documented. This effect, where there are strength reductions in composite materials and
where the damage has not to date been nondestructively detectable, is known as "incipient" heat
damage. Incipient heat damage requires further identification. A secondary goal is to define the
temperature and time-at-temperature scenario where "incipient" heat damage occurs.

2.2 MATERIALS

2.2.1 NEAT RESIN

Neat resin samples were prepared by first degassing Fiberite 977-3 resin in a vacuum oven at
35°C (95°F). The resin was then cast in aluminum cake pans and oven cured at ambient pressure
resulting in 2.54 mm (0.1 in.) thick panels. A convection oven was heated to 180°C (356°F) and
the degassed resin was then placed in the oven, brought to temperature, and held for 2 hr. The
ramp rate to temperature was approximately 5°C/min. To prevent sudden exothermic reactions
that were experienced by directly heating to 180°C (356°F), 1 hr temperature holds were
incorporated into the cure cycle at 100°C (212°F), 120°C (248°F), and 140°C (284°F). The neat
resin panels were subsequently cut into 7.62 x 2.54 x 0.25 cm (3 x 1 x 0.1 in.) coupons.

2.2.2 COMPOSITE LAMINATES

Composite laminates were made from Fiberite IM6/977-3 unidirectional prepreg material
containing 64% fiber volume content. Sixteen-ply unidirectional [Ojjg and quasi-isotropic
[0,±45,90,90,±45,0]s laminates were hand laid-up using unidirectional prepreg and autoclave
cured to Fiberite specifications. After cure, the laminates were cut into 7.62 x 2.54 x 0.25 cm
(3 x 1 x 0.1 in.) coupons.
NAWCADPAX-99-112-TR

2.3 EXPERIMENTAL PROCEDURE

2.3.1 ENVIRONMENTAL CONDITIONING

The samples were conditioned before thermal exposure to yield dry, ambient stored, and
saturated coupons. Drying was performed in a convection oven at 38°C (100°F) until no
appreciable weight loss occurred. The ambient samples were stored in open air at prevailing
(ambient) conditions. The saturated samples were held in boiling water according to the
ASTM D 570-81 testing procedure.

2.3.2 THERMAL EXPOSURE

The conditioned specimens were thermally damaged in a high-temperature furnace. The furnace
was heated to a known temperature, and coupons were then placed in the furnace. The coupons
were subsequently removed after a period of either 5, 20, or 45 min. Furnace temperatures of
274°C (525°F), 302°C (576°F), and 329°C (623°F) were used. These times and temperatures of
exposure were selected based upon a set of preliminary exposures at a wide variety of conditions.
The intent of the selected time/temperature exposures was to yield samples that exhibited all
forms of lamination-plane cracking, from no damage to extreme damage. Upon removal from
the furnace, the samples were air cooled to room temperature. Table A-8 identifies the moisture
condition of the specimens before heating and the temperature and time-at-temperature coupon
exposure conditions. All samples were stored in open air ambient conditions after heating.

2.3.3 SAMPLE NOMENCLATURE

The convention used to identify each individual sample should be explained. Table A-8
identifies each sample and the exposure conditions. These exposure conditions defined the
sample name.

The first character in each sample name identifies the laminate type. There are three different
characters in this position, a 9, U, or Q. The "9" stands for a 977-3 neat resin sample. A "U" in
this position means it was a unidirectional sample, and a "Q" denotes a quasi-isotropic sample.

The next three characters identify the temperature, in degrees Fahrenheit, of the exposure. There
are three different numbers in this position, 525, 576, or 623.

The next two numbers identify the exposure time at the particular temperature. The three times
are 5,20, or 45 min.

The last character in the sample's name identifies the environmental exposure prior to heat
damage. The three letters in this position are either "S," "A," or "D." "S" stands for a saturated
sample, "A" for ambient, and "D" for dry.
NAWCADPAX--99-112-TR

For example, there is the sample identified as 9-525-05-S. The "9" means that it was a 977-3
neat resin sample, exposed at "525" °F, for "5" min, and was fully saturated ("S") before heat
damage.

2.3.4 THERMAL GRAVIMETRIC ANALYSIS

TGA testing was conducted on a TA Instrument Model No. 2950. The temperature in the
furnace, with the sample mounted, was first raised to a temperature of 30°C and allowed to
equilibrate. Then the temperature was ramped to 900°C at 10°C/min. A sample size of 6-8 mg
was used for each run; one run was performed on each exposed sample.

2.3.5 DIFFERENTIAL SCANNING CALORIMETRY

Differential Scanning Calorimetry (DSC) testing was conducted on a TA Modulated DSC

Instrument Model No. 2920. The temperature in the DSC cell, with the sample mounted, was
ramped from room temperature to 300°C at 5°C/min. Typical sample size was 10-11 mg. The
modulation temperature was ±1°C at a rate of 60 sec/cycle. One run was made on each exposed
sample.

2.3.6 VISUAL INSPECTION

Visual inspection was performed on the samples. Damage in the semitransparent neat resin
samples was clearly visible when back-lighting was used. See section 2.4.5 for results.

2.3.7 ULTRASONIC INSPECTION

Ultrasonic testing was performed on a TechTrend International laboratory scanner using Arius II
software. Scanning of the samples was performed using a 10 dB gain level and a 5 MHz
concave transducer with a 5.08 cm (2 in.) focal length. Index and scan increments were 0.127
cm (0.05 in.) at a rate of 15.24 cm/sec (6 in./sec).

2.3.8 THERMOGRAPHIC INSPECTION

Thermographic testing was performed on an Ambervu infrared imaging system located 46 cm

(18 in.) from the coupons. Inspection of the samples was performed using two flash heat lamps,
each 2,400 ws, located 61 cm (24 in.) from the sample. Images were taken at 217 frames per
second focusing on every seventh frame, resulting in 200 frames of data.
NAWCADPAX-99-112-TR

2.3.9 FOUR-POINT FLEXURE TEST

Flexural testing was performed according to ASTM Standard D 790-86, "Flexural Properties of
Unreinforced and Reinforced Plastics and Insulating Materials." Four-point loading at one-third
point was used. The support span was 4.1 cm (1.6 in.) with a span-to-depth ratio of 16:1. The
tests were conducted on an Instron test machine at a cross-head rate of 1.27 mm/min
(0.05 in./min).

2.4 RESULTS AND DISCUSSION

2.4.1 EXPERIMENTAL DESIGN

This study was designed for two purposes, to evaluate the mechanisms of lamination plane
cracking and to determine the effect of absorbed moisture in heat damage. Temperatures in the
range of incipient heat damage were chosen to determine the effectiveness of nondestructive
techniques to evaluate this type of damage. As such, temperatures approximately 50°C to 100°C
below the onset of the polymer matrix decomposition temperature were chosen, and the samples
were exposed for 5 to 45 min. Three sample sets were evaluated, one set of cured neat resin
samples and two composite laminate configurations - unidirectional and quasi-isotropic. The
neat resin samples were used to isolate the TEP mismatching, which occurs in composite
laminates, from the other variables being studied. To provide a range of samples to test the
effect of absorbed moisture, the samples were treated under dry, ambient, and saturated
environmental conditions. Table A-8 identifies the various coupon configurations. After
exposure, the samples were evaluated using thermal gravimetric analysis and DSC. Three
nondestructive methods were used to assess the degree of damage resulting from the thermal
treatments: visual inspection, ultrasonic inspection, and thermographic inspection.

2.4.2 ENVmONMENTAL CONDITIONING

Table A-l lists the neat resin samples and their weight before and after saturation. Table A-2
lists the neat resin samples and their weight before and after drying. Tables A-3 through A-6
similarly list the weights before and after conditioning of the unidirectional and quasi-isotropic
samples. Table A-7 shows the average weight loss or weight gain for the different sample
groups. The neat resin samples gained an average of 4.2% in weight during the conditioning
compared to the composite samples in which the unidirectional samples gained 0.98% in weight
and the quasi-isotropic ones gained 0.84% over the 25 days of conditioning. The neat resin
samples lost an average of 0.63% in weight during the conditioning compared to the composite
samples in which the unidirectional samples lost 0.29% in weight and the quasi-isotropic
samples lost 0.32% over the 10 days of drying. The fiber volume content of the composite
laminates is the cause for the large difference between the neat resin and the composite samples.
Figure B-l shows the weight gain or loss during conditioning of the 977-3 neat resin samples.
Initially, weight gain or loss occurs rapidly and then levels off until equilibrium is reached. For
the saturated samples, equilibrium was reached in 25 days. Equilibrium was reached in 10 days
during drying.
NAWCADPAX-99-112-TR

2.4.3 THERMAL GRAVIMETRIC ANALYSIS

Thermal decomposition versus temperature was determined in order to correlate both the
temperature of thermal decomposition initiation (defined as the temperature where 95% of the
original weight remains) and the temperature where the maximum rate of decomposition occurs
for the different heat damage scenarios. Figure B-2 is a typical TGA plot showing the percent
weight loss versus temperature for a neat resin sample. The neat resin sample in this figure was
first saturated (section 2.3.1) and then thermally damaged at 274°C (525°F) for a period of
5 min. The onset of thermal decomposition is measured as 357°C. The first derivative of the
temperature versus time curve can be calculated resulting in a new curve also shown in
figure B-2. The peak of the derivative curve occurs at 420.6°C, indicating that this is the
temperature where the maximum rate of decomposition is occurring. These measurements were
taken for each of the samples in this study. The TGA plots for every sample are presented in
appendix C. Table A-9 summarizes the results of thermal decomposition initiation and the
temperature where the maximum rate of decomposition occurs for the different heat damage
scenarios for the 977-3 neat resin. Similarly, tables A-10 and A-l 1 represent similar data for the
unidirectional and quasi-isotropic samples, respectively.

Figure B-3 summarizes the results of the onset of decomposition for the neat resin samples. This
graph has the onset temperatures grouped according to the heat damage temperature. Comparing
the results for the 525 °F exposures, it can be seen from this graph that the dry and ambient
samples' onset of decomposition temperature stays constant. The saturated samples' onset of
decomposition temperature increases with time for the 525°F results. Note that the 5 min
exposure value is 357°C and increases to 386°C as the exposure time increases. A similar trend
is observed in the 576°F grouped samples; however, the values for the dry and ambient
temperatures increase to a smaller extent with the 20 and 45 min exposed samples. The 623 °F
exposed samples do not show a significant trend. This could be due to the higher temperature
exposure of this group. Figure B-4 compares the same data, but groups the samples by similar
time of exposure as opposed to temperature of exposure. Again, the shape of the saturated
samples' curve is vastly different from the dry and ambient curves. Both of these representations
of the data show that the onset of decomposition temperature has increased with both increasing
temperature exposure and time exposure.

Figures B-5 and B-6 present the data for the temperature reflecting the maximum rate of weight
loss for the neat resin. Figure B-5 groups the data by exposure temperature showing increasing
time, and figure B-6 groups the data by exposure time showing the effects of increasing
temperature. These two charts reflect no significant trend.

The results for the unidirectional and quasi-isotropic laminates are shown in figures B-7 through
B-14. Again, no trend can be observed in the temperature at which the maximum rate of weight
loss occurs. But, the onset of decomposition temperature data shows that this value increases as
the temperature exposure or the time of exposure increases. The highest temperature exposure,
623°F, shows the largest scatter in the data.
NAWCADPAX-99-112-TR

2.4.4 DIFFERENTIAL SCANNING CALORIMETRY

DSC was used to monitor the heat flow through the damaged sample and measure the residual
exotherm. From these data, it is possible to derive the glass transition temperature (Tg) and the
degree of conversion for the materials.

Figure B-15 shows the results from the degree of conversion measurements. This graph presents
data from the dry neat resin samples. To derive the degree of conversion for a sample, the
residual heat of reaction for the sample is correlated to the heat of reaction for an uncured
sample. A standard value of 300 J/g was used for the uncured resin. For comparative purposes,
this value suffices. As is shown on the graph, the specimens heat damaged at the 274°C
temperature exhibited further curing as evidenced by the increased degree of conversion from
95% for the 5-min exposure to 98% for the 20-min exposure and to 99% for the 45-min
exposure. The higher temperature exposures reveal a fully cured network at greater than 99%
degree of conversion.

Results of this increase in degree of conversion can be seen in the Tg measurements. The dry Tg
measurements are presented in figure B-16. The data show that the 274°C exposed samples
experience an increase in Tg with increasing exposure time rising from 200°C to 219°C, and this
is attributed to a postcure resulting from the thermal exposure. This is not experienced in the
higher temperature exposed samples. Both the 302°C and the 328°C exposed samples
experience a decrease in Tg. The 328°C samples degrade much faster than the 302°C samples.
The same trend was observed with the ambient conditioned samples. Figure B-17 presents the
results for the saturated samples. These results differ from the dry conditioned samples in that
all three temperature exposures for the saturated samples exhibit degradation, with the higher
temperature exposed samples showing more degradation than the lower temperature exposed
samples. Comparing figure B-16 to figure B-17, note the 274°C exposed Tg values. The 5-min
saturated exposure value clearly indicates an increase in Tg from an undamaged resin state. This
increase, which occurred over a 5-min span, is a larger increase in Tg than was experienced by
the dry sample exposed for 45 min at the same temperature. This is an indication that absorbed
moisture accelerates the postcure process when the time/temperature exposure is not great
enough to cause matrix degradation.

2.4.5 VISUAL RESULTS

The semitransparent nature of the neat resin lends itself to visual evaluation of the effects of the
temperature exposure on the polymer. Figure B-18 shows all of the coupons as they appeared
after thermal exposure. The unidirectional and quasi-isotropic coupons are shown in
figures B-19 and B-20, respectively. Figure B-21 shows three of the neat resin coupons after
thermal exposure. These coupons were saturated at 5-min time exposures with increasing
temperature exposure from the top of the figure down. The figure shows that the amount of
voids increase as exposure temperature increases. Using back lighting to aid the examination,
observations of void formation after heating were noted and are documented in figure B-22. The

8
NAWCADPAX-99-112-TR

degree of damage was then qualitatively rated as either having no damage, some to moderate
damage, or being completely damaged, figure B-24. As the temperature and time-at-temperature
increased, the degree of damage increased, but no visible damage was observed at the low
temperature and short time-at-temperature exposures. Also noteworthy is the comparison of the
ambient and dry conditions showing similar behavior, which is not surprising since their
moisture content are approximately equal. Typical damage modes observed are shown in
figures B-21, B-22, and B-23. Note the striation marks in figure B-22 indicating stress buildup
initiating in the middle of the resin and continuing to the surface. This spalling damage mode
was observed in all neat resin samples. As has occurred in this example, a piece of the neat resin
coupon was ejected during thermal exposure. The manifestation of this phenomena in composite
laminates is shown in figure B-23. The fibers contained within the matrix prevent the laminate
from spalling like the neat resin, and instead the damage mode is delamination.

2.4.6 ULTRASOUND AND THERMOGRAPHY INSPECTION

Ultrasonic and thermographic scans were made on each of the specimens. Signal attenuation in
the sonograms indicated damage from the thermal exposure. Figure B-25 shows a typical
ultrasonic c-scan for the saturated neat resin samples. All of the saturated samples are shown
and labeled in this figure. Similarly, all of the dry neat resin and ambient conditioned neat resin
c-scans are shown in figures B-26 and B-27, respectively. Figures B-28 through B-33 show the
results for the unidirectional and quasi-isotropic laminates. The c-scans were then rated by
estimating the percent of the total area that exhibited defects, as noted by decibel loss. This
grading system uses 25% increments in an effort to develop a tool for qualitatively comparing
the c-scan results with the visual, mechanical, and other evaluation techniques used in the
project. It also provides a way to determine overall trends in the c-scan data. Samples with less
than 25% inhomogenieties were classified as undamaged and greater than 25% were rated as
damaged to some degree. Samples with deterioration so extensive that they could not be
evaluated by these techniques were noted as totally damaged. This was done to distinguish intact
100% damaged samples from those that had entirely lost their structural integrity. The results of
this scheme are shown in figure B-43.

Note according to this evaluation protocol, ultrasound inspection indicated no detectable damage
at the lower temperatures and the lower time-at-temperature exposures for the dry and ambient
stored samples. Again, the dry and ambient conditioned samples were comparable for the most
part due to the fact that there is not an appreciable difference in their moisture content. The
saturated samples did tend to show damage under any time/temperature condition except at the
lowest temperature/time exposure of 5 min at 274°C. These ultrasonic results correlate well with
the visual results as shown in section 2.4.5 for all sample types. It is also apparent that the higher
degrees of damage were detected as temperature, time at temperature, and moisture content
increased.
NAWCADPAX-99-112-TR

The results of the thermography inspections are rated in the same fashion. The thermography
results are given in figures B-34 through B-42. Figure B-44 is the rated figure of the
thermography scans similar to figure B-43 for the ultrasonic c-scans. The general trends are the
same as those found by ultrasound inspection, damage detection increases with temperature, time
at temperature, and moisture content. However, the results of the saturated samples for the
unidirectional and quasi-isotropic materials yielded unusual results. The c-scan results show
those sample groups to be extremely damaged although the thermography results show little
damage for any of the coupons. Perhaps the extent of damage in these samples hindered
penetration of heat and thus effected detection by thermography in the most severely damaged
samples or perhaps they were uniformly damaged.

2.4.7 FOUR-POINT FLEXURE TEST

Limited mechanical testing was conducted on the specimens after all other testing was
completed. Flexure testing was conducted on the specimens to see if any trends could be
established. It must be noted that the flexure testing results are based on one sample at each heat
damage condition and, therefore, the results are not statistically based, but define trends in the
data. The flexure test was chosen because resin properties are assumed to degrade faster than
fiber properties under the influence of heat, and a flexure test is a matrix dependent property.
Table A-12 gives the results of the four-point flexure test for the neat resin samples. Similarly,
tables A-13 and A-14 give the results for the unidirectional and quasi-isotropic coupons.
Included in these tables are the physical dimensions of each coupon, the peak load that was
reached during testing, and the corresponding flexural strength. Note that in table A-13 many of
the unidirectional tests were aborted. This was due to the fact that the peak load needed to break
the specimen was greater than the limit of the load cell on the test machine. Figure B-45 is a
graphical representation of the flexure strength for the saturated neat resin samples. A large
decrease in Tg is observed from the 5-min 274°C saturated neat resin exposed sample to both the
20- and 45-min exposed samples. The same trend was observed in the 302°C sample set. The
highest temperature exposure, 329°C, exhibits total flexural strength loss immediately from the
5- to the 45-min exposure. These data demonstrate that greater temperature exposure leads to
greater structural damage in the resin. Figures B-46 and B-47 give the results for the dry
exposed and ambient exposed neat resin samples, respectively. These two graphs are almost
identical with little difference between the dry and ambient exposed samples, as is demonstrated
with all the other evaluation methods. It must be noted that the 329°C 20- and 45-min exposed
samples from each of these two groups have zero values for their flexural strength. As noted in
table A-12, these samples completely crumbled upon removal from the high-temperature furnace
after heating and, therefore, no sample was available to test. This also happened for the 329°C
45-min saturated sample. The 274°C exposed sample shows an increase in flexure strength from
the 5-min exposed sample. This could be explained by the increase in Tg that was experienced
by these samples. Figures B-48, B-49, and B-50 are the results for the quasi-isotropic coupons.
The same trends are observed as were shown in the neat resin samples.

10
NAWCADPAX--99-112-TR

Flexural strength decreased very significantly in most cases with increases in temperature, time
at temperature, and moisture content, which is very consistent with the damage detected by the
above inspection techniques. Some of the exposures evidenced loss in flexural strength when the
damage detected by NDI was either minimal or borderline. This was observed in the case of the
dry and ambient conditioned samples. The saturated samples almost immediately experienced
significant loss in flexural strength when compared to the decrease in the dry and ambient
results.

The test matrix chosen for this study does not allow comprehensive analysis and correlation with
the degree of damage detected by the above techniques; however, the results do illustrate some
very definite trends when the decrease in flexural strength is compared to the inspection results.

2.5 CONCLUSIONS

The visual results revealed that at the 274°C temperature, no damage occurs at any of the time
periods for either the dry or ambient samples. The 5-min exposure time yielded no visible
damage at any of the temperatures for the dry or ambient samples. The saturated samples did
show spalling in the neat resin at both the 20- and 45-min 274°C exposures and at the 5-min
exposure for the 302°C and 3289C temperatures. From this and the results from other inspection
techniques, it was concluded that internal pressure from volatiles and/or trapped moisture was
the primary degradation mechanism in the samples over the temperatures and times studied. All
of the samples showed the trend of increasing damage with both increasing temperature and
time-at-temperature exposures. The Tg of the dry samples at the 274°C exposure increased. This
increase is attributed to a post cure. All other samples showed a decrease in Tg when compared
to the undamaged samples. All tests showed that the dry and ambient conditioned samples
exhibited almost identical behavior, most likely due to the small difference in moisture content
between them. All tests revealed that the saturated samples exhibited degraded properties much
earlier and much more severely than the dry/ambient samples. Ultrasonic inspection was capable
of detecting heat damage that induced blistering, ply delaminations, and void formations.
However, NDE techniques were not capable of detecting changes in samples that showed
degradation of other properties.

11
NAWCADPAX-99-112-TR

SECTION 3
OUTGASSING OF EPOXIES

3.1 INTRODUCTION

This study focuses on developing a technique to detect and estimate heat damage in a
graphite/epoxy composite composed of Hexcel 8552 resin by STA-FTIR technique.
Simultaneous Thermal Analyses (STA) performs DSC and TGA procedures simultaneously.
DSC provides heat flow characteristics while TGA measures weight loss, both as a function of
temperature and time. FTIR identifies the presence of specific molecular groups or bonds by
their absorption of energy in the infrared range. Combining the three techniques allows
simultaneous quantification and identification of evolved decomposition products as a function
of weight loss, time, and temperature.

3.2 EXPERIMENTAL

3.2.1 MATERIALS

Sixteen-ply quasi-isotropic composite laminates were made from Hexcel IM7/8552

unidirectional prepreg material. The laminates were hand laid-up and autoclave cured according
to Hexcel specifications. The laminate ply layup is [0,±45,90,90,±45,0]s

3.2.2 THERMAL EXPOSURE

The laminates were thermally damaged using a high-temperature platen press. The lower surface
of the press was first heated to 315°C (600°F), and the laminates were then placed on the heated
surface. The laminates were thermally damaged for either 5, 20, or 45 min. Upon removal from
the press, the samples were air cooled to room temperature. All samples were stored in open air
ambient conditions after heating.

3.2.3 SIMULTANEOUS THERMAL ANALYZER

Thermal gravimetric experiments are performed with a Rheometric Scientific Instrument

"Simultaneous Thermal Analyzer 625" (STA). STA consists of a DSC and a TGA. The system
is calibrated for the base line, sample temperature, balance and furnace temperature. The TGA
furnace is equipped with a heated transfer line to the gas cell in the FTIR instrument. The
analysis is performed under dynamic and isothermal conditions to measure the kinetic
parameters of thermal decomposition. The heating rates for the dynamic runs are 3, 5, 10, 15,
and 20°C/min from room temperature to 550°C. The isothermal condition is reached by a rapid
heating rate of 60°C/min to the isothermal temperatures at 290, 300, 310, 320, 330, 340, 350,
360, and 370°C. The temperature of the transfer line and the gas cell is controlled by the gas cell
controller. The temperature of the gas cell is kept at 200°C and the transfer line at 155°C. The
composite sample was cut in thin slices by a water-cooled, diamond-bladed saw and then into

12
NAWCADPAX-99-112-TR

smaller pieces using scissors. The weight loss is measured by using 13 to 17 mg of crushed
composite material in an aluminum pan. The sample was purged with high-purity nitrogen gas
(99.998%) for 30 min before and during the analysis at a flow rate of 50 ml/min. Five samples
were analyzed at each condition.

3.2.4 FOURIER TRANSFORM INFRARED SPECTROSCOPY

The Nicolet 560 Magna FTIR Instrument in line with the STA system was used to obtain the
FTIR spectra of the evolved gases from the heated composite sample. The instrument is
equipped with an MCT-B liquid nitrogen cooled detector. The transfer line and the gas cell are
purged with nitrogen gas at a flow rate of 50 ml/min. The gas cell compartment is purged with
nitrogen gas at a flow rate of 100 SCFH for 10 min before the run and then reduced to 30 SCFH
during the run. A background spectra is collected before each experiment at 128 scans and
4 cm"1 resolution. The correction for carbon dioxide (CO2) gas and water moisture, as
determined by the background spectra, is programmed and automatically subtracted from the
final results. The sample spectra are collected every 30 sec at 32 scans per spectra at 4 cm"1
resolution. The Gram-Schmidt chromatogram is recorded for all experiments. The Gram-
Schmidt measures the total gases evolved as a function of time.

3.3 RESULTS AND DISCUSSION

The samples were studied under both isothermal and dynamic conditions in the TGA cell.
During these runs, the outgassed products were transferred to the FTIR cell and analyzed.
Figure B-51 shows the weight loss measurement of undamaged 8552 resin from the TGA
instrument as a function of temperature. The TGA data show a one-step weight loss of 20%
during the dynamic run from room temperature to 550°C at 10°C/min. Figure B-52 shows the
Gram-Schmidt chromatogram for this dynamic run. At approximately 25 min into thermal
decomposition, corresponding to an STA cell temperature of 280°C, evolution of gasses were
indicated. This corresponds with the TGA weight loss analysis in which weight loss begins at
approximately 280°C.

The evolved gases of 8552 resin during heating were identified by FTIR as CO2, carbon
monoxide (CO), water (H20), carbonyl sulfide (COS), acid anhydride (R-CO-O-CO-R), and
phenol (C6H5-OH). The decomposition products appear in two stages, first at 280°C and then at
340°C. Figure B-53 shows the FTIR spectra for the evolved gasses of 8552 resin at 290°C. This
is during the first stage of thermal decomposition and consists of CO2, CO, H2O, and R-CO-O-
CO-R. This grouping of evolved gasses continues from 280°C to 340°C. Table A-15 provides a
listing of the associated vibrational frequencies used to identify these products. The FTIR data
show three carbonyl groups at 1725, 1759, and 1790 cm"1 frequencies during the first stage of
decomposition. The possible identification of the carbonyl groups are acid anhydride and ester.
At 340°C, a second grouping of evolved gasses begins. Figure B-54 is a spectrum collected at
350°C identifying this stage, and consists of COS and C6H5-OH. Figure B-55 is a comparison

13
NAWCADPAX-99-112-TR

of the FTIR spectra for 290°C, 350°C, and 500°C showing how the peaks change between the
two stages. Note that the 500°C spectra is similar to the one at 350°C, indicating that the second
phase is the final phase of decomposition.

The first stage of decomposition causes up to 8% weight loss, as observed during an isothermal
TGA run at 330°C (table A-16). Figure B-56 is a TGA plot showing the total weight loss
percent associated with 8552 resin at isothermal temperatures ranging from 300°C to 370°C.
This amount of weight loss causes the mechanical properties of the composite to greatly decrease
(section 2.4.7). In section 2, MECHANISMS OF LAMINATION PLANE CRACKING, it was
shown that incipient heat damage occurs at temperatures near the onset of thermal
decomposition, which occurred in the 274°C and 302°C exposed samples in that study.
Therefore, this first stage of thermal decomposition characterizes heat damage situations that
induce incipient heat damage. This is the most difficult heat damage to detect nondestructively
because there is no visible damage, and delaminations in the composite do not occur due to the
relatively low-exposure temperatures.

To estimate heat damage, the peak height of the carbonyl groups and the C02 peak was tracked
over the temperature range of 290°C to 370°C, see table A-16. Figure B-57 is a graph of the
average peak height versus the TGA isothermal temperature. A good correlation is seen in both
the C02 and the carbonyl group peak heights with temperature. There is a definite slope change
for both groups in the range of 330°C to 340°C, which corresponds to the thermal decomposition
mechanism change identified from the FTIR spectra. This correlation can be used to develop a
calibration curve to estimate the heat damage of a composite. To test this approach, data were
collected on thermally damaged composites at 315°C for 5, 20, and 45 min, and analyzed by the
STA-FTIR technique at 330°C isothermal (section 3.2.2). The damaged composite data are
given in table A-17. The peak height/mg of the carbonyl group of the undamaged composite is
measured at 4.25, which compares to the damaged group with peaks of 3.92, 3.53, 2.91 as
damage time increases from 5 to 45 min and is plotted in figure B-59. There is not a good
correlation with the C02 peaks. A linear regression was plotted through the carbonyl data with
an R2 value of 0.978. By developing calibration curves, STA-FTIR has the capability to track
heat damage and to estimate the amount of heat damage in a composite.

3.4 CONCLUSIONS

Analysis of Hexcel IM7/8552 composite material by STA/FTIR shows two distinct stages of
degradation, beginning at 280°C and then at 340°C. The outgassed products of the first stage of
thermal decomposition consist of C02, CO, H20, and a carbonyl group identified as either acid
anhydride or ester. This first stage occurs from 280°C to 340°C. At 340°C, a second stage of
thermal decomposition begins and continues for the duration of the decomposition process. The
second stage is characterized by the outgassing of COS and C6H5-OH.

14
NAWCADPAX-99-112-TR

Heat damage can be evaluated by STA/FTIR by correlating the peak heights of the carbonyl
group to exposure temperature. There is the potential to develop a heat damage assessment
technique using STA/FTIR by developing more extensive calibration curves of this type. In
section 2, incipient heat damage was shown to occur near the onset of thermal decomposition.
Stage one of the heat damage process begins at the onset of thermal decomposition of the
polymer; this initial stage results in incipient damage. During stage 2, more severe damage
occurs resulting in delamination and blistering, which are detectable by ultrasonic techniques.

15
NAWCADPAX-99-112-TR

SECTION 4
STATIC AND FATIGUE MODEL OF UNIDIRECTIONAL COMPOSITES

4.1 INTRODUCTION

This section presents an analysis of fiber/matrix interface debonding and matrix property
degradation due to a single step-function of temperature, investigates the mechanisms of damage,
and assesses the degree of tensile strength and tension-tension fatigue life that might be lost due
to such damage.

In the analysis, the fundamental mode of unidirectional fiber composite tensile failure is assumed
to be that of the "chain of bundles" cumulative weakening failure mechanism proposed by Rosen
(reference 17) and extended by Zweben (reference 22), McLaughlin and Rosen (reference 14),
Phoenix, et al. (reference 15), McLaughlin (reference 13), and others wherein the "ineffective
length" (unstressed fiber length encompassing a fiber break) and appropriate fiber strength
Weibull probability distribution parameters control structural failure. It is clear from the work of
Zweben (reference 20), Zweben and Rosen (reference 23), and Zhou and Curtin (reference 19),
for example, that other mechanisms than cumulative weakening can be operative during
composite tensile failure, most notably a transverse fiber break propagation mode caused by
adjacent fiber overstress near single or multiple fiber breaks. However, it has been shown
(Zweben, reference 21) that the cumulative weakening mode is an upper bound to failure and
may be a good representation for glass/polymer and graphite/polymer composites with weak
interfaces (Hahn, reference 12).

The cumulative weakening model has been modified (McLaughlin, reference 13) to include a
linear elastic fracture mechanics micromechanics model of the growth of fiber disbonds and
hence ineffective length with both increasing quasi-static load and number of cycles of constant-
amplitude tension-tension fatigue load. The ineffective length damage growth model was
combined with Weibull fiber failure statistics to obtain a predictive tool for determining either
the life or the residual strength of a unidirectional fiber composite under any combination of
static or variable amplitude tension-tension fatigue loading. This work adds the effects of
thermal stress, residual and otherwise, to the analysis and, using temperature-dependent material
properties, predicts the reduction in static strength and fatigue life that might occur as functions
of the applied temperature and time at temperature.

16
NAWCADPAX--99-112-TR

4.2 CUMULATIVE WEAKENING WITH THERMAL STRESSES

4.2.1 CUMULATIVE WEAKENING AND CHAIN-OF-BUNDLES MODEL

In the cumulative weakening mode of tensile failure, a unidirectional composite is considered to

be a series chain of links composed of short lengths of dry fiber bundles. In the latter mode,
bundle strength is dictated by fiber strength (s) versus length (8) statistics that can be expressed,
for example, by the Weibull cumulative distribution function (oc,ß are constants):

F(s) = 1 e"85" (1)

which results in bundle strength 5/of

Sf = (aße8)J/ß (2)

In a composite, the effective bundle length, 8, is the ineffective length, which is the distance
from a fiber break over which the fiber is ineffective in carrying tensile load (figure B-60).
Remaining fibers in the bundle "link" of length 8 are assumed to share equally the broken fiber's
load as if they were in a dry bundle ofthat length. Until fiber stress is high enough to initiate and
propagate a crack in the fiber/matrix interface, the ineffective length is assumed to equal the
length 8# of an equivalent step function of zero stress extending in either direction from the fiber
break (figure B-61). This elastic ineffective length 8^ has been computed with a shear-lag
analysis in McLaughlin (reference 13) for a broken fiber in a hexagonal array of intact fibers that
have been "smeared" into an equivalent ring of surrounding fiber material (figure B-62):

ÖE /d = (l/2)pEf \n(d'/d)/Gm (3)

where Ef is fiber axial Young's modulus, Gm is matrix shear modulus, d is fiber diameter, and
d' = 2r' is inner diameter of intact ring. Once an average shear-lag shear stress of T is exceeded
at the crack tip (shown in McLaughlin, reference 13, to be equivalent to exceeding a critical
mode II energy release rate of Gnc), the crack propagates and the ineffective length becomes
equal to 8^ + 2a. In the cracked region, due to friction and/or mechanical interference, the shear
stress may maintain a constant value of T\T where TJ , the post-failure shear stress fraction, is
between 0 and 1.0. The ineffective length 8 as a function of applied far-field of fiber stress O/o
following fiber/matrix crack initiation at a fiber stress sj is shown in McLaughlin and Rosen
(reference 14) to be:

(<7f
S= SE +2a = 8E + ° SJ)d ; sr = 2T8E/d (4)
2r\T

17
NAWCADPAX-99-112-TR

As composite stress ac increases and, with it, fiber far-field stress G/o, the ineffective length
increases until the bundle strength Sf , given by equation (2), reduces to G/o. Equating
equation (2) solved for 8 to equation (4) with Sf in place of <5ß will give the fiber stress Sf at
composite failure, which in turn gives composite failure stress Sc from

Sc = SfEc/Ef (5)

McLaughlin (reference 13) developed a procedure for using the cumulative weakening model to
predict fatigue life and residual strength under any history of tension-tension composite axial
stress. If a Paris-type crack growth equation is applicable for the fiber/matrix interface, it can be
shown that the resulting rate of crack extension with cycles N as a function of amplitude fiber
stress AGJO is

da ,„ „ ,„
— = Ca(A<Jf0r (6)

and the growth of ineffective length with number of cycles for constant amplitude stress becomes

5 S, = Ca(Aaf0)m(N NO (7)

where CCT and m are constants from the Paris equation, and 8,- and Nt are the preexisting
ineffective length and total number of cycles, respectively, before a block of cycles at fiber stress
amplitude A<jyo.

The growth of ineffective length with static loading, equation (4), and constant-amplitude fatigue
loading, equation (7), are sufficient to determine the ineffective length that will occur under any
history of static and cyclic tension-tension stresses. The first instance where the ineffective
length reaches a value

Sf = Os0rJ (8)
~^e

at the same time the maximum fiber stress level is at Cßmax causes the composite to fail. Several
examples of this that include fatigue strength versus cycles (S/N) curve determination under
constant-amplitude loading and residual strength after a history of cyclic stressing are presented
in McLaughlin (reference 13).

4.2.2 CUMULATIVE WEAKENING WITH THERMAL STRESSES

The difference in thermal expansion properties of the fiber and matrix usually causes residual
thermal stresses in each phase. These stresses have not been included in the preceding analysis,
and it is important to determine their effect upon strength and fatigue life. Also, when subjected
to elevated temperatures, the properties of the matrix, fiber/matrix interface, and fiber change.

18
NAWCADPAX-99-112-TR

Therefore, high temperatures may cause damage in the composite because of stresses created due
to thermal expansion and the modified properties that affect the damage development. This
section includes thermal expansion in the cumulative weakening analysis .

Let To be the stress-free temperature (approximately the cure temperature) of a composite. The
composite is at instantaneous temperature T with the resulting temperature difference from the
stress-free-state being AT = T - T0. The composite (c), fiber (/), and matrix (m) are each
assumed to be represented by one-dimensional constitutive laws between stress F, strain e, and
temperature difference (oc is linear thermal expansion coefficient):

£i = Oi/Ei + at AT , i = c, f, or m (9)

Let the axial coordinate along a fiber be x with origin at a fiber break (figure B-61), axial
displacement be u(x), cross-sectional area be A, and subscripts c,f, and m refer to composite,
fiber, and matrix, respectively. The matrix has a shear modulus of Gm , and x(x) = Gm y(x) is the
shear stress at the fiber/matrix interface due to the shear-lag engineering shear strain y. Force
equilibrium in the ^-direction in the cracked and uncracked regions becomes, using 8/= duf/dx,

d2Uf
Ef Af =-?£ - T)Tml = 0, 0_x_a
dx2
(10)
Uf U
Ef As ^rf - x{xm = 0, T(X) = 2Gm ~ ' , a.
dx2 df ln(d/d)

To obtain Uf , these equations are integrated using uc — £<>* and the boundary/continuity
conditions

dus _ n
U
, —x = 0 —
dx
dus nn
-^-*->~ = GOT (11)
dx
us and —- continuous at x = a
dx
where

dor = o> + Ef as AT (12)

and the shear stress at the crack tip is found to be

m
G„
T(a) = [Gar - 4-V[T] (13)
2 Ef Md'/d) d

19
NAWCADPAX-99-112-TR

A comparison with McLaughlin (reference 13) shows that the difference between formulations
with and without thermal expansion is in the constitutive equation (9), the appearance of the term
COT in place of O/o in equation (13) and subsequent developments, and the variation of material
properties with temperature.

4.2.3 ISOTHERMAL STATIC STRENGTH AND FATIGUE LIFE

The growth of ineffective length with monotonic increasing fiber thermomechanical tensile
stress COT becomes

ö= SE+ (OOT ST)d ST =

2rfT

where &E remains unaffected by temperature and is still given by equation (3). Composite static
tensile strength is determined by first finding fiber stress Sf at failure using equations (2), (12),
and (14), and then computing composite failure stress from

Oc = —Oof- Ec((Xc - (Xf)AT (15)

Ef

with GC = Sc and Sf= o0f. Following McLaughlin (reference 13), the equation for isothermal
fatigue life under constant-amplitude tension-tension cyclic stress is obtained as follows. From
equation (13), it can be shown that the cyclic (maximum minus minimum) component of shear-
lag shear stress Ax(a) under isothermal conditions is proportional to the cyclic component of
fiber stress AG/Q. Therefore, the Paris equation (6) for fiber/matrix crack extension and the
resulting equation (7) for growth of ineffective length remain unaltered. Fatigue failure occurs
when ineffective length (equation (7)) grows and bundle strength given by equation (2) falls to
the maximum applied fiber stress Gßmax, resulting in

^^ 6, = C„(Acrf0r(N Ni) (16)

where 8, is the ineffective length immediately prior to the inception of cyclic loading and Nt is
the cycle number at the beginning of the particular block of cyclic loading defined by <Sßmax and
AGJO.

Two forms of equation (16) are of interest. The first is when the composite is in its virgin state
with no prior fiber/matrix interface damage, and the initial ineffective length is due solely to the
initial half-cycle of fatigue loading given by equations (12) and (14) with Gyo = <Sßmax :

Si = -^(ep™ + EfCtfAT - ST) (17)

20
NAWCADPAX-99-112-TR

The resulting fatigue life equation in terms of composite stress is, using equation (15) and
nondimensionalizing,

(a en + OCTIT) - CsOcn ' CgT

= CN(N 1/2) (18)

where

Ocn=0CISe

f \P+I

Cs=aße (19)
2r]T yEc c
j

CN = ccßeC(
KEc J
\ß
CST = aße (EfacAT-sT) + 8E
2r]T yEc C
J

The other form of equation (16) occurs when the composite is not in its virgin state due to prior
cyclic loading or static stressing to a level above the current cyclic stress. Then 8,- and JV,- have
predetermined values, and 8,- is not a function of Oßmax . In this case, equation (16) becomes

(aen + Gcrir) - C&

= CN(N Ni) (20)
1
ACTcn"

with

r
Ef Y (21)
C& = SiCcße
\Ee J

4.3 HEAT DAMAGE IN UNIDIRECTIONAL GRAPHITE/EPOXY COMPOSITES

4.3.1 MATERIAL-RELATED HEAT DAMAGE PROCESSES

In the temperature range from 20°C to 600°C, fiber properties do not change significantly. On
the other hand, matrix and fiber/matrix interface properties and those composite properties that
they affect will change significantly with temperature. Tests have been carried out by the

21
NAWCADPAX-99-112-TR

authors and others (references 1 through 11) on neat epoxy resin and graphite/epoxy composites
showing that:

a. Increasing temperature causes reductions in stiffness and strength properties in

epoxies. If the material is heated to a high enough temperature, there will be
permanent, residual changes. Tests were performed on Hercules 3501-6 and Fiberite
977-3 neat epoxy resin samples using a Rheometrics RDA II dynamic analyzer.
Storage and loss moduli were dynamically measured on a single specimen as
temperature increased from 20°C to above 300°C. Figure B-63 shows the temperature
variation of shear modulus (normalized to 40°C values) for both resins. Note that the
curves are nearly identical. At 300°C, the shear moduli of both resins were negligible
and remained so as the samples cooled back down to room temperature. Upon test
completion, the samples were observed to be severely cracked and oxidized with
significant mass loss.

b. Heat causes damage in the form of micro- and/or macro-cracks to form in the resin,
most probably caused by out gassing of water vapor and organic volatiles (Arafat,
reference 10). Figure B-64 shows c-scans of 25 x 50 x 4 mm 977-3 neat resin samples
subjected to temperatures from 270°C to 330°C for times varying from 5 to 45 min.
Greater darkness indicates greater damage. Figure B-65a shows the spallation cracks
(about 5-mm across) that typically appear in these samples. Figure B-65b is a
photograph of the surface of a laminated woven composite heated to 370°C. The dark
"craters" are holes through which gasses escaped from inside the composite after
causing the specimen to delaminate.

c. All of these phenomena are magnified with increasing time at temperature and
moisture content (see, for example, figure B-64 and Mehrkam, et al., reference 4;
Arafat, reference 10; and Tuttle, et al., reference 18).

In order to predict the static strength and fatigue life of a unidirectional composite with a given
moisture content, there are three material property issues to address. The first is the variation of
properties with temperature as it increases to a given level. These properties will control thermal
damage occurring during the heating process. The second is the degradation of properties as the
temperature is maintained at a given level. Many studies, including those at NAWCAD Patuxent
River on neat resin samples, have shown that greater time at temperature generally produces
more damage. Other work shows that mass loss occurs at elevated temperatures and the loss is
also time dependent. The third issue is whether the heat has permanently altered material
properties at room temperature once the heat has been removed. The altered properties will
affect the manner in which damage grows under mechanical loads following the heat exposure.
The consideration of temperature dependence, time dependence, and residual effects are all
necessary to determine the effects of heat exposure on residual strength and life of the composite.

22
NAWCADPAX-99-112-TR

From a practical standpoint, it will be important to determine the relative importance of the
following two main damage mechanisms:

1. Residual fiber/matrix interface damage may be caused during the heating process that
could manifest itself as an increased initial ineffective length and, therefore, reduce
fatigue life even if there were no residual matrix property alterations. Such damage is
practically impossible to detect in the field using current NDE techniques. If it is
important, such techniques will need to be developed.

2. Matrix property alterations that are nonreversible upon cool down will clearly affect
strength and life. It is necessary to know at which temperatures and for what
application times critical reductions in important material stiffness and strength
properties occur. Most of the important property variations are due to mass loss and
chemical changes, and techniques are under development that may allow surface
chemistry changes to be readily detected in the field and thus assist in determining
heat damage criticality.

4.3.2 THERMAL DAMAGE EFFECTS FOR A PARTICULAR GRAPHITE/EPOXY

SYSTEM

4.3.2.1 General

Test results for T300B, 6000-50B/AralditeLY553 graphite/epoxy from Radhakrishnan

(reference 16) are used in conjunction with data from the literature to estimate a consistent set of
properties for use in the current analysis to study the relative importance of the mechanisms
described above and to quantitatively estimate the effects of thermal history on strength and
fatigue life. A presentation is given here of available data and the methods used to estimate
unavailable properties. The temperature- and time-dependent properties are then used to
determine how much fiber/matrix damage occurs during the heating process. Finally, S/N curves
are constructed that result from thermomechanical damage and altered material properties for
two heat-application scenarios: a short time of less than 5 min and a long time of greater than
Ihr.

4.3.2.2 Time/Temperature Property Variations

Room-temperature properties of T300B, 6000-50B/Araldite LY553 graphite/epoxy from

Radhakrishnan (reference 16) are shown in table A-18. Since the fatigue parameters CN and m
were unavailable, they were calculated from constant-amplitude fatigue data that were presented
in his paper by using a least-squares curve fit and procedures outlined in McLaughlin
(reference 13), but with the current thermal development and a stress-free temperature of 180°C.

23
NAWCADPAX--99-112-TR

For short heating times of 5 min or less, the variation with temperature of Araldite LY553 epoxy
nondimensional shear modulus was assumed to follow that of Fiberite 977-3 since results for the
two resins shown in figure B-63 were so close. Matrix Poisson's ratio was assumed not to vary
with temperature, and Young's modulus was found from Em = 2Gm(l+v). While it is likely that
the epoxy coefficient of thermal expansion will be temperature-dependent, it is likely to be much
less so than the elastic constants as long as the material is not significantly chemically altered,
and was assumed constant here until above 300°C. Tests on both neat resin systems and
graphite/977-3 composites show that at 350°C and higher, the material rapidly ablates or
oxidizes, leaving effectively a bundle of dry fibers in the region to which heat is applied.

For long heating times of 60 min or greater, it was also assumed that matrix thermal expansion
coefficient and Poisson's ratio are unaffected by temperature until the matrix is destroyed. For
shear modulus, it was noted that the resins tested became fluid at a temperature near 300°C and
ablated within the hour, leaving a region of dry fibers. Turtle (reference 18) has shown that
significant mass loss (greater than 2%) and a drop of 80% in matrix-dominated composite
properties occur when composites are exposed to several hours at 260°C. Arafat (reference 10)
found significant mass loss at temperatures of 200°C. Following the data trends in these
references and tests performed under the current program, it was assumed for long-time heating
above 200°C that epoxy shear modulus suffers additional loss (10% at 210°C, 75% at 250°C,
100% at 300°C), and that any property loss is permanent upon cooling to room temperature. The
resulting variation in matrix shear modulus with temperature is shown in table A-19. Note the
differences between long- and short-time at-temperature and residual values.

To estimate the temperature variation of fiber/matrix interface properties, it is noted that (see
McLaughlin (reference 13)) the energy release rate for fiber pullout is primarily mode II and is
proportional to the square of the average shear stress at the crack tip calculated from a shear-lag
analysis of fiber pullout. Therefore, the fiber/matrix interface shear stress T at which a crack
extends is proportional to the square root of the critical mode II energy release rate Guc of the
fiber/matrix interface. Turtle (reference 18) found that, following exposure to 260°C, GIc of
graphite/epoxy panels reduced 7% after 15 min, 40% after 45 min, 33% after 1 hr, and 80% after
a 10-hr exposure. This is consistent with neat resin tests at NAWCAD Patuxent River that also
show a strong time effect and greater matrix cracking and apparent out-gassing effects at higher
temperatures. In addition, test data were examined from 11 unidirectional composite material
systems and from unpublished data from NAVAIRSYSCOM Structures Division and other
sources on the temperature variation of transverse tensile strength, transverse compressive
strength, axial shear strength, and interlaminar shear strength. These are all matrix- or
fiber/matrix-interface-dominated properties that should have similar variations with temperature
as does the shear-lag fracture stress T. The numerical values thus obtained and the results of
Turtle (reference 18) are fairly consistent with the degradation in epoxy shear modulus given
above. As a result, Tis assumed to decrease proportionately with shear modulus.

24
NAWCADPAX-99-112-TR

An epoxy-matrix composite is cured at a temperature of approximately 180°C. When it is cooled

to room temperature, the usually greater thermal expansion coefficient of the matrix will impart
radial normal compressive stress to the fiber/matrix interface. Heating the composite will lessen
this clamping force until at cure temperature, the radial stress at the interface becomes tensile.
This may do several things: the shear stress T at which a crack propagates along the fiber/matrix
interface may decrease because of the added mode I loading; and the cracked interface stress
ratio T| in the cracked region will decrease. As a result, the additional effects of thermal
microstresses must be dealt with.

A constant-axial-strain thermal stress analysis was performed on a three-phase composite

cylinder model consisting of a fiber surrounded by a ring of matrix, which is in turn surrounded
by an infinite cylinder of composite. Temperature-dependent material properties were used. It
was found that interface normal stress was significantly reduced with temperature and even
became slightly tensile as temperatures increased, but even the highest tensile and compressive
stresses were judged too small compared to epoxy fracture properties to affect the interface
fracture stress T, The cracked shear stress interface ratio, rj, on the other hand, should depend
heavily upon radial normal stress. In the absence of other data, it was assumed that T| is
proportional to the ratio of radial normal compressive stresses at temperature to that at room
temperature. Table A-20 shows the results of the analysis.

4.3.2.3 At-Temperature Fiber/Matrix Interface Damage

As previously discussed, it is useful for NDE purposes to know if significant fiber/matrix

cracking occurs during the heat application period. It is also a necessary preliminary to
determination of residual fatigue life once the heat has been removed. The procedure is to
determine, as described in section 2.3, the static fiber failure stress at temperature using
temperature-dependent properties and equations (2, 3, 12, and 14). The residual thermal fiber
stress at temperature is then found using equation (15) with oc= 0. Initially, fiber stress is
compressive due to residual stresses caused during cure. Results for both the short- and long-
heat application times showed that the fiber stress at which fiber/matrix interface begins to crack
is significantly reduced with increasing temperature. However, by the time temperature rises
above the stress-free state and begins to cause fiber axial tensile stress, matrix elastic modulus
has decreased to the point where fiber stress is considerably below that required to initiate
interface cracking. It is concluded that, for the graphite/epoxy composite material analyzed here,
no significant thermal stress-created fiber/matrix interface damage occurs throughout a thermal
cycle.

4.3.2.4 Residual (Upon Cool Down) Fatigue Strength Versus Cycles Curves

Since there is no thermomechanically induced fiber/matrix interface damage for either long- or
short-heat application times until the matrix is driven off by temperatures above 250°C to 300°C,
the appropriate equations for fatigue life are equations (18) and (19). For cyclic stress ratio
R = 0, S/N curves were calculated that give residual fatigue properties upon cool down from

25
NAWCADPAX-99-112-TR

maximum temperatures ranging from room (no applied heat) to the temperature at which the
matrix has been driven off (350°C for short-heat application times and 300°C for long-heat
application times). Results are shown in figure B-66. It is important to note that for short-
application times, the matrix was assumed to recover to its virgin state with no loss in properties.
The resulting short-application time S/N curves will be unchanged from the virgin one until the
matrix is gone at 350°C. The long-application time S/N curves will show changes from 100°C
reflecting matrix chemical and mechanical changes due to the long time at temperature.
Interestingly, at 150°C and below, strength reductions are limited to about 15%. Temperatures
above glass transition Tg (about 185°C here) produce a marked and sudden strength decrease:
nearly 50% at 200°C, 95% at 250°C. This is not unexpected due to the equivalent drop observed
in matrix and fiber/matrix interface properties. In addition, the S/N curves indicate that life of
the composite is not strongly affected for cyclic stress levels that are below the level of the heat-
degraded static strength.

Finally, it is important to realize that the results presented above pertain to the region of heating
only. This is important because in the damaged region, the fibers are at worst still continuous,
and the strength can be no less than the static strength of a dry fiber bundle of length equal to the
size of the damage zone. In fact, above 300°C for short-application times and 250°C for long-
application times, there is no matrix inside the damage zone. Outside the zone, however, the
matrix is still intact. This creates a scenario in which the initial (static) composite strength is
determined by an ineffective length that is equal to the size of the damage zone. Continued
cyclic stressing will cause cracks to form at the fiber/matrix interface and grow into the unheated
region where matrix properties are intact. This will further increase the ineffective length and
decrease residual strength. The effect of the size of the damaged region can be determined by
using equations (19, 20, and 21). For illustrative purposes, damage zone (and 8;) was varied
from 15 to 150 mm. Figure B-67 shows that the 150-mm long damage zone causes a drop of
nearly 70% in initial static strength, but the fatigue strength remains constant until about 1015
cycles where it rejoins the unheated material S/N curve.

4.4 CONCLUSIONS

A model has been developed for strength and fatigue life of unidirectional composite materials in
tension that includes thermal as well as mechanical loading. The model is capable of treating
any combination of thermal and mechanical stress histories as long as temperature-dependent
properties are known. The model has been applied to investigating the damage processes caused
in a particular unidirectional graphite/epoxy composite due to the application of heat and
maintaining a constant temperature in the composite for short-time (less than 5 min) and long-
time (greater than 60 min) scenarios. The following results show that:

1. According to the model developed, while the composite is at temperature, damage in

the form of fiber/matrix interface cracking due to thermal stresses probably does not
occur for either short- or long-time heat application, and the primary loss in strength
and fatigue life is due to matrix shear and fiber/matrix interface degradation with
temperature.

26
NAWCADPAX-99-112-TR

2. According to the model, heat application for less than 5 min at 300°C or lower will not
have a significant effect on residual matrix properties after cool down to room
temperature because matrix mass loss, chemical changes, and cracking do not occur to
a significant degree. Maintaining composite temperatures of greater than 150°C for
longer than 60 min will cause large reductions in strength due to matrix degradation at
temperature. Interestingly, life does not appear to be significantly affected for cyclic
stresses below the heat-degraded static strength level.

3. The model predicts that short-time application of heat resulting in temperatures higher
than 300°C and long-time heating resulting in temperatures above 250°C will remove
the matrix, leaving at best a dry bundle of fibers in the heated zone. Strength and life
of the composite in the immediate vicinity of this zone are strongly affected by the
size of the zone.

These conclusions are based upon one graphite/epoxy material system for which incomplete at-
temperature property data were available and for which many assumptions had to be made.
While care must be taken if applying them to other composites with larger fiber volume fractions
and stronger interface properties, it appears reasonable that less matrix and a stronger interface
will have little effect upon results 1 and 3. However, it is possible that such changes will push
the failure mode from cumulative weakening to fiber-break propagation, in which case, the
cumulative weakening results would be an upper bound (Zweben, reference 21).

27
NAWCADPAX-99-112-TR

SECTION 5
CONCLUSIONS

Heat damage occurs over a wide variety of temperature ranges in the naval environment. The
damage begins when composite structures are exposed to temperatures beginning near the Tg of
the material and continues with increasing temperature such as in the case of fire exposure. The
time of exposure is critical in determining the amount of damage. At temperatures near the onset
of thermal decomposition, the damage becomes so subtle that it becomes very hard to detect
using current evaluation techniques. The most critical of these cases is known as incipient heat
damage. This is damage that is undetectable using current nondestructive assessment techniques.
Higher temperature exposures leave visual clues and delaminations in the structure, but with
incipient damage, a composite structure may have reduced strength and life without any
indication.

Section 2, MECHANISMS OF LAMINATION PLANE CRACKING, addresses the

phenomenon of incipient heat damage. It is observed that at temperatures near the onset of
thermal decomposition, longer time exposures cause incipient heat damage. Matrix mass loss is
observed as the primary degradation mechanism in the case of incipient damage. When damage
is nondestructively detectable, outgassing from volatiles and/or moisture was the degradation
mechanism that caused voids and delaminations in a composite. The presence of absorbed
moisture in a structure was shown to lower the temperature/time exposure necessary to cause
delaminations and void formation.

In Section 3, OUTGASSING OF EPOXIES, the products that are given off during heat damage
causing matrix mass loss were shown to occur in two distinct ranges of temperature. The first
occurred over the temperature range of 280°C to 340°C. The evolved gases of 8552 resin were
identified by FTIR as C02, CO, H20, and a carbonyl group identified as either acid anhydride or
ester. The first stage of decomposition caused up to 8% weight loss in the composite and it is,
therefore, during this phase of damage that mechanical properties are reduced. Incipient heat
damage was shown to occur near the thermal decomposition temperature (section 2). This first
stage begins at the onset of thermal decomposition, therefore, it is in this stage that incipient heat
damage occurs. At 340°C, a second stage of thermal decomposition begins and continues for the
duration of the decomposition process. The second stage is characterized by the outgassing of
COS and C6H5-OH. Heat damage can be evaluated by STA/FTIR by correlating the peak
heights of the carbonyl group given off during heat damage to exposure temperature. The
STA/FTIR technique shows great promise as a means to detect and determine the degree of heat
damage in composites. Further studies to develop more extensive calibration curves correlated
to mechanical properties are necessary.

An analytical model was developed to aid in predicting heat damage. The model can predict
strength and fatigue life of unidirectional composite materials in tension, to include thermal as
well as mechanical loading. The model is capable of treating any combination of thermal and
mechanical stress histories as long as temperature-dependent properties are known. According

28
NAWCADPAX-99-112-TR

to the model developed, heat application for less than 5 min at 300°C or lower will not have a
significant effect on residual matrix properties after cool down to room temperature because
matrix mass loss, chemical changes, and cracking do not occur to a significant degree.
Maintaining composite temperatures of greater than 150°C for longer than 60 min will cause
large reductions in strength due to matrix degradation at temperature. The life of a composite
does not appear to be significantly affected for cyclic stresses below the heat-degraded static
strength level.

29
NAWCADPAX-99-112-TR

THIS PAGE INTENTIONALLY LEFT BLANK

30
NAWCADPAX--99-112-TR

REFERENCES

1. P. A. Mehrkam, E. Armstrong-Carroll, and R. Cochran, "Fire Damage Assessment of A-6

Composite Wing BuNo 152951", Report No. NAWCADWAR-93058-60, of Sep 1993.

2. F. D. Hardcastle, R. I. Johnson, and R. W. Brotzman, "Evaluation of Heat Damage In

Carbon/Epoxy Composites", TPL-2061-Fr, Jun 1994.

3. R. Collins, et al., "NDI for Heat Damaged Advanced Composites", Volumes 1 and 2,
Great Lakes Composites Consortium, Feb 1995.

4. Armstrong-Carroll, E., Mehrkam, P. A., and Cochran, R., "Heat Damage Evaluation of
Painted Graphite/Epoxy Composites", Conference on Characterization and NDE of Heat
Damage in Graphite Epoxy Composites, Organized by the Nondestructive Information
Analysis Center (NTIAC) located in Austin, Texas, Apr 1993.

5. L. B. Greszczuk, "Mechanical Properties and Thermal Degradation of Advanced

Composites Under Rapid Heating," Defense Nuclear Agency Report No. DNA-TR-85-71-
V2, of Jun 1985.

6. M. R. Tant, H. L. N. McManus, and M. E. Rogers, in M. R. Tant, J. W. Connell, and H. L.

N. McManus, eds., High-Temperature Properties and Applications of Polymeric Materials.
American Chemical Society, Washington, DC, 1995, pp. 10-12.

7. W. W. Wendlandt, Thermal Analysis. 3rd ed., Wiley, New York 1986, pp. 9-86.

8. C. J. Janke, J. D. Muhs et al., "Composite Heat Damage Spectroscopic Analysis," Oak

Ridge National Laboratory Report ORNL/ATD-42, Sep 1990.

9. P. A. Mehrkam and E. Armstrong-Carroll, SAMPE International Symposium. 38, 217

(1993).

10. Arafat, E. S., 1995, Rust College, Holly Springs, MS. Personal Communication.

11. Armstrong-Carroll, E., Mehrkam, P. A., and Cochran, R., 1994, A Characterization of Heat
Damage in Composites, 12th ASTM Symposium on Composite Materials: Testing and
Design.

12. Hahn, H. T., 1979, "Fatigue Behavior and Life Prediction of Composite Laminates," in
Composite Materials: Testing and Design (Fifth Conference), ASTM STP 674, S. W. Tsai,
Ed., pp. 383-417.

31
NAWCADPAX-99-112-TR

13. McLaughlin, P.V.D., Jr., 1994, Life and Residual Strength of Unidirectional Fiber
Composites, in Wetherhold, R. C, ed., Durability of Composite Materials, MD Vol. 51,
ASME, pp. 59-73.

14. McLaughlin, P. V., and Rosen, B. W., 1974, "Combined Stress Effects Upon Failure of
Fiber Composites," TFR/7404/1112, Materials Sciences Corporation, Final Report,
Contract N62269-73-0800, Naval Air Development Center, Warminster, PA.

15. Radhakrishnan, K., 1984, "Fatigue and Reliability Evaluation of Unnotched Carbon Epoxy
Laminates," Journal of Composite Materials, Vol. 18, pp. 21-31.

16. Rosen, B. W., 1965, "Mechanics of Composite Strengthening," in Fiber Composite

Materials, ASM, Metals Park, OH.

17. Turtle, M., et al, 1995, Thermo-Mechanics of Structural Composites Under Conditions of
Fire Impact, Navy Council on Materials and Structures.

18. Zhou, S. J., and Curtin, WA, (1995), A Failure of Fiber Composites: A Lattice Green=s
Function, Ada Met, Vol. 43, pp. 3093-3104.

19. Zweben, C, 1968, "Tensile Failure Analysis of Fibrous Composites," AIAA Journal,
Vol. 6, pp. 2325-2331.

20. Zweben, C, 1972, "A Bounding Approach to the Strength of Composite Materials,"
Engineering Fracture Mechanics, Vol. 4, pp. 1-8.

21. Zweben, C, 1974, "Failure Analysis of Unidirectional Fiber Composites under Combined
Axial Tension and Shear," J. of the Mechanics and Physics of Solids, Vol. 22, pp. 193-215.

22. Zweben, C, and Rosen, B. W., 1970, "A Statistical Theory of Material Strength with
Applications to Composite Materials," J. of the Mechanics and Physics of Solids, Vol. 18,
pp. 189-206.

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NAWCADPAX--99-112-TR

APPENDIX A
TABLES

33 APPENDIX A
NAWCADPAX--99-112-TR

Table A-l
SATURATING STATISTICS OF 977-3 NEAT RESIN SAMPLES

Ambient Weight Saturated Weight Weight Gain % Gain

Sample (g) (g) (g) (Ambient)
9-525-05-S 4.3211 4.5005 0.1794 4.15
9-525-20-S 4.3949 4.5790 0.1841 4.19
9-525-45-S 4.4514 4.6374 0.1860 4.18
9-576-05-S 4.3924 4.5896 0.1972 4.49
9-576-05-S 4.3494 4.5280 0.1786 4.11
9-576-05-S 3.4827 3.6265 0.1438 4.13
9-623-05-S 3.8963 4.0566 0.1603 4.11
9-623-20-S . 4.2336 4.4078 0.1742 4.11
9-623-45-S 3.8566 4.0157 0.1591 4.13
Avg=> 4.1532 4.3268 0.1736 4.18

Table A-2
DRYING STATISTICS OF 977-3 NEAT RESIN SAMPLES

Ambient Weight Dry Weight Weight Loss % Loss

Sample (g) (g) (g) (Ambient)
9-525-05-D 3.9869 3.9600 0.0269 0.67
9-525-20-D 3.9321 3.9094 0.0227 0.58
9-525-45-D 4.0273 4.0037 0.0236 0.59
9-576-05-D 3.9002 3.8759 0.0243 0.62
9-576-20-D 3.9001 3.8748 0.0253 0.65
9-576-45-D 4.2966 4.2704 0.0262 0.61
9-623-05-D 4.5908 4.5616 0.0292 0.64
9-623-20-D 4.6132 4.5850 0.0282 0.61
9-623-45-D 3.9541 3.9277 0.0264 0.67
Avg=> 4.1335 4.1076 0.0259 0.63

34 APPENDIX A
NAWCADPAX-99-112-TR

Table A-3
SATURATING STATISTICS OF UNIDIRECTIONAL COMPOSITE SAMPLES

Ambient Weight Saturated Weight Weight Gain % Gain

Sample (g) (g) (g) (Ambient)
U-525-05-S 3.9877 4.0255 0.0378 0.95
U-525-20-S 4.4007 4.4442 0.0435 0.99
U-525-45-S 4.4032 4.4469 0.0437 0.99
U-576-05-S 4.4036 4.4465 0.0429 0.97
U-576-05-S 4.4537 4.4975 0.0438 0.98
U-576-05-S 4.5609 4.6062 0.0453 0.99
U-623-05-S 4.4258 4.4701 0.0443 1.00
U-623-20-S 4.3643 4.4070 0.0427 0.98
U-623-45-S 4.3976 4.4405 0.0429 0.98
Avg=> 4.3775 4.4205 0.0430 0.98

Table A-4
DRYING STATISTICS OF UNIDIRECTIONAL COMPOSITE SAMPLES

Ambient Weight Dry Weight Weight Loss % Loss

Sample (g) (g) (g) (Ambient)
U-525-05-D 4.5226 4.5076 0.0150 0.33
U-525-20-D 4.3862 4.3721 0.0141 0.32
U-525-45-D 4.3276 4.3163 0.0113 0.26
U-576-05-D 4.2424 4.2308 0.0116 0.27
U-576-05-D 4.3911 4.3779 0.0132 0.30
U-576-05-D 4.4185 4.4059 0.0126 0.29
U-623-05-D 4.5125 4.4983 0.0142 0.31
U-623-20-D 4.5156 4.5029 0.0127 0.28
U-623-45-D 4.4004 4.3886 0.0118 0.27
Avg=> 4.4130 4.4000 0.0129 0.29

35 APPENDIX A
NAWCADPAX-99-112-TR

Table A-5
SATURATING STATISTICS OF QUASI-ISOTROPIC COMPOSITE SAMPLES

Ambient Weight Saturated Weight Weight Gain % Gain

Sample (g) (g) (g) (Ambient)
Q-525-05-S 4.6294 4.6688 0.0394 0.85
Q-525-20-S 4.3628 4.3994 0.0366 0.84
Q-525-45-S 4.1261 4.1590 0.0329 0.80
Q-576-05-S 4.6150 4.6547 0.0397 0.86
Q-576-05-S 4.3294 4.3665 0.0371 0.86
Q-576-05-S 4.3034 4.3397 0.0363 0.84
Q-623-05-S 4.2344 4.2693 0.0349 0.82
Q-623-20-S 4.3893 4.4266 0.0373 0.85
Q-623-45-S 4.4021 4.4405 0.0384 0.87
Avg=> 4.3769 4.4138 0.0370 0.84

Table A-6
DRYING STATISTICS OF QUASI-ISOTROPIC COMPOSITE SAMPLES

Ambient Weight Dry Weight Weight Loss % Loss

Sample (g) (g) (g) (Ambient)
Q-525-05-D 4.4575 4.4415 0.0160 0.36
Q-525-20-D 4.4003 4.3838 0.0165 0.37
Q-525-45-D 4.3629 4.3480 0.0149 0.34
Q-576-05-D 4.5276 4.5126 0.0150 0.33
Q-576-05-D 4.2894 4.2757 0.0137 0.32
Q-576-05-D 4.6505 4.6341 0.0164 0.35
Q-623-05-D 4.3769 4.3633 0.0136 0.31
Q-623-20-D 4.2767 4.2650 0.0117 0.27
Q-623-45-D 4.1944 4.1838 0.0106 0.25
Avg=> 4.3929 4.3786 0.0143 0.32

36 APPENDIX A
NAWCADPAX--99-112-TR

Table A-7
AVERAGE PERCENT WEIGHT GAIN OR LOSS RESULTING FROM
ENVIRONMENTAL CONDITIONING

Average Dry Average Wet

Weight Loss Weight Gain
Samples (%) (%)
977-3 Neat Resin 0.63 4.18
Unidirectional 0.29 0.98
Quasi-Isotropic 0.32 0.84

Table A-8
COUPON LEVEL IDENTIFICATION OF EXPOSURE CONDITIONS

Samp e Set Coupon Label Exposure Conditions

977-3 Neat Unidirectional Quasi-Isotropic Temperature Time Moisture
Resin Laminates Laminates (min) Condition
9-525-05-S U-525-05-S O-525-05-S 274 5 Saturated
9-525-20-S U-525-20-S O-525-20-S 274 20 Saturated
9-525-45-S U-525-45-S 0-525-45-S 274 45 Saturated
9-576-05-S U-576-05-S O-576-05-S 302 5 Saturated
9-576-20-S U-576-20-S O-576-20-S 302 20 Saturated
9-576-45-S U-576-45-S 0-576-45-S 302 45 Saturated
9-623-05-S U-623-05-S O-623-05-S 328 5 Saturated
9-623-20-S U-623-20-S 0-623-20-S 328 20 Saturated
9-623-45-S U-623-45-S 0-623-45-S 328 45 Saturated
9-525-05-D U-525-05-D O-525-05-D 274 5 Dry
9-525-20-D U-525-20-D 0-525-20-D 274 20 Dry
9-525-45-D U-525-45-D 0-525-45-D 274 45 Dry
9-576-05-D U-576-05-D 0-576-05-D 302 5 Dry
9-576-20-D U-576-20-D 0-576-20-D 302 20 Dry
9-576-45-D U-576-45-D 0-576-45-D 302 45 Dry
9-623-05-D U-623-05-D O-623-05-D 328 5 Dry
9-623-20-D U-623-20-D O-623-20-D 328 20 Dry
9-623-45-D U-623-45-D 0-623-45-D 328 45 Dry
9-525-05-A U-525-05-A 0-525-05-A 274 5 Ambient
9-525-20-A U-525-20-A 0-525-20-A 274 20 Ambient
9-525-45-A U-525-45-A 0-525-45-A 274 45 Ambient
9-576-05-A U-576-05-A Q-576-05-A 302 5 Ambient
9-576-20-A U-576-20-A 0-576-20-A 302 20 Ambient
9-576-45-A U-576-45-A 0-576-45-A 302 45 Ambient
9-623-05-A U-623-05-A Q-623-05-A 328 5 Ambient
9-623-20-A U-623-20-A 0-623-20-A 328 20 Ambient
9-623-45-A U-623-45-A 0-623-45-A 328 45 Ambient

37 APPENDIX A
NAWCADPAX-99-112-TR

Table A-9
ONSET OF DECOMPOSITION TEMPERATURE AND THE TEMPERATURE WHERE
THE MAXIMUM RATE OF DECOMPOSITION OCCURS FOR
THE 977-3 NEAT RESIN SAMPLES

Temperature at
Temperature Maximum
Exposure Exposure at 5% Weight Decomposition
Time Temperature Loss Rate
Sample (min) (°C) (°Q (°C)
Undamaged 0 0 379.5 433.8
9-525-05-S 5 274 357.1 420.6
9-525-20-S 20 274 368.3 426.5
9-525-45-S 45 274 386.2 428.6
9-576-05-S 5 302 357.1 424.8
9-576-20-S 20 302 377.2 421.3
9-576-45-S 45 302 393.9 430.1
9-623-05-S 5 329 373.9 428.8
9-623-20-S 20 329 385.0 428.8
9-623-45-S 45 329 390.6 425.7
9-525-05-D 5 274 386.2 436.1
9-525-20-D 20 274 385.0 433.3
9-525-45-D 45 274 388.4 430.5
9-576-05-D 5 302 381.7 429.8
9-576-20-D 20 302 388.4 427.5
9-576-45-D 45 302 395.1 425.3
9-623-05-D 5 329 381.7 413.2
9-623-20-D 20 329 371.6 423.9
9-623-45-D 45 329 358.3 425.2
9-525-05-A 5 274 379.5 417.6
9-525-20-A 20 274 379.5 421.9
9-525-45-A 45 274 381.7 425.5
9-576-05-A 5 302 377.2 410.7
9-576-20-A 20 302 383.9 420.5
9-576-45-A 45 302 397.3 428.1
9-623-05-A 5 329 377.2 424.7
9-623-20-A 20 329 390.6 415.9
9-623-45-A 45 329 363.8 415.9

38 APPENDIX A
NAWCADPAX-99-112-TR

Table A-10
ONSET OF DECOMPOSITION TEMPERATURE AND THE TEMPERATURE
WHERE THE MAXIMUM RATE OF DECOMPOSITION OCCURS FOR
THE 977-3 UNIDIRECTIONAL SAMPLES

Temperature at
Temperature Maximum
Exposure Exposure at 5% Weight Decomposition
Time Temperature Loss Rate
Sample (min) (°C) (°C) (°C)
Undamaged 0 0 410.7 421.4
U-525-05-S 5 274 413.0 428.2
U-525-20-S 20 274 413.0 428.0
U-525-45-S 45 274 417.4 428.2
U-576-05-S 5 302 410.7 425.9
U-576-20-S 20 302 413.0 422.1
U-576-45-S 45 302 412.9 425.1
U-623-05-S 5 329 410.7 426.1
U-623-20-S 20 329 417.4 422.7
U-623-45-S 45 329 415.2 425.0
U-525-05-D 5 274 408.5 423.7
U-525-20-D 20 274 413.0 424.0
U-525-45-D 45 274 413.0 422.5
U-576-05-D 5 302 410.7 423.0
U-576-20-D 20 302 414.0 421.9
U-576-45-D 45 302 417.4 430.5
U-623-05-D 5 329 415.2 424.7
U-623-20-D 20 329 417.4 422.0
U-623-45-D 45 329 416.3 418.2
U-525-05-A 5 274 410.7 420.5
U-525-20-A 20 274 415.2 425.5
U-525-45-A 45 274 411.8 421.3
U-576-05-A 5 302 409.6 417.7
U-576-20-A 20 302 414.0 423.8
U-576-45-A 45 302 416.3 422.6
U-623-05-A 5 329 413.0 423.9
U-623-20-A 20 329 412.5 422.5
U-623-45-A 45 329 417.4 427.4

39 APPENDIX A
NAWCADPAX-99-112-TR

Table A-11
ONSET OF DECOMPOSITION TEMPERATURE AND THE TEMPERATURE
WHERE THE MAXIMUM RATE OF DECOMPOSITION OCCURS FOR
THE 977-3 QUASI-ISOTROPIC SAMPLES

Temperature at
Temperature Maximum
Exposure Exposure at 5% Weight Decomposition
Time Temperature Loss Rate
Sample (min) (°C) (°C) (°C)
Undamaged 0 0 414.0 425.6
Q-525-05-S 5 274 415.2 431.0
Q-525-20-S 20 274 413.0 427.4
Q-525-45-S 45 274 418.5 427.8
Q-576-05-S 5 302 411.8 426.2
Q-576-20-S 20 302 413.0 427.0
Q-576-45-S 45 302 417.4 429.4
Q-623-05-S 5 329 413.0 428.5
Q-623-20-S 20 329 417.4 427.3
Q-623-45-S 45 329 419.6 428.9
Q-525-05-D 5 274 416.3 424.8
Q-525-20-D 20 274 415.2 427.9
Q-525-45-D 45 274 415.2 429.2
Q-576-05-D 5 302 416.3 429.6
Q-576-20-D 20 302 416.3 432.5
Q-576-45-D 45 302 413.0 425.1
Q-623-05-D 5 329 413.0 422.6
Q-623-20-D 20 329 417.4 426.6
Q-623-45-D 45 329 419.6 422.0
Q-525-05-A 5 274 410.7 425.9
Q-525-20-A 20 274 415.2 426.8
Q-525-45-A 45 274 420.7 428.2
Q-576-05-A 5 302 413.0 426.2
Q-576-20-A 20 302 415.2 428.3
Q-576-45-A 45 302 417.4 420.3
Q-623-05-A 5 329 413.0 426.2
Q-623-20-A 20 329 415.2 424.4
Q-623-45-A 45 329 409.6 422.5

40 APPENDIX A
NAWCADPAX-99-112-TR

Table A-12
FLEXURAL TEST RESULTS FOR THE 977-3 NEAT RESIN SAMPLES

977-3 Neat Resin (Four-Point Flex, ASTM D-790)

Temp Time Moisture Width (b) Depth (d) Length (1) Peak Flex Strength
(°F) (min) Condition (in.) (in.) (in.) Load (KSI)
(lb)
0 0 Ambient 0.421 0.109 1.600 25.49 12.338

525 5 Saturated 1.024 0.102 1.600 135.25 30.468

525 20 Saturated 1.019 0.101 1.600 26.08 6.021
525 45 Saturated 1.013 0.104 1.600 37.65 8.247
575 5 Saturated 1.025 0.107 1.600 100.76 20.607
575 20 Saturated 0.973 0.108 1.600 24.82 5.249
575 45 Saturated 0.960 0.092 1.600 7.36 2.174
625 5 Saturated 0.964 0.099 1.600 10.52 2.672
625 20 Saturated 0.980 0.111 1.600 13.88 2.759
625 45 Saturated Samples Crumbled Upon Cooling

525 5 Dry 0.983 0.098 1.600 84.56 21.497

525 20 Dry 0.956 0.100 1.600 130.42 32.741
525 45 Dry 0.964 0.100 1.600 82.88 20.634
575 5 Dry 0.959 0.102 1.600 120.95 29.094
575 20 Dry 0.961 0.096 1.600 21.67 5.872
575 45 Dry 0.952 0.108 1.600 15.99 3.456
625 5 Dry 0.978 0.112 1.600 176.48 34.525
625 20 Dry Samples Crumbled Upon Cooling
625 45 Dry Therefore Nontestable

525 5 Ambient 1.001 0.099 1.600 144.72 35.403

525 20 Ambient 0.990 0.116 1.600 177.11 31.908
525 45 Ambient 0.986 0.117 1.600 140.93 25.059
575 5 Ambient 1.009 0.100 1.600 157.76 37.525
575 20 Ambient 1.009 0.105 1.600 29.24 6.308
575 45 Ambient 1.009 0.105 1.600 12.62 2.723
625 5 Ambient 0.994 0.109 1.600 186.16 37.832
625 20 Ambient Samples Crumbled Upon Cooling
625 45 Ambient Therefore Nontestable

41 APPENDIX A
NAWCADPAX--99-112-TR

Table A-13
FLEXURAL TEST RESULTS FOR THE IM6/977-3 UNIDIRECTIONAL SAMPLES

Unidirectional (Four-Point Flex, ASTM D-790)

Temp Time Moisture Width (b) Depth (d) Length (1) Peak Load Flex Strength
(°F) (Min) Condition (in.) (in.) (in.) (lb) (KSI)
0 0 Ambient 1.003 0.089 1.600 1,003.89 303.261

525 5 Saturated 1.004 0.084 1.600 918.09 311.031

525 20 Saturated 1.002 0.089 1.600 795.69 240.607
525 45 Saturated 0.997 0.089 1.600 549.21 166.907
575 5 Saturated 1.005 0.090 1.600 875.6 258.146
575 20 Saturated 0.994 0.091 1.600 553.21 161.299
575 45 Saturated 0.996 0.092 1.600 528.39 150.429
625 5 Saturated 1.000 0.090 1.600 428.08 126.839
625 20 Saturated 0.989 0.090 1.600 497.06 148.915
625 45 Saturated 0.993 0.109 1.600 63.83 12.985

525 5 Dry 0.999 0.091 1.600 1,002.84 Test Abort

525 20 Dry 0.981 0.090 1.600 986.65 298.003
525 45 Dry 0.996 0.087 1.600 961.83 306.205
575 5 Dry 1.000 0.085 1.600 1,001.58 Test Abort
575 20 Dry 0.997 0.089 1.600 623.66 189.533
575 45 Dry 0.987 0.091 1.600 646.16 189.737
625 5 Dry 0.993 0.092 1.600 1,004.52 Test Abort
625 20 Dry 0.999 0.091 1.600 497.48 144.324
625 45 Dry 0.988 0.089 1.600 328.18 100.644

525 5 Ambient 0.998 0.089 1.600 1,002.84 Test Abort

525 20 Ambient 0.972 0.089 1.600 1,000.11 Test Abort
525 45 Ambient 0.985 0.087 1.600 951.31 306.238
575 5 Ambient 0.999 0.089 1.600 1,004.73 Test Abort
575 20 Ambient 0.988 0.092 1.600 584.96 167.882
575 45 Ambient 0.988 0.090 1.600 570.66 171.138
625 5 Ambient 0.988 0.090 1.600 1,002.21 Test Abort
625 20 Ambient 0.990 0.091 1.600 483.81 141.634
625 45 Ambient 0.990 0.101 1.600 105.68 25.115

42 APPENDIX A
NAWCADPAX-99-112-TR

Table A-14
FLEXURAL TEST RESULTS FOR THE IM6/977-3 QUASI-ISOTROPIC SAMPLES

Quasi-Isotropic (Four-Point Flex, ASTM D-790)

Temp Time Moisture Width (b) Depth (d) Length (1) Peak Load Flex Strength
(°F) (min) Condition (in.) (in.) (in.) Ob) (KSI)
0 0 Ambient 0.976 0.089 1.600 626.63 194.533

525 5 Saturated 0.999 0.089 1.600 666.35 202.101

525 20 Saturated 0.983 0.087 1.600 294.11 94.870
525 45 Saturated 0.983 0.083 1.600 267.61 94.843
575 5 Saturated 1.001 0.088 1.600 343.32 106.295
575 20 Saturated 0.989 0.087 1.600 214.62 68.809
575 45 Saturated 0.981 0.086 1.600 229.97 76.071
625 5 Saturated 0.991 0.086 1.600 217.35 71.171
625 20 Saturated 0.985 0.088 1.600 248.05 78.046
625 45 Saturated 0.971 0.092 1.600 60.04 17.533

525 5 Dry 0.981 0.089 1.600 628.94 194.255

525 20 Dry 0.982 0.088 1.600 540.81 170.679
525 45 Dry 0.987 0.088 1.600 383.47 120.409
575 5 Dry 0.994 0.088 1.600 740.85 230.988
575 20 Dry 0.992 0.086 1.600 287.76 94.131
575 45 Dry 1.000 0.088 1.600 305.22 94.593
625 5 Dry 0.997 0.084 1.600 517.67 176.608
625 20 Dry 0.989 0.085 1.600 248.84 83.579
625 45 Dry 0.991 0.084 1.600 110.43 37.902

525 5 Ambient 0.999 0.086 1.600 674.17 218.987

525 20 Ambient 0.994 0.087 1.600 523.98 167.148
525 45 Ambient 0.988 0.088 1.600 363.06 113.885
575 5 Ambient 0.999 0.089 1.600 684.27 207.536
575 20 Ambient 0.998 0.088 1.600 316.58 98.310
575 45 Ambient 0.981 0.088 1.600 249.89 78.945
625 5 Ambient 0.987 0.088 1.600 616.74 193.656
625 20 Ambient 0.985 0.090 1.600 227.6 68.464
625 45 Ambient 1.000 0.084 1.600 89.61 30.480

43 APPENDIX A
NAWCADPAX--99-112-TR

Table A-15
IR VIBRATIONAL FREQUENCIES OF 8552 OUTGASSED PRODUCTS

Vibrational Frequency
Compound Symbol (cm1)
Carbon Dioxide C02 672, 2,307, 2,372, 3,729
Carbon Monoxide CO 2,189,2,254
Water H20 1,337,1,379, 1,505,1,596
Acid Anhydride R-CO-O-CO-R 752, 1,170,1,721, 1,759,1,794,2,942
Carbonyl Sulfide COS 866, 2,045,2,068
Phenol C6H50H 1,250,1,486,1,623,3,011,3,383

44 APPENDIX A
NAWCADPAX-99-112-TR

Table A-16
RAW STA DATA FOR UNDAMAGED 8552 COMPOSITES

Samples Were Undamaged ]Prior to Testing

Isothermal Sample Weight Peak Peak
Temperature Weight Loss at Height/mg Height/mg
(°C) (mg) lHr (Carbonyl) (C02)
290 17.40 2.00 1.09 0.70
290 15.70 2.25 1.58 0.83
Average => 16.55 2.13 1.34 0.76
300 16.20 3.48 1.97 1.44
300 16.30 3.32 1.73 1.57
300 12.20 4.01 1.71 1.62
Average => 14.90 3.60 1.80 1.54
310 13.50 4.35 2.64 2.08
310 12.50 4.83 2.50 2.27
310 14.70 4.18 2.40 1.51
Average => 13.57 4.45 2.52 1.95
320 14.10 5.62 3.21 3.06
320 16.10 5.89 3.39 2.53
320 12.80 5.92 3.32 3.01
Average => 14.33 5.81 3.31 2.87
330 17.10 7.58 3.76 3.87
330 15.80 8.09 4.26 3.28
330 14.30 7.96 4.74 3.54
Average => 15.73 7.88 4.25 3.56
340 17.00 9.99 5.07 4.38
340 12.80 10.15 6.24 5.73
Average => 14.90 10.07 5.66 5.06
350 15.20 12.31 7.11 7.17
350 12.90 12.18 6.59 7.32
Average => 14.05 12.25 6.85 7.24
360 15.30 13.82 7.97 9.74
360 15.10 13.71 7.78 8.83
Average => 15.20 13.77 7.88 9.28
370 15.90 16.37 9.13 11.33
Average => 15.90 16.37 9.13 11.33

45 APPENDIX A
NAWCADPAX-99-112-TR

Table A-17
RAW STA DATA FOR PREDAMAGED 8552 COMPOSITES

Samples Were Predamaged at 315°C Prior to Testing

Damage Sample Weight Peak Peak
Time Weight Loss at Height/mg Height/mg
(min) (mg) lHr (Carbonyl) (C02)
5 15.20 7.90 3.98 2.98
5 13.10 8.47 3.86 3.17
Average => 14.15 8.19 3.92 3.07
20 13.70 7.47 3.41 3.61
20 13.10 7.22 3.66 3.62
Average => 13.40 7.35 3.53 3.61
45 13.10 6.97 3.07 3.50
45 14.60 7.03 2.76 3.34
Average => 13.85 7.00 2.91 3.42

46 APPENDIX A
NAWCADPAX-99-112-TR

Table A-18
PROPERTIES OF GRAPHITE FIBERS IN EPOXY

Fiber Axial Modulus, Ef 177 GPa(1)

Fiber Transverse Modulus, E2f 25 GPa(2)
Fiber Axial Thermal Expansion Coefficient, 0Cf -0.5xl0-6 °C"1(3)

Fiber Transverse Thermal Expansion Coefficient,(X2f 30xlO"6oC1(2)

Fiber Volume Fraction, Vf 0.35(1)
Fiber Diameter, d 0.0035 mm(3)
Weibull Fiber Parameter, a 6.89xl0-9MPa1-961mm-1(4)
Weibull Fiber Parameter, ß 1.961(4)
Matrix Shear Modulus, Gm 0.7 GPa(1)
Matrix Poisson's Ratio, vm 0.35(2)
Matrix Thermal Expansion Coefficient, am 65x10"6 °C"1(1)
Fiber-Matrix Interface Shear Strength, T 10 MPa(1)
Postfailure Shear Stress Fraction, r\ 0.035(1)
Fatigue Crack Propagation Exponent, m 22.5(1)
Fatigue Crack Propagation Constant, CN 3.9xl0"4 cycles"1(1)

NOTES: (1) Reference 16 (and micromechanics).

(2) Estimate.
(3) THORNEL Brochure.
(4) Reference 13.

47 APPENDIX A
NAWCADPAX-99-112-TR

Table A-19
DEGRADED EPOXY SHEAR MODULUS FOR
TWO-HEAT EXPOSURE HISTORIES

Matrix Shear Modulus, Gm,

MPa
Temperature Short-Time Exposure Long-Time ixposure
(°C) At Temperature Resid (Cool) At Temperature Resid (Cool)
20 700 700 700 700
100 607 700 607 607
150 568 700 568 568
200 301 700 301 301
250 23 700 6 6
—
300 23 700 0 0
350 0 0 0 0

Table A-20
CRACKED INTERFACE SHEAR STRESS RATIO FOR
TWO-HEAT EXPOSURE HISTORIES

Cracked Interface Dhear Stress Ratio, r|

Temperature Short-Time Exposure Long-Time Exposure
(°C) At Temperature Resid (Cool) At Temperature Resid (Cool)
20 0.0346 0.0346 0.0346 0.0346
100 0.0150 0.0346 0.0150 0.0299
150 0.0056 0.0346 0.0056 0.0281
200 0 0.0346 0 0.0150
250 0 0.0346 0 0.0003
300 0 0.0346 0 0
350 0 0 0 0

48 APPENDIX A
NAWCADPAX-99-112-TR

APPENDIX B
FIGURES

49 APPENDIX B
NAWCADPAX-99-112-TR

977-3 Neat Resin

Moisture Conditioning Averages
4.22

4.2 -•■■•-

4.18 4.2% Average Weight Gain

^1 4.16

4.14
f 0.63% Average Weight Loss
\
4.12
K -urn
Drying
Saturating
4.1
10 15 20 25
Days

Figure B-l
ENVIRONMENTAL CONDITIONING RESULTS FOR THE 977-3 NEAT RESIN
SAMPLES SHOWING THE AVERAGE WEIGHT GAIN AND LOSS DURING
THE DAYS OF THE CONDITIONING

50 APPENDIX B
NAWCADPAX-99-112-TR

&+/%} mHm 'AIJTO

a
«ft
P CS Q
vi 'ssM&m:;.-.-:-:•: >.-. ...J. ...J..
^4 £;;

*C

X.

8 s 1"
O

,, & «
O ö **
^> is
,, *9 O C
© i.

OP v tN

e j-

o
I,:

< Ok 3£

IP ^
fit i« +-I it
m m m HJ
m x
1
as "B 1 i 1
a ¥ü s O1 03 «3- ft!
6 H v l
Hi |ul?a^

51 APPENDIX B
NAWCADPAX-99-112-TR

977-3 Neat Resin

Temperature at 5% Weight Loss
400

390
A*
u Ä --4i
--.-1 • \
a
w
380 V
3
/
W A
1 ■' \
(B
1
1
A ^ \
®
Q.
370 §
\ \
A 1
\ \
E 1 1
1
a \ 1
t-
360 §
1
. - . . 1
1
— -♦—-Dry \
t
A A
—A-- Saturated
350
c in o in in o in in o in
c o CM ■* o CM ■«t
o o CM ■*
z in m in CO CD co CO co CO
C\l CM CJ i^ i^ r^ CJ CJ CM
m m in w in m CD co CO

Exposure Temp [°F]-Time [min]

Figure B-3
COMPARISON OF THE ONSET TEMPERATURE OF DECOMPOSITION FOR
THE 977-3 NEAT RESIN SAMPLES GROUPED BY TEMPERATURE EXPOSURE

977-3 Neat Resin

Temperature at 5% Weight Loss
400

390
o
o 380
"♦
3

S 370
E
a>
I- -♦—Dry
360
—■ Ambient
■-A-- Saturated
350
in in in o o o in in m
o o o CM CJ CM ■* •* ■*

in co CO in CD CO m co CO
CM c~ CM CM i^ CM CM r^ CM
in in co in in co m in co

Exposure Temp [°F]-Time [min]

Figure B-4
COMPARISON OF THE ONSET TEMPERATURE OF DECOMPOSITION FOR
THE 977-3 NEAT RESIN SAMPLES GROUPED BY TIME EXPOSURE

52 APPENDIX B
NAWCADPAX-99-112-TR

977-3 Neat Resin

Temperature at Max Rate of Weight Loss
440

Ü 430

•£
« 420
0)
a
£
ai
410 —-♦ Dry
—■ Ambient
—A-- Saturated
400
in o in
CM ■>!■

to ID CD CO CO CO
rv tv CM CM CM
CD CD CD

Exposure Temp [°F]-Time [min]

Figure B-5
COMPARISON OF THE TEMPERATURE AT WHICH THE MAXIMUM RATE
OF WEIGHT LOSS OCCURS FOR THE 977-3 NEAT RESIN SAMPLES GROUPED
BY TEMPERATURE EXPOSURE

977-3 Neat Resin

Temperature at Max Rate of Weight Loss
440

Ü 430

t; 420
<v
Q.
E
iZ 410
—■ Ambient
—A-- Saturated
400
CO in in o o in in in
o o o CM CM

m CD CO in
CM i^ CM CM CM
in in CO in CD

Exposure Temp [°F]-Time [min]

Figure B-6
COMPARISON OF THE TEMPERATURE AT WHICH THE MAXIMUM RATE
OF WEIGHT LOSS OCCURS FOR THE 977-3 NEAT RESIN SAMPLES GROUPED
BY TIME EXPOSURE

53 APPENDIX B
NAWCADPAX-99-112-TR

IM6/977-3 Unidirectional Laminate

Temperature at 5% Weight Loss
440

-♦ Dry
-■ Ambient
O 430
-A-- Saturated

~
to
420
w
0>
a
E
<t>
I- 410

400
in o in in o in in o 10
o CM ■* o CM ■* o CM ^J-
in in in CO CD (0 co CO CO
CM OJ M r»- i^ t^ CM CM CM
in in m in in in CD CO CD

Exposure Temp [°F]-Time [min]

Figure B-7
COMPARISON OF THE ONSET TEMPERATURE OF DECOMPOSITION FOR THE
UNIDIRECTIONAL LAMINATE SAMPLES GROUPED BY TEMPERATURE EXPOSURE

IM6/977-3 Unidirectional Laminate

Temperature at 5% Weight Loss
440

■-♦--Dry
—■ Ambient
Ü 430
■-A-- Saturated

■£
CD
420
k.
(D
D.
E
v
I- 410

400
CD CO in in o o o in w in
c o
o o o CM CM OJ ■* ■<* •*
Z in CO CO m co CO in co CO
CM i^ CM CM N CM CM r^ CM
in m CO w in CO in m co

Exposure Temp [CF]-Time [min]

Figure B-8
COMPARISON OF THE ONSET TEMPERATURE OF DECOMPOSITION FOR THE
UNIDIRECTIONAL LAMINATE SAMPLES GROUPED BY TIME EXPOSURE

54 APPENDIX B
NAWCADPAX--99-112-TR

IM6/977-3 Unidirectional Laminate

Temperature at Max Rate of Weight Loss
440

O 430

■S
» 420
01
o.
e ■-♦—-Dry
0>
410
—■ Ambient
--A-- Saturated

400
w o in in o m O in
o CM ■* o CM o CM

IT) in in CO CO CD CO CO CO
CM CM CM CM CM CM
in in in in in in CO CO CO

Exposure Temp [°F] ■Time [min]

Figure B-9
COMPARISON OF THE TEMPERATURE AT WHICH THE MAXIMUM RATE OF
WEIGHT LOSS OCCURS FOR THE UNIDIRECTIONAL LAMINATE SAMPLES
GROUPED BY TEMPERATURE EXPOSURE

IM6/977-3 Unidirectional Laminate

Temperature at Max Rate of Weight Loss
440

O 430

-*3^~
■2 420
IB
w
O
a.
E -♦—-Dry
a>
K 410
-■ Ambient
-A-- Saturated

400
o o CM CM CM Tt ■* ■*

CO CO m CO CO in CO CO
CM CM CM CM CM
in CO in in CO in in CO

Exposure Temp [°F]-Time [min]

Figure B-10
COMPARISON OF THE TEMPERATURE AT WHICH THE MAXIMUM RATE OF
WEIGHT LOSS OCCURS FOR THE UNIDIRECTIONAL LAMINATE SAMPLES
GROUPED BY TIME EXPOSURE

55 APPENDIX B
NAWCADPAX-99-112-TR

IM6/977-3 Quasi-lsotropic Laminate

Temperature at 5% Weight Loss
440

--• Dry

Ü 430 —■ Ambient
—A-- Saturated

- 420
k.
<D
Q.
E
CD
H 410

400
w o in m o in in o in
o eg •* o CO o CM ■*

m in m CD CO CO CO CO co
CO CO CO CO CO CO
in in in in m m CO CO co

Exposure Temp [°F]-Time [min]

Figure B-11
COMPARISON OF THE ONSET TEMPERATURE OF DECOMPOSITION FOR THE
QUASI-ISOTROPIC LAMINATE SAMPLES GROUPED BY TEMPERATURE EXPOSURE

IM6/977-3 Quasi-lsotropic Laminate

Temperature at 5% Weight Loss
440

-♦—-Dry
O 430 -■ Ambient
-A-- Saturated

- 420
0) .--.*
a.
E
£ 410

400
CD
C
m m in o o o m in in
o o o o CM CO CM -a-
z in CO CO in CO CO in CO CO
CO CM CO r-. CM CM CM
in m co m in CD in m CO

Exposure Temp [°F]-Time [min]

Figure B-12
COMPARISON OF THE ONSET TEMPERATURE OF DECOMPOSITION FOR THE
QUASI-ISOTROPIC LAMINATE SAMPLES GROUPED BY TIME EXPOSURE

56 APPENDIX B
NAWCADPAX--99-112-TR

IM6/977-3 Quasi-lsotropic Laminate

Temperature at Max Rate of Weight Loss
440

Ü 430

V. 420
at
a.
E
ai -♦ Dry
410
-■ Ambient
-A-- Saturated

400
in o in in o in in
s o CM ■* o CM o
z in in m CD
CM CM CM CM
tn in in ID

Exposure Temp [°F]-Time [min]

Figure B-13
COMPARISON OF THE TEMPERATURE AT WHICH THE MAXIMUM RATE OF
WEIGHT LOSS OCCURS FOR THE QUASI-ISOTROPIC LAMINATE SAMPLES
GROUPED BY TEMPERATURE EXPOSURE

IM6/977-3 Quasi-lsotropic Laminate

Temperature at Max Rate of Weight Loss
440

u 430
*—* iV
(B
^
3
a 420
w
a>
a
E -♦—Dry
0)
1- 410
-■—Ambient
-A-- Saturated

400
in in o in in in
o o CM

CO

Exposure Temp [°F]-Time [min]

Figure B-14
COMPARISON OF THE TEMPERATURE AT WHICH THE MAXIMUM RATE OF
WEIGHT LOSS OCCURS FOR THE QUASI-ISOTROPIC LAMINATE SAMPLES
GROUPED BY TIME EXPOSURE

57 APPENDIX B
NAWCADPAX-99-112-TR

~i—i—i—i—|—i—i—i—i—|—i—i—i—i—|—i—i—i—i—|—i—i—i—r-

© 525°F (274"C) exposure

• - 575°F (302°C) exposure
■- - 625-F (328°C) exposure

0.92
i i I i i i i_

10 20 30 40 50
exposure time (min)

Figure B-15
DEGREE OF CONVERSION VALUES FOR THE 977-3 NEAT RESIN SAMPLES
DRIED PRIOR TO HEAT DAMAGE

■ ■ ■ ■ ■ ■ ■

240 -9— 525°F (274°C) exposure

-• - 575°F (302°C) exposure
Wh - 625°F (328-Ci exposure
220 -—e
200
p
J» 180
160

140

120
10 20 30 40 50
exposure time (min)

Figure B-16
GLASS TRANSITION MEASUREMENTS FOR THE 977-3 NEAT RESIN SAMPLES
DRIED PRIOR TO HEAT DAMAGE

58 APPENDIX B
NAWCADPAX--99-112-TR

230
220
210
200
o
o 190
180
170
-6— 525°F (274°C) exposure
-# - 575°F (302°C) exposure
160 Wh - 625°F (328°C) exposure

150 ■ ■ I ■ I I I I I i I I i i i i

0 10 20 30 40 50
exposure time (min)

Figure B-17
GLASS TRANSITION MEASUREMENTS FOR THE 977-3 NEAT RESIN SAMPLES
SATURATED PRIOR TO HEAT DAMAGE

59 APPENDIX B
NAWCADPAX-99-112-TR

Figure B-18
977-3 NEAT RESIN SAMPLES AFTER ENVIRONMENTAL
AND THERMAL EXPOSURE

60 APPENDIX B
NAWCADPAX-99-112-TR

Figure B-19
UNIDIRECTIONAL SAMPLES AFTER ENVIRONMENTAL
AND THERMAL EXPOSURE

61 APPENDIX B
NAWCADPAX-99-112-TR

Figure B-20
QUASI-ISOTROPIC SAMPLES AFTER ENVIRONMENTAL
AND THERMAL EXPOSURE

62 APPENDIX B
NAWCADPAX-99-112-TR

Figure B-21
SATURATED 977-3 NEAT RESIN COUPONS 9-525-5-S, 9-576-5-S, AND 9-623-5-S
(FROM TOP TO BOTTOM) SHOWING INCREASING DAMAGE DUE
TO INCREASING THERMAL EXPOSURE

Figure B-22
SPALONG DUE TO OUT-GASSING IN 977-3 HEAT-DAMAGED NEAT RESIN

63 APPENDIX B
NAWCADPAX-99-112-TR

Figure B-23
AMBIENT (LEFT) AND SATURATED (RIGHT) CONDITIONED IM6/977-3
UNIDIRECTIONAL COMPOSITES EXPOSED FOR 45 MIN AT 625°F

5 min 20 min 45 min

Dry 274°C

■
Conditioning 302°C
328°C KEY TO DAMAGE

■1
5 min 20 min 45 min No Damage
Ambient 274°C ^H | Mild Damage
Conditioning 302°C ^H 1 Moderate Damage
328°C M Total Damage
5 min 20 min 45 min
Saturated 274°C
Conditioning 302°C
328°C M

Figure B-24
DEGREE OF DAMAGE RATING FOR 977-3 NEAT RESIN
VISUAL INSPECTION RESULTS

64 APPENDIX B
NAWCADPAX-99-112-TR

O0
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65 APPENDIX B
NAWCADPAX-99-112-TR

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66 APPENDIX B
NAWCADPAX-99-112-TR

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67 APPENDIX B
NAWCADPAX-99-112-TR

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68 APPENDIX B
NAWCADPAX-99-112-TR

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69 APPENDIX B
NAWCADPAX-99-112-TR

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70 APPENDIX B
NAWCADPAX-99-112-TR

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71 APPENDIX B
NAWCADPAX--99-112-TR

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72 APPENDIX B
 NAWCADPAX-99-112-TR

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73 APPENDIX B
NAWCADPAX--99-112-TR

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74 APPENDIX B
NAWCADPAX-99-112-TR

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75 APPENDIX B
NAWCADPAX-99-112-TR

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76 APPENDIX B
NAWCADPAX-99-112-TR

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77 APPENDIX B
NAWCADPAX-99-112-TR

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78 APPENDIX B
NAWCADPAX-99-112-TR

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82 APPENDIX B
NAWCADPAX--99-112-TR

Degree of Damage Detected by Ultrasonic C-Scan

<25%
[
25%-50% 50-75% 75-100% Total Damage
977-3 Neat Resin Unidirectional Ouasi-Isotropic
5 min 20 min 45 min 5 min 20 min 45 min 5 min 20 min 45 min
525°F 525°F 525°F
Dry 575°F
575°F
Conditioning:575°F
625°F 625°F 625°F

5 min 20 min 45 min 5 min 20 min 45 min 5 min 20 min 1 45 min

1 1
1
Ambient 525°F
Conditioning 575°F
625°F
5 min 20 min 45 min
525°F
Saturated
Conditioning 575°F
625'

Figure B-43
DEGREE OF DAMAGE DETECTED BY ULTRASONIC C-SCAN

Degree of Damage Detected by Thermography

<25% 25%-50% 50-75% 75-100% Total Damage

977-3 Neat Resin Unidirectional Ouasi-Isotropic
5 min 20 min 45 min 5 min 20 min 45 min 5 min 20 min 45 min
525°F
Dry
Conditioning 575°F
625°F

5min 20 min 45 min 5 min 20 min 45 min 5min 20 min 45 min

525°F 525°F 525°F
Ambient
575°F 575°F 575°F
625°F 625°F 625°F

5 min 20 min 45 min 5 min 20 min 45 min 5 min 20 min 45 min

525°F liiifill 525°F 525°F
Saturated
575°F
Conditioning 575°F 575°F
625°F i^o ^o^^is" ^ä..^^^^^^^B
625°F ^H 625°F ^H
Figure B-44
DEGREE OF DAMAGE DETECTED BY THERMOGRAPHY

83 APPENDIX B
NAWCADPAX-99-112-TR

977-3 Neat Resin

Saturated Exposures
40.0 -♦-274 [°C]
-«-302 [°C]
Ö) 30.0 ±-329 [°C]
c
0)

</) w
20.0
(8 *—

1 io.o

0.0
10 20 30 40
Exposure Time [min]

Figure B-45
FLEXURE RESULTS FOR SATURATED 977-3 NEAT RESIN COUPONS

977-3 Neat Resin

Dry Exposures
40.0 ♦-274 [°C]
«-302 [°C]
O) 30.0 A-329 [°C]
c
0)

C/> w
20.0
(0

1
2 oo

0.0
10 20 30 40
Exposure Time [min]

Figure B-46
FLEXURE RESULTS FOR DRY 977-3 NEAT RESIN COUPONS

84 APPENDIX B
NAWCADPAX--99-112-TR

977-3 Neat Resin

Ambient Exposures
40.0 ♦-274 [°C]
»-302 [°C]
*-329 [°C]
O) 30.0
c
CD

W OT
20.0
CO
l_
3
X 10.0
0)

0.0
10 20 30 40
Exposure Time [min]

Figure B-47
FLEXURE RESULTS FOR AMBIENT 977-3 NEAT RESIN COUPONS

IM6/977-3 Quasi-lsotropic
Saturated Exposures
250.0 -♦-274 [°C]
-»-302 [°C]
£ 200.0
O) A-329 [°C]
c
CD
£ -- 150.0

75 — ioo.o
3
X
ü 50.0
u_
0.0
10 20 30 40
Exposure Time [min]

Figure B-48
FLEXURE RESULTS FOR SATURATED IM6/977-3 QUASI-ISOTROPIC COUPONS

85 APPENDIX B
NAWCADPAX-99-112-TR

IM6/977-3 Quasi-lsotropic
Dry Exposures
250.0 274 [°C]

£ 200.0
c
0)
£ ^ 150.0

"Jo -J 100.0
3
X
2. 50.0
u.
0.0
10 20 30 40
Exposure Time [min]

Figure B-49
FLEXURE RESULTS FOR DRY IM6/977-3 QUASI-ISOTROPIC COUPONS

IM6/977-3 Quasi-lsotropic
Ambient Exposures
r
250.0

£: 200.0
c
<D
£ " 150.0

75
i_
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3
X
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0.0
10 20 30 40
Exposure Time [min]

Figure B-50
FLEXURE RESULTS FOR AMBIENT IM6/977-3 QUASI-ISOTROPIC COUPONS

86 APPENDIX B
NAWCADPAX-99-112-TR

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NAWCADPAX--99-112-TR

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92 APPENDIX B
NAWCADPAX--99-112-TR

12.00

10.00

^ 8.00

■; 6.oo

■* . ««
* 4.00
Q.

2.00 ■Carbonyl j
•Carbon Dioxide!
0.00
280 300 320 340 360 380
Isothermal Temperature

Figure B-57
PEAK HEIGHT OF CARBONYL AND CARBON DIOXIDE VERSUS TEMPERATURE

12.00

10.00

^ 8.00
4*
JZ

■; 6.oo
X y = 0.5628X - 0.0255
t 400 R2 = 0.998
ft.
■Carbonyl
2.00 Carbon Dioxide
■Linear (Carbonyl);
0.00
0.00 5.00 10.00 15.00 20.00
% Weight Loss

Figure B-58
PEAK HEIGHT OF CARBONYL AND CARBON DIOXIDE VERSUS WEIGHT LOSS

93 APPENDIX B
NAWCADPAX--99-112-TR

4.50
-0.0282X + 4.1481
R2 = 0.9777
4.00
en
E
3.50
.5*
*
it 3.00
19
0.
♦ Carbonyl
2.50
■ Carbon Doxide
— Linear (Carbonyl)
2.00
10 20 30 40 50
Damage Time

Figure B-59
UNDAMAGED VERSUS 315°C DAMAGED PEAK HEIGHT VERSUS DAMAGE TIME

1 * M- t t ♦

I I ! I 4 I I

W (b)
Figure B-60
(a) STRESS DISTRIBUTION NEAR FIBER BREAK (b) CHAIN-OF-BUNDLES MODEL

94 APPENDIX B
NAWCADPAX-99-112-TR

Qr

Figure B-61
EQUIVALENT STEP FUNCTION LENGTH FOR 8E

2a

■— x !=2r

Figure B-62
BROKEN FIBER IN INTACT FIBER RING SHOWING CRACKED
FIBER/MATRIX INTERFACE OF LENGTH 2a

Figure B-63
NONDIMENSIONAL STORAGE MODULUS g AS A FUNCTION OF TEMPERATURE
FOR HERCULES 3501-6 (gh) AND FIBERITE 977-3 (gf)

95 APPENDIX B
NAWCADPAX-99-112-TR

977-3 Neat Resin

Moisture Condition: Ambient

ü
^iS^i-i^iiiipSäH^

.6b5*F-Ö5itifc ^525:^ -.20» 525:"*■- 45 min

:;57;6i°j=:-;:05 rhini 576^20« -576 °F-45 min

Total Damage
(Sample Crumbled

■sfc* dm Upon Cooling)

:- 623 ^F - Co rirtin " Ks^aoÄSiv 623?Fi45;miri

DARKER AREAS ARE WOREDAMAGED

Figure B-64
C-SCANS OF FIBERITE 977-3 NEAT RESIN EPOXY SAMPLES SHOWING EFFECT
OF TEMPERATURE AND TIME AT TEMPERATURE

(a) (b)

Figure B-65
(a) HEAT-INDUCED CRACKS IN 3501-6 RESIN EXPOSED FOR 15 MIN AT 260°C
(b) OUT-GASSING VENTS IN WOVEN Gr/Ep LAMINATE EXPOSED
FOR 3.3 MIN AT 370°C

96 APPENDIX B
NAWCADPAX--99-112-TR

ym&m AND SHO(RT»TH*E TO »o*e

%m L0NS-

Figure B-66
RESIDUAL NONDIMENSIONAL FATIGUE STRENGTH, S, VERSUS CYCLES, N

Figure B-67
NONDIMENSIONAL FATIGUE STRENGTH, S, VERSUS CYCLES, N; MATRIX
GONE IN ZONE LENGTH b,

97 APPENDIX B
NAWCADPAX-99-112-TR

THIS PAGE INTENTIONALLY LEFT BLANK

98
NAWCADPAX--99-112-TR

APPENDIX C
THERMAL GRAVIMETRIC ANALYZER PLOTS

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