SANDIA REPORT

SAND99-8213 Unlimited Release Printed January 1999

Epoxy Foam Encapsulant: Processing and Dielectric Characterization

Linda Domeier and Marion Hunter

Prepared by Sandia National Laboratories Albuquerque, New Mexico 87185 and Livermore, California 94550 Sandia is a multiprogram laboratory operated by Sandia Corporation, a Lockheed Martin Company, for the UnJtedStates Department of Energy under Contract DE-AC04-94~~8jSOO0.

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SAN D99-8213 Unlimited Release Printed January 1999

Epoxy Foam Encapsulant: Processing Dielectric Characterization

Linda Domeier Materials Processing Department

and

Marion Hunter
Materials Chemistty Department Sandia National Laboratories P. O. BOX 969 Livermore, CA 94551-0969

Abstract

The dielectric performance of epoxy foams was investigated to determine if such

materials might provide advantages over more standard polyurethane foams in the Comparisons of the dielectric characteristics encapsulation of electronic assemblies. of epoxy and urethane encapsulant foams found no significant differences between the two resin types and no significant difference between as-molded and machined

foams. Blown epoxy foams are an alternative to the more prevalent and versatile polyurethane foams used as DP firing set encapsulant and in a range of other commercial applications. Epoxy resins are not as readily foamed and processed as
urethanes and have generally seen only limited use as encapsulant. Potential advantages for epoxy foams, however, might result from their dielectric properties and also elimination the of toxic and sometimes sensitizing isocyanates used in urethane formulations. This study specifically evaluated the formulation and processing of epoxy

foams using simple methylhydrosiloxanes as the blowing agent and compared the
dielectric performance of those foams to urethane foams of similar density.

Epoxy foams with densities ranging from 0.25 to 0.90 grams/cc were prepared and the influence of various formulation parameters on those foams was established. The alkylhydrosiloxane blowing agents used generate hydrogen gas during the epoxy curing process, much as urethane foams generate carbon dioxide from water during the curing reaction.

Dielectric properties were measured on these epoxy foams and also urethane foams over a range of densities and with both machined and as-molded, skinned surfaces. No significant differences were found. Both as-molded foams with skinned surfaces and machined foams showed little dependence of volume resistivity on foam density except at very low densities. Urethane foams generally had higher volume resistivities

than epoxy foams although all the samples, with and without skins, had resistivities

above 106ohm-cm measured at one minute. Urethanefoams were typically about an

order of magnitude higher at 1017 ohm-cm.

Acknowledgements
The contributions of Paul Beeson, now retired from Org. 1812, were invaluable in carrying out the initial foam dielectric tests and in guiding the establishment of that test capability at Sandia, California. The bulk of the work in setting up the California test capability was carried out by Marion Hunter with additional assistance from Bill Even and Bob Crocker.

Table

of Contents

Introduction Background on Epoxy Foam Technology Siloxane Blowing Agent 8

11

Foam Formulations:

Foam Formulations: Curing Agents and Epoxy Resins Foam Formulations: Processing Studies Foam Density and Structure Dielectric Testing Procedures Dielectric Testing Results Surfactants

14 15 15 16 22 23

Conclusions
References APPENDIX APPENDIX APPENDIX APPENDIX APPENDIX AStructure of Epoxy Formulation Ingredients BSurfactants Evaluated in Epoxy Foams CFoam SEM Pictures DDielectric Testing Equipment EDielectric Testing Data

36
37 38 39 40 53 54

Epoxy Foam Encapsulant: Processing Dielectric Characterization

and

Introduction
Blown epoxy foams are an alternative to the more prevalent and versatile
polyurethane foams used as firing set encapsulant and in a range of other DP and commercial applications (Ref. 1). Commercial epoxy foam applications have typically exploited the rigidity, adhesive strength, moisture resistance and toughness of epoxies, plus the lighter weight of a foam, in such structures as wind generator blades, windsurfing boards, automotive spoilers and in an aluminum honeycomb in the DC10, These applications often include sandwich structures or fibers for reinforcement. Commercial epoxy adhesives also employ added foaming agents in some applications to insure gap filling. Epoxy resins are not as readily foamed and processed as urethane foams and have generally seen limited use in encapsulant applications. Potential advantages of epoxy foam in encapsulant applications might lie in their dielectric properties and also the elimination of toxic or sensitizing isocyanates used in urethane formulations. DP programs have also cited the brittleness and dark color of the epoxy foams as advantages, either of which can be provided by appropriately formulated and filled urethane foams. The purpose of this study was to evaluate the formulation and processing of epoxy foams using simple alkylhydrosiloxanes as the blowing agent and, more importantly, to compare the dielectric performance of those foams to urethane foams of similar density. Epoxy foams with densities ranging from 0.25 to 0.90 grams/cc were prepared and the influence of various formulation parameters on the foam density and processing was established. Alkylhydrosiloxane blowing agents were used to generate hydrogen gas during the epoxy curing process, much as urethane foams generate carbon dioxide from water during the curing reaction. This technology appeared appropriate for encapsulant applications due to the formulation flexibility and the gentleness of the

foaming reaction.
Dielectric properties (volume resistivity, dielectric constant and dissipation factor) were measured on these epoxy foams and also urethane foams (CRETE formulations) over a range of densities and with both machined and as-molded, skinned sutiaces. Dielectric breakdown properties have not been determined as yet.

Background

on Epoxy Foam Technology

This section is meant to briefly review the various options available in creating epoxy foams and their relative advantages and disadvantages. The alkylhydro siloxanes selected as the blowing agent for this study is one of several could be used. A major consideration in this selection was the ease of formulation and processing and the similarity in behavior to current polyurethane foams. Polyurethane are readily foamed by the simple addition of various amounts of water that reacts with isocyanate groups to form the carbon dioxide blowing agent and amines. The resulting amines quickly react with remaining isocyanate groups to form urea linkages within the urethane matrix. Epoxies do not foam on the addition of water and have instead been foamed by the addition of various reactive and inert blowing

agents, each of which provides advantages and disadvantages. Both resin types also
utilize surfactants and catalysts as needed to modify the resin reactivity and foam morphology. (Note: Only blown foams are considered in this discussion. Syntactic epoxy foams, created by the addition of hollow spheres of glass, GMB, or other materials are a separate class of materials which generally cannot provide foam densities lower than about 0.7 g/cc) Heat activated blowing agents have included azo and hydrazide compounds (nitrogen generation) and carbonate salts, all of which usually require milling equipment to

insure a uniform distribution of the solid blowing agent and also refrigerated storage to prevent premature decomposition. High curing temperatures are often required to
activate the blowing agents although this can be modified by added catalysts (Ref. 2). AbleFoam 5, a now discontinued commercial product used in the W76 firing set, used ammonium carbonate as the blowing agent (Ref. 3). This proprietary product was sold in Semco cartridges which required storage below about 50F. The thawed cartridges could be injected into molds and had a potlife of about one hour. Curing at temperatures above 120F, preferably at about 150F, was required and heated molds appeared to be beneficial. Upon decomposition the salt would generate a mixture of

ammonia and carbon dioxide. This product was discontinued by the manufacturer, Ablestick, due to the unavailability of the triglycidyl ether of glycerin used in the formulation. This component is a cancer suspect agent. A backup product developed
at Bendix, KCP, was called Capoxyfoam and used the same blowing agent in a DEN 431 /Epon 828/phenyl glycidyl ether/Shell Z formulation (Ref. 4). Proper dispersion of the blowing agent was critical in this formulation and it has not apparently been used in any weapon applications. Many of the reactive blowing agents reported in the literature are integral components of the epoxy formulation and have included carbamate salts (Ref. 5), carbonate oligomers (Ref. 6), combinations of anhydride curing agents and tertiaty amine catalysts (ref. 7), and trialkoxyboroxines (Ref. 8), Carbamate salts are an intermediate reaction product of carbon dioxide and aliphatic amine curing agents and require a difficult synthetic/purification process. Upon heating, the original amine curing agent plus carbon dioxide are generated. Formulation stability and processability are

challenges with this class of materials. Carbonate oligomers also generate carbon dioxide upon heating (about 140-1 80C) and are specific epoxy resins containing multiple carbonate linkages that can be used in standard epoxy formulations. These oligomers, basically glycidyl-capped low molecular weight Lexan, do not appear to be commercially available. Tertiary amines and aliphatic anhydrides are standard ingredients in epoxy formulations and have been shown to react at elevated curing temperatures (at least 115C) to generate carbon dioxide and foam the resulting epoxy matrix. A patent in this area suggests the use of added auxiliary blowing agents (Ref. 7). Note: This reaction of anhydrides and tertiary amine catalysts was noted previously at Sandia and AS/FM&T when a prebiend containing such ingredients and used to cure a solid epoxy encapsulant system was found to slowly generate carbon dioxide and build up pressure during storage at room temperature. The chemistry of this reaction is not well defined but may involve loss of an allylic hydrogen and selfcondensation (Ref. 9). Finally, trialkoxyboroxines have also been described as combination curing/blowing (generated methane gas) agents. They must be used at high levels or supplemented with other blowing agents. Pot life after mixing was extremely short and the exotherms appeared to be substantial. Other reactive blowing agent additives, as opposed to simple heat activated agents, have included combinations of sodium borohydride and water (Ref. 10), and alkylhydro siloxanes (Ref. _l1-1 3). Sodium borohydride reacts with advantageous and added water to generate hydrogen gas and sodium metaborate (NaB02). This

blowing agent combination has also been used in thermoplastic foams. It was not
considered in this study on encapsulant applications due to the expected detrimental effect of the sodium salt formed during the foaming process on dielectric properties. Alkylhydro siioxanes are used as the blowing agent in a commercial foaming epoxy, RP-I 774, from Ciba-Geigy. This specific formulation includes Bentonite clay and calcium carbonate fillers along with dibutyl phthalate as a diluent or flow modifier. As received, it would be too viscous for most encapsulant applications. Data sheets indicate both Bisphenol A and diluent epoxies, perhaps Epon 815, and a Versamid type curing agent. The third component, the blowing agent, is a methylhydrosiloxane

homopolymerwhich reacts with the amine curing agent to generate hydrogen gas. Similar siloxane-blownsystems were the subject of a German study on the fatigue
behavior of fiber-reinforced epoxy foam laminates (Ref. 14). Russian work with this class of blowing agents has also been reported (Ref 15) including a patented formulation (Ref 16) using ethylhydrosiloxane as the blowing agent in a carbon black

filled conductive foam.

Because of the formulation flexibility, the absence of any ozone-depleting agents, the absence of added or generated salts, and the processing similarity to urethane foams, the alkylhydro siloxanes were chosen as the blowing agents for this study. Inert blowing agents include low-boiling solvents and Freons or injected gases and these have been used in numerous foaming applications with both thermosetiing and thermoplastic resins. Freons were used in the late 70s by Thorn EMI Electronics Ltd.

in Great Britain to specifically formulate epoxy foams for electronic encapsulation (Ref. 11-1 3). The advantages cited were low toxicity (no isocyanates) and removability with acetone solvents. This series of products (Feldex F3-6) utilized a range of amine (F3/4) and polymercaptan (F5/6) and anhydride curing agents with the F5 foam being the most recommended although it had poor load bearing capability above 60C. No performance advantages for these products over similar urethane foams were clearly

demonstratedor claimed. Their ready softening in the presence of acetone was

mentioned only briefly and no details such as ease of removal or possible correlation to poor mechanical properties were provided. Such ready dissolution of an epoxy by acetone usually suggests incomplete cure. All these products appear to have been discontinued or were never fully commercialized. In the 70s there was also work at

Ciba-Geigy on special aliphatic epoxy resins, not apparently commercialized, which

gave superior quality foams using inert blowing agents (Ref. 17). A program at Sandia/New Mexico has utilized an inert blowing agent, Fluorinert (from 3M), as a blowing agent in a replacement material for the discontinued AbleFoam encapsulant and will be reported elsewhere. FC-72

Finally, an extensive study was carried out at Y-1 2 (Ref. 18) on mechanically frothed epoxies which contained no blowing agents but relied on surfactants to stabilize air whipped into the formulation by a high speed mixer. These Versamid cured materials showed a range of foam morphologies depending on the surfactant used. The most successful was a pre-reacted mixture of stearic acid and the Versamid curing agent. No advantage was found in the present study for such a surfactant over commercially available surfactants.

10

Foam Formulations:

Siloxane

Blowing

Agent

The available literature did not define what range of alkylhydrosiloxane homopolymers and (alkylhydro)(dialkyl) siloxane copolymers might be useful in epoxy foam formulations. Both the level of siioxane additive and the type of homopolymer or

copolymer might be used to adjust the foaming action and final density and the effects
of these indicated Russian was not parameters were evaluated. The Ciba-Geigy data sheets for RP-I 774 the use of methylhydro homopolymers (confirmed by NMR) while the

work indicated the use of ethylhydro homopoiymers.

discussed in any of the references.

The use of copolymers

(Methylhydro)(dimethyl)siloxane copolymer Alkylhydrosiloxane homopolymer y i

O-~i

~
O-~i t 0<

yyyy
~-O-~i-O-~i-O-~i-O-f $ HHHH R = methyl or ethyl i-O $

-00

HnRm R = methyl

Initial foaming trials with hand-mixed samples used a standard 60/40 Epon 828/Versamid 125 formulation and various types and levels of siloxane additives. The various siloxanes shown in Table 1 were all screened in both room temperature and oven cured (150F) formulations at the 1 percent level and none showed significant foaming action other than the pure alkylhydrosiloxanes. Addition of a stannous octoate catalyst or water had no effect on the foam density and flame ionization analysis of the Ciba-Geigy RP-I 774 siloxane blowing agent showed no added metallic compounds. The methylhydrosiloxanes gave better foaming and lower densities than ethylhydro-siloxane and both PS-120 and HMS 991 gave identical

foaming behavior to the Ciba-Geigy additive. Based on these results, PS-120 was
selected as the foaming agent for the remaining work.

11

Table 1. Siloxane Polymer Additives Product percent percent

percent

Molecular Wt.

methylhydro 100 PS-120

PS-122.5 PS-123 HMS-151 50-55 30-35 15-18

dimethyl
45-50 65-70 82-85

ethyl hydro

Viscosity (Cps)

2270
900-1000 2000-2100

30
10-15 25-30 25-35

25-30 HMS-301 30-35 65-70 100 1500-1900 15-25 HMS-991 HES-992 100 75-125 RP-I 774 100 PS series from United Chemical Technologies, Inc. HMS/HES series from Gelest, Inc. RP-I 774 is the siloxane blowing agent supplied with Ciba-Geigys RP-I 774 3-part
epoxy foam The amount of added methylhydrosiloxane clearly had an effect on the level of foaming and further formulation tests varied the amount of PS-120 siloxane in order to obtain different foam densities. Figure 1 shows the results of early tests with the 60/40 Epon 828/Versamid 125 formulation. These included both hand-mixed and blademixed formulations as well as surfactant modified formulations. Use of a sutfactant

generally produced lower density foams although no further decreases in foam density
were obtained agent). above about 2 phr (parts per hundred resin including epoxy and curing

Figure 2 shows the foam densities obtained from several series of samples including the initial free-rise foams shown in Fig. 1 (blade-mixed, surfactant-free), two series of foam disks cut from small and large diameter molded foams, and also a series of molded 7 mm thick disks which were not machined and therefore included a higher density skin near the foam surface. All four series showed similar correlations of density with the level of added siloxane. Only siloxane levels up to 2 phr were used in most cases.

12

Figures 1 and 2. Epoxy Foam Density vs. PS-120 Siloxane Content

Free-Rise
1.2-

Epoxy

Foam

Density

vs. Siloxane

Content

Blade-mixed, A .

surfactant-free,

machined

samples

1.0{ } \ \ \
0.8 \ 0.6 - m \ Y 04 .AAi

Blade-mixed, plus 1.0-1.6 phr DC 5357 Hand-mixed, surfactant-free

A
A 0.2 A k t

0,0 * o

10

phr PS-120 Epoxy

1.2 I

Siloxane vs. Siloxane Content

I

Foam I

Density
I

+ Large Molded, Machined Foams (median disk density) mSmall Molded, Machined Foams (median disk density)
1.0 A Molded Foam Disks (as-molded with skin)

0.8

6 A A

Free-rise, Machined Foams

I I I I I

All samples blade-mixed, surfactant-free. 1 s~ 0

0.6

A +
q

0.4

$
0.2

q s

AL

0.0 0.0 0.2 0.4 0.6 0.8 1.0 1.2 1.4 1.6 1.8 2.0

phr PS-120

Siloxane

13

Foam Formulations:

Curing Agents

and Epoxy Resins

Both Versamid cured systems, similar to RP-I 774, and lower viscosity systems cured with Jeffamine D-230, Ancamine 2049 and PACM were investigated. The lower viscosity systems are similar to a solid epoxy encapsulant (Formula 459) now used in some DP applications. The epoxies and curing agents used are shown in Table 2. Table 2. Epoxy Resins and Curing Agents (Structures I Epoxy Resins: Viscosity (cps) Epon 826 6,500-9.500 I I Epon 828 11 ;000-15,000 Epon 830 17,000-22,500 Curing Agents: Versamid 125 6,500-9,500 @75C Versamid 140 8,000-12,000 Jeffamine D-230 9 120 I Ancarnine 2049 ! PACM 6 Changes in formulation shown in Appendix A) Epoxy Equi. Wt. 178-186 I

I I J

185-192
190-198 NH Equi. Wt. 100 125 60 60 52.5

viscosity can strongly effect the foaming behavior in both urethane and epoxy resin systems. Epon/Versamid formulations using Epon resins

826, 828, and 830 and Versamid curing agents V-125 and V-140 were evaluated and
clearly showed improved epoxy foaming behavior as the formulation viscosity was increased by going to Epon 828 and 830 and by using Versamid 125 in place of 140.

Lower viscosity formulations cured with Jeffamine/Ancamine/PACM mixtures showed

much poorer foaming behavior than the Versamid systems. Initial foaming tests with PS-I 20 in Formula 459 (a solid epoxy encapsulant formulation containing 75 parts Epon 826 and 25 parts of a 1/1 Jeffamine D-230/Ancamine 2049 blend) resulted in the hydrogen gas simply bubbling out of the mixture with little or no foaming action. Addition of a surfactant, stearic acid or DC-193, and nucleating additives such as CabO-Sil and glass microballoons, gave some improvement, but the foam level and uniformity were still poor. Other alkylsiloxanes, as expected, showed no improvement. Improved foaming was observed when Epon 826 was replaced with the higher viscosity Epon 828 and 830 and when the Ancamine 2049 curing agent was replaced by the more reactive PACM (his-( para-aminocyclohexyi) methane). PACM alone, without Jeffamine D-230, did not foam as well as the curing agent blend. While some preliminary dielectric tests were carried out on the Jeffamine/PACM cured epoxy foams, the quality (cell size and uniformity) of these foams was generally much poorer than in the Versamid cured foams, Most of the dielectric testing on epoxy foams, therefore, used a 60/40 Epon 828 or 830 mixture with Versamid 125.

14

Foam Formulations:
Surfactants are commonly

Surfactants
used in urethane and other foams to control the foaming

behavior, The effect of various commercial surfactants on the epoxy foam formulations

was investigated with a standard 30/20/0 .2/0.8 Epon 828/Versamid 125/PS120/surFacant formulation. Over thirty mixes were evaluated for foam quality using a
150F oven cure. The various surfactants used are shown in Appendix the most promising was DC-5357, a siloxane/gIycol ether copolymer. B. Of these,

In addition to the above trials, a pre-reacted blend of stearic acid with a mixture of Versamid 125 and 140 was evaluated. This surfactant, presumably a stearic acid salt, was found to have superior foam stabilizing properties in a prior study of frothed epoxy foams (Ref. 18). A 140/47/2.2 gram mixture of Versamid 140, Versamid 125 and stearic acid was stirred and heated to dissolve the stearic acid. When this curing agentkurfactant blend was used in place of standard Versamid in a PS-I 20 foamed mixture, the level and uniformity of the foaming was actually decreased and no further evaluations were carried out. Use of stearic acid alone, with no pre-reaction, provided better foam behavior, and both were surpassed by the siloxane/glycol ether type surfactants. While Versamid cured foams with surfactants showed slightly better uniformity in handmixed trials, blade-mixed samples showed only marginal differences with and without added surfactant, As noted earlier, the use of a sutfactant generally gave slightly

lower densities at the same PS-120 concentration, an effect that made adjustments of
the foam density more difficult due to the smaller range of PS-120 used. The molded foams prepared for dielectric testing were formulated without added surfactant. The lower viscosity Jeffamine/Ancamine 2049 cured formulations also showed lower densities and better uniformity when 1 phr of DC-193 surfactant was added. Higher surfactant levels gave no further improvement and other surfactants were not This improvement was less noticeable when investigated with this formulation. Ancamine 2049 was replaced with the faster curing PACM and those materials were also molded without surfactant for dielectric testing.

Processing

Studies

Many of the initial screening evaluations was carried out on simple hand-mixed formulations. An overhead mixer with 2-3 inch Corm blades was used during later formulation trials to determine the density vs. siloxane blowing agent relationship and to prepare samples for dielectric testing. Blade mixing generally gave slightly lower densities due to air entrapment and also better uniformity. Most of the epoxy foams, when cured at room temperature and then post-cured in an oven, showed some shrinkage of the foam. More stable and uniform foams were obtained with oven cures at 125-150 F with pre-heated molds. Larger samples

15

showed darkening at 150F.

in the foam interior, evidence of a significant

exotherm, when cured

The molds used consisted of a bottom steel plate, a top steel plate perforated with small holes to allow gas and foam escape, and steel cylinders of various heights between the plates. Two series of molds were fabricated, an initial series with

cylinders having a 5 inch diameter and a second series having a larger 6 inch diameter. The large diameter molds were required to provide samples for the larger
electrodes fabricated for the dielectric testing. Cylinders of 1-3 inches in height were used to prepare foams that were later machined into 7 mm thick disks. Densities were measured on the individual test disks and did show some variance from the top to bottom of the molded sample in some of the larger molds. Very thin, 7 mm, steel cylinders were used to mold the individual dielectric samp]a- n-+-~ *:+k h- molded skin Perforated Top Plate

Bottom Plate

Steel Molds: Side View

Foam Density

and Structure

Foam density in the epoxy foams was controlled by the level of added PS-I 20 methylhydro-siloxane up to levels of about 2 phr. Comparison polyurethane foams were made from a standard CRETE formulation (Ref. 19) based on varying levels of:

Isonate 143L (modiiied methylene diisocyanate from Dow Chemical, isocyanate equivalent weight, 144.5; functionality 2.1; viscosity 33 cps)
Voranol 490 (propylene oxide polyol from Dow Chemical formed by extension of a sucrose /glycerin base; functionality 4,3; avg. molecular wt. 460; viscosity 5572 cps) Polycat 17 (tertiary amine catalyst from Air Products) DC-1 93 (siloxane/glycol ether surfactant from Air Products) water (generates carbon dioxide blowing agent) This polyurethane foam is one of several which have been evaluated as replacement encapsulation foams for DP applications. The urethane foams were typically more exothermic and were cured several hours at room temperature before an overnight post-cure at 150F. Foams were prepared over the same general range of densities as the epoxy foams.

16

Visual and SEM examinations of the epoxy and urethane foams showed the
urethanes to have smaller and more uniform cell sizes. Figures 3 and 4 show low magnification and SEM (50x) crosscuts of both foam types over a range of densities. Figures 5 and 6 show similar side-by-side comparisons of three sets of foams at the same density. The difference in cell size at similar densities is most apparent in the side-by-side comparisons. At the lowest densities, both the epoxy and urethane foams were less uniform and showed the presence of large cells, particularly in the lower magnification pictures. Additional foam pictures are contained in Appendix C. While it was anticipated that cell structure might have a strong influence on dielectric properties, the results as a whole did not show such trends for these particular samples. Earlier epoxy foam samples made with the Jeffamine D-230/PACM curing agent were significantly more non-uniform and did show poor performance in some tests that might be attributed to the poor foam morphology.

17

Density (gr.lee)

Fiq.3. Cross-Section Views of Foams Used in Resistivitv Tests

0.23

Epoxy Foams (Versamid Cured)

Urethane Foams (CRETE)

I
+

0.30
Density (gr.lee)

0.44

0.15

0.51

0.22

0.53

0.31

0.61

0.37

0.69

0.50

18

Density (grmlcc)

Fiq. 4. SEM Cross-Section Views of Foams Used in ResistivitV Tests

0.23

0.30

Density (gr.lee) 0.44 0.15

0.51

0.22

0.53 0.31

0.61 0.37

0.69 0.50

19

F&J .5.

Cross-Section

Foam Comparisons: Cured)

EPOXV vs. Urethane

at Same Densitv (a rlcc] Urethane Foams (CRETE)

Epoxy Foams (Versamid

9L@

Ilr@2

0.23

0.22

Iv

0.30

0.31

0.51

0.50

Fiq. 6. SEM Cross-Section

Foam Comparisons: Cured)

EPOXV vs. Urethane

at Same Densitv (qrlcc) Foams (CRETE)

Epoxy Foams (Versamid

AH SEMS at 50X

Urethane

grin/cc

gr.lc c

0.23

0.22

Iv

0.30

0.31

0.51

0.50

Dielectric

Testing

Procedures

Dielectric tests were carried out with cylindrical brass electrodes and a guard ring such as described in ASTM DI 50-94 and 257-93 and shown below. Foam samples were either machined disks cut from large molded billets or as-molded disks of the appropriate diameter and a thickness of about 7 mm. A detailed description of the test

equipment and procedures in given in Appendix

D.

Polymers, i.e., plastics, have often been utilized because of their insulating capabilities. This capability is often characterized by dielectric constant, dissipation factor and volume resistivity. Dielectric constant is the ratio of the capacitance of a capacitor, such as the test assembly above, containing the material of interest relative to the same system in which air (dielectric constant of 1) is the dielectric medium. It is measured with an alternating current. Values of 2-10 are typical of insulators and are generally sensitive to temperature and also the frequency. It is a dimensionless parameter and lower values are preferred for high frequency insulation. Dissipation factor, also called the power factor in some cases, is the tangent of the dielectric loss angle. It describes the power lost, rather than stored, in an alternating current in which the material must rapidly change polarization. It is again a dimensionless and lower values are preferred. Volume resistivity, measured in ohm-cm, directly measures the resistance in a nonaltemating current of the material of interest. A high voltage, 1000 volts in most of the

tests described here, is applied across the insulating material and the resulting current is measured. Most unfilled and unfoamed plastics have volume resistivities in the 100
to 1015 range. A few plastics such as DAP (diallyl phthalate) and Teflon have values in the 101s and 1017 range which was also observed for the more highly insulating foam samples studied here. Currents were measured in the pico (1012) amp range.

22

Dielectric

Testing

Results

(Data in Appendix

E)

Initial tests with 4 inch x 7 mm machined disks of two epoxy and two urethane foam formulations were carried out with the smaller electrodes in Sandia, NM. The epoxies were the Versamid cured formulations and the Jeffamine/PACM cured formulations while the urethanes were either the TD1-based foam now prevalent in the stockpile or

the newer CRETE family of urethanes. The density range of these samples was
limited and the quality of the foams was also variable. As shown in Fig. 7, however, there was a strong correlation of dielectric constant with foam density, independent of the resin type or the test frequency (1-1000 KHz). Dissipationfactors, shown in Fig. 8, showed much greater scatter in the results with no clear correlation to resin type or density. The test frequency was clearly more dominant in this case although values measured a 1 KHz were considered too erratic to be reliable. The initial volume resistivity tests were made at 3 kilovolts (KV) due to the sensitivity required and, as shown in Fig. 9, were largely in the 1016 ohm-cm range. Values were also measured at 1 KV on this series of samples but the data was erratic and in the same range as the noise. These initial results showed varying dependence of the resistivity on foam density. The poorer quality of the epoxy foams cured with Jeffamine/PACM appeared to result in lower resistivity for that group of samples. Overall, no clear conclusions could be drawn about the effects of resin type and foam density on volume resistivity from these tests. It was because of the high sensitivity required that the electrodes fabricated for further testing in California were made with a larger surFace area, roughly four times the area of the smaller electrodes. A second series of foams with the larger 5 inch diameter

were fabricated and tested both in California using these larger electrodes and also in

New Mexico. While the electrodes used in New Mexico were still the smaller size, the
higher quality of the foam samples in this series did provide less erratic data and the agreement between the two test locations was, ultimately, very good. These larger foams were prepared from only the Versamid cured epoxies and the CRETE family of urethanes. One series of tests in New Mexico measured the dependence of volume resistivity the applied voltage. As shown in Fig. 10, neither the epoxy or urethane samples showed a strong dependence on the applied voltage. The resistivity values shown resistivity vs. voltage comparisons in Fig. 10 are clearly higher than seen in Figure particularly at lower densities. This is attributed primarily to improvements in the quality of the samples. All the volume resistivity tests at California were conducted kilovolt. Numerous Round Robin comparisons were made between the test equipment and procedures gave good agreement. was the insertion of a carbon cloth insert between the foam provide better electrical contact. As shown in Figs. 11 and little difference in the volume resistivity measurements and on the 9, at 1

the two Sandia Labs until One procedure considered and electrode surfaces to 12, such inserts resulted in an average increase in the

23

Figures 7 and 8. Dielectric Constants and Dissipation Factors of Preliminary Samples

(Sandia, NM Data)

Foam 3.00!

Dielectric ,

Constant

vs.

Density

(Small,

Machined

Disks,

NM

Data)

2.75-

(0 %
s

9 CRETE3olyurelhane, O KHz Q TDI PO!} urethane, 10 <Hz

2.25A V,ar~ W-b

AJeff/PA~M epoxy, 10b KHz

/3 0 ~ ; ~ n

2.00q

Versam$ epoxy, 1 M~z

1.75-

O TDI

flOl)

urethane, 1 ~Hz

1.50-

1.25-

1.00 ~ 0.0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.6

0.9

Foam
0.016

Dissipation

Factor

vs.

Density

(Small,

Machined

Disks,

NM

Data)

0.014q

* e A A
A

0.012k ~
o

0.0,0AA
q

o A
A& A

If
~ .= 0.006

~:

A o

m Versamid epoxy, 10 KHz

S
0 ~ 0.006

B4 o $[
E F
0.004-

* B *SI

o
u

Jeff/PACM epoxy, 10 KHz mM CR~E polyurethane, 10 KHz

u

u TDI polyurethane, 10 KHz AVersamid epoxy, 100 KHz

AJeff/PACM epoxy, 100 KHz A CRETE polyurethane, 100 KHz

ATDI polyurethane, 100 KHz

. Versamidepoxy,1 MHz 0.002 0 Jeff/PACMepoxy,1 MHz

e CRETE polyurethane, 1 MHz O TDI polyurethane, 1 MHz I I

0.0000.0

0.1

0.2

0.3
Foam

0.4
Density

0.6
(grams/cc)

0.6

0.7

0.8

0.9

24

.. <

Figures 9 and 10. Volume Resistivity of Preliminary Samples (Sandia,NM Data)

Volume Resistivityat3 KV(Small, Machined DiSKS,

5.0-

.-

. ..-

. .

. .. . .
NM

uata~

. .

4.5-

4.0q q q

3.5

6 6 w +

q A q * q A

3.0 -

2.5 -

q
9

q + Epon/Versamid a Jeff/PACM epoxies

2.0 -

1.5 -

M m

epoxies

1.0 -

A CRETE poiyurethanes
q

0.5 m 0.0 +

TDI

polyurethane

0.0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

Volume
80-

Resistivity

vs. Voltage

(Large,

Machined

Disks)

-E+ 703 u + 60-

Epoxy Foams at 1 kV Epoxy Foams at 3 kV Foams at 2 kV

x E y E E o ~
.> .(n .(n

-m-Urethane Foams at 1 kV +Urethane

50 + 40 1 I

Urethane Foams at 3 kV

30

\\

1$1 g 20.4
>

I
I

I
I M

1>1
I

I
I

I I

I
I

10

0.0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

Foam Density (g/cc)

25

Fiawres 11 and 12. Volume Resistivity and Dielectric Constant vs. Carbon Cloth Insert (Sandia, NM Data)

Volume
50

Resistivity

With/Without

Carbon

Cloth

Insert

Epoxy Foams: 1 Min. VR With Cloth

-E- Epoxy Foams: 1 Min. VR Without Cloth

40

+ +
30

Urethane Foams: 1 Min. VR With Cloth Urethane Foams: 1 Min. VR Without Cloth

20

10

0 0.0

0.1

0.2

0.3

0.4

0.s

0.6

0.7

0.8

1000 KHz Dielectric

2.25
+ [ I I

Constant
I

With/Without
1

Carbon

Cloth

Insert

Epoxy Foams With Cloth f

-E- Epoxy Foams: Without Cloth

2.00

+
I

Urethane Foams: With Cloth F

-e- Urethane Foams: Without Cloth

1.75

e
1.50.

Average All Foams Nith Cloth: 1.77 Average II Foams Viithout Clott : 1.65
1.25. 0.0

* 0.1
0.2 0.3 0.4

I
0.5

I
0.6 0.7 0.8

Foam Density (g/cc)

26

dielectric constant of only 0.12. Further measurements were all made without the carbon cloth insert.
Measurements on 7 mm thick machined foam disks showed a strong correlation of dielectric constant with foam density for both the epoxy and urethane materials. This is shown in Figs. 13 and 14. A slight dependence of dielectric constant on frequency is apparent. As noted above, the agreement in test values between NM and CA was generally good. Dissipation factors for these same samples, shown in Figs. 15 and 16, were less well behaved although a generaI correlation with density was again observed.

Volume resistivity measurements at both one minute after the voltage was applied

(ASTM procedure) and three minutes are shown in Figs, 17 and 18 and indicated little
dependence on foam density. All the samples had very high resistivity. The values measured in CA tended to be slightly more conservative that those made in NM, but the agreement was generally good. All these resistivities required sensitivity in the picoamp range and all showed the expected increase in resistivity between one and three minutes. The resistivity was approaching equilibrium at three minutes with much less variability. When used as an encapsulant, the foams would not be machined and would possess a skin of higher density and varying thickness near the mold or substrate surface. A series of molded foam samples, again 7 mm thick, were prepared and tested in the same manner as the machined foams to determine the effects of such skins on the dielectric performance. As shown in Figs. 19 and 20, the dielectric constant of the as-molded foams again showed a strong correlation with density. Two series of epoxy samples were prepared, one with Epon 828 and a second with Epon 830 and slightly higher levels of siloxane blowing agent to insure more uniform mold filling. Both series gave similar results which are combined in Fig. 19.

The dissipation factors of these same as-molded foams were better behaved than in
the machined samples and are shown in Figs. 21 and 22. There was a slight correlation with foam density and a strong correlation with test frequency, particularly between 100 and 1000 KHz. The volume resistivity results on these as-molded samples, as in the machined samples, showed little dependence on foam density except at the very lowest urethane density of about 0.2 g/cc. These results are shown in Figs. 23 and 24.

Pulling all the above results together, Figs. 25 and 26 compare, at 100 KHz, the
dielectric constant and dissipation factor of both the epoxy and urethane foams with both machined and as-molded samples. The dielectric constant of all these materials was, again, clearly dependent on foam density only with no significant differences due to the material or the presence or absence of a surface skin. The dissipation factors

27

Figures 13 and 14. Dielectric Constants of Machined Epoxy and Urethane Foams (Sandia, NM and CA Data)

Dielectric
3.00-

Constant

of Machined

Epoxy

Foams

~
2.75-

1 KHz (NM) 10 KHz (NM) 100 KHz (NM) 000 KHz (NM) KHZ (CA) 00 KHz (CA)
/ 0 9 A

~
~

2.50

~1 +--1

2.25.

+-1

2.00.

1.75

1.50

1.25

1.00

0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9

0.0

Dielectric
3.00

Constant of Machined Polyurethane

Foams

,
~ 1 KHz (NM) KHz (NM) 100 KHz (NM) 1000 KHz (NM) 1 KHz (CA) 100 KHz (CA) ~10 ~

2.75

2.50

~ +-

2.25

-e--

2.00

1.75

/$/ .Afl / /

1.50

1.25

d~ ?=*

1.00

0.0

0.1

0.2

0.3

0.4 Foam Density

0.5 (g/cc)

0.6

0.7

0.8

0.9

28

Figures 15 and 16. Dissipation Factors of Machined Epoxy and Urethane Foams (Sandia, NM and CA Data)

Dissipation
0.020

Factor

of Machined

Epoxy Foams

--A-IO
0.018

KHz (NM) 100 KHz (NM) 000 KHz (NM)

~
0.016

~1
0.014

-e-- 100 KHz (CA)

b % 2 c o .% a .(/) .: 0.012

-1

0.010

0.008

0.006

0.004

0.002

0.000 0.0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.6

Dissipation
0.020-

Factor

of Machined

Polyurethane
I

Foams

I -+-10
~ 100

1 KHz (NM) KHz (NM)

0.016-

0.016-

0.014-

1000 KHz (NM)

-100

0.012-

0-
0.010-

A \ \ \
\

KHz (CA)

0.008-

0.006 -

0.004 -

0.002 -

0.000 *

0.0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.6

Foam Density (g/cc)

29

Figures 17 and 18. Volume Resistivity of Machined Epoxy and Urethane Foams (Sandia, NM and CA Data)

Volume
1.E+19

Resistivity

of Machined

Epoxy Foams

~One -.--One 8-Three =-Three

1.E+18-

Minute -NM Minute - CA Minutes - NM

Minutes - CA

K,

1.E+17

* \ \ \\ \

8-..

+*--

A.

.-*

1.E+167 0.0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.6 0.9

Volume
1.E+19-

Resistivity

of Machined

Polyurethane

Foams

.-One
-+-one

Minute - NM Minute - CA Minutes - NM Minutes - CA

=-Three
1.E+18-

--=--Three

h----------%
1.E+17 1.E+16

0.0

0.1

0.2

0.3

0.4 Foam Density

0.5 (g/cc)

0.6

0.7

0.8

0.9

30

Figures 19 and 20. Dielectric Constants of As-Molded Epoxy and Urethane Foams (with skins) (Sandia, CA Data)

Dielectric
3.00q

Constant

of Epoxy Foams with Skin (Epon 828 & 830 Series)

1 KHz 10 KHz 100 KHz

1000 KHz Linear (1 KHz) Linear (10 KHz) Linear (100 KHz) s n

2.75-

A
+

s
2.50- 2.25 - ------

---2.00 -

Linear(lOOO KHz)

1.75 -

1.50 -

1.25 -

1.00 ? 0.0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

Dielectric
3.00 q
2.75A

Constant

of Polyurethane

Foams with

Skin (CRETE Series)

1 KHz 10KHz
100 KHz 1000 KHz Linear (1 KHz)

q
2.50 9

2.25 -

---

Linear(lo KHz) Linear(100KHz)

linear (1000 KHz)

-----2.00 -

--

./ fltm .

,. . . .- . / .0

1.75 -

1.50 -

1.25 -

1.00 ~ o

0.1

0.2

0.3

0.4
Foam Density,

0.5
glee

0.6

0.7

0.6

0.9

31

Figures 21 and 22. Dissipation Factors of As-Molded Epoxy and Urethane Foams (with skins)

(Sandia, CA Data)

Dissipation 0.040

Factor of As-Molded

Epoxy Foams

m 0.035-..W -. ---- ~
---0.025 H --- -.. --- -- m--

-... -% 4 -*@-

0.030-

A +

10 KHz

100 KHz 1000KHz

Linear (1 O KHz)

0.020 -

--
0.015 ------

Linear (100 KHz) Linear (1OOOKHZ)

0.010 0.005 -

0.000 ~ 0.0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

DissipationFactor of As-MoldedPolyurethaneFoams
0.040

0.035----. .-- b

0.030-. ---.P---1

0.025 -

~ ,----

A q =

..0.020 m

----

,.JL.

I ~-----

IO KHZ 100 KHz

10OOKHZ

Linear
0.015 -

(1OKHz)

Linear (100 KHz) Linear (I OOOKHZ) I ! _.

q 1

------

0.010 0.005 ~ 0.0001 0.0 0.1 II 0. AL

-_ -+--A

-+---

-----

3-A

0.2

0.3

0.4

0.5

0.6

0.7

0.6

0.9

Foam Density (g/cc)

32

Figures 23 and 24. Volume Resistivity of As-Molded Epoxy and Urethane Foams (with skins) (Sandiz CA Data)
Volume
1.E+19 ~ -*~Three -m-1.E+18 One Minute - Epon 828 Series

Resistivity

of As-Molded

Epoxy

Foams

(with skin)

One Minute - Epon 830 Series

Minutes - Epon 828 Series Three Minutes - Epon 830 Series

n- - ___ T=

1.E+17

? I

[ .

0 ne Minute Avg. = 6.8 E16 Three Minute Avg. = 1A E17

A.

1.E+16 ~

J? ~ s = 0.70 t Thickne
0.2

0.1

Volume
1.E+19 1

1.E+18 -

\ \ 4
Resistivity
l\
\ * \ \ \ \

cm
0.4 0.5 0.6 0.7 0.8 0.9

0.3

of As-Molded

Polyurethane
I

Foams
,

(with skin)
t

~
-4 --

One Minute - Series A

One Minute - Series B

Minutes Three Minutes - Series - Series A B

~Three *-

1.E+17

Minute

,AVg. = 24 Avg. = 1. Avg

E17 (or El 8 (or 4.8 E17 o nitting Thlcknes 0.4 Foam Density, = 0.716 cm 0.5 glee 0.8 0.7 0.8 0.9 IOMest densit y)

Tt ?e Minute

1.E+16

,11,

0.1

0.2

0.3

33

Figures 25 and 26. 100 KHz Comparisons of Epoxy and Urethane Foams (Sandia,CA Data)

100 KHZ Dielectric Constant of As-Molded/Machined

Epoxy 3.00m
2.75 n

and

Polyurethane

Foams

,
Machined Epoxy Foam Machined Polyurethane Foam

q
2.50 - 2.25 - --------

As-Molded Epoxy Foam (with skin) As-Molded Polyurethane Foam (with skin) Linear (Machined Epoxy Foam)

q
..-

q
Linear (Machined Polyurethane Foam) Linear (As-Molded Epoxy Foam (with skin)) Linear (As-Molded Polyurethane Foam (with skin)) ..

,.

2.00 - ----

1.75

1.50 /0 8 -, / y

/ , ytl

1.25

CY

1.00

0.0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

Foam Density, g/cc

100 KHZ

Dissipation Factor of As-Molded/Machined Epoxy and Polyurethane Foams

0.025

n u 0.020
+ 0 Linear

Mashined Epoxy Foam Machined Polyurethane Foam As-Molded Epoxy Foam (with skin) As-Molded Polyurethane Foam (with skin) (Machined Epoxy Foam) Linear (Machined Polyurethane Foam) Linear (As-Molded Epoxy Foam (with skin)) Linear (As-Molded Polyurethane Foam (with skin)) /
a

~ 0.015

---------

cl---! _____
0.010

- -

1L---.- e --- .--

4-

------w+

*- . -------0.005 ------66

-0

0.000 . 0.0

0.1

0.2

0.3

0.4

0.5

0.6

0.7

0.8

0.9

Foam Density, glee

34

Figures 27 and 28. Volume Resistivity of Machined and As-Molded Epoxy and Urethane Foams (Sandia,CA Data)

One Minute Volume

1.E+20

Resistivity

of Epoxy and Polyurethane

Foams

Machined Epoxy Machined Polyurethane As-Molded Epoxy (with skin)

o
s 1.E+19

1 As-Molded Polyurethane (with skin)

Expon.

(MachinedEpoxy)

Expon. (Machined Polyurethane)

------ Expon, (As-Molded Epoxy (with skin))
1.E+18

-- Expon. (As-Molded Polyurethane (with skin))

_ u

13--- ---------

--Q
1.E+17

-;dcr:-~.. --------~G--
q

---q q

%-0.5

1.E+16

0.0

0.1

0.2

0.3

0.4

0.6

0.7

0.8

0.9

Three Minute Volume Resistivity of Epoxy and Polyurethane

1.E+20~ q Machined

Foams

Epoxy

o s
u u

MachinedPolyurethane

As-Molded Epoxy(withskin)
As-Molded Polyurethane (with skin) Expon. (Machined

1.E+19

Epoxy)

13___
1.E+16

Expon. (Machined Polyurethane) Expon. (As-Molded Polyurethane (with skin)) -+..

u

------ Expon. (As-Molded Epoxy (with skin)) --+.=1 -~--&_ --4 -.\ 1

-\%-

1 -+ .-.

z ----- n----_-QDn --=_ ---~+

q

.:

1.E+17

~4:.iL__-_J 9

.0

1.E+16~

0.0

0.1

0.2

0.3

0.4 Foam Density

0.5 (g/cc)

0.6

0.7

0.8

0.9

35

were more erratic throughout these tests, but did indicate a slightly higher dissipation factor for the epoxy foams and also higher dissipation factors in the machined samples than in the as-molded samples. There was again a clear dependence on foam

density.
Again pulling all the above results together, Figs. 27 and 28 show that both the one minute and three minute volume resistivities showed only a slight dependence on foam density and slightly higher values for the urethane foams. All the foams had very

high volume resistivity values with the as-molded foams showing slightly higher
resistance than the machined foams.

Conclusions
No dielectric advantages were found for the epoxy foams over polyurethane These comparisons are evident in Figures 25-28. foams.

Both as-molded foams with skinned surFaces and machined foams showed little dependence of volume resistivity on foam density except at very low densities. Urethane foams generally had slightly higher volume resistivities than epoxy foams although all the samples, with and without skins, had resistivities above 1016 ohm-cm (measured at one minute). Urethane foams were typically about an order of magnitude higher at 1017 ohm-cm. Dielectric constants were clearly dependent on foam density in both the machined and as-molded samples with all samples falling along the same trendline. Neither the resin type or the presence or absence of the foam skin had additional significant effects on dielectric constant. The cell sizes and foam morphologies were also examined and did not appear to have significant effects on the dielectric constant and volume resistivity. Processing of the siloxane-blown epoxies was similar to water-blown urethanes although the cell size of the epoxies was generally larger and less uniform.

36

Jleferences

10
2. 3. 4. 5. 6. 7. 8. 9. 10.

D. Klempner andK. C.Frisch,Handbookof PolymericFoamsandFoamTechnology, Hanser,1991.

A. Schrnitter and W. Seiz, US Patent 4,031,043 (1977). H.M. McIlroy and C. H. Smith, SPE Journal, pp. 39-44, Vol. 26 (1970). F. C. Ayres, H. M. McIlroy and W. E. Richardson, Rigid Epoxy Foam Encapsulation: PDO 6984436 (1971). A. Kiihlkamp et al, US Patent 3,406,131 (1968); Offenlegungsschrift 1570573 (1970); Brit. Patent 1,143,644 (1966) M. Hashirnoto et al, US Patent 5,166,184 (1992) W.T. Gormley and G.J. Gillespie, US Patent 4,090,986 (1978). H. L. Lee, US Patent 3,378,504 (1968) Michelotte, Knuth and Bauley, J. Chem. Eng. Data, 79, Vol. 4 (1959). R. C. Wade and C. Letendre, J. Cellular Plastics, pp. 32-35, Jan/Feb (1980). M. Hajim.ichael et a.1,.BritishPolymer Journal, pp. 307-311, Vol. 18 (1986). M. Hajimichael et al, UK Patent Application GB 2,187,745 (1987). M. Hajirnichael et al, UK Patent Application GB 2,200,357 (1986). K. Kurek and A. K. Bledzki, Proceeding of the 47ti Annual Conference, Composites Institute, The Society of the Plastics Industry, pp. 1-12, Section 17-D (1992) A.A. Berlin et al, Foam Based on Reactive Oligomersj Chapter 5: Epoxy Oligomer Based Foams, pp. 215-261, translated from Russian by Alec Odinsk, Technomie Publications (1982) M. I. Topchiashvili et al, US Patent 3,956,195 (1976) A. Schmitter et al, US Patent 3,941,725 (1976) G. F. Dorsey et al, Studies of Foamed Epoxies, UC-25/Y-1833, Sept. 14, 1972. S.H. Goods, C.L. Neuschwanger, C.C. Henderson, D.M. Skal% J. of Applied Polymer Science, Vol. 68, pp 1045-1055 (1998) or SAND98-8490, March 1998.

11. 12. 13. 14. 15.

16. 17. 18. 19.

37

Append~

A. Structures of Epoxy Formulation

Ingredients

i&HCH20~+~0-CH,:CH,0~ ~~ -:-CHJCH2
Epon 826/828/830 (increasing value of n and molecular weight in series)

NH,- C,cfi
,

CH,cy:
,

--EEF!CH2CH2
.+=~p
C , 2- N,

NH,- 24 H

24: H

Versamid 125/140 (complex reaction product of acid dimer and diethylenetriamine)

CH3
Jeffamine D-230

CH3

%H6

2NOCH20NH2

Ancarnine 2049

PACM

38

Amendix B. Surfactants Evaluated in Epoxv Foams

Identification
;ilicone polymer/copolymer? ;ilicone polymer/copolymer? ;ilicone glycol copolymer silicone glycol copolymer ]ilicone glycol copolymer silicone glycol copolymer silicone polymer silicone glycol copolymer? silicone glycol copolymer? ;ilicone glycol copolymer? silicone glycol copolymer? silicone glycol copolymer? silicone glycol copolymer? non-silicone polymer non-silicone polymer silicone polymer silicone polymer

Manufacturer
Air Products

Trade

Name

Type

Dabco DC-56 Dabco DC-57 Dabco DC-193 Dabco DC-197 Dabco DC-5098 Dabco DC-5103 Dabco DC-5164 Dabco DC-5320 Dabco DC-5357 Dabco DC-5367 Dabco DC-5384 Dabco DC-5385 Dabco DC-5454 LK-221 LK-443 Q2-5200 Q2-8075 L-5420
Tergitol 7

non-ionic non-ionic non-ionic non-ionic non-ionic non-ionic non-ionic non-ionic non-ionic non-ionic non-ionic non-ionic non-ionic non-ionic non-ionic

Dow-Corning

Union Carbide

anionic

0Z!6%0 monoheptadecylsulfate, water

sodium salt in

Tergitol NP-1O Tergitol 15-S-7 Niax L-6906 Niax Y-10762

Triton 100

non-ionic non-ionic

nonylphenol ethoxylate (1O EO) secondaty alcohol ethoxylate (7 EO) polyalkylene oxide/dimethylsiIoxane copolymer silicone

Icl

Tween Tween Tween Tween

20 40
60

80

non-ionic non-ionic non-ionic non-ionic non-ionic non-ionic non-ionic

polyoxyethyene polyoxyethylene poiyoxyethylene polyoxyethyiene

(20) sorbitan monolaurate (20) sorbitan monopalmitate (20) sorbitan monostearate (20) monooleate

Shin-Etsu Aldrich

KF-865 Sorbital Monoloeate Glycerin HandiMan water

amine functionalized polysiloxane sorbital monoloeate glycerol (1,2,3-propanetriol) hand soap formulation

39

Armendix C: Foam Pictures

40

42

EPOXVFoam, 0.44 gr/cc (1 12497AI )

44

EPOXV Foam, 0.53gr/cc(110397D1

46

Epoxy Foam, 0.69 @cc (111 397C3)

-1

Polyurethane

Foam, 0.1 5gr/cc(120897A3)

Polwrethane

Foam, 0.22 q-Ycc (120897B2)

Pol~urethane

Foam, 0.31 qr/cc (120897C2)

o-l

Polyurethane

Foam, 0.37 gr/cc (120397B2~

Polyurethane

Foam, 0.50 gr/cc (120897D7)

K)

Am endix

D: Dielectric Testing

hitial dielectric testswerecarried outbyPaulBeeson atSandia, M. Thistestingcapability N

was later set up in Skndia CA where most of the tests were run. Round-Robin comparisons

between the two labs showed good agreement after some early trouble-shooting. The early tests carried out by Paul Beeson in Sandi% NM used smaller brass electrodes with a 2 inch diameter top electrode, 4 inch bottom electrode and guard ring with an inner diameter of 2.3 inches. A larger set of electrodes with a 4.25 inch top electrode and 5 inch bottom electrode was designed by Paul Beeson and fabricated in the SandiZNM machine shop for use in SandiL CA. The guard ring had an inner diameter of 4.5 inches and the effective electrode area uses a diameter midway between the upper electrode and guard ring or 4.375 inches. The CA electrodes therefore had an effective surface area of 96.99 sq. cm. and the area of the NM electrodes was 23.55 sq. cm. The electrodes were enclosed in a oven for both faraday shielding and heating. Low noise test leads were used and all cable connections as well as the elec~odes were carefully insulated. The specific equipment used in California, all from Hewlett-Packard, consisted of a Model 4339B High Resistance Meter and a Model 4284A Precision LCR Meter along with low-noise leads (16117C).

n
Guard Ring Sample Bottom ~ ~ ~

Top electrode+

Electrode

Tests using carbon cloth inserts between the foam sample and electrodes to improve contact showed slightly higher conductivity. The differences were minor, however, and the reported tests were carried out without these inserts, unless otherwise noted, for simplicity. All volume resistivity measurements except for some early tests and comparisons of resistivity vs. voltage in Sandi@M were carried out at 1 kilovolt. Volume resistivities were measured both one minute, as called for in the ASTM procedures, and three minutes after the voltage was applied. The conductivity, as expected, dropped rapidly during the first minute and more slowly during the next two minutes. Calculations: Volume Resistivity = (Voltage x Electrode Area)/ (Measured Current x Sample Thickness)

DielectricConstant= (MeasuredCapacitancex SampleThickness)/ (ElectrodeAreax EO)

where q = electric field constant (8.854x 10-12Fr-l)

53

Awendix

E: Dielectric Measurements

54

Dielectric

Measurements density (gr/cc)

on Machined thick. (cm)

Foam Samrdes

(Sandia,CA Diel. Con.

and NM data. with/wi riout carbon

cioth insert)

I
Cap (pf) IX

Machined Epoxy 111997-D2 11 1697-D6 11 2497-Al 11 1697-Al I10397-DI 11 1197-D2 11 1397-C3 11 1997-D2 111697-D6 112497-AI 111697-A1 110397-DI 11 1197-D2 11 1397-C3 11 1997-D2 11 1697-D6 112497-A1 11 1697-Al I10397-DI 111197-D2 11 1397-C3 I 0.23 0.30 0.44 0.51 0.53 0.61 0.69 0.23 0.30 0.44 0.51 0.53 0.61 0.69 0.23 0.30 0.44 0.51 0.53 0.61 0.69 0.700 0.698 0.704 0.695 0.702 0.703 0.708 .

1 KHz 4.12 4.51 5.42 5.65 5.72 6.14 6.51 inserts 0.0020 0.0020 0.0045 0.0040 0.0050 0.0060 0.0057 1.38 1.51 1.83 1.88 1.93 2.07 2.22

10KHZ I 4.10 4.47 5.35 5.58 5.65 6.06 6.41 0.0047 0.0061 0.0100 0.0099 0.0115 0.0115 0.0113

I 1.38 1.50 1.81 1.86 1.90 2.04 2.18

NM data with no carbon cloth inserts

5d%H=-l=t=l=6.29 0.0137 I 2.14

NM data with usinci carbon cioth

I 0.702 [ 0.703 [ 0.708

EI G l-lmii!Bii EiE ,:: 3

. 6.05

0.0050

I 2.04

6.53

0.0060

! 220 m
2.33 1.47 1.56 1.83 1.91 2,03 2.18 2.36

::;

6.86

0.0060

6.76

0,0114

2.30

aiiu
I
6.31 6.63 0.0137 0.0140 :;: =1==1=

6.21

0.0134

I 2.11

CA data with no carbon cloth inserts 0.700 0.698 0.704 0.695 0.702 0.703 0.708 18.0 19.2 22.3 23.6 24.8 26.6 28.6 0.0030 0.0040 0.0060 0.0100 0.0050 0.0070 0.0080

JzLLMLkl

ata, with/without I

carbon cloth insert] I

density (grlcc) Machined 120897-A3 120897-B2 120897-C2 120397-B2 120897-D7 120897-A3 120897-B2 120897-C2 120397-B2 120897-D7 0 0 120897-A3 120897-B2 120897-C2 120397-B2 120897-D7 Polyurethane 0.15 0.22 0.31 0.37 0.5.0 0.15 0.22 0.31 0.37 0.50 0.15 0.22 0.31 0.37 0.50

thick. (cm)

Cap (pf) Im

Diel. Con.

Cap (pf) 10 KHz

CF

Diel. Con.

Cap (pf) 100 KHz

D=

Diel. Con.

NM data with no carbon cloth inserts 0,672 0.698 0.700 0.702 0.685 0.672 0.698 0.700 0.702 0.685 0.672 0.698 0.700 0.702 0.685 15.6 16.0 18.6 21.2 24.2 0.0020 0.0030 0.0280 0.0040 0.0050 1.22 1.30 i .52 1.73 1.93. 15.4 15.9 19,5 20.8 24.2 0.0100 0.0110 0.0120 0.0090 1.21 1.29 1.59 1.70 1.93 4.41 4.11 4.57 4.77 4.83 4.71 4.79 4.97 0.0000 0.0000 0.0020 0.0030 1.56 1.58 1.61 1.67 4.82 4.69 4.77 4.94 0.0021 0.0030 0.0045 0,0054 1.56 1.57 1.60 1!66 4.80 4.67 4.72 4.89 0.0040 0.0052 0.0081 0.0091 1.55 1.56 1.59 1.65 0.0000 0.0000 0.0020 0.0020 1.42 1.38 1.54 1.61 4.41 4.10 4.54 4,74 0.0021 0.0027 0.0047 0.0054 1.42 1.37 1.53 1.60 4.39 4.08 4.50 4.69 0.0039 0.0049 0.0081 0.0093 1.41 1.37 1.51 1.58

=l=E4.39 4.08 4.48 4.65 0.0035 0.0042 0.0076 0.0094 1.42 1.37 1.50 1.58 1.66 4.81 4.66 4.70 4.85 0.0036 0.0053 0.0078 0.0091 1.55 1.56 1.58 1.63 1,77

NM data with usina carbon cloth Inserts

CA data with no carbon cloth inserts

=l=i=

IDielectric

Measurements
density

on As-Molded thick, (cm) 0.575 0.724 0.720 0.720 0.720 0.720 0.711 0,716 0.716 0.700 0.703 0,710 0.708 0,714 0.715 0.731 0.720 0.714 0,716 0,719 0,714 0.713 0.721 0,711 0,716 0.712 0.719 formulated

Foam Samples

(all 3andia.CA

data with no carbon cloth Diel. Con. 2,32 2.04 2.28 2.31 2.45 2.49 1.53 1.56 1.92 1.84 2,14 2.16 2,27 2.32 2.55 2.67 1,40 I

inserts) Diet. Con. Diet. Con.

I IAs-Molded ,82598EP3A 82598EP4B 182598EP5B

i 82598EP5A

(gr/cc) EDOXV* ] I I \ [ I B I ] I \ I [ ] 0.56 0.58 0.66 0.67 0.74 0.74 0.28 0.28 0.46 0.46 0.59 0.60 0.68 0.68 0.83 0.82 0.19 0.32 0,39 0.53 0.63 0.75 0.19 0.30 0.40 0.52 0.63 samples Polyurethane

Cap

(pf)

DF 0.0036 0.0032 0.0038 0.0038 0.0039 0.0041 0.0023 0.0026 0.0031 0.0032 0.0035 0,0037 0.0036 0.0038 0,0042 0.0042 0,0011 0.0016 0.0020 0.0024 0.0028 0.0029 0.0013 0.0018 0.0019 0.0025 0.0028

Diel. Con.

Cap (pf) IOKHZ

DF

Cap

(pf)

IX

Cap (pf) 1 MHz

DF 0.0369 0.0305 0.0332 0.0337 0.0351 0.0353 0.0241 0.0243 0.0293 0.0290 0.0326 0.0326 0.0338 0.0342 0.0370 0.0374 I 0.0205 j

1 KHz 34.87 24.35 27.38 27.71 29.43 29.86 18.51 18.84 23.17 22.71 26.34 26.23 27.68 28.13 30.89 31.55 1 KHz 16.67 19.47 20.65 23.56 25.45 28.49 16.30 19.13 20.51 23.80 26.05 1.40 1.62 1.72 1.97 2.12 2.37 1.37 1.58 1.71 1.97 2.18 2.34 2.05 2.30 2.32 2.47 2.50 1.53 1.57 1.93 1.85 2.16 2.17 2.28 2.34 2.57 2.69.

100KHz 0.0067 0.0060 0.0067 0,0070 0.0072 0.0072 0,0047 0.0045 0.0058 0.0056 0.0067 0.0065 0.0068 0.0068 0.0077 0.0075 ] 0.0020] 34.24 23.96 26.88 27.19 28.85 29.27 18.28 18.62 22.81 22.37 25.86 25.78 27.17 27.61 30.24 30.90 100KHz 16.59 I 0.0032 ] 1.39 I 0.0094 0.0085 0.0095 0.0099 0.0103 0.0102 0.0063 0.0060 0.0082 0.0079 0.0096 0.0093 0.0099 0.0098 0.0112 0.0109 2.29 2.02 2.25 2.28 2.42 2.46 1.51 1.55 1.90 1.82 2,12 2.13 2.24 2.30 2.52 2.63

34.63 24.21 27.19 27.52 29.21 29.64 18.43 18.76 23.04 22.59 26.16 26.06 27.49 27.94 30.65 31.31 IQ!&& 16.65

32.68 23.09 25.80 26.08 27.61 28.02 17.77 18.10 22.01 21.61 24.84 24.77 26.05 26.48 28.86 29.48 w 16.21

2.19 1.95 2.16 2.19 2.32 2,35 1.47 1.51 1.84 1.76 2.03 2.05 2.15 2.20 2.40 2.51 1.36 I

,82598EP6A 82598EP6B 82798EPIA 82798EPI 82798EP3A 82798EP3B 82798 EP4AI m

-1

82798EP4B 82798EP5A 82798EP5B 82798EP6AI 82798EP6B As-Molded 90298PU1A 90298PU2A 90298PU3A 90298PU4A 90298PU5A 90298PU6A 90298PUIB 90298PU2BI 90298PU3B\ 90298PU4BI 90298PU5BI

qFirst

6epoxy

with Epon 828.

Last10

~oxysamples

formulated

with Epon

830.

Iume Resis t ivltv Measurement s x z

Sandia, NM cald VR resuits only 0.23 11 1697-D6 112497-AI 111697-AI

-l~la:r7:iRfioid=;l: ? ;: IJJ2L Q--Lb !p_l %:qji

n Machln les { andia. A and NM data withl ithcwt car on clo h inse rts

Three min. One min. Three min. One min. ohm-cm) (ohm-cm) (ohm-cm) (ohm-cm)
ertq 1 KV 2 KV 1,53E+17 9.92E+16 6.03E+16 6.33E+16 5.20E+16 5.15E+16 5.41 E+16 Voi. Rest One min. 2 KV 3.96E+17 2.41 E+17 I,49E+17 I,21E+17 1.43E+17 1.24E+17 1.30E+17 Vol. Res. Three min. m 1.53E+17 7.61 E+16 6.87E+16 5.56E+16 5.33E+16 5.52E+16 4,60E+16

Three min. (ohm-cm)

One min.

-:= = = = = Three min. One min. Three min. One mtn. Three min. hphm;cm) car on ciot 2 KV 2KV 1.20E+17 7.56E+I 4.32E+16 4.64E+16 3.95E+I 4.89E+I 3.82E+I 6 6 6 6

;1 1997-D2

0.700

1000

1s with m~ carbon 1 KV 23.55 23,55 23.55 23,55 23.55 23.55 23.55

Ot

3 KV 4.04E+17 1.49E+17 1.65E+17 1.36E+17 1.26E+17 1.50E+17 1.28E+17

(ohm-cm ~ohm-cm e t th using JJMrsulsw --1 KV lKV1.35E+17 8.09E+16 6.31 E+16 5.47E+16 4.60E+I 5.49E+16 3.91 E+16 Vol. Res. One min. 6 4.81 E+17

(ohm-cm)(ohm-cm)
3 KV 8.34E+17 6 6 6 6 1.03E+17 9.94E+16 6.35E+I 6 8.32E+I 6 8.04E+I 6 8.05E+l 6

1.98E+17 7.67 E+161 9.84E+161 6,05 E+161 5.89 E+16[ 5.74E+161 3.78E+I 6/

[ 6.73E+17 1.35E+17 2.57E+17 1.09E+17 1.53E+17 1.72E+17 1,23E+17

2.93E+17 1.41 E+17 1.08E+17 1.09E+17 9.32E+I 1.22E+17 l.ol E+17 6

w 8.48E+17 5.22E+I 4.33E+I 3.77E+I 3.46E+16 3.05E+I 3.26E+16

0.30 .0.698 1000 0.44. ~ ~ 0.51 0.695 1000 0.53 0.61 ~ den. grlcc 0.702 ~ ~ thick. cm 1000 1000 1000

1.21 E+17 1.52E+17 1.26E+17 1.20E+17 1.46E+17 1.04E+17 Vol. Res. Three min.

110397-D1 11 1197-D2 1 11397-C3

Sample No.

volts

Electrode Area

1:1 min.

1:3 min.

1:1 min. ~4/28/98

1:3 min. measurements)

Sandia, CA Raw data

CA data with no carbon cloth measurements)

in serts. all alIKV

CA data w th no carbon cloth inser ts, all at 1 KV

(4/24/98 and cal d VR results 11 1997-D2 0.23 0.700 ~

111697-D6 112497-A1 11 1697-AI 110397-D1 111197-D2 111397-C3

0.30 = 1000 0.44 0,704 1000 0.51 0.695 1000 0.53 0.702 1000 0.61 0.703 1000 0.69 0.708 1000

96.987 96.987 96.987 96.987 96.987 96.987 96.987

1.25E-1 2 2.04 E-I 2 3,98E-12 4.40E-12 4.30E-12 4.07 E-I 2 4.73E-12

4.90E-13 9.30E-13 2.20E-12 2.23E-12 2.02E-12 1.86E-12 2. IOE-12

1.II E+17 6.81 E+16 3.46E+16 3.17E+16 3.21 E+16 3.39E+16 2.90E+16

2.83E+17 1.49E+17 6.26E+16 6.26E+I 6 6,84E+I 6 7.42E+16 6.52E+16

1.16E-12 2.05E-12 4.32E-12 4.69E-12 4.28E-12 3.25E-12 4.25E-12

4.70E-13 8.IOE-13 2.27E-12 2.24E-12 2.05E-12 1.23E-12 1.94E-12

1.19E+17 6.78E+I 6 3.19E+16 2.98E+16 3.23E+16 4.24E+16 3.22E+I 6

2.95E+17 1.72E+17 6.07E+16 6.23E+16 6.74E+I 6 1.12E+17 7.06E+I 6

Sandia, CA Raw data and cald VR resui t s 11 1997-D2 s. Avera9 e of CA 4124 and 412 E measurerr en t all at 1 KV 0.23 .0.700 1000 0.30 0.698 1000 0.44 .0.704 1000 0.51 0.695 1000 0.53 0.702 ~ 0.61 0.703 1000 0.69 .0.708 1000

11 1697-D6 112497-A1 111697-AI 110397-D I 111197-D2 111397-C3

96.987 96.987 96.987 96.987 96.987 96.987 96.987

1.21E-12 2.05E-12 4.15E-12 4.55E-12 4,29E-12 3.66E-12 4.49E-12

4.80E-13 8.70E-13 2.24E-12 2.24E-12 2.04E-12 1.55E-12 2.02E-12

1.15E+17 6.79E+16 3.32E+I 6 3.07E+16 3.22E+I 6 3.77E+16 3.05E+16

2.89E+17 1.60E+17 6.16E+16 6.24E+16 6.79E+I 6 8.93E+I 6 6.78E+16

Vol u me Re s stivitv Yleasurements on Machine d Poiyure t %ane Foam Samples iS$ndia.cA ar d NM data with/without carbon cloth insert s) den. Sample No. 9rlcc thick. cm Electrode Area (sq. cm.) Sandia, NM csld VR resul t s only 120897-A3 120897-62 120897-C2 120397-B2 120897-D7 0.15 0.22 0.31 0.37 0.50 den. gricc 0.672 0.698 0.700 0.702 0.685 thick. cm Vol. Res. One min. Vol. Res. Three min. Vol. Res. Vol. Res. Three min. (ohm-cm) 2 Kv 3.50E+18 1.12E+18 7.48E+17 8.39E+17 Vol. Res, One min. Vol. Res. Three min. Vol. Res. Voi. Res. Voi. Res. Vol. Res. Vol. Res. Vol. Res.

volts

One min.
(ohm-cm) 2 KV 7.01E+17 4.22E+17 3.54E+17 2.40E+17

(picoamps) ( picoamps) 1 KV

NM re$WI ts with n I carbon CI oth inserts

1 KV
1.17E+18 8.44E+17 6.73E+17 1.66E+16

1000 1000 1000 1000 1000

23.55 23,55 23.55 23,55 23.55 Electrode Area

4.38E+I 7 3.37E+I 7 3.06E+I 7 2.24E+17 -

One min. Three min. One mint Three min. one rnin hree in (ohm-cm) (picoamps) (picoamps) (ohm-cm) NM resul ts with using carbon clot lhySgJ&5 3 KV 3 KV 1 KV 2 KV 1 KV 2 KV LLKY MY 1.70E+17 1.00E+18 7.97E+16 8.76E+17 3.19E+17 7.01 E+17 1.75E+18 2.92E+17 2.81 E+17 3.21 E+17 1.16E+17 9.64E+17 1.23E+17 3.69E+17 1,12E+18 3.37E+17 3.61 E+17 2.80E+17 9.18E+17 6.29E+17 2.80E+17 1.53E+17 6.73E+17 4.44E+I 7 2.49E+17 1.77E+17 5.61E+17 4.47E+17 1.77E+17 1.09E+17 3.74E+17 1.94E+17

Sample No.

volts (4/24/98 1000 1000 1000 1000 1000

i: 1 min.

i: 3 min.

Vol. Res. One min.

Vol. Res. Three min.

1:1 min.

1:3 min.

Vol. Res. One min.

Voi. Res. Three min.

Sandia, CA Raw data and cald VR res Uita 120897-A3 0,15 0.672 120897-B2 Ul m 120897-C2 120397-B2 120897-D7 0.22 0.31 0.37 0.50 0.698 0.700 0.702 0.685

GA data with no carbon CIOt b inserts. measurements) 96.987 96.987 96.987 96.967 96.987 6.70E-13 7.20E-13 8.70E-13 I,17E-12 1.22E-12

ell at 1 KY 2,15E+17 1.93E+17 1.59E+17 1.18E+17 1.16E+17 4.37E+17 3.56E+17 3.65E+17 2,66E+17 2.72E+17

CA data W h no car b on cloth ins f!rts. all at 1 KY (4/28/98 measurements) 5.90E-13 5.90E-13 8.20E-13 1.50E-12 1.32E-12 2.50E-13 3.50E-13 3.50E-13 4.60E-13 5.30E-13 2.45E+17 2.36E+I 1.69E+17 9.21E+16 1.07E+17 7 5.77E+17 3.97E+17 3.96E+I 3.00E+17 2.67E+17 7

3.30E-13 3.90E-13 3.80E-13 5,20E-13 5.20E-13

AVer@3eof CA 4124 m
120897-A3 120697-B2 120897-C2 120397-B2 120897-D7 0.15 0.22 0.31 0.37 0.50 0.672 0,698 0.700 0.702 0.665 1000 1000 1000 1000 1000 96.987 96,967 96,987 96.987 96.967

4128 measureu 1.E@5 2.90E-13 3.70 E-I 3 3.65E-13 4.90E-13 5.25E-13 , 2.29E+17 2.12E+17 1.64E+17 1.03E+17 1. II E+17 4.98E+17 3.76E+17 3.80E+i7 2.82E+17 2.70E+17

6,30 E-I 3 6055E-13 6.45E-13 1.34E-12 1.27E-12

Volume

Resistivltv

I-=d=d
Samp[eo. N
~-Molded

Measurements l___l__l____ (cm) 0.575 0.724 0.720 0.720 0.720 0.720 0,711 0.716 0.716 0.700 0.703 0.710 0.708 0.714 0.715 0.731 0.72 0.714 0.716 0.719 0.714 0.713 0.721 0.711 0.716 0.712 0.719
I I

on As-Molded

Fo

n Samdes

fall Sandia.CA

data with no carbon cloth inserts] Vol. Res. One min. Johm-cm) 6.09E+16 . 8.59E+16 ... 5.96E+16 8.75E+16 5.24E+16 5.12E+16 1.20E+17 7,65E+16 7.74E+16 6.89E+16 4.98E+16 6.83E+16 6.88E+16 7.19E+16 5.34E+I 4.13E+16 1.04E+18 2.19E+17 2.60E+17 1.55E+17 1. II E+17 2.03E+17 3,28E+17 1.41 E+17 1.65E+17 1.14E+17 1.07E+17
I [

Electrode
Area

I (gr/CC)

ErIoxv* 0,56 0.58 0.66 0.67 0.74 0.74 0.28 B 0.28 0.46 0.46 0,59 0,60 0.68 0.68 0.83 0.82 Polyurethane 0.19 0.32 0.39 0,53 0.63 0.75 0.19 0.30 0.40 0.52 0.63
I

82598EP3A 82598EP4B 82598EP5B 82598EP5A 82598EP6A 82598EP6B 82798EP1A 82798EPI 82798EP3A 82798EP3B 82798EP4A g 82798EP4B 82798EP5A 82798EP5B 82798EP6A 82798EP6B As-Molded 90298PUIA 90298PU2A 90298PU3A 90298PU4A 90298PU5A 90298PU6A 90298PUIB 90298PU2B 90298PU3B 90298PU4B 90298PU5B

---L
volts 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000 1000
I

1: 1 min. _IF?!Q@i& 2.77E-12 1.56E-12 2.26E-12 1.54E-12 2.57E-12 2.63E-12 1.14E-12 1.77E-12 1.75E-12 2. OIE-12 2.77E-12 2.00E-12 1.99E-12 1.89E-12 2.54E-12 3.21 E-12 1.30E-13 6.20E-13 5.20E-13 8.70E-13 1.22E-12 6.70E-13 4.1 OE-I3 9.70E-13 8.20E-13 1.20E-12 1.26E-12
I I

1:3 min. (P icoamps) 1.12E-12 7.00E-13 1.02E-12 3.50E-13 1.12E-12 1.06E-12 5.50E-13 5.30E-13 6. IOE-13 7.90E-13 1.38E-12 8.00E-13 6.60E-13 6.50E-13 9.00E-13 1.28E-12 1.00E-14 2.40E-13 1.50E-13 3.40E-13 2.60E-13 2.40E-13 8.00E-14 4.40E-13 2.50E-13 5.50E-13 4.60E-13 formulated

Vol. Res. Three min. (ohm-cm) 1.51 E+17 1.91 E+17 1.32E+17 3.85E+17 1.20E+17 1.27E+17 2.48 E-I-17 2.56E+17 2.22E+17 1.75E+17 1.00E+17 1.71 E+17 2.08 E-I-17 2.09E+17

sq. cm.) 96.987 96.987 96.987 96.987 96.987 96.987 96.987 96.987 96.987 96.987 96.987 96.987

96.987 96.987 96.987 96.987 96.987 96.987 96.987 96.987 96.987 96.987 96.987 96.987 96.987 96.987 96.987

1.51 E+17 1.04E+17 1.35E+19 5.66E+17 9.03E+17 3.97E+17 5.22E+I 5.67E+17 1.68 E+18 3.1 OE+I7 5.42E+I 2.48E+I 2.93E+17 7 7 7

First 6 epoxy samples formulated with Epon 828.

Last 10 epoxy samples

with Epon 830.

UNLIMITED

RELEASE

INITIAL DISTRIBUTION:
AlliedSignal, Inc. Federal Manufacturing & Technologies Mark Wilson, D/834-2C43 to: David Spieker Maxine Pennington, D/834-SC4 PO Box419159 Kansas City, MO 64141-6159 MS 0367 Ed Russick, 1815

Division (FM&T)

MS 0367
MS MS MS MS MS MS MS MS MS MS MS MS MS MS MS MS MS MS MS MS MS 0479 0481 0533 0834 0958 0958 0958 0958 0961 1407 1407 1407 1405 9001 9002 9003 9004
9007

Randall Saunders, 1815

Roy HoIt, 2151 Randy Harrison, 2167 Doug Weiss, 2343 Andy Kraynik, 9112 Carol Adkins, 1472 Matt Donnelly, 1472 John Emerson, 1472 Ramona Myers, 1472 John Sayre, 1403 Jim Aubert, 1815 Bob Lagasse, 1815 Tamara Ulibarri, 1811 Cliff Renschler, 1812

T. O. Hunter, 8000 Attn: P. N. Smith, 8500 D. L. Crawford, 5200 M. E. John, 8100

MS 9005
9031 9031 9054 MS 9405 MS 9420 9042 9403 9403 9403 9403 9405

J. B. Wright, 2200
R. C. Wayne, 8400/8900 P. E. Brewer, 8600 L. A. Hiles, 8800 W. J. McLean, 8300 T. M. Dyer, 8700 L. A. West, 8200 Wei-Yang Lu, 8746 Bill Even, 8713 Steve Goods, 8712 Marion Hunterj 8713 Jim Wang, 8713 Linda Domeier, 8230 (5)

MS MS MS MS MS MS

61

MS MS MS MS MS

9405 9405 9405 9405 9405

Craig Henderson, 8230 Jill Hruby, 8230 David Irvin, 8230 Pat Keifer, 8230 Dawn Skala, 8230

MS 9405
MS 9420 MS 9107 MS 9133 MS 9409 MS 9409 MS 9409 MS 9430 MS 9430 MS 9018 MS 0899 MS 9021 MS 9021

LeRoy Whinnery, 8230

L. A. West, 8200 Attn: V. Barr, 8210-2 B. E. Affeldt, 8210

G. Kubiak, 8250 C. Oien, 8260

R. Stulen, 8270 L. Tallerico, 8204 A. J. West, 8240 Central Technical Files, 8940-2 (3 copies) Technical Library, 4916 Technical Communications Department, 881 5/MS 0899, Technical Library, 4916 Technical Communications Department, 8815, for DOE/OSTl

62