B AD-A150 455 I, I

R TECHNICAL REPORT BRL-TR-2630

A COMPREHENSIVE REVIEW OF BLACK POWDER

Ronald A. Sasse'

January 1985

DTICELECTE

3 Reproduced From S 2Best Available Copy B

US ARMY BALLISTIC RESEARCH LABORATORYABERDEEN PROVING GROUND, MARYLAND

.. 02 21 026

Destroy this report when it is no longer needed.Do not return it to the originator.

Additional copies of this report may be obtainedfrom the National Technical Information Service,U. S. Department of' Commerce, Springfield, Virginia22161.

The findings in this report are not to be construed as an official.Department of the Army position, unless so designated by otherauthorized documents.

The use of trade names or manufacturers' names in this reportdoes not constitute indorsement of any. coamexrciaL product.

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TECHNICAL REPORT BRL-TR-2630 _____________

4. TI~44wd~bdI&$ fPE9 y REPORT A PERIOD COVERED

A COMPREHENSIVE REVIEW OF BLACK POW~DER 5 EPRIOOG EOTNNE

7. AUTHOR~s) S. CONTRACT OR GRANT NUMBER(.)

2onald A. Sasse'

9. -PERFORING NORN tZATjON NAMIE AND ADDRESS I0. PROGRAM ELEMENT. PROJECT,. TASKU.S. Amyý Ballistic Res earch Laboratory AREA & WORK UNIT NUMBERSATTN: AVMXR-IBD IL161 102AN43Aberdeen Proving Ground, ND 21005 -5066

11. CONTROLLING OFFICE NAME AND ADDRESS 12. REPORT OATSUS Army Ballistic Research Laboratory Jnr'18ATTN: AI4YBR-OD-ST 12. NUMBER OF PAGESAberdeen Proving Ground, HD 21005-5066 40

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Approved for public release; distribution unlimited.

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IILSUPPLEMENTARY NOTES

1913 f&iEckwFdwAeT' m Jm9ueemow"Y old" tt mw~smp "d 'eId.f'll by Slek mubw)

Flame Spread Rat** Closed BombPyrotechnics , QuicknessPyialroetsBurn Rates Relative Quickness CharcoalArmy A munition Plant

2L - AMTXA51 MuwRwme em main w IsiU- N subseek en h1..J M0R iTjnt a ttempt has been made to scrutinize black powder and thecharcoal it contains as fully'S asPossible,utilizing modern testing techniquesand various analytical chemical procedures. Although the tests performed arewell established, their application to define a porous propellant representsa new point of view for investigating structure. from 86.N.1. microphoto-graphs and'compactioa studiee,it is*'suggested that the pressipig Action usedto miake black powder results in Plastic flow that producies a conglomerate

D JASW 143 m ee'evssesmUNCLASSIFIED5EOUfrTV CLASSIICATION OP ThIS PAGE (VNin Do& S Ma~m

UNCLASSIFIED -

SWCUM"y CLASSIFICATION OF THIS PAG6(ftM Da" A"O

0. Abstract (Cont'd):

d cohesive mass containing a ltrix of inter-connecting passageways. Theeegree of openness of black powder grains and, in particutlar, internal surfacerea, pore volume, internal free volume, &and density were all found to belated to burn rate. Thermodynamic calculations were cited that relate

omputed theoretical values to experimentally determined quantities. Closednab combustion was compared to strand burn-rate*, and it wa suggested thatlosed bomb data embrace more than one combustion mode and as such do notiirectly, relate to bulk values. From this interrogation; chemical andphsical properties wrte related to combustion phenmena. As wortk progressed

t became evident that material produced by the Indiana Army Ammunition Plant,ill be, or has becom, the soot successfully characterised black powder *

roduced in the United States.'*

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1.

UNCLASIVZE

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.TABLE OF CONTENTS

Paste

LIST OF ILLUSTRATIONS ...... ... 5 -

I *INTRODUCTION.... 00*eees ~ge 6SS0000000007

II. CRARACTERIZATION.OF BLACK POWDER... .e.,g°.....o. ,10

III. COMPACTION OF BLACK POWDER MEAL. e.o- * .*........ I . . .....

IV. ATMOSPHERIC STRAND BURR ..TES******.. ....*******......***e******o 7

V. HIGH PRESSURE STRAND BURN RATES...********.***go************.*

VI. CLOSED BOMB EVALUATION,.,....... ........ e.................... .20

VII QUICKNESS VALESo..o e00ooo..o......0 00...oooo .oo .24

VlIII FLANESPREAD T egg.egOO OooOOe.24

IX. STRUCTURAL STRENGTH OF BLACK P-WDER*,**..*****g************** *.*

X. COMBUSTION TEMPERATURE*..........* o.000.********.........** 27

XI. GENERAL CO-NE*NTS gg**.*..*****.****.*g********g**.****** ****

XII. ACKNOWLEDGMENTS.... ... 0.00.....

REFERNCES. 000 O O O • 0000 oOeO'ooog 0000"00 OO@000060000,000.3

DISTRIBUTION LIST. oo..ooooo.*o ooooooo ,oo.ooo*000oooooeo33

Accession For

NITiS' C71kiiDTIC , TV I

L TJustification

FES 2 1I% .0 ByDistributicn/-Availsbility CodesAva-l and/or

Diat Specil&

.oN" @I

LIST OF ILLUSTRATIONS

vigure- Page

1. Interior of Black Powder Grain Produced by Wheel Kill Process.... ... 13

2. Interior of Black Powder Grain Produced by Jet-Hill Process.s.. ..... 14

3. Effect of Pressure on Black Powder Meal.............................16

4. Strand Burn Rates at Atmospheric Pressure as a Function of Density..18

5. Strand Burn Rates at High Pressures........................ ....... 21

6. One Atmosphere Flimespread Rates for Various Classes ofBlack Powder .................... ,.........................25

7. Strength of Black Powder...........................................28

tL.

5-'p.

1.* INTRODUCTION

Black powder was made in production mills in Europe as early as 1340 inAugsburg, 1344 in Spandau and 1348 in Legnica. The process, traceable to the Z.early B.C. efforts of the Chinese, evolved as an "art form" havig historical -

rather than scientific origins. The development of the craft has beenreconstrujted by various authors ald excellent accounts hav;e been given by'Urbanski, Karthall, and Vieille. The subject has been reviewed by Fedoroffand Sheffield, who prov de numerous references, and a very recent work byGray, Marsh and McLaren reproduces detailed historical drawings of the earlygun powder facilities.

In essence, black powder is made by grinding potassium nitrate, sulfur,and charcoal into a fine powder. This meal is transformed into a cohesiveconglomerate mass by either forming a paste which is forced through anddivided by a screen, or it is directly pressed into a cake. Both forms aresubsequently broken into pieces of .a particular size. The small lumps orgrains of black powder are then coated with graphite to retard the absorptionof moisture and to prevent the grains from adhering. This process has beenstandardized t) some degree, in accordrnce with prevailing technology, but theoperator adds water, adjusts temperatu¶?e, selects grinding time, or changescompression pressur. based on personal experience, which is guided byindividual judgment of color, odor, or general perception of the condition ofblack powder as it undergoes its various transformations. Such judgments areexchanged from experienced operator to journeyman.

Although the productio., of black powder was as great as 10.6 millionpounds during World War I, the advent of smokeless powder diminisheddemand. This fact, together with the inherent dangers of production marked byoccasional explosioLs, has resulted in the closing of most manufacturingfacilities in North America. The only production plant supplying the militaryis the Belin Pouder Works in Noosic, PA, which was built in 1911-12.embracingthe technology of 1850. The method of manufacture is termed the "standardprocess" and incorporates a ball and wheel-mill to prepare the meal. The

T.Urbanaki,, 42.ksmAfrj1 -W"O 'nwtg o t~lava Vol. .5, Pergauro Pressa,MY, Op. ;i22-346, 2937..

2A. •,9,halZ,a&,b adjm, 2nd. M., Vol. 1, makisto•is Sn and Co.,Philadelplh, PAS 101?.

'1.o z asAudva0 # Ps pat,#•a Vol. 6, Chapter 2 by P.,Vieille, Gauthier-Vallare 9t rile, !mpVm 's-LUbraires, Pav,,pp. 256-591, 1893.

8B.7. Pedovoff and 0.9. Sheffield, mhvlao~ Q~rs fn oftL00 &!~loia t latedZemte, Vol.. 2, PATR'2700, Pioatinny Arsenal, Dover, NJ,. pp. B165-BI78, 1962.

59. Gr'ay, H. Mrarh, -and M. AtoLaren, _F- A92*&Pidl St Ridawn, Vol. 17?, PP. -3385,Deoeaber2' 982.

6A.P. Van gelder and H. Sgoatter, I~*w~ ftm~t~a nridua*~ nAaiaCotuobia Univ'ersity Press,,NI, 192?.

7

plant vas operated by E.I. DuPont de-Nemours &Co-., who sold the facility to p ~~VGOEX Inc. in April of 1973. Because black powder still play* an importantrole in fuses and ignition devices, the U.S. Army Corps of Engineers startedto construct a production plant in Charlestown. IN, in 1974. The installationwas completed in 1978 and it was operated by ICI America* Inc. One principal-departure from standard practice was 5ho inclusion of a jet--mill to grindmaterial as developed by [jell Lovoldwhich has been used in Norway tomanufacture black povder. Every effortwas made to modernize the newblackpowder manufacturing process and to make production as safe as possible.These concupts were translated into hardware that resulted in the firstarted "production cycle completed in early 1983. In the planning stage, various- -'.studies were conducted to: (1) elucidate the ball and wheel-mill processes, n2(2) investigate new techniques and equipment, and (3) compare the ballistic..properties of black powder originating from this agd other countries.. This.work was r~ported in palb by the Chromalloy Cory,, Battelle Meimorial .Institute, Olin Corp., and IQ America* Inc. Battelle publishedabstracts of 50 articles and 60 patents describing the wheel-mill process infine detail and gave particle size distribution as a function of grinding timand moisture content for both the jet and wheel-mill processes.- Theaccumlated knowledge was used as a foundation t or the design of the Indiana.Plant.

The performance of black powder, in contrast to, i1 t erparation. has beencharac rorzed in the classic papers of Noble and Abel l Recently,Williast sumrtized burning characteristics and discussed several. foreign

K. Lovosd, U.S. Patent No. M6t0546, e Prdocee- for the prossaeion of BlackPowder," 2 Mdy 1972.

8cuomalloy Corp., NA Studyj of moderniued Techniques for the ds nofacth e ofBZla:k Powder," Pop,-.lew Clwmial Div.iion, pnaZ Report 0o. DA-_23-?_-o01-_ORD-P-43, Chromwzoy Corp., &MardevilZe, IL, am•anuay 1960.

H9H.. Carlton, B.8. Boh pep, and H. Hack, "Battezz 11.a.roiat InstituteXnaZ Report on Advisory Service. on ConceptuaZ Design and DeveZopnmen of 5Newr and Iiprqioved Processes for' the MaknUfacftur of Blaok Povder, attllMeopwiaZ Institute, Columbus, OH, Oetober 1970..

I 0 .%% .o. I* 10JR. Plessinger and L.W. B'raniff, "PinaZ Report on Development of IpoePwocees for the MWnuacture of Black Pow~der," 11RS AIu-g1 0*, -Olin Cor'p.,Indiana Arsj Awmozition Plant, Charlestown, IN, 3; Deceube, 19fl.

"lindiana Anuuouition Plant, "Black Powder Mznztfatu.~gReUt, o. n ,:'..:=

2s. Indian Avw Anunition Plant, Charleetooi IN, 1975. '1 2 R.A. Noble and ?.A. Abel, Til. T- .D218 o. Sbc.. L0Umed. Seri" A. Vol. ,-

1865, pp. 49-155, 1871.T

"R.A. Noble and P.A. Abel, A•i. t, an.e* o.•M 229. London, Serie A, Vol. " -"171, pp. 203-279, 1880. 0.

AP.A. Wilzlia, "The Role of Black Poder. in lpopesZing • 0zrge, Pioatinn'"Arsenal Tech. Report No. 4770, PFcatinny Arsenal, &urn, NJ, mi. 197,.

8

' ;I.., %

. . . . . .. . . . . . • • - ."-7 -. -4- -7 , " ,.

references. Rose1 5 studied the effects of various charcoals on performanceand concluded that volatile untent was an j•portant parameter; he also wrotean excellent review article., Kirshenbaum concluded from differentialthermal analysis, DTA, that even when volatiles were removed from variouscharcoal samples this treatment did not alter the order of ignition; thus, itwas concluded that some property other than volatiles also affectedignition. He also reported that ignition was not a property of surface area,ash content, or sulfur content. Blackwood and Bowden Tsuggested sulfurreacts with volatiles as an initiation step, but Kirshenbaum showed all threecomponents, potassium nitrate/sulfur/charcoal, must be present to induce thelow temperature pre--ignitioygexotherm. Clearly, volatiles affect burning rate,and this is shown by Hintze who recommends 82% carbon while Blackwood andBowmen suggest 70%. Neither work relates these values to the standard form ofwater or ash-free basis, and it is not clear as to the exact state of thestarting material; therefore, these recommendations cannot be compareddirectly. However, both studies recommend a high volatile content. DuPonthas maintained astandard of 75% carbon since the 1930's and this practice hasbeen followed by GOEX.

In this discussion it is emphasized that the properties of charcoal areimportant, but the exact requirements to make a good ballistic'product areelusive. Present practice is that charcoal be made from hardwood, currentlymaple being selected in the United States, and that it be of low, 51 or less, •-aash content. No American specification exists citing volatile content but-.urrent practice uses material of 20-30%. The current specification does notcite the type of wood, particulars relating to pyrolysis, nor any requiredphysical property. One control on black powder is it must conform to thedensity range of 1.72 to 1.80 g/cm . The amounts of potassium nitrate/sulfur/chartoal are given, but compaction pressure and particle size are not. Suchgeneral criteria result in a large latitude of allowable variance in makingblack powder.

From 6he historical significance of black powder, it would appear that

the manufacturing technology has been developed; however, one general.observation is the same manufacturing procedure, using the s"we ingredients,

results -..n lots exhibiting Jifferent burning rates. This has been the

experience of GOEX and DuPont where fast ane slow lots have been blended to "iachieve a particular result. Although some of the factors that affect burnrate are known, the lot-to-lot variations have not been identified. It Was 215 J.R. Rose, "Investigation of Black Powder and Charcoal," HTR-433, Naval

ordnance Station, Indian Head,'MD, September 1975.1 60Rose, MBackc Powder - A modern Cmmwrntazry," Proc. of the loth Symvposium

on f&plosivee and Pyrotechnics, Franklin Research Institute, Phiadetphia,PA, pp. 14-16, 1979.

17A.D. Kirhenbawm, Thezm, himioa.- Acta Vol. 16, p. 1.3, 1977.J..

18J.D. BZackwood and F.P. Bowden, Proc. Rog,. Soc.. ondon. A213, p. 285, 19.2.

"19W. Hintse, AZoivjeoyff,', Vol. 2, p. 41, 1966.

9 .. •-,

I

for these reasons that the BkIlistic Research Laboratory (DIL) has initiatedseveral black powder studies to elucidate the sensitive parmeters thatcontrol combustion. From scanning electr" microscopy (S.R.Q., it wasinferred that structure was importantt ar. in developing this hypothesis, itsoon became clear that correlations e% st between physical properties andcombustion. This review will blend both past and current research, focusingon ingredients, physical structure, and combustion, in an attempt to replacesome of the mysticism associated with black powder and black powderproduction.

It. CHARACTERIZATION OF BLACK POWDER ,

A. Ingredients

No comment is directed to sulfur or potassium nitrate; these chemicalspropose no particular technological problem. However, charcoal, a naturallyderived substance which contains approximately 35% "tar-like constituents,varies from one source to another and from one-lot to another., Such variancehas been studied in ietail for maple charcoal," where ten samples frommaterial supplied by one producer and used by t!e Idiana Slack Powder Plantwere analyzed. Hydrogen, carbon, itrogen, sulfur, and oxygen were measuredand the elemental composition of ash was determined. Results are given inTable I on a weight-percent basis. Physical properties were determined andinclude true density, volatiles, heat content, surface area, and porevoluz2. The extreme ranges of ten aamples are summarized in Table I, whereasindividual values for each analysis are given in Reference 20. Freedmanused averages of this data, where the empirical formula for charcoal was takento be Ct 4 5 H7 1701 00 to compute thermody~mic properties; his results werethe data tase or closed bomb evaluations. The empirical formula used torepresent DuPont and GOEX charcoals was C8.604.901.00-

An interesting obscrvation is the low surface area of this charcoal, andthus, it is inferred that most of the pores must be plugged, f r a completelycarbonized material would have a sirface area of about 1000 N'/1g.

Another disturbing aspect of thia data is the range~of carbon andvolatile content where some values are at the extreme limits of what. isbelieved to make good black powder. The data, illustratas the problem ofmaking a reproducible product using an ingredient the composition of which

2R.A,. Sasse', "CA apateriaation of Mzp~e Charcoal Used to Ahke Back Por ,"ARBRL-MR-0332 Ballstic Research Laboratory, USA-A RAD4lf1, Abezdwe " ProvingGround, MD, November 1983.* ADA-lU.-S 13.

9E. Freedma~n, "The Themody~namics of Real and Unreal Stack Powrder,'" Pzoc.of the 20th JANNAF Combustion Meeting, CPIA Publicatiou• No. 388,, Vot. r. ppSii, October 198.93

2 2RA. Sasas', M. Holmes, D. Hansen, N. Aungat, 0. Dbo,, and H. Bo&wRma,

"EaZiation of zaok Powdaer Produced by As indiana Az, A•unition Plan,"ARBRL-TR-in press, Ballistic Research Laboratory, USA-ARRALDO. AberdeenProving Ground,. D, 1..4.

10- • I

-. I- -

TABLE 1. CHARACTERIZATION OF MAPLE CHARCOAL

carbon 72-- 81 SiS2 16----43 enthalpy 11400-130G0

hydrogen 2.9--3.5 CaO 28---"4 Btu/lb

nitrogen 0.30-0.48 A1 2 03 12---14 surface area 2.2-15.7

sulfur 0.01-0.02 K20 8.4-12.9 M2 /g

oxygen 12.6-15.4 Na2 0 1.0-1.8 pore volume 2---10

ash 2.5--10.4 Fe.O, 2.3-4.9 = 3 /g

volatiles 22- 30 M&O 1.9-3.7 true d nsity 1.444-1.56P2 05 1.2--2.1 g/ca

Valuesare in weight percent unless otherwise noted.

cannot be closely controlled. To address this problem, research has beendirected to i4nti.y pure organic compounds that could be substituted directlyfor charcoal. Polyphenols, diacids, and phthaleins gave promising results.Testing mist be conducted before such propellants can be properly consideredas viable black powder substitutes to include: card gap, drop veight, andfriction sensitivity.

B. External Structure of Grains of Black Powder

The size latitude of class one black powder is larg% and it is defined asmeteri4 which will pass through a number four sieve (4.75 m) and not anumber eight sieve (2.36 me). Even though lots of black powder met thiscriteria, some lots appear to be composed of different size grains fromothers, suggesting that a more quantitative meas•'re be undertaken. Sizedistributions were determined for DuPont 111-12, WX 75-44, and Indiana1983 -lack powders and resultb are giveu in Table 2. These materials are

-referred to later without using Li- identifiers. Each sample had a slightlydifferent distribution, and in all cases, the function was not pronounced.This broad distribution should be taken into account in combustion modelingstudies and will be addressed later.

Another characteristic of black powder is its graphite coat, and Uttleinformation exists to describe this envelope or its function. Onecharacteristic of- tbe coating is to keep the grains from adhering to one

*a)S. Mie and R.A. -Sdesee', "Organic Subet'itutee for 4zarecaZ -In OtaekPow~der 2WWp Pyr~otechnic Formulations, N Proco. of the 19th J.4NNAP CombustionMeeting, CMIA Publication No. 368,6 Vol. II, pp. J05, Oatobei 1982.

(b) S. Vies, R.A. Sao*#e', and H.S. Ho7.mes, 11rai Substitutee for charwoaZin 'Bl~ak Powoder' AT"ype Pyr~otechnic Formulations,, ARBR&-.TR-02580,ftlZistia Rosaraih Labor'atoryj, VSA-ARAIDCO, A ber)dee~n Proving Gr'ound,

MD, July 1984.

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11%,

KI-7 77 7

TABLE 2. MRAIN SIZE DISTRIBUTION

Largest Size 4.?5 4.00 3.35 2.80 2.36 2.36in an

GOEX 0.31 9.48 26.69 22.25 28.46 11.70

DuPont ý3.39 33.23 36.13 17.31 8.82 0.65

Indiana 2.24 22.20 29.80 25.58 18.02 1.53

another, and'a second role is to prevent absorption of vater. From high speedcinematography of a single burning grain, it appears that the coating aets asan inhibitor~and as such, it is a very important part of black powder. Toahoy the influence of this coat, &amples-of black powder were obtained justbefors graphite was added to the glaze barrel; these are called green grains.and later the corresponding graphited material was also selected. The flame-spread rates of these tvo samples differed by a factor of two shoving t~heretarding effect of the graphite coat. One attempt to examine this coatingwas undertaken in which but one DuPont grain vas examined using S.K.N.techniques. Microphotographs were taken of the flat side of the hemispherecreated by cleaving the grain in half, much like snapping a twig, such thatthe surfaces vere not marred by a tool. From the pictures, the graphite coatvas judged to be about five microns thick. Future work will attempt to -

correlate electric conductance of a black powder bed to graphite filmthickness.

C. Internal Structure of Black Powder

24S.E.N. microphotographs of class one black powder were abtained, by

first cleaving the Stair~ in half as described. Two mamples fromn the jet andwheel-mill are given in Figures 1 and 2 at two different magnifications.,Comparison of the figures shows the jet-mill produces a smaller and more,uniform distribu~tion of particles. Io addition, the charcoal Pores were, notfilled with either potassium nitrate or sulfur, aproperty that had beenascribed to. the pressing action of the whel-mill by the concept termed"incorporation*" From these ard other such photographs, it.. was noted that. the,degree of openness of the -grain increased as did Lits burning rate* Ar~evealing feature of the photographs was the lack of crystalline sharp edtms,and it became apparent that a dominant feature was plastic flow that createdvoids and porosity in the grain. This feature was quantified by determininginternal surface area and pore volume. Brupauer, Emett, and Teller, B*E.T.,

*gas absorption techniques were used to measure surface areavanid values of 0.5 Vto 1.0 14'/gwere obtained where the larger surface 'areas were proportional to

2 4 (a) R.A. Sass*', "fThe InfZuence of PhytaicaL Pro pezftic of Black ftuvier an5um~ing Rate," Seventh Trnt eanationaZ Pyrotechnics S~wnixar, Vol. 2, 12?Research Institute, Chicaggo, IL, p. 536, July~ 1950.

(b) R.A. Sass.', "The Influence of Physical Properties of Black Powder onBurning Pate," ARBRL-TR-02308, ftltiatio Research Tabovntoip, USAm.ARRAXCI',Aberdeen ProVing Ground'. MD, March 15,(AD. A100*7).

12

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the faster. burning material.* The same result was found with pore volume asdeterr~iued by mercury intrusion p~rosimetry, where values ranged between 0.01to 0 .04 c=3 /g for both whole and cleaved grains. Thus, the mercury penetratedthe entire grain without hindrance from either the graphite coat or internalstructure. -In addition, the merecury intrusion data showed that passagewayshad mean diameter@ of about 0.1 micron at the narrowest cross-section.

Another method of determining the degree of opienness of black powder isto determine internal free volume. This quantity can be calculated from thebulk and true densities where sample volumes are measured two different ways:bulk density is Aetermined from the volume taken equal to the amount ofmercury displaccd by the sample, and true density is given by the amount ofheliumn displaced. Since mercury does not enter the pore* as does helium,these differenccs can be related to void space. Indiana, DuPont and GOEX

* black powders '4had bulk densities. of 1.75 to 1.79, true densities of 1.94 to1.97, and internal fret volumes were 4.10 to 5.75Z. Also, the maximumtheoretical density for this black powder would be 1.97 using the average truedensity 'of 1.43 for charcoal (see Table 1) and the density values for sulfurand potassium nitrate. The calculated value is almost equal to the =sasured

*values of triu* dens ity.

All of these measurements support the conclusion that the compattion stepused in making black powder induces local plastic flow producing a fusedconglomerate and cohesive mess containing a matrix of interconnectingpassageways and that the degree of openness of a black powder grain isdirectly related to burning rate. These concepts immediately suggest the

* question addressed in the next section, "How do we quantify the compactionproceus and apply this knowledge to make reproducible laboratory sample* andreproducible production lots?"

11I. COMPACTION OF BLACK POWDRR -A

Black powder meal is pressed into a cake using various pressures anddifferent moisture contents to rheea particular grain density. Thisprocess was examuined in detail by pressing meal slowly in a 'material testinginstrument, an I tron, and recording both the pressure and density of theample., The seaml displacement rate of 0.254 i/min was selected and a total

'load of 3,000 g/ wes applied slowly to samples of different moisture- .. content. Results are given in Figure 3r.vbere the early portion of 'the curve

represents Imoveme t of material into a close packed geometry and the linearportion reflects lastic flow. Had the experiment been extended to higher

25(a) R.A a. &W"" Stal &irgM'tes to *to Mo~dred Atawephez'.e"- fight*

(b) R.A. &we*', Strapd aa"R,ftPtee to OWMo wdred Atweophern.,* P'oe. ofthe U;t; JAINNA Cohta NeetipV, CPIA Nubtoation No. j66k Vot. r, p. is.,GOctober' 1952.

(a) L.A. &ous*'. "Srp &ALn Rates to awMo Adred Atavephe'..AROAL-?R-O2ESO, hLUtitio RossaroF, Labomvt ory* USA-ARRAXOW, Aberdeeny2 , n# GQp4,P4 A~s At 1993.- (A-A120-087).

15

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0.10 20 30' 40 50 60COMPRESSION(%

*Figire 39. Effect of pressure on Black Powder Real:0.0; *. 1%; +,22; 0, 32; aod* 42 Waetr

* 16

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pressures, the curve would approach a Vertical asymptote near values of 65%compaction. A direct relationship is shown between the logarithm of appliedglobal pressure to density; this functionality was suspected to be 2 he resultof compressing bounded spheres. This idea is 3upported by Knudsen who showethat porosity is a logarithmic function of the contact area between spheres.To evaluate these concepts and assess the effect of particle size, a

collection of two different diameter copper spheres, 50 and 125 microns, wereindividually compressed. The resulting curves were logarithmic and could besuperimposed one upon the other. Apparently, particle size does not influencegrain density at particular compaction pressures and particular watercontents. Also, these experiments indicate the logarithmic relationship isthe result of plastic flow among a collection of spheres. This samerelationship was even shown for the much larger class one grains where suchresults can be applied to the fabrication of fuse and time delay elements.

The application of physical testing to evaluate the compaction processhas been successful, and the results can be applied to fabrication technology,dwell-time studies, and to the preparation of laboratory samples. Sinceplastic fliw was found to be dominant, an equivalent' process was adopted wheresamples were pressed in a constant volume die using a spacer to control pistontravel; this avoided the eifficulty of simultaneously controlling bothpressure and water content. The technique offered the ,advantage offabricating a series of samples having predictable densities by placing knownweights of meal into a perallelepiped die forming "sticks" 4x5x20 me. Due toa slight degree of elasticity, bulk densities were calculated from the finalmeasured dimensions of the extruded samples. These samples were inhibitedwith a coat of cyanoacrylate-based glue for strand-burn rate studies.

The preceding sections presented the chemical and physical properties ofblac! powder; subsequent data and discussion will pertain to combustion.

IV. ATMOSPUERIC STRAND BURN RATES

Inhibited black powder sticks of different densities were made from mapleand oak charcoal meals that were ground in the Indiana pilot plant jet-mill.ThMy were burned in air, at atmospheric pritsure and photographed bycinematography at 2000 frames per second. The position history of the'burning interface was plotted's. a function of time and the least square slopewas used to calculate burning rate. The deviation of the slope was- takes asthe precision of one measurement and is given as an error bar on the datapoints drawn in Figure 4, Later, it was found that some deviations amongthese measurements was traceable to a poor inhibitor coat, indicated in themovies by a growing crown forming at the burning interface.. These instancescould be identified and discarded. From the remaining zubset, burn-rates ofabout one centimeter per second were obtained, and they ate shown to be alinear function of density. Black powder containing maple charcoal burnedabout 202 faster than oak. One additional experiment was performed to comparethe burning rates of two sticks of black powder that were made to equaldensities where one was compressed damp and the other was pressed dry at a

286 pp Mudsei 1 J, AR, Cez'amo &Vc.. Vol. ERft Io. 5 e p.371, hAgut 1959.

17

1.1r

1.0

0 .71- •ILI

ow I ,I

6 .6

0.51-- 1.3 1.4 1.3 1.6 1.7 1.8 1.9

DENSITY (g/cm 3)

FiSure 4. Strand surn Rates at Atmospheric fressure as a Functton ofDensity. Lower Curve Oak and Upper Curve Maple BIack Powders.

18 ,

• ' Ib

higher pressure. Both vere dried acd the two burning rates were found equal,and, in effect, the samples did not reflect their different respectivepreparation histories. J-.'

In a further attempt to evaluate class one black powder, Indianagraphited class, gra-ins were ground, sieved, pressed into sticks, and strand-burn rates measured. A similar sample was mode using Indiana green grains, andthe two burn rates were similar, 0.89 and 0.91 cu/s. It was concluded thatthe small amount of graphite in one sample did not effect the result. GOEXand DuPont samples had equal but slightly higher values of 1.00 cu/s. Inthese measurements, original grain size or distributi )n of sizes is negated asis any effect related to the graphite coat or original density of thegrains. Under these circumstances, burn rate is only proportional to chemicalcomposition, original fine degree of grinding, and density of the stick. :2Thus, these measurements reflect an inherent burning quality. Advantages ofthe technique are that in photographing burning, one can. be certain of themode of combustion and insure that the inhibiting coat is adequate. For thesereasons, the test appears to have merit and parallels the older DuPont andGOEX methods in which black powder is placed in a lead tube, and its diameteris reduced by drawing the sample through an extrusion bench.

Even t~hough few samples were evaluated, this intrinsic combustionmeasurement ranks Indiana black powder olver than the others. This issomewhat surprising, for the Indiata meal was ground to a smaller particle ,size, ca 15 microns, than the other meals; hence its burning rate, nov

.dependent on, just particle size, chemical composition and density, should bethe fastest. Such a result mast be attributed to either a non-optinmuivolatile content in the charcoal or some other unidentified variable.

To et-tain surface burn rates, 2 5 non-inhibited sticks were evaluated. Thesurface burned faster than the bulk material and thus a pyramid formed, thesides of which became steeper as combustion progressed. This resulted in fourdistinct gas plumes jutting outward and normal to the burning surface. Thesurface that had been adjacent to the movable piston burned three timesfaster, and the surface formed by the bottom of the die burned six timesfaster than the bulk burn rate.

One 16m motion picture frame was enlarged and particle sizes were 25cmeasured by Nathan Klein of the BRL gsing a Quantimat 720 ImageAnalysor. 2 5 cThe. larger particles were found to be near perfect spheres having a sizedistribution that peaked at diameters of 225 to 300 microns; they are believedto be frozen droplets of -unreacted material. A second distribution of smallporous material of irregular shape and sharp edges was collected and examinedby S.3.N. techniques. In this case diameters were between 0.4 to iL0 micron,and these bodies are thought to be the result of condensation of reactionproducts.

19

v.t

V. HIGH PESSURE STRAND BURN RATES

Inhibited maple stick samples were bVned while being photograrhed in &windowed chamber of the d~gign of Kubota. Pairs of samples, of differentdensities were evaluated at several different nitrogen pressures to 100atmospheres. To minimize the obscuration effects of smoke, the optical pathinside the chamber was reduced to 8 m- by inserting two plastic spacers.Results are given, in Figure 5. The data contain some scatter and are comparedto the ay rage response curve derived from several jeferences summarized by 2 9Williams using t% values of Belyaev and Naznev, Glaskova and Tereshkinand Belyaev et al. The excellent agreement between the Russian and presentstudy is surprising considering the different charcoals and differentpreparation. procedures employed. The burn rate, or ao preciseLy, theregression rate fnction, r (cm/s), was determined for pressures, P (at=m),between 3 to 100 atmospheres. The relationship:

r i 1.72 P(O.164 1 0.017) (1)

was obtained. The burn rate curve exhibited a sharp decrease in slope atpressures of a few atmospheres. The films were examinet to see if a differentcombustion mode, such as deconsolidation, was associated with this transitionand no change was recorded. The only physical difference noted was that atlow pressures th. cell had a carbonaceous deposit on the' wall, whereas athigh pressures, large frozen droplets were seen; however, film, in either caselooked much alike. In otE experiments, where phenolphthalein wassubstituted for charcoal,' its burn-rate curve also bad a decrease in slopeand was similar to those reported here. Since the selting point of theorganic, 258 C, and that of potassium nitrate, 334 C, ae both below theignition temperature, ca 450 C, the substituted system could be a liquid-liquid reaction in contrast to the liquid-solid black powder system. Thiscould imply that the "break" in the burn-rate curve could be -due to nitratechemistry as opposed to the nuances ,of charcoal.

V1o CLOSED BOMB EVALUATION

Closed-bomb techniques and subsequent data reduction have been a concern tof several laboratories. To insure equivalent data proessing, laboratoriesexchanged propellant samples and results are given in a JNAXt Combustion.

27N. Kubota, T.J. CAleamfllev, L.M. . Cavenv. and M., Suiwnrfietd, fThe Msoehaniauiof supev-Riate Burning, of Catatyswl Dou~ble Bass Propellants.," Report No. ANS2027 * Dept. of Aerospace and moahanicat Sotenoss, Ppineston University,,'Prinoeton, AV, Naoi'd 1973.

2*A.?. Bel yaev and s.F. At~z v Vependenoe Iof Burning Rate of Swk*ceFormingPowder on Pressure, DAoL. Akad. Nauk SSSR, Vol. 1, p. M8?, 1960.

29 A.P. Glaxkova and Z.A. Treeshkin, "Relation Betwen Ppreure adu• au!ning

Vatoeity of 9xploeivz'ee." Zhsur. Fix. Xhim.1, Vol. 3.5,, pp'. 1682-1628, 1951. 4

OAr. Belyaev, A.Z. Kovotkov, A.K. Parfarfenov, and A.A. .kumou, "Theairning Rate of Sowlu A'ploetue Subetancess and Mixzturee at Very~ NighPressures," ?),ur Pu.Xhin., Vol 370 P. 150, Iv63.

20,

r".."

-. 7-.::

10

*L

,o op

I f

1 10 100 1000

PRESSURE (atm)

C.~

Figure 5. Strand Burn Rates at High Pressures; Dashed Line,References 14, 28, 29, and 30.

21 '

S31••Report. Although black powder was not considered, this document does.reflect closed-bomb evaluation methods and the description is a vtablereference tool. The calculated maximum pressure, flame temperature and otherquantities have been predicted by various thermodynamic computer codes thatrequire the chemical composition of the propellant. In the case of blackpowder, the composition of charcoal,as well i the other including ash,ingredients,must be specified. Eli Freedman performed such calculatioas forthe Indiana, GOEX, and DuPont samples. For the first time, charcoal wasrepresented by its elemental composition as opposed to only carbon as had been .t!'e custom. For the GOEX and, DuPont timples, Freedman used the elemental L.composition of charcoal given by Rose as "Roseville I" made by the RosevilleCharcoal Co. of Zanesville, OH, and obtained 'the potassiumnitrate/sulfur/charcoal concentrations from the data sheets supplied by % .Indiana. In a like manner, the chemical composition of the charcoal used 'atIndian (also made by Roseville) was taken by averaging the values reported bySasse' and summarized in Table I of this chapter. Again, potassiumnitrate/sulfur/ charcoal concentrations were2 obtained frof Indiana datashiets. The computed results were comparedZ to closedmbenb data where an 88

ca bomb, at a loading density of 0.14 g/cm;, was employed to produce peak,'pressures of 472 atmospheres. For one example, a flame temperature of 1765 Cand an impetus of 95583 (FT-lb/lb) was calculated. To calculate burn-rateequations, thermodynamic quantities were used,and the grains were consideredto be perfect spheres with a diameter chosen at the midpoint of the size rangeof the original screening,and a value of 0.14 inch, or 0.55 mm, was assumed.Closed bomb burning-rate equations were derived for four samples each of GOEX,DuPont, and Indiana black powders and they are given in Table 3. Equationswere fitted to the data between 136 and 408 atm.

One major concern of this and other closed-bomb black powder experiments ;'is the large value of the burning-rate exponent, 0.5 to 0.6, iii the burning-rate equation,as contrasted to the supposedly equivalent value' derived fromstrand burn-rate experiments where a smaller value of 0.164, Eq. 1, has beenreported. Such differences have been pre ioualy observed in other work.wndthey have been discussed, first by Rose and later by hite and Sasse.'1The diflf rent values in exponents has to reflect a different burning, mode in,the clos d bomb than is normally assumed, and hence, these burning ratesshould considered as pseudo-burning rates.

In e strand-burning experiments, room temperature gas pre-pressurized .the chamer and sample as contrasted to the closed bmb where hot combustion

31JANSF, Combuatio,, &ooemitt.., &m 1zte Measw...snt. a .wi ta ReductionProosd• Panel, "Round Robin Results of the CZosed Boub a t l ' 'an.Str-n

Burne,w CPIA. Publication No. M61, edited by A. Mf'ass, Mly 1989..3 2 (a) X. W/hit. and Rf.A. Sass*, "Combuetio" and FTZa~r Chazaoteristio. of Blackc

'Dowde., Pvoo. of the 18th JAAVNAF' Combustioni Me~ting, CPIA Publication No.

M . L,'• .'*:

347, Vol. II, p. 253, October 1981.

(b) X. White and R.A. Sase., "R#1,iationship of Conbu ,tion and PFytsioaLPropert.i of Blaok Powder,' ARBRL-MR-0.3219, Baltistic Researoh ,abova.o .."USA-"LW, Abeldwi Ppopig around AV, Novae 1982. (AD A123,264)

22

.. 1

TABLE 3. COFWFICIENTS FOR THE BURN-RATE EQUATION AND QUICKNESS VALUES.

b n Peak AverageSampXe Pressure QuicknessType ---- at. atm/s

MOEX• , 20.3 0.671 454 44.480.551 0.531 455 44.81 ..0.287 0.660 454 44.650.326 0.641 453 45.63

DuPont 0.561 0.493 469 38.410.518 0.485 466 34.030.457 0.503 462 32.050.251 0.547- 465 32.19

Indiana 0.179 0.661 459 29.140.309 0.553 .459 28.340.328 0.542 463 28.270.345 0.533 467 29.09

Burning rate, r(cm/s) is given by the 'function r-bPn where pressure, P, is in.atmospheres.

gases had this effect. It was thought that this different temperature andpressure history might influence combustion to a degree that would changeburning-rate exponents. Unpublished data of a single inhibited black powdercylinder, burned in the same closed bomb at pressures to 110 atm, had anexponent of 0.192, a value near 0.164 derived by cinematography from strand-burner experiments. From this relationship, it was concluded that thedifference in gSa temperature and pressure history does not induce a different ,combustion mode, and furthermore, deconsolidation or porous burning does nottake place. Similar confirmation was obtained in high pressure steady-staterocket motor experiments. Tnerefire, the 11-rge burning-rate exponent must bean' artifact of burning a collection of grains of black powder.

To explain this discrepancy, one must invoke mechanisms whereby surface %area increases during combustion and two substantive suggestions have beenoffered. One is that grain break-up or fracture is the root cause for:increasing surface area,and a second hypothesis is all black powder grains donot ignite at the instant of ignition. Either explanation could account for ahigh value of the exponent ft tie burning-rate equation. Another approach tothis problem is to consider that the graphite con't acts as an inhibitor andcombustion progresses from a-sitgle point ignition source that results in-increasing' surface area during c'-ic burn. Nigh-speed movies of single burninggrains suggest this effect. If this idea is mechanistically correct, thengreen grains (where surface burn-rat'e are greater by a factor of 5 then bulkvalues) should burn with smaller burn rite-exponents than graphited material.Closad-bomb experiments exerting a maxinm, pressure of 100 atm followed thispattern and the approach seemed promising; however, in the present work, andat pressures to 500 atm, green ane graphited grains gave the same combustion '

curves. The contradiction of the two sets of experiments is unresolved and

.23 0.1

the concept of single-point ignition is not supported even though this processmay be operative. Work in this area should continue for this contradiction isthe behavior of black powder.

In dealing with combustion of black powder, it is recognized thatcombustion rates are proportional to grain size and the size distributionshould be known. Thebe functions were measured for all samples and they aregiven in Table 2. Each sample had a slightly different distribution and inall cases the function was not sharp. Under these conditions one worries thatthe numerous small or large grains dominate the calculation and invalidate theassumption of "average radius." Since an average and particular radius waschosen for data evaluation, it seemed worthwhile to perform a mathematicalsensitivity analysis using different radii. This was accomplished using oneset of COEX data and the various radii of the sieve sixes, four through eight,embracing the sub-sizes of class-one black powder. The burn-rate curves hadsimilar exponents but were displaced one from another where the pre-exponentchanged by a factor of 2.5. Clearly, the distribution function should befolded into the calculation, but the main point is grain size distributionrelates to the pre-exponent and not to the buraing-rate exponent.

VII. QUICKNESS 'VALUES

The derivative of the closed bomb pressure-time curve was formed as afunction of the percent of maximum pressure achieved. Each point o. the curveJs a quickness value relmted to a particular correspondiug pressure. Foursuch points at 25.0, 37.5, 50.0, and 62.5Z of maximum pressure are customarilyselected to represent quickness and the average of these f•yr points istermed, by the propellant community, as average quickness. Such values aregiven in Table 3. Since these values are extracted from the c*osed bomb data,comments concerning burning mode in that device also apply to the-interpretation of quickness. In presentation of relative quickness values,test samples have been normalized to a reference standard run under exactlythe same conditions. The quotient between these values renders a relativegasification rate that to some degree integrates and compensates for differentburning modes, whatever they may be.

VIII. FLAKESPREAD RATES

Open air flamespread rates were obtained by measuring the time requiredto burn 16 g of class one black powder strung in a straight line 46 on long.A recording TV camera was geed to measure burn times. Examples are given byWhita, Holmes, and Kelso. The technioue-was improved by placing the grainson a plastic strip and using a mirror to photograph the underside of -thesilhouetted bu-ning string. This placed the black powdie between the cameraand the light. Flamespread rates of 63 ca/s ware neasured for DuPont, 74 cm/s,for GOEX and 63 cm/s for Indiana samples.

3•3., White, H.9. Hotme, and J.R. Xelso, ".ffect of Elk Po,•e. Combustion onHigh and Low Pr'essure igniter System.", Proc. of thme 18th Comb'ustionMeeting, CPZA Pubtioation N o. 3058, Vol. r, p., 4?, Septsember 1979.

24

1.5

09

0O.5 0. E- E E EE E EO in on In in

UV.4 V~it.H0 K

14 63 5 808BLC PODE SIZ BY CLS

0 0 0 0

N ~~~ ftq* on C

Figure 6. Oue Atmosphere Fime00pread Rates for lariousClasses, of Black Powder

'25

I?

Kev~in White32 extended these measurements to different classes of blackpowder and his results are shown in Figure 6. The very small grains had theslowest rates, for the burning grains emitted gas jets that blew light materialout of the straight propellant line and retarded flme propagation. The fastflamespread rate noted wab suggested to be the result of individual, grainsoscillating, causing the gas-V-..ticle jets to interact to a greater degree withadjacent surfaces. This concept was confirmed by gluing grains to a plastic '

sheet and then the flamespread, rate dropped to 20 cm/s from the free value of60 cm/s. When two sheets were placed in opposition, such that the gas-particle jets from one sheet sprayed on the other, then the flamespread rateincreased to its free value of 60 cm/s.

A great deal of effort has been devoted to develop a flamespread "tester"where most of the urk was performed by the Princeton Combustion ResearchLaboratories of NJ and White, et al. "'ontributed to this abject. Theseresults have been extended and summarized in a recent report. The overallobjective was to devise a relatively quick and functional test that could be .exercised during the production of black powder such that results would beavailable before material was packaged. It was envisioned that this testwould enable one to determine, in a timely manner, if a production cycleproduced a ballistically acceptable product or would indicate if process orraw material changes were required. Most experiments measured black powdersflamespread rate in a 19 ca tube with open slits and used soft igniters thatfirst vented into a small plenum expansion chamber. This is the functional'design of the Princeton Research Laboratory "Flamesptead Tester." Otherapplications have used this tube as received with the holes plugged with a"wax-like" substance, and measurements have been made with an electric matchor a brisant configuration using the M61 primer as found in the M2852 iguitionsystem of the 105 -m Howitzer. Since these experiments are very specific inLature, and strongly depend on the particular geometry and venting conditiontemployed, they will not be described here but ace in Reierence 22. Ingeneral, it was found that soft ignition using vented tubes resulted inpressure pulses of 34 atm, uniform combustioa, and flamespread rates of 2000-3000 cm/s whereas plugged tubes and soft ignition gave pressures to ")0 atmand rates to 10000 cm/s. In this latter case, non-uniform combustion wasindicated by the rear pressure gnuge, wh'c!'. at times, recorded pressure ..-pulses twice as large as normally recorded. Harsh ignition and plugged tubesresulted in fracturing the grains that led in some cases to_ plugged flow andslow propagation rates, 5000' cm/s, non-uniform combustion, and thermalexcursions. It would appear that using soft igniters and either open air otsemi-confined conditions result in reliable flame propagation rates.

IX. STRUCTURAL STRENCTH OF BLACK PO•.,

In semi-confined plugged tubes and closed-bomb experiments, occurrence of Cgrain fracture could, in itself, explain both extraordinary pressure pulsesand enhanced gas generation rates. Such fracturing will be dependent on the

3NW.A. Mossima, L.S. Ingram, M. &iiPwmrfield, and J.C. Allen, "F1.amespreadPropagation Rates of Vari(ous Btaek pcn~ere Using the RpeR.J1cinapvaTustor' "' Seventh International Pyr~otechnics Seminar, Vol. , IT. fesearahInstit•te, Chioago, IJ, p. 388, July 1980.

26

(.i

.ii

_.-7

intrinsic strength of the propellant. To assess this parameter, several 1.0cm long black powder cylinders having diameters of 1.3 ca were prepared eachof a different density. They were slowly compressed on a Materials TestingMachine until they shattered and that pressure is given as a .function of"density in Figure 7. Additionally, dynamic effects were obtained with a

Ssimilar series of samples using a modified Drop Weight Testor where sampleswere mounted on top of a piezo-electric force gauge. A 2.0 kg weight wasdropped on the cylinders from a 20 cm height and force was recorded as a"function of time; displacement was also measured byan Optron ilectrc-Optical

r. Displacement Follower using the technique described by Lieb. 3 The dynamiccrushing strengths are also given in Figure 7, and they are slightly smaller."than quasi steady state values where both functions are steep functions ofdensity. By extrapolating the data, it is inferred that black powder mast be

*.• at least as dense as 1.3 to form a cohesive mass. From helium densitymeasurements Of carbon, density of 1.45, and density values for sulfur andpotassium nitrate black powder can be no more dense than 1.97.' The militaryspecification requires the higher' values, and it is suspected that the"specification was originally cited to achieve a minimm strength for. black

* powder. From these dynamic experiments, stress-strain curves were derivedthat were nearly linearý indicating that black powder crushes by a brittlefracture mode, mach like glass.

s. COMBUSTION TDEPERATUKE

Although combustion rates and mode have been discussed, no coment hasbeen directed to the heat released by various exothermic reactions. Thetemperature of the igs stream We* measured by the sodium line reversaltechnique by Harris, and he reported a value of 1549 1 25 C for burning 37black powder in air at one atmosphere. From arc image experiments, lmnchitim3

found - ignition tempeogture of 469 & 50 C for a DuPont. sample which agreeswell with [irshenbaum's" value of 420 C obtained by differential thermalanalysis. Another, but simpler, experiment was attempted, where a thin0.127 - diameter chromel-alumel thermocouple was placed in the center of meal

"- just before being pressed into a stick. Even within the general limitations-. of thermocouple measurements, the burning of this composite should give som

lower bound estimate for heat propagation within the stick. During combustionthe indicated temperature rose to 480 C in 22 me before the bead entered the,gas stream and melted. Assuming the bead was twice the thickness of the wire,

,'" mid a burning rate of 1.0 m/s, heat penetrated about 220 microns into the

- ~ ~ 34a... Lieb'.gd Jr.Jr. RwohoO, wStanoisdfr~atio, of a.-Drop Uei git MechaiaroaLPr~operties 2..tor for GOu Propstl~a'tef' ARML-TR-25 15, Batlistio ReesoxoJLabor'atoryi, USA -ARRAXN, Aberdeen PmvoiPng Crouaid, V, Aty 1983s,(AD A132-086).

* #e* 3 LI. aazies J*A. Laamo',, Re Field, ed D. Iftstd, e7. of B211istiasa Vote 1,p 553, 19??.

Fc. 'Laitoiits and if. HNaye., "Ignition Pr'operti~es of Btaok Padier, Phaee .1,w*Proo. of tile 15th JANNE Cambustion Noeting, CPIA Pubtioatime No. 308a Vol.*3 Sp. 1809, December 1979.

35"4D. Kirshlenba~we,.,- atf PA11takla, Vol . 1, p.; l71,Jklif 1975.

27-

I

I

I

1400

1200 +

* .1000++

sw

m600-* +

~400-

200

1.40 .40 1.60 1.70 1.8.D.-W (9/cm3 )

Figure 7. Strength of Black Powder; *, Static pbeoureuenti,

.q

and 0, Dynamic easuremmets

28-

grain. Clearly, the thermocouple was too thick, and the measurement was notcorrected for heat losses, b'ut one can conclude that the heated black powdershell is very thin.

XI3. GENEAL CXOENTS

The several functional and physical tests, each of which relates to aparticular combustion mode, have been presented. The relationships andproperties discussed in this chapter each characterize black powder; however,complete characterization will only become finalized when this work is coupledto Sun performance. This latter program is now in progress and is sponsoredby an Engineering Study (ESP IA-3-a428) funded by the office of WSMC-LE(R).Firings of DuPont, GOEX, and Indiana black powders will be evaluated inrelation to actual ballistic performance. of igniting a propellantand onlyfrom these results can we determine the adequaey or inadequacy, of the blackpowder. It is hoped that from the merging of laboratory and performance dataone or more of the laboratory tests can be identified to predict this quality.

MI. ACK•OMLDQIE3TS

To my friends Kevin White and Eli Freedman, I extend my gratitude fortheir personal and scientific support. I also dedicate this report to mydaughter Chris.

2

S

* \\

* 2,? \ 1

REFERENCES

1. T. Urbanski, Chemistri and Technology of Explosives. Vol. 3, PergamonPress, NY, pp. 322-346, 1967.

2. A. Marshall, Eplosives, 2nd. Ed., Vol. l1' Blakiston's Son and Co.,Philadelpha, PA, 1917.

3. Memorial Des Poudres It Salpetres, Vol. 6, Chapter 2 by F. Vieille,Cauthier-Vallars It File, Imprineurs-Libraires, Paris,, pp. 256-391, 1893.

4. B.T. Fedoroff and 0.1. Sheffield, Encyclopedia of Nkplosives and RelatedIteul Vol. 2, PATR 2700, Picatinny Arsenal, Dover, N, pp. 3165-BI78,1962.

5. E. Gray, H. Harsh, and M. McLaren. J. Material Scienceb Vol. 17, p. 3385,December 1982.

6. A.P. Vangelder and H. Schatter, Ristory of the Explosive Irdustry inAmerica Columbia University Press, NY, 1927.

7. K. Lovold, U.S. Patent No. 3660546, "Process for the Preparation of, BlackPowder," 2 May 1972.

S. Chromalloy Corp.,"A Study of Nodernised Techniquee for the Manufacture ofBlack Povder," Propellex Chemical Division, Final Report No. DAI-23-072-501-ORD-P-43, Chromalloy Corp., Edvardsville, IL, January 1960.

9. R.E. Carlton, B.S. lohrer, and R. lack,' "Battelle esmorial InstituteFinal Report ox Advisory Services on Conceptual Design ad Development ofRNe and Improved Processes for the Manufacture of Black Powder," •attelleMemorial Institute. Columbus, O, October 1970.

10. J.1. Plessinger and L.V. Braniff, "Final Report on Development ofImproved Process for the Manufacture of Black Powder," RCS hNURE-109,Olin Corp., Indiana Ar•y Ammunition Plant, Charlestown, IN, 31 December1971.

II. Indiana Ammunition Plant,. "Black Powder Manufacturing Facility," Vols. Iand 2, Indiana Army Amnition Plant, Charlestum, I, 1975.

12. R.A. Noble and F.A. Abel, Pbil. 'Trans. Soy. Soc., London, Series A,Vol. 165, pp. 49-155, 1875.

13. R.A. Noble and F'oA. Abel, Phil. Trans. Roy. Smc.. Londoun Series A,Vol. 171, pp. 203-279, 1860.

14. F.A. Williams, "MThe Role of Black Powder in Propelling Charges,*Picatinny Arsenal Tech. Report No. 4770, Pictimuny Arsenal, Dover, NJ,May' 1975.

15. J.9, Rose, "Investigation of Black Powder sad Charcoal,* ZRTU-433. NavalOrdnance Station, Indian Read, ND, September 1975.

30

Jt

REFERENCES (continued)

16. J.E. Rose, "Black Powder - A Modern Comentary," Proc. of the 10thSymposium on Explosives anl Pyrotechnics, Franklin Research Institute,Philadelphia, PA, pp,. 14-16, 1979.

17. A.D. Kirshenbaum, Thermochinica. Acta, Vol. 18, p. 113, 1977.

18. J.D. Blackvood ano V.P. Bowden, Proc. Roy. Soc., London A213, p. 285,1952.

19. W. Hintze, Explosivatoffe. Vol. 2, p. 41, 1968.

20. R.A. Sasse', "Characterization of Maple Charcoal Used to Make BlackPowder," ARBRL-MR-0332 Ballistic Research Laboratory, USA-ARRADCOK,Aberdeen Proving Ground, MD, November 1983. (AD A136 513).

21. 2. Freedman, "The Thermodynamics of REal and Unreal Black Powder," Proc.of the 20th JANKAI Combustica Meeting, CPIA Publication No. 388, Vol. 1,pp. 511, October 1983.

22. R.A. Sasts', H. Holmes, D. Hansen, V. Aungst, 0. Doali, and L Bowman,"Evaluation of Black Powder Produced by the Indiana Army AmunitionPldnt," ARBRL-TX-in press, Ballistic Research Laboratory, USA-ARADCON,Aberdeen Proving Ground, ND, 1984.

23. (a) S. Wise and L.A. Sass*', "Organic Substitutes for Charcoal in BlackPowder Type Pyrotechnic Formulations," Proc, of the 19th JANUA?Combustion Meeting, CPIA Publication No. 366, Vol. I1, pp. 305, October1982.

(b) S. Vise, LA. 3-az', ad H.. Ulmes, "Organic Substitutes forCharcoal in 'Black Powder' Type Pyrotechnic Formulations," AnRBL-T&-02569, Ballistic Research Laboratory, USA-ARRADCON, Aberdeen ProvingGround, ND, July 1984.

24. (a) L.A. Sasso', "The Influence of Physical Properties of Black Powder onBurning late," Seventh International Pyrotechnics Seminar, Vol. 2, ITTResearch Institute,* Cicago, IL, p. 536, July 1980.

(b) R.A. Sa"e', "The Influence of Physical Properties of' Black Powder onBurning Rate*' AnRL-TR-02308, Ballistic Research Laboratory,. UA-ARRADCOM, Aberdeen Proving Ground, MD, March 1981, (AD A100273).

25. (a) L.A. Sasse', "Strand Burn Rates to On. Hundred Atmospheres," EighthInternational Pyrotechnics Seminar, 1TT Research Institute, Chicago,IL,p. 588, July 19"2.

(b) I.A. Sasse', "Strand Burn tates to-One Hundred Atmospheres," Proc. ofthe 19th JANNAF Combustion Meating, CPIA Publication No. 366, Vol. 1, p.13, October 1982.

Wc) l.A. Sasse', "Strand Burn Rates to One Hundred Atmospheres," ARBRL-TR-02490, Ballistic Research Laboratory, USA-ARRADCON, Aberdeen ProvingGround, MD, May 1983, (AD A129 087).

31

REFERENCES (continued)

26. F.P. Knudsen, J.'Am. Ceramic Soc.0 Vol. 42, No. 8, p. 376, August 1959.

27. N. Kubota, T.J. Ohli :iller, L.H. Caveny, and N. Sumerfield, "TheMechanism of Super-I te Burning of Catalyzed Double Base Propellants,"Report No. AMS 1087, Dept. of Aerospace and Mechanical Sciences,Princeton University, Princeton, NJ, March 1973.

28. A.F. Delyaev and S.F.. Maznev, "Dependence of Burning Rate of ooke-Forming Powder on Pressure," Dokl. Akad. Nauk SSSR Vol. 1, p. 887,'1960.

29. A.P. Glazkova and I.A. Tereshkin, "Relation Between Pressure and BurningVelocity of Explosives," Zhur. Fiz. Khim., Vol. 35, pp. 1622-1628, 1961.

30. A.F. Belyaev, A.I. Rorotkov, A.K. Parferfenov, and A.A. Sutiowv, "TheBurning Rate of Some Explosive Substances and Mixtures at Very HighPressures," Zhur. Fiz. Khim., Vol 37, p. 150, 1963.

31. JANNAF Combustion Subcommittee, Burn Rate Measurements and Data ReductionProcedures Panel, "Round Robin Results of the Closed Bomb and StrandBurner," CPIA Publication No. 361, edited by A. Juhass, July 1982.

32. (a) K. White and L.A. Soese, "Combustion and Fime raracteristics ofBlack Powder," Proc. 18th JANNAY Combustion Meeting, CPIA PublicationNo. 347, Vol. I1, p. 253, October 1981.

(b) K. White and R.A. Sasse, "Relationship of Combustion and PhysicalProperties of Black Powder," ARBRL-NR-03219, Bellistic Research ILaboratory, USA-ARRADCON, Aberdeen Proving Ground , MD. November 1982.(AD A122 264).

33. R. White, R.I. Holsies. and J.. Weoso, "Effect of Black PowderCombustion on High and Low Pressure Igniter Systems," Proc. 16th of theCombustion Meeting, CPIA Publication No. 308, Vol. I,p, 477, September1971.

34. N.A. Messina, L.S. Ingram, N. ummerfield, and J.C. Allen, "FlamespreadPropagation Rates of Various Black Powders Using the ?PCL-FlaiespreadTestor," Seventh International Pyrotechnics Seminar, Vol. 1, ITT ResearchInstitute, Chicago, IL, p. 388, July 1980.

35. 1.J. Lieb and J.J. Rocebio, "Standardzation of a Drop Weight MechanicalProperties Testor for Gun Propellants," ARBRL-TI-02516, BallLstic

SResearch Laboratory, 3A-AIRADCON, Aberdeen Proving 9cound, M, July1983,. (AD A132-966).

36. L.I Harris. J.A. Lannon, R. Wield,, and D. Busted, J. of lallisticsoVol. 1, p 353, 1977.

37. C. Lenchits and t. Hayes, "Ignition Properties of Black Powder, Phase I,"Proc. 16th of the JANNAF Combustion Meeting, CPIA Publication No. 308,Vol. 3, p. 160, December 1979.

38. A.D. Kirshenbaum, J. 'of Ballistics, Vol. 1, p. 171, July 1978.

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