insulation for solid rocket motor

7/29/2019 Insulation for solid rocket motor

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TECHNICAL REPORTEUSTOMXRIC INSULATION FCR SOLID PROPELIANTROCKET MOTORS

ByD. H. Sale

"Departent of the Army Project No. IO124401AAMC Code No.- 5025.11.8 4 2 03Report No. 64-3158 Copy No. .EL 1-9-100-2 Date 27 October 1964

DISTRIBUTED BY THE rHIS REPORT MAY BE DESTROYED WHENOFFICE OF TECHNICAL SERVICES NO LONGER REQUIRED FOR REFERENCEU. S. DEPARTMENT OF COMMER(CEWASHINGTON 25. D. C.


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The findings in this report are not to be construtedas an official Departm-nt of the- Army poxsitIon.

"(kxpies Available at Office of Technical Ser' ices S . 75


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Repcrt No, 64-3158Copy No.

ELASTOMERIC INSULATION FOR SOLID PROPELLANTROCKET MOTORS

By

D. H. SaleApprcved by:

A. C. HANSONLaboratory Dlrector

27 October 1964

DA Projec Nc. 1CO-24401-All0AMC Code Nn. 5025 11.84203

Rock IslaDd ArsenalRock Islandd !lltnois

DDC AvaIlabilltv Notice:Quailfied requesters may obtaincopies of this report from DDC.


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ABSTRACTThe 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 dis-persing fibrous compounding ingredients, are reported.Oxyacetylene torch and static motor firing test datafor 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 standardizedby the Flame Ablation Test Group of Section III-L of ASTMCommittee D-20.

A material with 40 percent elongation, 1.34 gm/ccdensity, performance ind3x of 95 cm2 sec/gm and erosionrate of 2.0 mils/sec was the most promising insulationdeveloped. The material is a 55/45 butadiene/acrylo-nitrile compound containing phenol furfural resin, asbestosand oxyazoline wetting agent. It has been satisfactorilybonded to aluminum and to steel by conventional bondingagent. The thermal properties of this vulcanizate arenot affected by oven aging for one week at 70 0 C.

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RECOMMENDAT IONSIt is recommended that this project be discont inued.It is believed that the insulation m ater ia ls developed

during the course of this investigation represent anadvancement in the state of the art and that furtherinves t lgat ions under the approaches outlined in this andearlier work would result in only marginal improvements.

I-- is recommended that th e oxyacetylent torch testeqipment be retained in a usable condition, in order thatpromising new commercial insulation materials might beevaluated and that cooperat ive work to further improve*his screening test might be conducted, if necessary

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ELASTOMERIC INSULATION FO R SOLID PROPELLANTROCKET MOTORS

CONTENTSPage No.

Object IInttroduction 1Procedure 2Results ard Discussion 4Literature References 14Appendix I 16Appendix II 17Distribut icn 18

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ELASTOERIC INSULATION FO R SOLID PROPELLANTROCKET MOTORS

OBJECTTo develop improved, flexible, thermal case insulation

for solid propellant rocket motors.INTRODUCTION

The need fo r flexfl rocket motor case insulation nasbeen well established, Elastomers have played animportant role in meeting this need, as evidenced by themany types of elastomeric-based insulations which have beendeveloped for use in solid propellant missiles. The widespectrum of commercially available insulation ranges fromlightly filled rubbers with excellent flexibility butminimal ablation resistance, to highly loaded compoundswith little Alexlbility but outstanding resistance to thehigh temperatures and erosive gases found within rocketmotors.

Present day elastcmeric insulations are not consideredadequate for future neeas. especially needs related to theuse of end burning grains. It is anticipated that longerburning times at higher temperatures will necessitate morethermally resistant insulations and that higher internalpressures will require higher degrees of flexibility. Acontinuing need exists frr l ighter weight materials,

I-, ppears that maximum flexibility and resistance toth e environments within rocket motors are mutuallyexclusive properties. insofar as rubber-based insulationsare concerned, since tmprcvements in one property areattainable only It the expense of the other. Earlier workat this Arsenal, -8,9) as well as more recent studies, hasled to the development of r-'bber-based insulations havinga compromise In these two properties, namely, the highestdegree of ablative resistance which could be attainedtogether with flexibility which, when measured in terms ofelongation, amounts to 20 to 50 percent. Results of thesestudies have led to the following conclusions:

1. By far the cost effective filler combination forimparting ablation resistance to rubber vulcanizates is acombination of a phenolic resin and long fiber asbestos.2. This filler combination is most effective in a

high nitrile content, butadiene/acrylonitrile elastomer.Of the more than 400 combinations of elastomers, fillers

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and other compounding ingredients tested, none has led toa material having a better compromise between flexibilityand abltion resistance than that exhibited by the nitrile-phenolic resin-asbestos fiber system.

3. The degree of ablation resistance of this , or anyother asbestos-containing rubber compound, is directlyrelated to th e fiber length of the asbestos in the finishedproduct.

These findings largely influenced the direction ofeffort described in this report. Minimum effort has beendevoted to seeking more effective combinations of rubberand fillers. Major emphasis has been placed on developingmeans for incorporating long fiber asbestos into rubber-resin matrices without significantly reducing fiber length.PROCEDURE

Insulation resistance was determined with an oxy-acetylene torch test (Figure 1) using the conditons citedin Table I. The equipment and procedures duplicate thoseof the test currently in the f inal stages of standardizationby th e Flame Ablation Test Group of Section III-L of ASTMCommittee D-20.

The effectiveness of candidate insulation materialswas meawured by two test criteria; (1) the temperaturerise on the back side of the specimen while the frontside was exposed to the oxyacetylene torch flame and (2)th e time required for the flame to burn through th especimen. These criteria are reported as performanceindices and erosion rates, respectively. The index,referred to as P 2 0 0 , is computed by dividing the time(seconds) required for the specimen back side to reach200 0 C. by the original specimen thickness (centimeters)and by the specimen specific gravity The erosion rate,E, is computed by dividing th e original specimen thickness(mils) by the burn through time. It should be noted thathigh values of P 2 0 0 and low values for E are indicative ofgood insulation properties. Unless otherwise noted, th eperformance indices and erosion rates reported are theaverage of four test results

Rock Island Arsenal Laboratory has been an activemember of the aforementioned ASTM Test Group. The torchtest facility at this Laboratory was among those utilizedin a recent round robin. The round robin results showedan average variance among laboratories of less than 5% fo reacn of th e Iwo test criteria. The Rock Island Arsenaltest facility produced results well within this variance.

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TABLE ITORCH TEST OPERATING CONDITIONS

Oxygen flow rate, standard cubic feet/hour (SCFH) 123Acetylene flow rate, SCFH 102Volume ratio oxygen to acetylene 1 2Impingement angle between flame and specimen, degrees 90Specimen size, inches 4 X 4 X 1/4Distance from torch tip to specimen, inches 3/4Method of determining moment of burn through Visual

Several materials which exhibited excellent resistanceto the torch test were evaluated (see Table VII) In staticmotor firings conducted b,, the AtlantIc Research Corporationand the Allegheny Ballist ics Laboratory at their respectivetest facilities.The major compounding ingredients for each materialtested may be found in the tables pertaining to th ematerial. 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 twobladed sigma type mixer (Figure 2), with mi.xing armsoperating at differential speeds. All solid polymer-based compounds were mixed on a two roll rubber mill.Stress-strain properties were determined in accordancewith applicable ASTM(lO) proceduresRESULTS AND DISCUSSION

Previous evalua.cn( 9 ' of several types of inorganicand organic fibers had shown that asbestc3 was the mosteffective fo r imparting thermal resistance tc rubbervulcanizates Curren, studies were made to determine th eeffect of the type cf asbestcs on the properties ofinsulation materials Amosile, crocadolite and chrysoti leasbestos of approximately equal fiber length "major con-centration of fiber lengths. 3/4 to 1 inch long) wereevaluated in a nitrile r.ibber..phenol.c resin based compcuindChrysotile samples from three different suppllers wereincluded The results in Table II show that the threechrysotile-based vulcanizates differ from one anotherconsiderably, but that all three are superior to eitherthe amosite or crocidolite-based insulations. The supe-riority of chrysotile is attributed to its flexibility(both amosite and crocidolite are brittle and tend tosuffer fiber breakdown during compounding), higher specificheat and fusion temperature, lower density and higherpercent of bound water- Hereinafter, the word "Asbestos"

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99Tin this report refers to chrysotile #1.

The problem of obtaining a uniform dispersion of longasbestos fibers in a rubber matrix while et th e same time *minimizing th e reduction in fiber length was attacked *through the use of the following classes of materials:(1P wetting agents, to wet th e asbestos fiber and thusfacilitate fiber dispersion; (2) plast icizers , to softenthe rubber matrix; (3) liquid polymers, to reduce shearingforces which prevail when solid polymers are mixed; (4)s lvents, to dissolve th e unvulcanized rubber prior to th e 0asbestos addition.

Evaluationsof wetting agents were made as shown in (Table 1I1. The wetting agents were added to th e mixture Cjus# prior to th e asbestos. Although most of th e wetting Wagents tested were useful in dispersing th e asbestos,not all improved insulation properties. However, oxyazoline#1. a heterocyclic cationic wetting agent, produced vul-canizates with excellent thermal properties. A compoundccntairning 30 PH R of this wetting agent produced a 25 percentimprovement In thermal properties and a 100 percent increasein elongation over th e control material containing nowetting agent.

Oxyazoline #1 at 30 PH R concentration showed no evidenceof 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 unagedcontrols. Insulation containing oxyazoline #1 has beenbonded to both aluminum and steel using a two part, roomtemperature curing, general purpose epoxy adhesive. Bondstrengths (tensile shear on one inch lap joints) greaterthan th e tensile strength (1730 psi) of the insulationwere achieved.

Data for plasticized solid elastomer-resin-asbestosccmpounds and unplasticized control compounds are presentedin Table IV. Small amounts (5 and 15 PHR) of phosphateesters served to increase elongation but larger amountsdecreased elongation. None of the vulcanizates hadimproved thermal properties over th e controls.Liquid irgredients offer a means of compounding with

Icv shear forces. Data for liquid elastomer-asbestosvl;canizates, as well as th e appropriate controls basedon solid polymers, are given in Table V. The data revealedthe following results: vulcanizates based on l iquidelastomers have better thermal properties, greater tensilestrength but shorter ultimate elongation than the controlsbased on solid polymers. The liquid elastomers consistedcf low molecular weight, short chain molecules which required

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a high state of cure to produce good thermal resistance.Although these elastomers did facilitate th e incorporationof fibrous asbestos without appreciable fiber breakdown, th ehigh degree of crosslinking required for proper vulcanizationproduced lower elongations than are inherent with solid| polymers.

Further evaluation of liquid elastomers included th eaddition of thermosetting resins (liquid and solid) asfillers. The resins used in this stuoy were all polarand enhanced th e erosion resistance of NBR-based compounds,but they were too incompatible with th e less-polar SB Rto be effective. Because of the lack of non-polar resinsand th e low elongations obtained with th e liquid elastomers,work with SB R and NBR liquid elastomers was di3continuedo

The two carboxy modified polymers listed in Table Vwere vulcanized using an epoxy resin at a concentration of13 PH R as a curative. The low elongations obtained fromthese two compounds eliminated the need for investigatingthe effect of adding more resin.

The method of incorporating asbestos by adding it toa methyl ethyl ketone solution of the polymer and othercompounding ingredients proved unsuccessful. The asbestosin th e resultant vulcanizates was non-uniformly dispersedin th e rubber matrix after air and vacuum evaporation of thesolvent. These vulcanizates had properties inferior to theproperties of vulcanizates prepared by conventional millingprocedures.

Torch test data for several commercial insulationmaterials tested are presented in Appendix II. Of thesen-aterlals, one has properties comparable to the bestRock 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 materialsand two commercial products, were evaluated in static motorfirings by Atlantic Research Corporation. Erosion rates,densities, elongations and major constituents fo r each arepresented in Table VII. The erosion rates from th e staticfiring tests correlate reasonably well with the torchtest erosion rates, at least for the best five or six andthe poorest compounds. The erosion rates from th e statictests cover a range of only 2.4 units, as compared to 10.4units for the torch test.

Unfortunately th e insulation containing oxyazoline #1wetting agent was not included with th e above materials.

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TABLE VIEVALUATION DATA FO R THE BEST ROCK ISLAND ARSENALAND COMMERCIAL INSULATIONS

Property Measured Rcck Island Arsenal Commercial #IP200- Cm 2 sec/gm 95 79Time to backside 127 101temperature of 2000C.for 1/4" specimen, sec.E, mils/sec 2.0 2.0Elongaticn, % 40 50Density, gm/cc 1.34 1.28Major constituents Rubber, Resin, Rubber.

Asbestos, Oxyazoline #1 Resin, AsbestosHowever, this material was submitted to Allegheny BallisticsLaboratory fo r evaluation in their test facilities Theirata indicates that it compares favorably yh materialsthey class as "current better materials."(11 t

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LITERATURE REFERENCES

1. Batchelor, J. D. and Vasileff, N., "Solid PropellantRocket Motor Insulation," Conference on Behavior ofPlastics in Advanced Flight Vehicle Environments,WADD Technical Report 60-101, September 1960.

2. Dervy, A. J., "Reinforced Plastics of High Strength/Weight Ratio for Space Applications," Society of th ePlastics Industry, Inc., 17th Anrual Techn.Lcal andManagement Conference, Reinforced Plastics Division,Chicago, Illinois; 6,7,8 February 1962.3. Epstein, G., Cecka, A. M. and Robbins, D. L., "Plastics

in Rocket Nozzle Environments," Conference on Behaviorof Plastics in Advanced Flight Vehicle Env:!ronments,WADD Technical Report 60-101, September 1960.

4. Epstein, G. and Jaffe, E. H., "M aterials for InternalTnermal Protection of Rocket Motor Cases. A State-of-the Art Survey," Society of the Plastics Industry, Inc.,17th Annual Technical and Management Conference,Reinforced Plastics Division, Chicago, Ill; 6,7,8February 1962.

5. Hazelrigg, W. K., "Design Criteria for InsulationMaterials " a paper presented to th e Refractory MaterialWorking 6i-iup, Aerojet-General Corporation, Sacramento,Califcrnia, 14 July 1960.

6. Headrick, R. E., "Ablative Elastomeric InsulationM aterials," Directorate of Materials and Processes,W right-Patterson Air Force Base, ASD-TDR-62-400,August 1962.7. Sewell. J. J. and Kuno, J. K., "Aerospace Use of PlasticHardware and Thermal Insulation," Society of th e PlasticsIndustry, Inc., 17th Annual Technical and Management

Conference, Reinforced Plastics Division, Chicago,Illinois; 6,7,8 February 1962.

8. Rack Island Arsenal Laboratory Report No. 61-2315,2 August 1961. "Evaluation of Flexible Insulation fo rSolid Propellant Rocket Motor Cases."

9. Rock Island Arsenal Laboratory Report No. 62-2366,6 July 1962, "Development of Flexible Insulation fo rSolid Propellant Rocket Motor Cases."

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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.isticsLaboratory to Rock Island Arsenal, Subject:'Evaluation of Car didate Insulation Material"(U),25 June 1964.

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D1)TRIBUTIONNo. o0 Copies

A. Department oi befenseOffice oi tfae Director ou DeienseResearch & -.nineeringATTN: Mr. J. C. i3arrettRoom JD-10i5, The PentagonWashington 25, D. C. ICo,-m,.ma n ,e rDelense Documentation CenterATT 'N: T' DRCameron - ationAlexanuria, virginia 22314 20

G. Department of the Arms - Technicai . ,ervicesCommanding GeneralU,.. Arny 41.ateriel CommandRoom 25J2, Bldg. T-7ATTN: AMCRD-RS-CMWashington, D. C. 20315 1Commanding OfficerU... Army Coating and Chemical LaboratoryATTN: Dr. C. Pickett 1Techpical Library IAberdeen Proving Ground, Maryland 213)5Commanding GeneralU.:. Army Tank Automotive CenterATTN: SMOTA-REM. 2 iEMOTA- R'M. 3 1Warren, Michigan 4b990Commanoing eneraiU.s. Army Weapons CommandATTN: AMS WE-RD I

AM'I WE-PPRock Island ArseralRock Island, Illinols

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Commanding GeneralU.S. Army M issile CommandATTN: Documentation & Technical

Iniormation Branch 2Mr. R. E. Ely, AMSMI-RRS 1Mr. R. Fink, AMSMI-RKX 1Mr. W. K. Thomas, AMSMI 1Mr. Z. J. Wheelahan, AMSMI-RSM 1

Redstone Arsenal, Alabama 35b09Commanding OfficerFrankford ArsenalATTN: SMUFA-1330 1Library-0270 IPhiladelphia, Pa. 19137Commanding OfficerU.3. Army M aterials Research AgencyWatertown ArsenalATTN: RPDWatertown, Mass. 02170 1Commanding OfficerPicatinny ArsenalATTN: Plastics & Packaging Lab. 1

PLASTEC 1Dover, New Jersey 07801Commanding OfficerSpringfield ArmoryATTN: SWESP-TXSpringf ie ld, Mass. 01101 1Commanding OfficerWatertown ArsenalATTN-. SMIWT-LXWatertown, Mass. 02170 1Commanding OfficerW atervl iet ArsenalATTN: SWEWV-RDRWatervliet, New York 12189 1Commanding GeneralU.S. Army Munitions CommandDover, New Jersey 07801 1

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Commanding OfficerU.S. Army Environmental Health LaboratoryArmy Chemical Centvr, Maryland 1Commanding OfficerU.S. Army Chemical Warfare LaboratoriesATTN: Technical LibraryArmy Chemical Center, Maryland ICommanding OfficerHarry Diamond LaboratoryATTN: Technical LibraryWashingtoxA, D, C. 20436 1Commanding OfficerU.S. Army Engineer R&D LaboratoriesATTN: Chemistry Research Section,

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Commanding OfficerU.S. Army Research Office (Durham)Box CM, Duke StationDurham, North CarolinaChief of Research & DevelopmentU.S. Army Research & DevelopmentLiaison GroupATTN: Dr. B. SteinAPO 757New York, N. Y. ICommanding OfficerU.S. Army Aviation SchoolATTN: Office of the -ibrarianFort Rucker, Alabama 1

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CommanderU.:. Naval Ordnance Test StationATTN: Technical Library BranchChina Lake, California 1CommanderU.6. Naval Reseaech LaboratoryATTN: Technical Information CenterAnacostia StationWashington 25, D. C. 1CommanderMare Island Naval ShipyardATTN: Rubber LaboratoryVallejo, California 1

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and DevelopmentATTN: Lt. Col. J. B. Shipp, Jr.Room 4D-313, The PentagonWashington 25 , D. C. I

CommanderWright A ir Development DivisionATTN: ASRCZE-1 1WWRCO 1Materials Central 1Wright-Patterson Air Force Base, Ohio6593 Test Group (Development)ATTN: Solid Systems Division, DGSCEdwards Air Force Base, California 1CommanderAMC Aeronautical Systems CenterATTN: Manufacturing & Materia.sTechnology Division, LM!BMOWright-Patterson Air Force Base, Ohio 2Commanding OfficerBrookley Air Force BaseATTN: Air Force Packaging LaboratoryAlabama 1

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E. Other Government AgenciesScientific & Technical Information FacilityATTN: NASA Representative (SAK/DL) IMr. B. G. Achhammer 1Mr. G. C. Deutsch 1Mr. R. V. Rhode 1P.O. Box 5703Bethesda, Maryland 20014George C. Marshall Space FlightATTN: M-S&M-MI

M-R?-AE-M IHuntsville, Alabama 35800Commanding GeneralU.S. Army Weapons CommandATTN: AMSWE-RD 3Rock Island Arsena.lRock Island, Illinoisforrelease toCommanderBritish Army StaffATTN: Reports Officer3100 Massachusetts Avenue, N. W.Washington b, D. C.Commanding GeneralU.S. Army Weapons CommandATTN: AMSWE-RD 3Rock Island ArsenalRock Island, Illinoisforrelease toCanadian Army Staff, WashingtonATTN: GSO-l, A&R Section2450 Massachusetts Avenue, N. 11.Washington 6, D. C.Prevention of Deterioration CenterNational Academy of ScienceNational Research Council2101 Constitution AvenueWashington 25, D. C.

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