UNCLASSIFIEDW0-r-

AB2 1 a 138

ARMED SERVICES TECHNICAL INFORMWflON AGENCYAlINTON HALL SIATIONARLINGTON 12, VIRGINIA

UNCLASSIFIED

NOTICE: When government or other drawings, speci-fications or other data are used for any purposeother than in connection with a definitely relatedgovernment procurement operation, the U. S.Government thereby incurs no responsibility, nor anyobligation whatsoever; and the fact that the Govern-ment may have formulated, furnished, or in any wayaupplied. the said drawings, specifications, or otherdata is not to be regarded by implication or other-wise es in any manner licensing the holder or anyother person or corporation, or conveying any rightsor permission to manufacture, use or sell anypatented invention that may in any way be relatedthereto.

NOLTR 6 1-153

A LOW GASSING IGNITER MIXTURE FORVARIOUS PYROTECHNIC DELAYCOMPOSITIONS

C/D

cc RUZASM) TO k.ryAS2f NAVAL ORDWAROK LAfOR.~njM

For Release to Military and (Govea-monn-Agencies Only.

0Approvi i fptAppral. by Butwps ,q, jrIz d.r0X ,,,6abuo~qu.t releaa*.

~ ~ I jI NOVEMBER 1961]NotUNITED STATES NAVAL ORDNANCE LABORATORY, WHITE OAK, MARYLAND

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NOLTR 61-153

A LOW GASSING IGNITER MIXTURE FORVARIOUS PYROTECHNIC DELAY COMPOSITIONS

Prepared by:

E. Eugene Kilmer

ApprovedChief, Exposon Dynamics Divison

ABSTRACT: Mixes of zirconium and lead monoxide have beeninvestigated for use as hot wire sensitive gasless ignitermixes for igniting gasless delay powders. A (50/50) zirco-nium/lead monoxide composition is sensitive to hot wireignition; it reliably initiates molybdenum and manganesebase delay mixtures; it acts essentially as a gasless delayigniter for such delay mixtures used in systems having delaysup to several seconds in time. It does not act gasless whenigniting long burning tungsten delay mixes. It will notsatisfactorily ignite all delay compositions so that itsselection for use must be based on knowledge of its specificbehavior with the particular delay composition contemplated.

PUBLISHED DECEMBER 1961

Explosions Research DepartmentU. S. NAVAL ORDNANCE LABORATORY

WHITE OAK, MARYLAND

i

NOLTR 61-153 1 November 1961

This report presents information concerning the search for a"gasless" igniter to be used in electro-explosive devices.The work was carried out in the Explosion Dynamics Divisionof the Explosions Research Department, U. S. Naval OrdnanceLaboratory, White Oak, Maryland, in connection with Wep TaskRUME 3E000/212 1/V008 10 004, Problem 016, Applied Researchfor Underwater Detonators. The results of this investigationare intended for the information and use of the Naval OrdnanceLaboratory and should be of interest to others working withelectro-explosive devices.

W. D. COLEMANCaptain, USNCommander

C. ARONSONBy direction

li

NOLTR 61-153

CONTENTSPage

IntZtroduction ........ . 1SelJleation and Preparation of'Mixes. .e . . ......... 2Selaettion of Final Mix for Further Tests. . . . . . . 2Tesitng in Delay Devices . . . . . . . . . . . . . . 3Serr,-.sLtivity to Hot Wire Ignition. . . . . . . . .. . 4Corrncjusions . . . . . . . . . . . . . . . .. . . . . . . . 5Retffer-ences . . . . . . . . . .. . . . . . . . . . . . 6

ILLUSTRATIONS

Fiaure s Title Page

i Light Output During Burning of SeveralZirconium/Lead Monoxide Ignition Mixtures . . .10

2 The Test Vehicle Used for Testing the FastBurning Delay Compositions . . . . . . . . . . 11

3 The Test Vehicle Used for Testing the SlowBurning Delay Composition. . . . . . . . . . . 12

4 Percent Firing vs. Constant Current forZr/PbO 50/50 Igniter Mix . . . . . . . . . . . 13

Tall bles

1 Preliminary Tests of Firing Voltages forZr/PbO Compositions . ........ . .... 7

2 Observed Delay Times for Delay CompositionsIgnited from (50/50) Zirconium/LeadMonoxide Igniter Mixture. . . . . . . . . . . 8

3 Determination of the Firing Characteristicsof Igniter Mix (50/50) Zr/Pb by the BrucetonSensitivity Method ........... .. 9

~iii

NOLTR 61-153

A LOW GASSING IGNITER MIXTURE FORVARIOUS PYROTECHNIC DELAY COMPOSITIONS

introduction

1. The designs ofelectro-explosive devices (EEDs) containing"gasless" delays have almost exclusively used primary explo-sives heated by a bridgewire to effect initial reaction.Primary explosives, when they react, produce liberal quanti-ties of gaseous combustion products. If these gases areallowed to materially increase the internal pressure of theEED, the burning rate of the gasless delay, which is pressuresensitive, is considerably increased over its rate at ambientpressureand inefficient use of the delay (with respect totime/length) results. In addition, if the internal gas pres-sure is not controlled, time uniformity may not be obtained.

2. To overcome these difficulties practical designs have allowedfor venting the primary explosive gases through vent holes tothe exterior or have incorporated a fully contained internal ventchamber (1). The former expedient reduces the shelf life of theEED in moist environments and also prevents potting of the EED.The latter solution overcomes the moisture and potting diffi-culties but requires increased volume or length (for the ventchamber) and this space in a weapon system is often at a pre-mium.

3. Another method of overcoming the problem would be to elimi-nate the primary explosive and substitute an igniter materialsensitive to ignition by a hot wire and having combustionproducts which are essentially gasless. Such igniter materialshave not been generally available. Two possibilities, however,exist:

Metal acetylides.

"Gasless" mixes similar to the gasless delays butwith sufficient sensitivity to be initiated byhot wires.

The acetylides had been previouslyoinvestigated (2) but abandonedbecause of their extreme static sensitivity and difficulty ofpreparation. Gasless igniter materials of sufficient sensitivitywere unknown; however, some gasless igniter mixes, A-lA forexample (3), were known to be marginally close to the sensitivitydesired*

*KA-A could be initiated by a hot wire some of the time but notalways. In some cases the wire could be burned out withoutinitiating the A-lA.

NOLTR 61-153

4. The Universal Match Corporation in 1959 was assigned aproblem under Contract NOrd 13466, Task 2, to develop hot wiresensitive gasless igniter mixes for use in non-vented delaysystems. The results of their work are summarized in theirfinal contract summary report (4). In brief, they found anumber of mixes which could be ignited by hot wires. Theycentered their testing on the most promising; mixes of boronand lead dioxide and mixes of zirconium and lead dioxide. Theboron mix was found to introduce appreciable non-uniform delaysitself so zirconium/lead dioxide was the final igniter materialselected. When it was used in non-vented delays appreciablereduction in time over the vented system resulted.

5. The work reported herein is a continuation of the workstarted at the Universal Match Corporation. It was hoped toobtain a sensitive gasless igniter capable of being incorporatedinto non-vented delays without appreciably decreasing the burn-ing time below that of identical vented items. It has beenfound that a (50/50) zirconium/lead monoxide igniter mix actsas if it were gasless when igniting molybdenum and manganese*base mixes in systems with delays up to several seconds. Thismix, however, does not satisfactorily ignite all delay compo-sitions and affects the burning times of long burning tungstenbase delays in obturated systems.

Selection and Preparation of Mixes

6. After reviewing the work performed by the Universal MatchCorporation and all other pertinent literature and information,it was decided that mixtures of zirconium and lead monoxidewould be investigated. An approximate stoichiometric mixtureof these ingredients, (17/83) Zr/PbO, as well as several oxygendeficient combinations were prepared. The zirconium powder con-formed to specification JAN-Z-399A. The lead monoxide wasreagent grade obtained from Merck and Co. It was finer than325 mesh. For reasons of safety, mixing was performed with theingredients wet. The wetting fluid was ethyl acetate. Quanti-ties of 10 grams or less were wetted with the fluid and mixedin a Waring blender for twenty minutes. The mixtures were thenfkItered and dried in an oven.

Selection of Final Mix for Further Tests

7. The selection of the final mix for further testing wasbased on two criteria:

The ignition sensitivity at a selected size hot wire.

2

NOLTR 61-153

The rapidity of the combustion sensed by a phototubedetector.

Preliminary sensitivity tests were conducted by pressing themixtures about a 0.0004-inch diameter Tophet-C wire, 0.050inch long, and then determining, by a few exploratory tests,the potential needed on a 1-microfarad capacitor to causesamples to fire. The results of this testing are given inTable 1. From this table-it can be seen that the (20/80), and(50/50) Zr/PbO mixes could be ignited without sufficient dif-ference in sensitivity to choose between them. The (95/5)Zr/PbO mix could not be fired even at 6 microfarads and 250volts, and was thus eliminated.

8. The (20/80), (40/60), and (50/50) Zr/PbO mixes were thansubjected to hot wire ignition testing in which the light ou-put was viewed as a function of time using a photoelectricdetector tube and an oscilloscope. Typical traces for thethree mixes are shown in Figure 1. The (20/80) Zr/PbO mixshowed no output 'for the full sweep of the oscilloscope, whichwas 5 milliseconds in these tests, although the mix, of course,was ignited. The inherent delay was felt to be too long and theburning, which finally did occur, too erratic for further con-sideration of this mix as an igniter material. The (40/60)mixture and the (50/50) mixture ignited within the sweep time;however, the (40 0 mixture showed a rather slow build-up inintensity while the (50/50) mixture showed an even, rapidbuild-up to its final intensity. On the basis of these resultsit was decided to use only the (50/50) mixture for furthertesting.

Testing in Delay Devices

9. Tests in delay devices, both obturated and vented, wereconducted with delay mixes of various burning rates. Compari-sons were made between burning times in the vented and non-vented devices. Two types of test vehicles were chosen forthese tests.

For the obturated condition the fast burning compositions(molybdenum and manganese based mixes (5), (6)) were testedin the unit shown in Figure 2, and the slow burning compo-sition (tungsten based mix (5)) was tested in a larger bodyshown in Figure 3. The test devices were loaded such thatthere was no internal free volume for venting of gases duringburning.

3

NOLTR 61-153

The vented devices were identical to the obturated onesshown in Figures 2 and 3 except that the charge holder wasreduced in diameter and a vent hole 0.025 inch in diameterwas drilled in the delay body slightly above the igniterlevel to allow gases to escape to the exterior.

10. On the basis of preliminary tests, the igniter mix wasloaded at 10,000 psi. The initiator assembly contained 30milligrams of (50/50) Zr/PbO igniter mix. The quantity ofigniter used for the fast burning molybdenum and manganese basemixes was 100 milligrams while the slow burning tungsten base,delay composition required 250 milligrams of the igniter mix.The delay compositions were loaded at 30,000 psi and the unitstested over a temperature range of -65@F to + 160°F. Theenergy from a 1-microfarad capacitor charged to 60 volts wasused to produce ignition and the ability of the mixture toignite the delay compositions and the delay times were deter-mined. Table 2 summarizes the results observed.

The manganese delay compositions were reliably initiatedover the temperature range +160°F to -650F in both theobturated and vented systems.

In the case of the molybdenum base delays, there was nosignificant difference in the observed delay timesbetween the obturated and vented systems.

For the manganese delay compositions there was a smallreduction of the burning time in the obturated system.

The slow burning tungsten base delay composition wasignited satisfactorily in the obturated system but inthe vented system failures occurred at the igniter-delaymix interface. The failures were probably due in partto the loss of pressure caused by the venting. There wasa considerable reduction in time in the obturated systemas compared to the vented system. This can be seen fromthe tests conducted at 160*F where all items ignitedproperly. The table shows also that ignition reliabilityat the igniter-delay interface is a function of the opera-ting temperature.

Sensitivity to Hot Wire Ignition

11. Two methods were used to determine the sensitivity of the(50/50) zirconium/lead monoxide mix to ignition by a hot wire.

The first was a capacitor Aischarge Bruceton type test (7)using a fixed 1-microfarad capacitor and a variable potential.

4

4

0

0 NOLTR 61-153

The second was a variable-amplitude, constant-current,run-down type test.

12. The data for the capacitor dfscharge test are shown inTable 3. The mean firing potential was determined to be 57.4volts which corresponds to an energy of 16,500 ergs. If theassumed log normal distribution is correct, the 99.9% firingpoint is at 63.1 volts corresponding to an energy of 19,900 ergs.

13. The constant-current data were obtained on two groups ofelements containing the igniter mix. The results are shown ingraphical form in Figure 4. From this curve it can be seen thatthe current characteristics of the two groups were rather uni-form, that virtually no primers fire below approximately 340milliamperes, and that virtually all can be expected to fireabove 420 milliamperes. The number at each point plotted onthe curves indicates the number of igniters tested at this point.

Conclusions

14. From the-experiments conducted it is concldded that the150/50) zirconium/lead monoxide igniter mix acts as if it were'gasless" when igniting molybdenum and manganese base mixeshaving times up to several seconds. When igniting long'burningtungsten base delays, there is an appreciable reduction of timein the obturated system over that of the vented system.

15. This igniter mix does not satisfactorily ignite all delaycompositions; auxiliary igniters such as A-lA on top of thedelay column may be necessary in some cases. The igniter mixmay be satisfactorily ignited from hot wires. The energyrequired is somewhat more than that needed for sensitive primaryexplosives.

5

a 5

INOLTR 61-153

@0

REFERENCESS

*(I) NavOrd Report 5724, "An Investigation of InternalVenting for Delay Actuators", H. S. Leopold andE. E. Kilmer,,i0 Sep 1957, Confidential

(2) NOLM 10487, "Development of Gasless Delays for LowEnergy Electric Primers", Progress Report (NOL-26-Re2b-222-5), W. W. Rymer, 15 Nov 1949

(3) NavOrd OS 8976, "Powder Ignition, Gaslesa", 13 $ov 1959

(4) Universal Match COrp., "Contract NOrd 13466, Task 2,Summary Retort No. 3", Period 1 jan 1958 to 30 Apr 1961,Confidential

(5) Universal Match Clorp., "Contract NOrd 13466, Task 2, SummaryReport No. 2", Period 1 Dec 1955 to 1 Jan'1958, Confi-dential

(6) MIL-M-21383-NOrd, "Manganese Delay Composition", 28 Apr 1958;and NavOrd OD 9360, "Preparation of Manganese Delay Compo-sition", 5 May 1956

(7) Princeton University, Statiitical Research Group,"Statistical Analysis for a New Procedure in SensitiVityExperiments", AMP Report No. 1O1.IR SRG No. 40, Jul 1944

6

6

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NOLTR 61-153

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NOLTR 61-153

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NOLTR 61-153

Table 3

Determination of the Firing Characteristics ofIgniter Mix (50/50) Zr/PbO by the Bruaeton Sensitivity Method

Volt Fire Failure

± X's Oles

6 61 - 1 .0 0 36_0

-5. _60 3J_ _1 * *

459 4 3__ _12 16 ____

3. __587 4 512- '163L-257 5 7 :14 ..4

1 56 5 5____ 1 5-------0 5 0 550 _ 0

c-log howl674.036 'Sum Sum Sum-A __m-

d- &1og h-0.007 ____N2 2 2 20

M=c + d A - I )or -c d A( + I

m - 1.74,036 + 6007 -+ - 1.75870

Antlq m- 5714 Volts_ _ -Capac itance w 1 mf'd.

-N - Us.A e Nx or No From Table or 6- d (0.05 + 1.6M)as above -rph p. 51-54*6- 07(5+.(16N2 1AMP Report No. S'= 0.01363-

K K__6__ m+Kr Eo(% point) =5CV2 *

-- 3090 -0.042111( 1.71658. 5(l) (52.O)2-136520

--50 1 X)57.4) -ui6,47-99-2 j +3.090 +0.01421171 1 8008: 5(1)(-6312-19-P910

*C microf'aradsV-volts

~-.ergs.

9

NOLTR 61- 153

20/80Zr/PbO

40/60

* Zr/PbO

50/50Zr /PbO

TIME (0.5 MS/Cim

FIG. I 'LIGHT OUTPUT DURING BURNINA OF SEVERALZIRICONIUM /LEAD MONOXIDE IGNITION MIXTURES

- - 10

NOLTR 61-153

"K 2 -GLASS KOVARPLUG.

SOLD ER.

C HARG0E HOLDER'---

Zr/PbODELAY CARRIERM

DE LAYCOMPOSITION

BRASS BAFFLEAdiA-IA IGNITER

BRASS CUP-V~j -PISTOL POWDER

SR 4990

REF

jFIGURE 2. THE TEST:VEHICLE USED FOR*TESTING, THE FAST BURNING

DELAY COMPOSITIONS.,

NOLTR 61-153

100

801

01

00

30 0. L~TEST NO.1I3010 TEST NO. 2

20

-

.340 .350 .360 .370 ..380 .390 .400 .410 .420CONSTANT CURRELNT (ILLIAMPRS

FIGURE 4. PERCENT FIRING VS CONSTANT. CURRENT FOR Zr/PbO 50/50 IGNITER

'MIX. 13

NOLTR 61-153

GLASS KOVAR SOLDERPLUjG.

-'~CHARGEHOLDER

,BRASS

FRIGNITER BD* Zr/PbO

DEA

COMPOSITION1.5

IGNITER

PISTOLPOWDERSR 49 90

.500 CLSR-IC* S -~~~~ REFCOUEDS

FIGURE 3. THE TEST VEHICLE USED FORTESTING THE SLOW BURNING

4DELAY COMPOSITION.

04

NOLTR 61-153

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