Fermilab-TM-2366-A

Measurement of mechanical properties of three epoxy adhesives at

cryogenic temperatures for CCD construction
H. Cease, P.F. Derwent, H.T. Diehl, J. Fast, D. Finley
Fermi National Accelerator Laboratory
Batavia IL 60510

November 6, 2006

Abstract

Materials testing of an adhesive for bonding Silicon to a substrate is presented. Test results
include Young’s Modulus, Poisson’s Ratio, and the coefficient of thermal expansion at temper-
atures ranging from room temperature to 100 K. Data for 3 epoxies (Tra-Con F113, Epotek
301-2, Hysol 9361) are presented.

1 Introduction
The SNAP CCD focal plane has to meet stringent performance requirements, especially on
flatness. As the CCDs are manufactured at room temperature and will operate at 130 K in
space, it is necessary to characterize their behavior as a function of temperature. In addition, it
is expected that the CCD focal plane will undergo thermal cycles in space. As the construction
materials (Si, AlN, SiC) have different coefficients of thermal expansion (CTE), there may
be stress on all of the epoxy joints. NASA has criterion on the stress/strength relation for
such joints [1]. This note details tensile strength tests and coefficient of thermal expansion
measurements on proposed epoxies for use in the CCD assembly.
Tensile strength tests to measure Young’s Modulus and Possion’s Ratio [2] were performed
at Precision Measurements and Instruments Corporation (PMIC) [3] at 5 temperatures (295K,
250K, 200K, 150K, 100K). An additional measurement was made at Fermilab at 295K. Mea-
surements of the CTE from 77 K to 295 K were made at Fermilab.
Three epoxies were measured, Hysol 9361, Tra-Con F113, and Epotek 301-2. The Hysol is
being considered for the AlN-SiC joint, the Tra-Con and Epotek for the CCD-AlN joint. In
Table 1, we summarize the properties of the glue joints as reported by the manufacturer.
The Hysol sets in 24 hours, with a full cure in 7 days at room temperature. The epoxy samples
used in the tensile strength tests had a 7 day cure. For the Hysol CTE measurements, we used
a sample with am accelerated 2 day cure. For the Epotek and Tra-Con CTE measurements,
measurements were made with samples with both a 2 day cure and a 7 day cure. The Epotek
epoxy has an additional manufacturing specification on residuals ions (salts) in the resin which
is important for silicon bonding applications.

1
 Epoxy Modulus Viscosity CTE @ 295 K
Hysol 9361 723 MPa 1000 Pa s -
Tra-Con F113 - 180 cps @25 C 55 ppm/C
Epotek 301-2 - 225-425 cps 37 ppm/C

Table 1: Epoxy properties as provided by the manufacturers.

Ambient
Elastic Modulus (psi) 356886± 12523 3.51%
Tra-Con F113 Poisson’s Ratio 0.401±0.003 0.64%
Maximum Stress (psi) 2539± 86 3.40%
Elastic Modulus (psi) 531427± 6166 1.16%
Epotek 301-2 Poisson’s Ratio 0.358±0.001 0.35%
Maximum Stress (psi) 3751± 45 1.21%
Elastic Modulus (psi) 154678± 1526 0.99%
Hysol 9361 Poisson’s Ratio 0.433±0.007 1.67%
Maximum Stress (psi) 1153± 9 0.77%

Table 2: Epoxy properties as measured at ambient temperatures.

2 Tensile Tests
Tensile tests were performed by PMIC and also the Fermilab Material Testing Group. Both
tests used samples prepared at Fermilab. The samples were dogbone shaped and machined out
of cast plates of epoxy. The samples were degassed to minimize the number and size of air
bubbles. We note that the Hysol samples did have visible bubbles on the machined surfaces.
PMIC measurements were performed per ASTM method D-638. Five dogbones of each
epoxy were measured at 5 temperatures (295K, 250K, 200K, 150K, 100K). The sample modulus
was calculated using the Secant Method at a 0.68% strain (or the highest strain achieved if the
sample failed before that level). The Hysol samples did fail before 0.68% strain was achieved
for the lower temperature measurements. Tables 2, 3, 4, 5, and 6 summarize the measurements.
The full report from PMIC is included as Appendix 1.
The Fermilab Material Testing group also performed a tensile measurement at ambient tem-
perature on the three epoxies. The steepest slope over a series of ranges was used to calculated

250 K
Elastic Modulus (psi) 519361± 16547 3.19%
Tra-Con F113 Poisson’s Ratio 0.372 ± 0.005 1.25%
Maximum Stress (psi) 3527± 120 3.41%
Elastic Modulus (psi) 595903± 16547 3.19%
Epotek 301-2 Poisson’s Ratio 0.365 ± 0.004 1.05%
Maximum Stress (psi) 4115± 79 1.91%
Elastic Modulus (psi) 239242± 4375 1.83%
Hysol 9361 Poisson’s Ratio 0.435 ± 0.004 1.02%
Maximum Stress (psi) 1736± 35 2.02%

Table 3: Epoxy properties as measured at 250 K.

2
 200 K
Elastic Modulus (psi) 615588± 26807 4.35%
Tra-Con F113 Poisson’s Ratio 0.368 ± 0.003 0.69%
Maximum Stress (psi) 4272± 198 4.64%
Elastic Modulus (psi) 648860± 12482 1.92%
Epotek 301-2 Poisson’s Ratio 0.349 ± 0.005 1.32%
Maximum Stress (psi) 4471± 99 2.22%
Elastic Modulus (psi) 560786± 11976 2.14%
Hysol 9361 Poisson’s Ratio 0.357 ± 0.005 1.27%
Maximum Stress (psi) 3912± 84 2.15%

Table 4: Epoxy properties as measured at 200 K.

150 K
Elastic Modulus (psi) 886035± 40429 4.56%
Tra-Con F113 Poisson’s Ratio 0.367 ± 0.008 2.28%
Maximum Stress (psi) 5983± 264 4.42%
Elastic Modulus (psi) 833220± 14089 1.69%
Epotek 301-2 Poisson’s Ratio 0.334 ± 0.007 2.16%
Maximum Stress (psi) 5681± 106 1.87%
Elastic Modulus (psi) 822654± 14072 1.71%
Hysol 9361 Poisson’s Ratio 0.357 ± 0.012 3.46%
Maximum Stress (psi) 4641± 79 1.71%

Table 5: Epoxy properties as measured at 150 K.

100 K
Elastic Modulus (psi) 1105895± 40675 3.69%
Tra-Con F113 Poisson’s Ratio 0.348 ± 0.005 1.44%
Maximum Stress (psi) 7092± 649 9.15%
Elastic Modulus (psi) 1014310± 14384 1.42%
Epotek 301-2 Poisson’s Ratio 0.350 ± 0.008 2.34%
Maximum Stress (psi) 6783± 162 2.39%
Elastic Modulus (psi) 1132056± 13051 1.19%
Hysol 9361 Poisson’s Ratio 0.353 ± 0.016 4.55%
Maximum Stress (psi) 4225± 201 4.76%

Table 6: Epoxy properties as measured at 100 K.

3
 Ambient
Elastic Modulus (ksi) 384.84 ±85.7 22.2%
Tra-Con F113 Ultimate Tensile Strength (psi) 4798.2±569.1 11.9%
Elastic Modulus (ksi) 650.6± 176.2 % 27.1
Epotek 301-2 Ultimate Tensile Strength (psi) 9664.2±1769.6 18.3%
Elastic Modulus (ksi) 137.5± 17 12.3%
Hysol 9361 Ultimate Tensile Strength (psi) 2400.4± 190.6 7.94%

Table 7: Epoxy properties as measured at ambient temperatures by the Fermilab Ma-

terial Properties Testing group.

the modulus. The crosshead pull speed was greater than 0.05 inches per minute. The results
are summarized in Table 2.

3 Coefficient of Thermal Expansion Measurements

CTE measurements were made at Fermilab. The measurements were performed in the spirit of
ASTM-E831. Samples were approximately 8 mm × 8 mm × 20 mm, machined from samples
cast in a mold. Each sample was vacuum degassed during the casting to minimize the size and
number of trapped gas bubbles.
The CTE was measured by placing the sample in a holder inside of a cryostat. Liquid
nitrogen is poured into the cryostat. Once the temperature stabilized at 77 K, a heater is used
to ramp the temperature to ambient temperature with a rate of 1-2deg C/minute. An LVDT [4]
at the top of the sample measured the change in sample length. The length and temperature
were recorded during the cooldown and the warmup. In Figure 1, we show a picture of the
sample in the holder. The LVDT is at the top of the picture, connected via quartz rods to
the sample holder. The sample holder is installed inside the cryostat. We report the integral
fractional change in length (dL/L) of the sample as a function of temperature in Table 8. In
Figures 2, 3, and 4, we show the fractional change in length as a function of temperature for one
sample of Tra-Con F113, Epotek 301-2, and Hysol 9361. In Figure 5, we show a representative
time ramp for one of the measurements.

4 Stress/Strength Ratios
The NASA guideline for epoxy joints [1] is a safety margin of a factor of 2 on the stress. With
the measured modulus and CTE, we can calculate the expected stress on the joint and compare
to yield strength, using the following logic:

Stress
Modulus =
Strain
dL
Strain = (1)
L
dL
(epoxy) = CTE (epoxy) × ∆T
L
With the assumption that the CTE of the substrate is small compared to the epoxy, the stress
on the joint is simply:

Stress = Modulus × CTE (epoxy) × ∆T (2)

4
Figure 1: The sample holder for use in the dL/L measurements.

5
 Ambient Temperature
Tra-Con F113 dL/L (×10−3 ) – –
−3
Epotek 301-2 dL/L (×10 ) – –
Hysol 9361 dL/L (×10−3 ) – –
250 K
Tra-Con F113 dL/L (×10−3 ) -3.27 ± 0.13 3.94%
Epotek 301-2 dL/L (×10−3 ) -2.83 ± 0.04 1.52%
−3
Hysol 9361 dL/L (×10 ) -4.69 ± 0.04 0.8%
200 K
Tra-Con F113 dL/L (×10−3 ) -6.20 ± 0.11 1.73%
Epotek 301-2 dL/L (×10−3 ) -5.45 ± 0.03 0.59%
Hysol 9361 dL/L (×10−3 ) -8.69 ± 0.02 0.3%
150 K
Tra-Con F113 dL/L (×10−3 ) -8.71 ± 0.06 0.76%
Epotek 301-2 dL/L (×10−3 ) -7.70 ± 0.11 1.37%
Hysol 9361 dL/L (×10−3 ) -11.3 ± 0.003 0.2%
100 K
Tra-Con F113 dL/L (×10−3 ) -10.7 ± 0.08 0.72%
Epotek 301-2 dL/L (×10−3 ) -9.66 ± 0.18 1.88%
−3
Hysol 9361 dL/L (×10 ) -13.3 ± 0.03 0.2%

Table 8: Integral dL/L for the three epoxies as measured at the 5 temperatures.

Figure 2: The integral dL/L vs temperature for a representative Tra-Con F113 sample.

6
Figure 3: The integral dL/L vs temperature for a representative Epotek 301-2 sample.

Figure 4: The integral dL/L vs temperature for a representative Hysol 9361 sample.

7
 Figure 5: The temperature vs time for a representative CTE measurement.

Ambient 250 K 200 K 150 K 100 K

Tra-Con F113 – 2.8 1.1 0.76 0.65
Epotek 301-2 – 5.9 2.7 1.5 1.0
Hysol 9361 – 2.1 0.83 0.5 0.29

Table 9: The ratio of strain to stress as defined in equation 3.

A criterion that the yield strength must be more than twice the stress leads to the requirement
that

yield strength (epoxy)

> 2. (3)
Modulus × CTE (epoxy) × ∆T
The stress reported in the data sets is not the epoxy yield strength, it is the strength at
0.68% strain. A conservative guideline can still be determined if the maximum stress achieved
is used in the calculations as a proof stress. We will use either the room temperature ultimate
strength or the maximum stress applied to the sample at temperature, whichever is larger. As
the strength is known to increase with decreasing temperature, this selection is a conservative
approach. In Table 9, we show the ratio of strength over stress as defined above.
The Epotek has the lowest bond strain and, at ambient temperature, the highest ratio
of maximum strength to strength at 0.68%. Although none of the epoxies meet the criteria
for temperatures below 200 K, it does not mean the joint will fail. We have chosen to take a
conservative approach in the calculation of the maximum stress. In addition, the tensile strength
data collected was taken at high pull rates (0.10 inch/minute for the PMIC tests). Epoxies, as
with most plastics, are visco-elastic materials which respond differently based on how quickly
the load is transferred to the material. The high rates of strain applied to the samples during
testing will have a much higher modulus and stress than in the actual application. During
flight, the CCD focal plane will have a cool down rate of 3 degrees per minute, taking at least
20 minutes to achieve operating temperature and allowing the epoxy to creep and relieve some

8
of the stresses.

5 Conclusions
We have presented measurements on epoxy properties for use in the SNAP CCD assembly,
covering temperatures from ambient to 100 K. Test results on Young’s Modulus, Poisson’s
Ratio, and integral dL/L have been presented. A criterion for the epoxy has been proposed.

References
[1] NASA-STD-5001 - Structural Design and Test Factors of Safety for Spaceflight Hardware
[2] Young’s Modulus is the ratio of tensile stress to tensile strength and is a measure of how
a material changes length under tension or compression. Poisson’s Ratio is defined as the
strain normal to an applied load divided by the strain in the direction of the applied load
and is a measure of the material’s tendency to get thinner as it is stretched or thicker as it
is compressed.
[3] Precision Measurements and Instruments Corporation, 3665 SW Deschutes Street, Corval-
lis, OR 97333
[4] LVDT stands for Linear Variable Differential Transformer, outputting a voltage dependent
upon physical displacement.

9
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