22 Stevenson

Methods for the Evaluation of Carbon Based
Composite Surfaces for Subsequent Adhesive

Bonding
Bill Stevenson
Dept. of Chemistry
Wichita State University
PASTE
SCHOOL
LOGO
HERE
The Joint Advanced Materials and Structures Center of Excellence
Water uptake, cure state and kinetic evaluation of
candidate prepregs for composite repair
• Motivation and Key Issues - To help US Aero Space

manufacturers of large composite parts produce and maintain a better
product in a more cost effective manner
• Objective - To remove some of the qualitative judgements that

have to be made concerning composite repair and replace them with
quantitative measurements
• Approach - To adapt spectroscopic based technology for the

analysis of cure state and water content in composites and to transfer
this technology to industry
The Joint Advanced Materials and Structures Center of Excellence 2

FAA Sponsored Project
Information
Principal Investigators & Researchers

• William T.K. Stevenson1, Irish Alcalen1, Sarah Hall1, Lamia Salah2, John Tomblin2, Mike
Borgman3, Robert Bohaty4, Dennis Burns1
• 1. Chemistry, Wichita State U, (Bill.Stevenson@wichita.edu)
• 2. NIAR, Wichita State U.
• 3. Spirit AeroSystems, Wichita, KS - contractor
• 4. Spirit AeroSystems, Wichita, KS
FAA Technical Monitor

• Curt Davies
Other FAA Personnel Involved
• Larry Ilcewicz
Industry Participation
• Spirit AeroSystems

Topics
Diffuse Reflectance Near IR spectroscopy for composite
surface water content
Diffuse Reflectance Near IR spectroscopy for surface resin
cure state
Diffuse Reflectance Near IR spectroscopy for prepreg aging
studies
Contact angle measurement with mechanical testing
Candidate repair prepreg analysis and cure


Water uptake, cure state, surface free energy
analysis, and kinetic evaluation of candidate
prepregs for composite repair
Near IR studies
Background

A composite sample is placed on top of the integrating

sphere module for analysis
Antares II
1. Transmission
module 2
2. Integrating
sphere 3 1
reflectance
module
3. Remote
triggered
diffuse
reflectance
module

0.40 1.00
0.90
0.35
0.80
0.30
0.70
0.25 0.60
0.20 0.50
0.40
0.15
0.30
0.10
0.20
0.05 0.10
0.00 0.00
10000 9000 8000 7000 6000 5000 4000 10000 9000 8000 7000 6000 5000 4000
0.50 0.45
0.45
0.40
0.40
0.35
0.35
0.30
0.25 0.30
0.20
0.15 0.25
0.10
0.20
0.05
0.00 0.15
10000 9000 8000 7000 6000 5000 4000 10000 9000 8000 7000 6000 5000 4000
All x – wavenumbers (cm-1) All y – absorbance. Lomod thermoplastic elastomer (3.01mm thick), upper left
– near IR spectrum in transmission, lower left - diffuse reflectance near IR spectrum obtained using the
integrating sphere module. Uncured 934/T300 prepreg (1 layer), upper right – near IR spectrum in
transmission, lower left - diffuse reflectance near IR spectrum obtained using the integrating sphere
module.

Conventional calibration curve – peak area is ratioed to

near IR my720-dds resin
that of an invariant peak after baseline correction 1.00
0.75 mm
0.90 0.93 mm
uncorrected vs baseline corrected spectra for wet Toray T300/934 1.04 mm
resin composite 0.80 1.49 mm
2.0 2.00 mm
0.70 2.70 mm
1.8 uncorrected spectrum
3.38 mm
absorbance
baseline corrected spectrum
1.6 0.60 4.29 mm
arbitrary units
6.75 mm
1.4
0.50 0.09 mm
1.2 0.63 mm
1.0 0.40
0.8 0.30
0.6
0.20
0.4
0.2 0.10
0.0
0.00
10000 9000 8000 7000 6000 5000 4000
10000 9000 8000 7000 6000 5000 4000
wavenumbers wavenumbers
Chemometrics calibration curve – second derivative

spectra are subjected to partial least squares analysis Second derivative spectra of curing T800/3900 prepr
0.0010
uncorrected vs second derivative spectra for wet Toray T300/934 resin
composite 59% cured
uncured
2.0
0.0005
1.8 uncorrected spectrum
second derivative spectrum
1.6
arbitrary units
1.4
0.0000
1.2
1.0
0.8
-0.0005
0.6
0.4
0.2 -0.0010
0.0
10000 9000 8000 7000 6000 5000 4000
wavenumbers -0.0015
4800.00 4700.00 4600.00 4500.00 4400.00
wavenumbers
(Top left) Conventional diffuse reflectance and baseline corrected diffuse reflectance spectra of wet
934/T300 prepreg. (Top right) conventional diffuse reflectance spectra of MY720-DDS resin versus plaque
thickness. (Bottom left) Conventional diffuse reflectance and second derivative spectrum of 934-T300
prepreg. (Bottom right) Second derivative spectrum of curing T800/3900 prepreg.

Near IR studies
Water uptake
and desorption

1.00
0.90
OH
O 0.80
[ ]n
Absorbance
O O O O O 0.70
0.60
0.50
0.40
Mid performance engineering epoxy resin NH2 NH2
0.30
(top) diglycidyl ether of bisphenol A (DGEBA)
0.20
(left) meta phenylene diamine (mPDA)
NH2 0.10
(right) para phenylene diamine (pPDA)
0.00
NH2
10000 9000 8000 7000 6000 5000 4000
Wavenumber (cm‐1)
(Left) DGEBA/m&pPDA resin constituents. (Right) Near IR spectrum of the resin before (hatched
line) and after (full line) exposure to water. The arow denotes the absorption band at 5215 cm-1
attributed to water in the resin

1 1
Normalized peak area

0.5 sample1 0.5

sample2
sample1
sample3 sample2
sample4 sample3
sample5 sample4
sample6 sample5
sample6
0 0
0 0.5 1 1.5 2 2.5 3 0 0.5 1 1.5 2 2.5
% water content % water content
Chemometrics calibration Curve for Water uptake in 825/mpd/ppd resin Chemometrics calibration Curve for Water uptake in 825/mpd/ppd resin
3 3
2.5 2 2.5 2
R = 0.9941 R = 0.9941
2 2
Calculated
Calculated
1.5 1.5
1 1
0.5 0.5
0 0
0 0.5 1 1.5 2 2.5 3 0 0.5 1 1.5 2 2.5
Actual Actual
(Top left) Beeer plot of normalized absorbance at 5215 cm-1 versus water content during water uptake.
(Top right) Similar plot but obtained during water desorption cycle. (Bottom left) Chemometrics calibration
plot for water absorption. (Bottom right) Chemometrics calibration plot for water desorption

O O
1.00
H2
0.90
N C N
0.80
O 0.70
Absorbance
O
0.60
H 2N 0.50
0.40
0.30
High performance epoxy resin O 0.20
(top) TGDDM (MY720) resin S 0.10
(right) DDS curative O 0.00
10000 9000 8000 7000 6000 5000 4000
-1
H 2N Wavenumber (cm )
(Top left) MY720 and DDS resin constituents. (Top right) Near IR spectrum of the resin before
(hatched line) and after (full line) exposure to water. The arow denotes the absorption band at 5215
cm-1 attributed to water in the resin

3 3
Normallized peak area

2 2
sample 1 sample 1
sample2 sample 2
1 1 sample 3
sample3
sample4 sample4
sample5 sample5
sample6 sample6
0 0
0 2 4 6 0 2 4 6
Chemometrics Calibration Curve for Water uptake in Chemometrics Calibration Curve for Water uptake in
MY720/DDS resin MY720/DDS resin
6 6
5 5
R2 = 0.9919 R2 = 0.9919
Calculated
Calculated
4 4
3 3
2 2
1 1
0 0
0 1 2 3 4 5 6 0 1 2 3 4 5 6
Actual Actual
High performance MY720/DDS resin (Top left) Beer plot of normalized absorbance at 5215 cm-1 versus
water content during water uptake. (Top right) Similar Beer plot but obtained during water desorption
cycle. (Bottom left) Chemometrics plot for water absorption. (Bottom right) Chemometrics plot for water
desorption.
vacuum bag
breather
release film
peel ply
laminate
to vacuum
sealant tape
tool
release film
Sketch of vacuum bagging setup used to prepare small

plaques of prepreg for testing purposes.

1.00 1.00
0.80 0.80
Absorbance
0.60 0.60
0.40 0.40
0.20 0.20
0.00 0.00
10000 9000 8000 7000 6000 5000 4000 10000 9000 8000 7000 6000 5000 4000
Wavenumber (cm‐1) Wavenumber (cm‐1)
1.00
Tool face 0.80
Absorbanc
Resin rich
regions are 0.60
over
0.40
exposed
due to
0.20
charging
0.00
Bag face 10000 9000 8000 7000 6000 5000 4000
‐1
Wavenumber (cm )
Near IR spectrum of (Top left) 934/T300 cured woven composite tool face, (Top right) Near IR spectrum of
934/T300 cured woven composite bag face, (Bottom left) SEM of cross section of uncoated 934/T300
cured woven composite bag face down with resin rich regions overexposed. (Bottom right) Diffuse
reflectance near IR spectrum of cured T800/3900 composite bag face. Water at 5215 cm-1 is denoted by the
arrows
1.00
20

0.90 dry
5.57% water
0.80
0.70
15
absorbance
0.60
0.50 10 5 layers
0.40 7 layers
11 layers
0.30
5 layers-b
5
0.20 5 layers-c
0.10
0.00 0
10000 9000 8000 7000 6000 5000 4000
0 2 4 6 8 10
wavenumbers
% water content

10 20
5 layers
7 layers
8 2
R = 0.9922 11 layers
15 5 layers-b
Calculated
6 5 layers-c
5 layers-d
10
4
2 5
0
0 2 4 6 8 10 0
Actual 0 2 4 6 8
% water content
934/T300 composite - plots of normalized 5215 cm-1 peak areas versus water content (Top left) Near IR
spectrum of dry and wet composite with 5215 cm-1 peak arrowed (Top right) Normalized Beer plots during
water absorption cycle (Bottom left) Chemometrics plot during water absorption cycle (Bottom right)
Normalized Beer plots during water desorption cycle.


Normalized peak area 16 16
14 14 7 layers
12 12
10 10 11 layers
8 8
5 layers
6 5 layers-b
6
4 5 layers-c 4
2 5 layers-d 2
0 0
0 2 4 6 8 0 2 4 6 8
9
5.6

5.1 8
4.6 7
Calculated
Calculated
4.1 6 2
R = 0.9974
2
R = 0.9954
3.6 5
3.1 4
2.6 3
2.6 3.1 3.6 4.1 4.6 5.1 5.6 3 4 5 6 7 8
Actual Actual
934/T300 composite - plots of normalized 5215 cm-1 peak areas versus water content during water
desorption (Top left) Normalized Beer plot during water desorption cycle of 5 layer composite (Top right) )
Normalized Beer plot during water desorption cycle of 7 and 11 layer composite (Bottom left) Normalized
Chemometrics plot during water desorption from 5 layer composite (Bottom right) Normallized
Chemometric plot during water desorption from 7 and 11 layer composite
Near IR spectroscopy
Resin and composite
cure studies

1.00 1.00
0.80 0.80
Absorbance
Absorbance
0.60 0.60
0.40 0.40
Top – uncured
Middle – 42% cured
0.20 0.20
Bottom- 98% cured
0.00 0.00
10000 9000 8000 7000 6000 5000 4000 5000 4800 4600 4400 4200 4000
Wavenumber (cm-1) Wavenumber (cm-1)
adhesive-cure 1.2
0.3
1
0.25 R 2 = 0.987
Calculated
0.8
normalized peak a
0.2
0.6
0.15
0.4
0.1
0.2
0.05
0
0 0 0.2 0.4 0.6 0.8 1 1.2
0 0.2 0.4 0.6 0.8 1 1.2
degree cure
Actual
Fiberite FM377U aluminum filled adhesive cure. (Top left) Uncured Fiberite FM377U aluminum filled
adhesive with 4530 cm-1 band annotated. (Top right) Stacked spectrum for curing adhesive (Bottom left)
Fiberite Fm377U adhesive % cure by DSC versus (Beers law) normalized peak area at 4530 cm-1 (Bottom
right) Chemometrics calibration curve for adhesive cure. The 4350 cm-1 peak is indicated by the arrow.

1.20
uncured 934/T300 prepreg
1.00
1.00 Top – uncured
0.90 Middle – 42% cured
0.80 Bottom – 94% cured
Absorbance
0.80
0.70
0.60
absorbance
0.60
0.50
0.40
0.40
0.30 0.20
0.20
0.10
0.00
0.00
5000 4800 4600 4400 4200 4000
10000 9000 8000 7000 6000 5000 4000 Wavenumber (cm-1)
wavenumbers
934/T300 resin cure Chemometrics Calibration Curve for cure of T300/934

105 prepreg
30
95 R2 = 0.983
Calculated % cure
25
85
20
75
peak area
15
65
10 55
5 45
35
0
0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 35 45 55 65 75 85 95 105
degree cure actual % cure
934/T300 prepreg cure. (Top left) Uncured 934/T300 prepreg with 4530 cm-1 band annotated. (Top right)
Stacked spectrum for curing prepreg (Bottom left) 934/T300 prepreg % cure by DSC versus (Beers law)
normalized peak area at 4530 cm-1 (Bottom right) Chemometrics calibration curve for prepreg cure. The
4350 cm-1 peak is indicated by the arrow.
O
O O curing Toray T800/3900 prepreg
O
1.00
O NH2
0.90 uncured
N CH2
0.80 54% cured
72% cured
absorbance
0.70
0.60
O
0.50
N O SO 0.40
O O 0.30
0.20
0.10
0.00
NH2 5000 4800 4600 4400 4200 4000
wavenumbers
Chemometrics Calibration Curve for cure of T800/3900 prepreg

T800-3900 cure
2 1.05
1.8
normalized peak area
0.95
Calculated % cure
1.6
0.85 R2 = 0.9896
1.4
0.75
1.2
0.65
1
0.8 0.55
0.6 0.45
0.4 0.35
0.2 0.25
0 0.25 0.35 0.45 0.55 0.65 0.75 0.85 0.95
0 0.2 0.4 0.6 0.8 1
degree of cure Actual % cure
(top left) Components of T800/3900 prepreg. (top right) Spectra of curing prepreg. (bottom left) Beer plot
of cure versus normalized peak area (bottom right) Chemometrics plot for the cure reaction. The 4350 cm-1
peak is indicated by the arrow.


Surface Master 905 face adhesive Surface Master 905 face adhesive
0.14 0.14
0.12 0.12 uncured

uncured
34.52% cured
absorbance
0.10 0.10
absorbance
86.24% cured
0.08
0.08
0.06
0.06
0.04
0.04
0.02
0.02
0.00
0.00
10000 9000 8000 7000 6000 5000 4000 6000 5500 5000 4500
wavenumbers wavenumbers
Calibration Curve for Surface Master 905 Cure Calibration Curve for Surface Master 905 Cure
(Integrating Sphere) (Fiber Optic Probe)
1
1
0.9 0.9
0.8 0.8 R2 = 0.9921
0.7 0.7
Calculated
Calculated
0.6 R2 = 0.9877 0.6
0.5 0.5
0.4 0.4
0.3 0.3
0.2 0.2
0.1
0.1
0
0
-0.1 0 0.2 0.4 0.6 0.8
0.000 0.200 0.400 0.600 0.800 1.000
Actual Actual
(top left and top right) Cure of Surface Master 905 face adhesive by near IR spectroscopy. A comparison
of the performance of the diffuse reflectance probe (bottom left) and the integrating sphere probe (bottom
right) during cure of the adhesive. The 4350 cm-1 peak is indicated by the arrow.

Near IR spectroscopy
Prepreg aging studies

Correlation of chemometrics plots of second derivative spectra with prepreg Tg for uncured but aged
T800-3900 prepreg.
Surface analysis and repair of

contaminated T800-3900
composite

•T800-3900 composite is formed and scarfed

•Cleaned with acetone – lint free cloth
•Contaminated
•Cleaned with acetone – lint free cloth
•Surface free energy measured by contact angle analysis
•Repair made using ACG T800MTM-45 prepreg w Cytec
FM300-2 adhesive, 32 plies w 7.7 msi stiffness
•Subjected to tensile testing

Contaminents
Skydrol
Paint stripper
Jet fuel
Perspiration
Water
0%
25%
50%
75%

repair surfaces 10/1 & 20/1 scarfed
70
surface free energy (milliN/m)
60
50 Skydrol
Paint Stripper
jet fuel
40 perspiration
water 0%
30 water 25%
water 50%
water 75%
20 good surface for bonding
10
0
Contaminent

failure loadings, 10/1 scarf
60,000
53100+ 2100 lbs
50,000
Ultimate load (lbs)
40,000 Skydrol
Paint Stripper
jet fuel
30,000 perspiration
water 0%
water 75%
20,000 control
10,000
0
Contaminent

Characterization and cure

kinetics of T700-2510PW
prepreg, a candidate material for
the repair of epoxy based
composites

Structural analysis
Cure kinetics by DSC

•Ramped
•Isothermal
•Ramp and soak
DMA

Mid infrared
spectrum of
resin
extracted
from T700-
2510PW
prepreg

HNMR T700/2510 PW in CDCl3

Proton NMR of
T700-2510PW
prepreg with
DGEBA
resonances
arrowed
10 9 8 7 6 5 4 3 2 1 0
ppm

analysis, and kinetic evaluation of candidate prepregs
for composite repair
2.0
A 1.5
B A
Differential Heatflow (mW) - Endo Up

1.0
Scanning
0.5
0.0
Calorimeter -0.5
(DSC) -1.0
Output -1.5
0 10 20 30 40 50 60
Time (min)
B
Degree of Cure at time t, α = ------
A+B 34
Flores,
The Joint Advanced Materials and Structures Center of Excellence
Gandikota,
Cure of T700- degree of cure vs temperature (T700-5210PW prepreg)

2510PW Prepreg
under Ramped 1.2
conditions by
DSC 1
Extent of cure
0.8
degree of cure
1c/min
0.6 2c/min
3c/min
4c/min
5c/min
0.4
10c/min
15c/min
20c/min
0.2
0
80 100 120 140 160 180 200 220 240
temperature (C)

Degree of cure (α)

versus temperature
o
( C) for resin in T700-
2510PW prepreg and
resin in three other
common high
performance aviation
prepregs, all cured
under programmed
conditions at
5oC/min,

Rate of cure
(dα/dt) versus
temperature
(T) for T700-
2510PW
prepreg

Flynn Wall kinetics

⎛ − Ea ⎞
⎜ ⎟
K = Ae ⎝ RT ⎠
dα
= K [ f (α )]
dt
⎛ dα ⎞ ⎛ Ea ⎞ 1
ln ⎜ [ ( )]
⎟ = ln A + ln f α − ⎜ ⎟
⎝ dt ⎠ ⎝ R ⎠T

m=Ea/R

Ea versus
conversion (α)
for resin in
T700-2510PW
prepreg, M21
pultrusion
unitape, for
resin in
TORAYCA(IM3
50F) prepreg,
and for resin
in T300/934
prepreg

Plot of
conversion
(α) versus
time for
cure, over a
range of
isothermal
temperature
of T700-
2510PW
prepeg

Plot of rate
(dα/dt) versus
time for cure,
over a range of
isothermal
temperature of
T700-2510PW
prepeg

Kamal kinetic scheme for isothermal kinetics

dα/dt = (K1 + K2αm)(αf – α)m
Where…
K1 = rate constant for uncatalysed cure of resin
K2 = rate constant for cure of resin catalysed by
products
α = intermediate level of cure at isothermal
temperature
αf = ultimate level of cure at isothermal temperature
Isothermal experiments were performed from 120oC
to 180oC in 5oC increments
Plot of rate of cure versus

degree of cure for resin in
T700-2510PW prepreg at
140oC. Black squares –
experimental data, red line
– Kamal model prediction.
The gradient of the best fit
straight line is set to –
Ea1/R.
Poor fit to Kamal kinetics

External catalysis

Plot of rate of cure

versus degree of cure
for resin in T700-
2510PW prepreg at
180oC. Black squares –
experimental data, red
line – Kamal model
prediction.
Good fit to Kamal
kinetics
Relative effect of
external catalysis is
diminished

Plot of ln{K1}
versus 1/T for T700-
2510PW prepreg
using data points
collected at 150oC
or above. The
gradient of the best
fit straight line is
set to –Ea1/R.

Plot of ln{K2} versus

1/T for T700-2510PW
prepreg using data
points collected at
150oC or above. The
gradient of the best fit
straight line is set to
–Ea1/R.

Values of Ea1 and Ea2 for T700-2510PW prepreg calculated

according to the Kamal method.
All Kj/mole
System Ea1 Ea2
T300/934 53.8 (2 parameter) +~0
64.3 (1 parameter)
TORAYCA(IM350F) 74.7 53.8
T700-2510PW 102.5 96.3

Combined ramp and soak experiments were performed using T700-

2510PW prepreg using a method developed previously. The
experiment is summarized below
Ramp from room temperature Heat of reaction to Heat of reaction to soak

to soak temperature intermediate temperature = temperature = ΔH(Ts)
ΔH(Ti)
Fast cool to room temperature
Fast re-heat to soak
temperature
Isothermal at soak temperature Heat of reaction to Ultimate isothermal heat of
intermediate time = ΔH(ti) reaction = ΔH(t∞)
Fast cool to room temperature

Ramp to 300oC @ 3oC/min for Heat of reaction =ΔH(r)
residual cure

Examples
Extent of reaction to an intermediate cure temperature during the first ramp cycle
α = ΔH(Ti) / (ΔH(Ts) + ΔH(t∞) + ΔH(r) )
Extent of reaction to soak temperature

α = ΔH(Ts) / (ΔH(Ts) + ΔH(t∞) + ΔH(r) )
Extent of reaction at intermediate soak time

α = (ΔH(Ts) + ΔH(ti) ) / (ΔH(Ts) + ΔH(t∞) + ΔH(r) )
Ultimate extent of reaction after soaking to long times

α = (ΔH(Ts) + ΔH(t∞) ) / (ΔH(Ts) + ΔH(t∞) + ΔH(r) )

Ramp and
soak of
T700-
2510PW
prepreg to
125oC over a
range of
heating
rates.
Conversion
(α) versus
time

Ramp and soak of

T700-2510PW
prepreg to 125oC
over a range of
heating rates. Rate
of reaction (dα/dt)
versus time

Ramp and soak experiments were performed at

125, 130, 135, 140, 145, 150, and 155oC
it may be concluded that a good compromise

cure cycle, minimizing both reaction rates and
reaction time, may be constructed by heating to
150oC at 2oC/min followed by a 20 min soak at
that temperature.

Sample configuration for the DMA experiment

(Alpha Technologies ATD 2000 encapsulation rheometer)

1.0oC/min to 155oC & hold
DMA of uncured 1.0E+09 180
T700-2510PW 160
prepreg from G'

140
G'' X 10
room
Temperature (oC)
T (oC) 120
G', G" + 5E6
temperature to 100
155oC @ 1oC/min 5.0E+08
80
then held at 60
155oC for 120
40
min.
20
Temperature
0.0E+00 0
(oC), G’, and G” 0 50 100 150 200 250 300
are plotted as a Time (min)
function of time

DMA of uncured 1.0oC/min to 155oC & hold
T700-2510PW
5.0E+08 180
prepreg from
room 160
4.0E+08
temperature to G' 140
155oC @ 1oC/min
Temperature (oC)
T (oC) 120
G', G" + 5E6
3.0E+08
then held at 100
155oC for 120 80
2.0E+08
min.
60
Temperature (oC),
40
and G’, are 1.0E+08
20
plotted as a
function of time. 0.0E+00
0 50 100 150 200 250 300
0
Time (min)

Cure cycle Initial buildup of physical 100% cure achieved at

properties
1oC/min to 155oC & hold for 120 min 125oC on ramp segment 147oC on ramp segment
2oC/min to 155oC & hold for 120 min 134oC on ramp segment 6 min at 155oC soak temperature
2oC/min to 165oC & hold for 120 min 134oC on ramp segment 6 min at 165oC soak temperature
By comparing the results of DSC and DMA experiments, the gel point can be
approximated at 40-45 % conversion of T70/2510PW prepreg.

A Look Forward
• Benefit to Aviation
• Ability to accept/reject prepreg and adhesive “on the role”
• On site numerical based identification of water in composite
• Quantitative on site measurement of adhesive and composite
cure
• Future needs
• Low cost extension to develop new applications, complete FAA
– NIAR scarf repair project, and complete technology transfer
to Spirit AeroSystems (Doug Lewis) and other companies



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Methods for the Evaluation of Carbon Based

Composite Surfaces for Subsequent Adhesive

• Motivation and Key Issues - To help US Aero Space

• Objective - To remove some of the qualitative judgements that

• Approach - To adapt spectroscopic based technology for the

The Joint Advanced Materials and Structures Center of Excellence 2

Principal Investigators & Researchers

FAA Technical Monitor

The Joint Advanced Materials and Structures Center of Excellence 3

The Joint Advanced Materials and Structures Center of Excellence 4

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A composite sample is placed on top of the integrating

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Conventional calibration curve – peak area is ratioed to

Chemometrics calibration curve – second derivative

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Normalized peak area

0.5 sample1 0.5

% water content % water content

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Normallized peak area

Sketch of vacuum bagging setup used to prepare small

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Tool face 0.80

Normalized peak area

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934/T300 resin cure Chemometrics Calibration Curve for cure of T300/934

degree cure actual % cure

Chemometrics Calibration Curve for cure of T800/3900 prepreg

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0.12 0.12 uncured

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Surface analysis and repair of

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•T800-3900 composite is formed and scarfed

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repair surfaces 10/1 & 20/1 scarfed

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failure loadings, 10/1 scarf

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Characterization and cure

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Cure kinetics by DSC

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HNMR T700/2510 PW in CDCl3

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Differential Heatflow (mW) - Endo Up

Cure of T700- degree of cure vs temperature (T700-5210PW prepreg)

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Degree of cure (α)

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Flynn Wall kinetics