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Presented at the Joint Meeting of the International Association for the Advancement of High Pressure Science and Technology

and the American Physical Society Topical Group on Shock Compression of Condensed Matter June 28 - July 2, 1993
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SHOCK RESPONSE OF POROUS 2AI + Fe2Os POWDER MIXTURES G.T. Holman, Jr., R.A. Graham, and M.U. Anderson, Sandia National Laboratories, Albuquerque, NM. 87185 Time-resolved pressure measurements have been conducted on 2AI + Fe2Os powder mixtures using the (PVDF) stress-rate gauge. These measurements were made on samples which were 53% of solid density. Measurements were made at pressures from 0.67 to more than 10 GPa utilizing both impact loading with a compressed gas gun and direct contact high explosive loading. The sample is pressed to the desired density in a copper capsule. PVDF gauges were positioned in front of and behind the powder sample in direct contact with the sample. These gauges measure the input and propagated stress-rate and are used for a precise measurement of velocity through the 4 mm thick sample. In the case of high explosive loading, gauges are also installed on the explosive side and on the capsule side of a metal driver plate to measure the shock velocity through the driver so that the driver pressure can be determined. The response of 2Al + Fe2Os under shock compression appears to demonstrate a more complex behavior than other materials. At approximately 4.6 GPa, the material compresses to beyond solid density. There was no evidence of chemical reaction. ....... INTRODUCTION /

For more than ten years, sbock-compression studies have been performed on highly porous powders and powder mixtures. Early experiments used the sample preservation technique. The experiments subjected the sample to a controlled shock using a plane wave generated by a high explosive. The sample was then recovered and analyzed using X-ray diffraction (XRD), scanning electron microscopy (SEM), differential thermal analysis (DTA), as well a_ other techniques._-s Later, the need for tirne-resolveO measurements on porous powders became essential to understand the dynamic response of porous materials under shock compression. This h,:ed led to a measurement technique being developed which utilizes the piezoelectric polymer, PVDF, as a gaugee to measure the time-resolved response of these porous materials under shock compression.7 The present study is one of three papers describing parallel work performed on three different materials, One material is a single component sample, TiO_.s The second material is a powder mixture which has a relatively low pressure for initiation of reaction, 5TJ + 3Si.0 The third is the classical thermite 2AI + Fe2Os which reacts at a pressure greater than 15 GPa based on earlier sample preservation work.l EXPERIMENTAL CONFIGURATION The aluminum and hematite (Fe_Os) powder in the mixture were acquired from the Aluminum Company Of America, ALCOA, and Fisher Scientific, respectively. The aluminum powder was manufactured and shipped as ALCOA lot #1401/$280202. ALCOA quoted 90% of the powder (by.

weight) between 3_,m and 12.8_m. A sample of the 1401 aluminum powder has been measured, and has a narrow size distribution ranging from 2_m to 17_m with 15_m making up.the largest volume, (25%)..,. The hematite in tile mixture was t,isner bcteminc stock #1116-3. Fisher quotes 100% of this material to be 15_m or smaller. The measured sample shows a distribution volume at a size of 22_m.and 45% of the sample per from lem to 27_m The porous powder sample is pressed into a capsule in three layers using a hardened steel plug. The top of each ortho first two layers is loosened before the next layer is added to lessen the chances of a layered effect of the sample. After ali three layers are pressed, the back capsule plug is pressed against the sample. A 50 mm diameter, 9.5 mm thick disc of KeI-F is mounted to the back plug between the gauge and the copper plug. This polymer provides a closer impedance match to the sample than the copper. Delaying the time of re-shock from the copper plug provides for a longer viewing time of the propagated wave. There is approximately + 1.5% thickness uncertainty with this design rather than the usual + 0.5%. The polymer deflects at a lower pressure than the pressure needed to compress the powder to 53% of solid density. Since the length of the hardened steel packing plug is known to + 5 _m, and the powder level with respect to the top of the capsule can be determined to + 10 _m, the sample thickness can be measured to the accuracy stated above. As shown in Figure 1, a PVDF gauge package is placed on either side of the sample. The gauge packages are comprised of different thicknesses of either KeI-F or Teflon along with the 25 _m PVDF gauge itself. Approximately 0.2 _m of aluminum is vapor deposited on the powder side of the package to provide an opaque barrier.

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Shock.._..p,. Loading

packages Copper fixture Powder

measure the projectile velocity to an accuracy of + 0.1%. Each gauge output goes to a current viewing resistor (CVR). There are two signal lines from each CVR. These signals are monitored using digitizing signal analyzers operated at one nanosecond per point. analyzer at the each CVR is monitored by the same The output of same horizontal sweep. One sensitivity based on the expected output. The other signal analyzer monitors the outputs at 10 or more analyzer monitors the two gauge outputs at a times the sensitivity of the first. These currentversus-time signals are a measure of the input and signals determines the wave velocity. The signals from the primary and sensitive channels are combined to increase resolution. The stress-rate signals are integrated and processed with a numerical fit using the software propagated stress-rates.program time between the The The PVDF Stress.:: two propagated stress measurement is characteristic of Several shock reverberations were observed during impa,_t loading. The front gauge typically remained loading for more than eight microseconds. EXplos#e active

le Input 0 E < [ ___ 0 _" a. 4 _ , l t_0 4 , , _. Propagated 0 -2 .4 4 __ 0 2OO Wave


' _ 's_z ' 100

2 0

' 0


Time (nammeeonete)

Time (nanoseconds)

Figure 1. The copper capsule containing the porous powder sample. Gauge packages are shown on both sides of the sample. Typical input and propagated stress-rate current waveforms are shown at the top and stress profiles are shown at the bottom, Two loading experimental configurations were utilized to measure the time-resolved response. The first technique utilized a gas gun facility which provides well controlled symmetric impact loading.:0 This method of impact loading also has the advantage of enabling small incremental pressure changes to be achieved. The second method is explosive loading where a P-40 plane wave generator, and a 102 mm diameter, 25 mm thick high explosive are used to provide the input stress wave into the target, Explosive loading offers the advantage of higher input stress, but has at least two distinct disadvantages: 1) limited selection of input stress levels, and 2) electrical noise radiated by the explosive to the data acquisition system at the lower signal levels. Measured current-time pulses and resulting stress-time records are shown in Figure 1. Impact loading In this configuration, an aluminum projectile with a copper impact face is accelerated into a copper capsule which contains a 50 mm diameter, 4 mm thick porous powder sample. Charged pins are used to

As shown in Figure 2, a P-40 plane wave generator and a 102 mm diameter, 25 mm thick high explosive are used to produce the input stress to the sample. A 114 mm diameter, 12.7 mm thick metal driver plate (aluminum or copper) is placed between the explosive and the copper capsule containing the sample. The explosive, the driver plate, and the capsule are in direct contact. PVDF gauge packages are mounted on the explosive side and on the capsule of the driver plate. The time difference between the two gauges measures the shock velocity in the driver plate so that input pressure in the driver can be determined. The gauge package on the explosive side of the driver plate is coated with approximately 0.2 ,m of aluminum to provide ar_opaque shield between the explosive and the gauge. The capsule containing the sample and the method used to monitor the ,torrent output from the gauges are essentially the same as that used in impact experiments. Late time signal reverberations have not been observed during explosive loading experiments. There is evidence of the Taylor wave from the explosive as seen by a slow decay on the back side of the stress signal. At pressures of approximately 17.5 GPa into the gauge package, the gauge output begins to become erroneous. This pressure range is coincident with the explosive driving configuration of Composition B with an aluminum driver plate. More work will be needed on the gauge packaging before higher input stresses can be successfully measured.

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_ uncertainty of compression is notsolids is As large, the Since the compression ofporous large. so shown in i , Figure 4,crushp-v plot for 2Al lower pressures (up to different the up slopes. At + Fe=O_ exhibits two 0.67 GPa), pressures large 0.67 GPa towardsolid isa between compression 3.2 GPa density. At there and the slope becomes more steep, and there is a smaller compression toward solid density. There have been two possibilities suggested to explain this phenomenon. One possibility suggests that the initial aluminum and the sec_ nd slope due to the crush

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// _.. ...___ ___ copper capeule t-rut gauge paCKage------ powder sample Figure 2. An established method of planar loading as seen above. A plane wave generator is used to change a point detonation into a plane wave over the surface of the HE. Explosive loading resultsinhigher pressm'es than can be achieved with impact loading, Two gauges are used to measure the shock velocity through the metal driver plate. RESULTS The propagated waveforms in the porous samples are observed to be dispersive when compared to a solid. A comparison of the propagated stress waves through 2AI + Fe=O_ at different input stresses is shown in Figure 3. The risetimes, though long, are virtually constant at input pressures above 3.3 GPa.e The measured input stress and sample wave speed are used to calculate a point on the pressure-vsrelative volume curve.Conservation momentum of equations are used in these calculations even though thepressureulse theporouspowder is p in nota true on the curve For this reason, the p-v shock wave. are somewhat uncertain. points as plotted

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could be the effect strength of Fe=O_. ofAnotherbeing f'flled asis that this voids possibility a result of particle size differences of the two materials resulting in the initial jump toward solid density. At an input pressure of 4.6 GPa, the sample has been compressed beyond solid density. Prior sample preservation studies on 2AI + Fe=O_ indicate a pressure of reaction threshold above 15 GPa: CONCLUSION_I The propagated wave in 2AI + Fe=Os is quite dispersive as is the case with mo_t porous materials. The response of this material under shock compression appears to be more complex than TiO_e or 5TJ + Si_ as indicated by the wave dispersion and the data plotted in the pressure-va-volume plane. Modeling of this material response is being done by Baer:= _T t i ! _J + r-_o, _

,=.......... _......... _............. _....... __:,t t _ ,o........ i .. ........ : ......... _ \ I








FI4dllt_o Volunm

200 400 "rime(Mnomco_=)


Figure 4. A plot of pressure-rs-relative volume. The solid symbols represent calculations based on the wave speed being measured from the breakaway of the input signal to the breakaway of the propagated signal. The open symbols represent calculations based on the wave speed being measured from halfmax to half-max.

Figure 3. The propagated stress waveforms show small changes in risetime with increased loading pressure above 3 GPa.

Table 1. Experimental parameters and results from shock compression experiments powder mixtures with unshocked density of 2.245 + .026 grams/cms (53%) of solid. Experiment Number,'.... Input Condition_ Configuratione Input StressD (GPa) Wave Velocity_ (km/s) Risetimer (nsec) Output Stressa (GPa)

on 2Al + Fe2Os Relative Volume_ ....

2485 (a) 2484 (a) BE-227 (b) BE-057 (b) BE-059 (b) BE-233 (b)

0.314 0.635 Baratol/Cu TNT/Cu Comp B/Cu PBX9404/A1

1 1 4 3 3 5

0.67 1.94 3.32 4.59 5.75 13.21

1.050 1.795 2.198 2.059 2.168 3.128

300 (162) 132 (78) 100 (44) 90 (39) 89 (40) 96 (48)

0.95 3.02 4.01 4.11 5.05 7.89

Kel-F KeI-F KeI-F KeI-F KeI-F Kel-F

1.385 1.377 1.293 0.977 0.861 0.755

A: (a) Impact Loading; (b) Explosive Loading; B: Symetric impact velocity (km/s) copper on copper or explosive loading; C: Configuration, nominal thicknesses in parentheses: 1: Cu (6.5mm)/FEP (12.7_m)/PVDF (25_m)/FEP (12.7m)/2Al + Fe#Os (4mm)/FEP (12.7_m)/PVDF (25_m)/FEP (12.7_m)/Kel-F (8.9mm)/Cu (6.35mm);2: P-40/Explosive (25.4mm)/Cu (12.7mm)/Cu (6.3mm)/Kel-F (125_m)/PVDF (25_m)/FEP (251am)/ZAl + Fe2Oa (4mm)/FEP (25_m)/PVDF (25_m)/FEP (25_m)/Kel-F (9.52mm)/Cu (6.35mm); 3: P-40/Explosive (25.4mm)/Cu (12.7mm)/Cu or Al (6.5mm)/FEP (12.7_m)/PVDF (25_m)/FEP (12.7pm)/2Al + Fe2Os (4mm)/FEP (12.7_m)/PVDF (25_m)/FEP (12.7_m)/Kel-F (9.52mm)/Cu (6.30mm); D: PVDF Measurement; E: Wave speed: Toe-Toe/10-90%; F: Propagated wave; G: PVDF measurement in polymer backing material; H: Calculated from PVDF input stress and wave speed; I: Value calculated using Hugoniot program rather than the actual measurement. ACKNOWLEDGEMENTS The authors would like to thank Heidi Anderson and Dave Wackerbarth, Ktech Corporation for their excellent technical assistance. The authors would also like to acknowledge New Mexico Tech for their firing site support. Work supported by USDOE Contract #DE-AC04-76DPOO789. REFERENCES 1. 2. R.A. Graham, Solids Under High Presazre Shock Compression: Mecham'cs, Physics and Chem/stry, Springer-Verlag (1993). R.A. Graham and N. N. Thadhani, "Solid State Reactivity of Shock-Processed Solids", in Shock Waves in Materials Science, edited by A.B. Sawaoka, Springer-Verlag (1993). N.N. Thadhani, _Shock-Induced Chemical Reactions and Synthesis of Materials", Progress in Materials Science, 37. 117-226, 1993. R.A. Graham, "Issues in Shock-Induced Solid State Chemistry", in Third International Symposium on High Dynamic Pressures, edited by R. Cheret' CEA, Paris (1989)pp 175-180. R.A. Graham, B. Morosin, Y. Horie, E. L. Venturini, M. Boslough, M. J. Carr, and D. L Williamson, "Chemical Synthesis Under High Pressure Shock Loading", in Shock Waves in Consensed Condensed Matter, edited by Yo M. Gupta, Plenum (1986) pp 693-711. 6. R.A. Graham, M.U. Anderson, F. Bauer, and R.E. Setchell, "Piezoelectric Polarization of the Ferroelectric Polymer PVDF from 10 MPa to 10 GPa: Studies of Loading-Path Dependence", Shock Compression of Condensed Matter-1991, eds. S.C. Schmidt, et al, North-Holland, (1992), pp 883-886. 7. R.A. Graham, M.U. Anderson, Y. Horie, S-IC You, and G.T. Holman, "]PressureMeasurements in Chemically Reacting Powder Mixtures With The Bauer Piezoelectric Polymer Gauge", Shock Waves, in press. 8. M.U. Anderson, R.A. Graham, and G.T. Holman, present proceedings, in press. 9. E.W. Dunbar, R.A. Graham, M.U. Anderson, G.T. Holman, N.N. Thadhani, present proceedings, in press. 10. R.E. Setchell, "Sandia 25-Meter Compressed Helium/Air Gun", Shock Waves in Condensed Matter-1981, eds. W.J. Nellis, L. Seaman, and R.A. Graham, (AIP, 1982) 657-660. 11. D. E. Wackerbarth, M. PI_ Anderson, R. A. Graham, SAND9243046, February, 1992, Sandia National Laboratories. 12. M.R. Baer, present proceedings, in press.

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