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Lfl
N OFFICE OF NAVAL RESEARCH
IContract: N00014-85-K-0222
Work Unit: 4327-555
Scientific Officer: Dr. Richard S. Miller
Technical Report No. 22
BLOW-OUT OF RUBBER BLOCKS DUE TO INTERNAL HEATING
by
A.N. Gent and M. Hindi
Polymer Engineering CenterThe University of Akron ,
Akron, Ohio 44325
November, 1989
Reproduction in whole or in part is permitted for
any purpose of the United States Government
Approved for public release; distribution unrestricted
89 12
SECURITY CL.ASSIFICATION OF THIS PAGE OW$N- S-. 4 Enfr.__
I READ DLSTRUCTIONSREPORT DOCUMENTATION PAGE BEFORE CCMPLE724G FORM
1. REPORT NUMBER 2, GOVT ACCESSION NO 3. RECIPIENT'S CATALOG NUMBER
"Lchni I. Re 1 ,;rr X.', 22
4. TITLE (anc SblIil.) S. TYPE OF REPORT & PERIOD COVERED
Blow-out of Ro,ibber B cOc('- ie t lhlical Report
6. PERFORMING ORG. REPORT NUMBER
7. AUTHOR(#) I. CONTRACT OR GRANT NUMBER(@")
A."'. (',nt anI I.d . i cl i "0001l-6-j- -K-0222
I. PERFORMING ORGANIZATION NAME AND ADORESS 10. PROGRAM '.-E " TASK
olvner E,,i eerin, a 'nttr ARLA A WCRK UNiT NUMBERS
Flh University i Akro; 7-5Akr., Oio 4",325
II. CONTROLLING OFFICE NAME AND ADCRESS 1Z. REPORT DATE
. avai Rose a c Vemb" r 1989
13. NUMBER OF PAGES
.rMi: .ton, VA 221 7-3000 1714. MONITORING AGENCY NAME & AODRESS-(I dllfefrl ro. CMnmit llnj 0tflc.) 35. SECUJRITY CLASS. (of LhII. repot)
Unclassi r ied
isi. CECLASSI FICATION/ DOWNGRADINGSCEDUL E
16. DISTRIBUTION STATEMENT (of Lhis Report)
According to attached distribution list.
Approved for publ"ic release; distribution unrestricted.
17. DISTRIBUTION STATEMENT (of Lh.e absr rct .,t.,d In ftlock 20, If dtaffrt frm Report)
1I. SUPPLEMENTARY NOTES
-ubmitted to: lournal of Applied Polymer Science
It. KEV WORDS (Continue on reve..s aide I1 moce.aw7. a Idently b hlock rmbo,)
B low- ut, BtIr; tinv, Decompostion, Elast omers, }at'igue, leat Build-Up
Rubber , The rma I Dtecompo-, t 4 oil
20. ATSI RACT (C iImin- . "w es id If noese..a mild Idenfrify b i b
hocA nm br)
Boubber blocks undcrg o explosive blIow-cit when hatd a mi rowave
yen ,n. '['he process appears to be the same as th i ow-out . aused by
ie, O,, ted v-anp lie d, ,ovr ,. -,re ssive ],,;ids. -t a It-rihuLteLl to higbInternal pressures lelera ted 4-v I voiatije Rroduct or thermal decompos t ion.
(over)
DD , Nf. 1473 EDITION OF I NOV .- . OLE I
S/N 0102- LF- 011- 6601 &ECU ITY CLASSIFICATION OF TwIS PAGE (AC lh- D e * )
3 Lr s ti a~~)ci iL tr rcr4'Ar P.1 :-, t :14
tfl ut l11Q - -i 0 1 L 11 ~1 :1: I C K d 1 V '114 11 1 1 'I A?. .- : 1)v4I 111-
i-ubbr, 11bouL I.SO de)1,r>>-. In. mBR .- I:.1 f:n) pI mp1I11 t. I; XB m
-Accesst on For
NTIS ~A~DM2, TA?
p -!
SNC 107- LF- 014- 6601
SECURITY CL ASSIFICAT;CN OF T,,IS P AGEfl4I,- D.Im Enr.,.d)
2
BIcw-Cut C,: Ru bber 71CC. s .iue 77zer:a ean
nx t.
Instituate off Pclxvner Sc.-ence *:aiovmer anee rinq Ca_-nter
Th n- :ersiJt' afni 4kon Aon 3i -12
~Nen ruber Is cieformed, cart of t-e work or iscna7Cn:
transc~ed in o 'eat. -3ecalise r,.bor-er is a rather zoor ccrr:nuctc--
of:; heat, the internal temn=erature under rnael-'
ce or-ataocns can reach hich ye] uies. oes-ecaallv fcr hi c
ar icles. Ta4re treads and tank track ac can 'becc-,, so hot a
'blow,-out." 3ut the mecn-anaqsn or failu:re is not well -understocca-
7t h-as been attraztuted to 7nechanical fatigue [11 , and ba~,
tensile fracture acgravated b y high temperature (2,31 . n on
trast, it is attributed here to high internal pressure of
volatile substances, sufficient to burst ccen the surrocunding
material. The volatiles are thoucht to be a product of thermal
decc77.positaor.,. Zha ow that blocw-out can be P -cd~uced !b;y d4irect
neatano: of rub;ber co.-rzounds in. a macrowave oven, and to sc-e
extent by internal heating a rnboer sheets by embedded
resistance hezating wires,.,:ithout any -nechanical stressing.
2. 7xzerarental dle:
Vulcanized rubber .:ylinders, 5anhich and 17.-'-.-n in
u-ameter, and sheets of various thicknesses were made in a corn-
cression :rold using conventional recipes. Atypical mix formu-
lataon ."as as folloJjWsr. in parts by wei-cet: SB'R 1502, 100; car!bon
black, (N330, Vulcan 3, Cabot Corp.) , 53; ::,7 cxace, E; stearic
ici. , 2; processing oil (Sundlex 7 9OT, Sun~ oen Cj .) , 5 ;
sulur,1;accelerator (S antocure MCR, >onsanto Co.), 35.-
I:laiztc IC'~ efe1e by htiCT ror ,3 in at 1500C.
Values of %ouno's modulus S were etermne from streSs-
strain relations in comzression, at a mient and elevated
temperatures.
Cylindrical specimens were subjected to reneated ccmnresscn
using a Goodrich Fexoi~eter, as described in ASTM D623 - 67 [4].
The freuency cf loading was 30 Wz and the double-am" i,4 e t:
oscillation was 6.35mm. Static compressive loads of either 32 cc
43 kg were acolied to the sample by attaching weichts to the
macnine beam. Experiments were terminated when the sample faile
by blow-out, typically within !5 min. Veasurements cf blow-cut
temperature were made by means of a orobe tnermocci.e 7 nsert d
into the samole immediately after blow-out.
Other samples were heated in a microwave oven without
imposing any deformation. Blow-out similar to that obtained with
the Goodrich Flexometer occurred in less than one minute.
Some vulcanized sheets, about 6-m thick, were heated by
passing an electric current through a fine straight cooper wire,
about 125m long and 160 'm in diameter, embedded in the center
of the sheet before vulcanization. The pcower nput was adjusted
to heat the sample at about the same rate as in the microwave
oven, 3-5cC/sec. Internal temperatures were determined from the
measured resistance of the wire and the temperature coefficient
of resistance of copper. At temperatures between 200 and 300cC,
the rubber sheet showed surface discoloration, followed soon
aft. rwar~s by apearance of a blister, which is ccnsocren
ecuivalent to blow-out.
Thermocravimetric analysis was carried cut on sone cc:oOunds.
and the volatiles released by hblow-out were isolated and onalyzeA
by -as chromatography and -ass spectrometry.
(i) Blow-out ':rnm repea- e. :!cmressicn a=nd so~le-ly tron heatz:ng
Blow-out temceratures for Gloodrich flexometer sam'.Des are
-vn n Table 1 . They reached values of 7CO'C or more,
Ecutcs _ng Lhat bDIuw-QuL ias d consequence of thermal d3econ7Osa-4
tion of t".3 Lolvoer.
Blow-out temperatures for sanwol.es subjected to ',irect
neatang in the microwave c-:en -were a Droximately the- same, Table
1, arnd the a-.Dearce or t-oe failed sann,.les was also cuitle
-'. r I n i re1. -hu:- e criterion for blocw-out seems -: be
a sac-ae one: -hintr'c c z: te sample ou,,st reach a critical
tem,.erature. VMeco-nicaI vworkinq is only a means or: cenerating
heat internally; -it is not essential for blow-out.
Significant differences were noted in the anpearance of:
sarnoles . F :lexed saac-oles became barral-shaoe d, due to cconpression
set, Ficure 1, and decomcosition was concentrated in the center.
in contrast, nacrowave sa-noles deconnosed over larcer internal
recions, \-serever seveore '-.ating h-ad occurred.
(i4i) Elc-w-o'.t teno :era=tu res -for typicztl rubb-!er coroncu nd s
Blow-out tenerat-.:ros are given in Table 1. They ranged
fromn about l800C to about 250--c, 4epcencing u:pon th-e poly.7er a-nd
the mix formulation.
Two coeneral featuro:s -,.ere noted. First, the ilow-outl
teorature was higher for harder materials. For example, con-
rounds _R2 and S3R3 had d~ifferent amounts :E lfuz _n ccel-
erator, while :;1 nd s3? 3 d iffered in carbDon black content,
ga:-:cang v-ulcana.zate:S of th - so-me nolvoer with -ar*-edb,' different
eIeS t Ic od ulu'_s . Bwottook plaoe at hicher temeratu.res rr
a ycu;;_ a nodulIS H 3 tQ-creratureS Icse to
blcw- out temoerature are inciuded in Table i; they; ccnfrm this
ceneral conclusion. Moreover, this feature _ s consastent wath
the proposed mechanism o: low-out. The critical pressure at
which a small internal cavitv in a rubber block w;ill excand
indefinitely as uiven apprrximately by 5E/6 (5,6]. Thus, a
harder material would be expected to withstand higher internal
pressures without rupturiiq.
Some materials appeared to soften markedly at high tempera-
tures and undergo blow-mut at the same time. For example, butyl
rubber compounds turned into a soft, buttery consistency at the
blow-out temperature, about 18O'C. in contrast, NBR and SR com-
pounds were found to be stiffer than others initially and to
retain their stiffness at high temperatures. They were found to
have higher blow-out temperatures also.
Natural rubber compounds became soft and sticky as a result
of thermal decomposition, whereas NBR and SBR compounds remained
relatively dry. In both cases, however, blow-out took place
explosively, especially for NR materials with C-C or monosulfide
crosslinks (,,R2 a;;d NR4) which blew out at relatively high
temperatures, Table 1.
Polybutadiene compounds did not undergo blow-out, even after
long periods of heating in the microwave oven. instead, the
samples softened, swelled, and became porous in the interior,
Ficure 2. Apparently, the vapor pressure of the products of
decomposition is significantly lower for this polymer. "Blow-
cut" temoeratures were taken as the temperatures at which
7rcnounced swelling occurred.
Thus, two factors appear to govern the susceptibility of
rubber compounds to blow-out. The first is their propensity to
cenerate high-vapcr--pressure volatiles. The second is their
6
tenrnyo soften on -e at Ing and tnus I cse r es Is _,Cance
sion cf a oressurized internal cavitv.
(iii) Possible nature orf volatiles causing bo-u
Certain ingredients in rubber formulations would b-e exnecte8
to volatilize at hich temneratures and create a nn,: internal
pressure. For examole, If water is present, high internal pres-
sures woulId be generated at L -mperatures mu,,ch abcve 100'C. In
order to test this tossibility, 0.5 operceiit cK salt was included
4n several mix formulat-4ons and the vulcanized samoles werc
Qcaked in water :oc _-e." -ral days befcre testing, so that they
ar-soro-ed 1-21, *z; weiarht of water. Blow-out took< place at
virtually tie s ame temroerature as for dry samo.les, indicatinq
t"hat absorbed water is not the main cause of blow-out.
Another 0:ossible volatile ingredient of many rubber com-
pounds is a hydrocarbon proce ssing oil. However, when an other-
wise identical formulation was prepared with no processing oil,
blow-out took place at ab)out the same tem;eratu,,re as before.
Thus, the p-rocessing oil itself was not resoonsiblte for b-low-out.
A.nother possibility iS dissolved air. Samoles that h-ad been
stored in vacuo for four weeks were foun:-d to h'-;:.e sicnificantli
nigne r blow-out temperatures, by about 30'C, Table 2. COn exposing
them to air again for several weeks, the blow,-out tempcratures
were reduced almost back to the original values. TLhese results
suQuest that air is at least partially responsible for blow-out,
pcably by catalyzing thermal decomoopsition.
Different formuolations are known to differ in susceptiboility
to tner7mal decomposition. For exa-mole, 'ulcanizates with ccolv-
Gsulfide crOsslankzs will soften at lower, temteratures than those
with 7onosulfide or with carbon-carbon crosslir.;,s because of the
lower strenath of such linkaces. IfI crosslink rupture Is also
7
a cc c.7an Ied 2:cv 1oie I=ccto of a vol atrle subsoa-:I:onb Z
z;L ~ x ace when a significan: -.ecree o: c:asstn.,:
ruzct"re Occurs. -7n accord with this hvnothesls, c Er c;: _ -e
rec-, es, x'e dn aC -C c r oss 1 i ks , a nd 7,o r cs u 1f __5e (sl re ss)
recipes cave the highest b~cw-out temeratures, Table 1,
ar~zro acnhirg the temperatures at which zoivmer dcr~oiincl
be exoected. I-nd differences observed between ela stooers can, '-e
attribut_-ed to differences In stabZility of the crcsslin k s-cm-
wotnonr them.
-- as, oalthouzh he-eact natu,.re or: the vojato -
is not clear, the hxyzothesis that it is a caseous cof --he
3ecoozosltion of crcssln]- accou.nts -for the main _za__rsc
bDlow-outz, namely, the general temperature rance -4n w-toch it
oc-curs, its close relatioo~shiD with softening -eatrote
lower tlwottempzeratures fcr - terials ccntaiunc cx sooo
crcsslin}:s i.n compcarison with C-C crosslinks, and the markle-
4ifferences observed between cj.::"erent cjolvcmers.
(!'.) Decom-csition by he ating with an --mbecoeo resootan_=cewre
Temneratures of surface discoloration are coven in oe-
l~~r ccr~d ~=4t t '---u-reS or t 'e cr-oer
of 5001C. These temneratu.res are much noon)-er tohan toose :or
blow-out tut they are considered to be over-estimates so:
actlual t=-,erature because of heat losses t-roucoa te
rubber and severe d ecoocs it ion of rubber in the ot'oate
wocnit C'o thewie
: eOCoS1-ton temnzer: tures measured on tnos waw were fotu no
'_o be less reproci=ble than -ccrowa'e blo1w-out temoeratu;res and
th:,ey cended stroncly on the rate of heating. Thus, althouch
the wiore-heati~nq 7-etod is a:ooealincly simple,' :oe -to'-
-ess satlsfactcr: --,-an -,.crowave heating for determininz:
s I I- Ca 2 I <:' I
2 C .... __..W, at
-~~~ ~ s-- - - n---. C-. tC f u n.-d
7- , . V-: .e .r n_21 5
CCC t- 7 eV r eswee -
C 3 Sc e1 e 7C n I
77. r rec tc -.
aren== Ced~ to 7. .I c-r120_,t, cC2:stIf 200203 ..
_nc S er cser .- :f r tsc:1.fer e n ec -
i I e a t e ecz ,Du n2j~a~ a - r I.
e pr n, -j00 cas cw- t 4s t*-e ceneraticn c
I le, 51 c-;e c0512: C: ca7tc z.2. C l n:r: e
-'C: e a nd t zr~t
icse resistance to cavity ex,-ansion.
Differc-7 eatn r .2.'rtdifrn
9
- ~~~~~~~~~~ ... ca7r:s c .... n ru "z c ~ ' s Ico'" cu t r l t ''i" .
te.cera-" s at tS0C, 0 C w e- eas BR asd SE , cc2 o'rnas R1:'w cut
2 a t f r e s cfa'-- t c' C or .- n C- r vz a lene c
c U:-,ns i , d 1 c bc w cut c sister. they 4eve c e i r n a
a : te s -at crew I sze ns -zbr ....dmer t. ever burst Z;e t o the
xte r , '- ecau se t'-e va-cr cres sre neaver reachcd
s wrk s s,,; crteubh The £ffizecf cava
&r-' ) nd a :rant-!n- a .. . . -
.e a crh s .re lso n4etc -d o 2r . . Pcrter, . c
n- ;trczIer f: 1 -, 7 :e
w.- as resented at t'e Szsring tee2in.. (D t-e-
-eican Chemical Society, :al'as, Acrsl 19-22, 198 -
i. J. E. 7 u.:h ]n .7 r ,-nscn, Tranns. ,t . R h . i d 7
C32s -a a .....
,3 : 941).
i.~~~~~~~~~~~~~ c. 2.n c: 1- m -o - s=:, Tlrc -- i ''r n,- ...
t - - X... . . ... . . . . t " . .
*'er .OZ. , T <r.n o [a. -* 9
_.__.___ea , _5. __inh 2 2~ 5cL c anr, j %2art,'A7olm. ?ln 7 .
-., .- Z 19 7)
-- - .. . . t * -- C.. .. . .
. .. .. . .. .,: , E' . . . zj OC. I_.n .), e. .
I-:-.I6. :. :. en an D. A. 'c cki s, . .7-) .cch y.i. _, }-O r c{9
anz .xiscoc ra -c -- - . '~e: .... ,- -- - * ...,:- -
-W C> -t C . - ,,- .i . - -i -sci --r -
R4.5 .2 2 1-
gR2 {-.n-.su!-
cil x <re 15 4 5 2
':R4~ ~ 4 er:.ii
fii- }:r&-5 - - 1-- - - -
5 2 2.5 -4 2-- .
5 R2 3.6 .5. 7: 0 ..
-, c._ 4 A f7.e s- 1- . ; r
c., E 4 --
4 4
}RI ~4 1 3 .. 0 C 3 9 'i
2-= 2 2 ! 2 4 ..
(a) (b)
cure_ Samnlies ~fNR2 after blw-u. a)F'exoreter,
(b,) Xicrcwave iieating.
r-iaure 2. Cross-section or PB sample after mricrcwave h'
Revised January 1985
12
(DY:)DISTRIBjUTON LIST
Dr. R.S. Mtiller Dr. L.V. Schmidt
Office of Naval Research Office of N'aval Technology
Code 432P Code 07CT
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(10 copies)
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Naval Sea Systems Command ATTN: CPIA (Mr. T.W. Christian)
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Hercules Aerospace Division Dr. R. McGuire
Hercules Incorporated Lawrence Livermore Laboratory
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P.O. Box 210 Code L-324
Cumberlana, MD 20502 Livermore, CA 94550
Mr. Otto K. Heinev P.A. Miller
AFATL-DLJG 736 Leavenworth Street, 16
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Atlantic Research Corp. Naval Research Lab.
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Revised January 198513
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Ser 432/84/211DY-IRevised January 1985 14
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University of AkronAkron, OH 44325
Herb Richter
Dr. D.A. Shockey Code 385
SRI International Naval Weapons Center333 Ravenswood Ave. China Lake, CA 93555
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G.A. ZimmermanG. Butcher Aeroject Tactical SystemsHercules, Inc. P.O. Box 13400
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Prof. Kenneth Kuo
W. Waesche Pennsylvania State University
Atlantic Research Corp. Dept. of Mechanical Engineering
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T.L. BoggsDr. R. Bernecker Naval Weapons Center
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