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TECHNICAL REPORT
EUSTOMXRIC INSULATION FCR SOLID PROPELIANT
ROCKET MOTORS By
D. H. Sale
IO124401A 03
Copy No.
.
27 October 1964
Date
The findings in this report are not to be construted as an official Departm-nt of the- Army poxsitIon.
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ELASTOMERIC
By
D.
H. Sale
Apprcved by:
27 October 1964
DDC AvaIlabilltv Notice: Quailfied requesters may obtain copies of this report from DDC.
ABSTRACT The development of flexible, elastomeric-based, solid propellant rocket motor case insulation is discussed. The effect on insulation properties of type of asbestos, of liquid versus solid elastomers and of methods of dispersing fibrous compounding ingredients, are reported. Oxyacetylene torch and static motor firing test data for some of the better insulation materials developed, as well as for souie commercial materials, are presented. The torch test, the principle screening tool used in this study, conforms to the test currently being standardized by the Flame Ablation Test Group of Section III-L of ASTM Committee D-20. A material with 40 percent elongation, 1.34 gm/cc density, performance ind3x of 95 cm2 sec/gm and erosion rate of 2.0 mils/sec was the most promising insulation developed. The material is a 55/45 butadiene/acrylonitrile compound containing phenol furfural resin, asbestos and oxyazoline wetting agent. It has been satisfactorily bonded to aluminum and to steel by conventional bonding agent. The thermal properties of this vulcanizate are not affected by oven aging for one week at 70 0 C.
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RECOMMENDAT IONS project be discontinued. It is recommended that this It is believed that the insulation materials developed investigation represent an during the course of this and that further of the art advancement in the state and inves t lgations under the approaches outlined in this improvements. only marginal in would result work earlier I-- is recommended that the oxyacetylent torch test eqipment be retained in a usable condition, in order that promising new commercial insulation materials might be evaluated and that cooperative work to further improve might be conducted, if necessary *his screening test
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ELASTOMERIC
Object Inttroduction Procedure Results ard Discussion Literature References Appendix I Appendix II Distribut icn
I
1 2 4 14 16 17 18
iii
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ELASTOERIC
ROCKET MOTORS
OBJECT To develop improved, flexible, thermal case insulation
are concerned,
Earlier work attainable only It the expense of the other. at this Arsenal, -8,9) as well as more recent studies, has led to the development of r-'bber-based insulations having a compromise In these two properties, namely, the highest degree of ablative resistance which could be attained together with flexibility which, when measured in terms of Results of these elongation, amounts to 20 to 50 percent. studies have led to the following conclusions: combination for 1. By far the cost effective filler imparting ablation resistance to rubber vulcanizates is a combination of a phenolic resin and long fiber asbestos.
2.
high nitrile
fillers
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and other compounding ingredients tested, none has led to a material having a better compromise between flexibility resistance than that exhibited by the nitrileand abltion phenolic resin-asbestos fiber system. 3. The degree of ablation resistance of this, or any other asbestos-containing rubber compound, is directly related to the fiber length of the asbestos in the finished product. These findings largely influenced the direction of Minimum effort has been effort described in this report. devoted to seeking more effective combinations of rubber and fillers. Major emphasis has been placed on developing means for incorporating long fiber asbestos into rubberresin matrices without significantly reducing fiber length. PROCEDURE Insulation resistance was determined with an oxyacetylene torch test (Figure 1) using the conditons cited in Table I. The equipment and procedures duplicate those of the test currently in the final stages of standardization by the Flame Ablation Test Group of Section III-L of ASTM Committee D-20. The effectiveness of candidate insulation materials (1) the temperature was meawured by two test criteria; rise on the back side of the specimen while the front side was exposed to the oxyacetylene torch flame and (2) the time required for the flame to burn through the These criteria are reported as performance specimen. The index, indices and erosion rates, respectively. referred to as P 2 0 0 , is computed by dividing the time (seconds) required for the specimen back side to reach 200 0 C. by the original specimen thickness (centimeters) The erosion rate, and by the specimen specific gravity E, is computed by dividing the original specimen thickness It should be noted that (mils) by the burn through time. high values of P 2 0 0 and low values for E are indicative of Unless otherwise noted, the good insulation properties. performance indices and erosion rates reported are the average of four test results Rock Island Arsenal Laboratory has been an active The torch member of the aforementioned ASTM Test Group. test facility at this Laboratory was among those utilized The round robin results showed in a recent round robin. an average variance among laboratories of less than 5% for The Rock Island Arsenal eacn of the Iwo test criteria. test facility produced results well within this variance.
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TABLE I TORCH TEST OPERATING CONDITIONS Oxygen flow rate, standard cubic feet/hour (SCFH) 123
102 1 2
degrees 90 4 X 4 X 1/4 3/4 Visual resistance In static Corporation respective
Several materials which exhibited excellent to the torch test were evaluated (see Table VII) motor firings conducted b,, the AtlantIc Research and the Allegheny Ballistics Laboratory at their test facilities.
The major compounding ingredients for each material tested may be found in the tables pertaining to the material. Curing systems are given in Appendix I. Test specimens were compression molded in a four cavity mold. The liquid polymer-based ccmpounds were mixed in a two bladed sigma type mixer (Figure 2), with mi.xing arms operating at differential speeds. All solid polymerbased compounds were mixed on a two roll rubber mill. Stress-strain properties were determined in accordance with applicable ASTM(lO) procedures RESULTS AND DISCUSSION Previous evalua.cn( 9 ' of several types of inorganic and organic fibers had shown that asbestc3 was the most effective for imparting thermal resistance tc rubber vulcanizates Curren, studies were made to determine the effect of the type cf asbestcs on the properties of insulation materials Amosile, crocadolite and chrysotile asbestos of approximately equal fiber length "major concentration of fiber lengths. 3/4 to 1 inch long) were evaluated in a nitrile r.ibber..phenol.c resin based compcuind Chrysotile samples from three different suppllers were included The results in Table II show that the three
chrysotile-based vulcanizates differ from one another considerably, but that all three are superior to either
the amosite or crocidolite-based insulations. The supe-
riority of chrysotile is attributed to its flexibility (both amosite and crocidolite are brittle and tend to suffer fiber breakdown during compounding), higher specific
heat and fusion temperature, lower density and higher percent of bound waterHereinafter, the word "Asbestos" 4 64-3158
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The problem of obtaining a uniform dispersion of long asbestos fibers in a rubber matrix while et the same time minimizing the reduction in fiber length was attacked through the use of the following classes of materials: (1P wetting agents, to wet the asbestos fiber and thus facilitate fiber dispersion; (2) plasticizers, to soften the rubber matrix; (3) liquid polymers, to reduce shearing forces which prevail when solid polymers are mixed; (4) s lvents, to dissolve the unvulcanized rubber prior to the asbestos addition. Evaluationsof wetting agents were made as shown in The wetting agents were added to the mixture Table 1I1. Although most of the wetting jus# prior to the asbestos. agents tested were useful in dispersing the asbestos, However, oxyazoline not all improved insulation properties. #1. a heterocyclic cationic wetting agent, produced vulcanizates with excellent thermal properties. A compound ccntairning 30 PHR of this wetting agent produced a 25 percent improvement In thermal properties and a 100 percent increase in elongation over the control material containing no wetting agent. Oxyazoline #1 at 30 PHR concentration showed no evidence of migration after aging for 7 days in an air oven at 700 C. Aged specimens when evaluated in the oxyacetylene torch "est. exhibited thermal properties equivalent to unaged Insulation containing oxyazoline #1 has been controls. bonded to both aluminum and steel using a two part, room Bond temperature curing, general purpose epoxy adhesive. greater one inch lap joints) shear on (tensile strengths than the tensile strength (1730 psi) of the insulation were achieved. Data for plasticized solid elastomer-resin-asbestos ccmpounds and unplasticized control compounds are presented in Table IV. Small amounts (5 and 15 PHR) of phosphate esters served to increase elongation but larger amounts None of the vulcanizates had decreased elongation. improved thermal properties over the controls. Liquid irgredients offer a means of compounding with Data for liquid elastomer-asbestos Icv shear forces. vl;canizates, as well as the appropriate controls based The data revealed on solid polymers, are given in Table V. vulcanizates based on liquid the following results: elastomers have better thermal properties, greater tensile strength but shorter ultimate elongation than the controls The liquid elastomers consisted based on solid polymers. cf low molecular weight, short chain molecules which required
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a high state of cure to produce good thermal resistance. the incorporation Although these elastomers did facilitate of fibrous asbestos without appreciable fiber breakdown, the high degree of crosslinking required for proper vulcanization produced lower elongations than are inherent with solid polymers. Further evaluation of liquid elastomers included the
addition of thermosetting resins (liquid and solid) as polar The resins used in this stuoy were all fillers. and enhanced the erosion resistance of NBR-based compounds, but they were too incompatible with the less-polar SBR to be effective. Because of the lack of non-polar resins and the low elongations obtained with the liquid elastomers, work with SBR and NBR liquid elastomers was di3continuedo The two carboxy modified polymers listed in Table V were vulcanized using an epoxy resin at a concentration of The low elongations obtained from 13 PHR as a curative. these two compounds eliminated the need for investigating the effect of adding more resin. The method of incorporating asbestos by adding it to a methyl ethyl ketone solution of the polymer and other The asbestos compounding ingredients proved unsuccessful. in the resultant vulcanizates was non-uniformly dispersed and vacuum evaporation of the in the rubber matrix after air These vulcanizates had properties inferior to the solvent. properties of vulcanizates prepared by conventional milling procedures. Torch test data for several commercial insulation Of these materials tested are presented in Appendix II. n-aterlals, one has properties comparable to the best Rock Island Arsenal insulation, as shown in Table VI, The work discussed he...in and work previously reported(8,9) has resulted in several excellent thermal insulation materials. The nine best of these, along with five poorer materials motor and two commercial products, were evaluated in static Erosion rates, firings by Atlantic Research Corporation. densities, elongations and major constituents for each are The erosion rates from the static presented in Table VII. firing tests correlate reasonably well with the torch test erosion rates, at least for the best five or six and The erosion rates from the static the poorest compounds. tests cover a range of only 2.4 units, as compared to 10.4 units for the torch test. Unfortunately the insulation containing oxyazoline #1 wetting agent was not included with the above materials.
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TABLE V I EVALUATION DATA FOR THE BEST ROCK ISLAND ARSENAL AND COMMERCIAL INSULATIONS Property Measured P200- Cm 2 sec/gm Time to backside temperature of 2000C. for 1/4" specimen, sec. E, mils/sec Rcck Island Arsenal 95 127 Commercial #I 79 101
2.0
Elongaticn, Density,
gm/cc
Major constituents
However, this material was submitted to Allegheny Ballistics Laboratory for evaluation in their test facilities Their data indicates that it compares favorably yh materials they class as "current better materials."(11 t
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LITERATURE REFERENCES 1. Batchelor, J. D. and Vasileff, N., "Solid Propellant Rocket Motor Insulation," Conference on Behavior of Plastics in Advanced Flight Vehicle Environments, WADD Technical Report 60-101, September 1960. Dervy, A. J., "Reinforced Plastics of High Strength/ Weight Ratio for Space Applications," Society of the Plastics Industry, Inc., 17th Anrual Techn.Lcal and Management Conference, Reinforced Plastics Division, Chicago, Illinois; 6,7,8 February 1962. Epstein, G., Cecka, A. M. and Robbins, D. L., "Plastics in Rocket Nozzle Environments," Conference on Behavior of Plastics in Advanced Flight Vehicle Env:!ronments, WADD Technical Report 60-101, September 1960. Epstein, G. and Jaffe, E. H., "Materials for Internal Tnermal Protection of Rocket Motor Cases. A State-ofthe Art Survey," Society of the Plastics Industry, Inc., 17th Annual Technical and Management Conference, Reinforced Plastics Division, Chicago, Ill; 6,7,8 February 1962. Hazelrigg, W. K., "Design Criteria for Insulation Materials " a paper presented to the Refractory Material Working 6i-iup, Aerojet-General Corporation, Sacramento, Califcrnia, 14 July 1960. E., "Ablative Elastomeric Insulation Directorate of Materials and Processes, Wright-Patterson Air Force Base, ASD-TDR-62-400, August 1962.
Materials,"
2.
3.
4.
5.
6.
Headrick,
R.
7.
Sewell. J. J. and Kuno, J. K., "Aerospace Hardware and Thermal Insulation," Society Industry, Inc., 17th Annual Technical and Conference, Reinforced Plastics Division, Illinois; 6,7,8 February 1962.
8.
Rack Island Arsenal Laboratory Report No. 61-2315, 2 August 1961. "Evaluation of Flexible Insulation for Solid Propellant Rocket Motor Cases." Rock Island Arsenal Laboratory Report No. 62-2366, 6 July 1962, "Development of Flexible Insulation for Solid Propellant Rocket Motor Cases."
9.
14
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10.
American Society for Testing Materials, October 1961. "*ASTM Standards on Rubber Products," 1916 Race Street, Philadelphia, Pa.
il.
Confidential Communication, Allegheny Ball.istics Laboratory to Rock Island Arsenal, Subject: 'Evaluation of Car didate Insulation Material"(U), 25 June 1964.
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D1)TRIBUTION No. A. Department oi befense Office oi tfae Director ou Deiense Research & -. 'nineering ATTN: Mr. J. C. i3arrett Room JD-10i5, The Pentagon
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