JOURNAL OF APPLIED PHYSICS

VOLUME 88, NUMBER 1

1 JULY 2000

The initiation of fine grain pentaerythritol tetranitrate by laser-driven flyer plates
S. Watson,a) M. J. Gifford,b) and J. E. Field
Physics and Chemistry of Solids, Cavendish Laboratory, Madingley Road, Cambridge CB3 0HE, United Kingdom

Received 10 February 2000; accepted for publication 5 April 2000 Charges of pentaerythritol tetranitrate PETN were impacted by laser-driven flyer plates launched from substrate backed aluminum films. The flyers were produced by single pulses from a Q-switched Nd:YAG laser. The aluminum flyers were between 3 and 5 m thick, had diameters of 1 mm, and achieved velocities up to 8 km s 1. The stresses were intense but of only nanosecond duration. This falls into an interesting regime since the shock thickness of a few microns is of the order of typical hot-spot sizes and less than the grain size of conventional explosive powders. Ultrafine PETN 1 m grain size was readily initiated, whereas conventional, 135 sieve PETN with a grain size of 106 m was not, although limited reaction was observed in some cases. Environmental scanning electron microscopy was carried out to help elucidate the differences in behavior. © 2000 American Institute of Physics. S0021-8979 00 09213-6

I. INTRODUCTION

The processes involved in shock initiation of solids have been studied over a number of years. If a shock is incident on a reactive material, the shock will decay as it would in an inert material unless reactive decomposition is induced in the explosive and energy is released to support the shock. For low pressure shocks with sufficient duration, reaction can occur following an induction period inversely dependent on the shock strength. Detonation will then propagate in the explosive. Prompt initiation occurs when the shock pressure and duration are sufficient such that the induction period is not required to accelerate the shock to a full detonation. The critical shock initiation pressure depends on the likely production of ignition hot spots within the material. Inhomogeneities in the explosive medium act as localization centers for hot-spot formation. The principal hot-spot mechanisms acting in a granular bed of material are frictional heating as grains rub against each other, localized shear deformation,1,2 and heating caused by rapid compression of gas spaces.3–7 These hot-spot mechanisms must produce their energy prior to the arrival of the release waves following the shock, if they are to sustain the reaction. The short shock wave imparted by a 3 m thick flyer will have a duration of around 1 ns as calculated from the Hugoniot of the aluminum and an estimate of the Hugoniot of the granular pentaerythritol tetranitrate PETN . The hotspot mechanisms must therefore be able to cause release of energy within 1 ns of the impact. Shock initiation by thin flyers is an interesting regime since the shock thickness is similar to that of hot-spot sizes and less than the grain size of all but ultrafine powders.
a

Now at: Department of Physics & Astronomy, University of British Columbia, 6224 Agriculture Rd., Vancouver, B. C., V6T 1Z1, Canada; electronic mail: watson @physics.ubc.ca b Author to whom correspondence should be addressed; electronic mail: mjg49@phy.cam.ac.uk 0021-8979/2000/88(1)/65/5/$17.00 65

Work has been carried out in a number of groups on the initiation of energetic materials by thin flyer plates. In studies which looked at the difference in shock sensitivity of different grain sizes of the same material conflicting results have been obtained. Setchell8–10 found that hexanitrostilbene was more sensitive to shock initiation when the material had a low specific surface area. In contrast Hayes11 found that the opposite was true. Honodel et al.12 found that ultrafine 1,3,5trinitrobenzene was more sensitive to prompt shock initiation from thin flyers approximately 0.51 mm than coarser material. However for relatively long lived shocks produced in gap tests and with thicker flyers approximately 3.3 mm the coarser material was more sensitive. Waschl13,14 argues that due to the small voids present in fine grain material, higher shock pressures are required for initiation. High pressure shocks are less long-lived than low shocks from flyers of the same thickness. There is a tradeoff between initiation from a short duration intense shock and a longer duration, lower intensity shock. Grain size is important in this case as the grain burning time is the critical factor when looking at the shock duration required. Laser-driven flyer plates can be produced by the irradiation of a metal film with a high fluence laser pulse focused at the interface with the substrate on which the film is deposited. The substrate should be transparent at the laser wavelength and the laser radiation is absorbed in the metal film which generates a plasma at the interface.15,16 The unvaporized layer of film is driven off as a flyer plate. Figure 1 illustrates the technique used to produce the flyer plates in our experiments.17 The laser is focused onto the film to the required spot size and the flyers typically achieve velocities of a few km s 1. For explosive initiation, the explosive surface is positioned a short standoff distance from the metal film, permitting the flyer to achieve maximum velocity before impacting with the explosive.
© 2000 American Institute of Physics

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J. Appl. Phys., Vol. 88, No. 1, 1 July 2000

Watson, Gifford, and Field

FIG. 1. A laser-induced plasma is produced at the interface with the metal film and the substrate, to launch a flyer of the unablated metal towards a target explosive. FIG. 2. Assembly used to launch flyers over small distances onto the explosive confinement.

Explosive initiation has been the prime motivation for research into laser-driven flyers.18,19 However there is also interest in using the high-pressure shocks generated by laserdriven flyers for high strain rate materials testing.20,21 Laserdriven flyers have also being used in micrometeorite simulations for research into spacecraft materials.22 Some researchers have reported improvements in flyer performance by launching them from metal films deposited onto the end of optical fibers.23,24 A study was made of the sensitivity to shock initiation by the laser-driven flyer technique, of fine and large grain PETN. Detonations were recorded using streak photography. Environmental scanning electron microscopy ESEM techniques were used to image the surface of the charges in order to provide insight into the differences in initiation behavior.
II. MATERIALS USED

C. Streak photography

A Hadland Imacon 790 electronic image converter camera was used to record high-speed events. The photographs were recorded on 3000 International Standards Organization Polaroid type 667 film. For the experiments described below, the module used provided streak operation with continuously variable speed between 10 and 1000 ns mm 1. A total record length of 75 mm was available.
D. Apparatus for initiation studies

The conventional PETN used in this investigation was a powder of single crystals of standard sieve size 135 with a mean grain size of 106 m. The ultrafine PETN that was used has a primary particle size of 1 m and was produced by a proprietary process. It has a loose powder density of 15% theoretical maximum density TMD . Both powders were supplied by ICI Nobel Enterprises, Ardeer, U.K.
III. EXPERIMENT A. Laser

The laser used was a Lumonics YM800 Nd:YAG laser operating at the fundamental wavelength of 1.064 m. It had an oscillator–amplifier configuration and provided a horizontally polarized TEM00 output. The beam diameter was 9 mm and Q switching produced 10 ns FWHM pulses with energy up to 1 J. Flyer plate performance and characterization and other details of the experimental techniques used to launch the flyers have been described previously.15–17
B. Target film

Figure 2 shows the explosive confinement which was held together in a steel clamp. The target film substrate is on the left and the aluminum film is separated from the surface of the explosive column by a lip in the base of the substrate holder which defined a standoff distance of approximately 100 m. The explosive was pressed into a 5 mm diam column in a polymethylmethacrylate chamber 25 mm long and 25 mm in diameter. A brass or copper witness plate was held at the other end of the explosive and served mainly to reduce damage to the clamp. The laser beam was focused with a 500 mm focal length lens and was incident on the center of the aluminum film at a spot size of approximately 1 mm diameter. The laser beam was maintained perpendicular with the film surface to within 1.5° by measuring the angle of reflection of the HeNe guide laser beam, which followed the same optical path as the Nd:YAG laser. The flyer, which was approximately 1 mm in diameter and between 3 and 5 m thick traversed the standoff distance and impacted centrally with the end of the explosive column. A complete description of those parts of the apparatus not directly involved with the explosive column is not included here but can be found in previous publications.15–17 The 100 m slit of the streak camera was oriented such that it was parallel with the center of the explosive column. The target film and the length of the column were imaged through the slit.
E. Triggering

The aluminum target films were deposited on circular substrates 15 mm in diameter and 3 mm thick. The substrates were UV grade fused silica, which had high transmittance at the infrared wavelength of the Nd:YAG laser. The films were deposited onto the substrates by magnetron sputtering in an Edwards E306A vacuum system. The thickness was measured in situ and controlled with a Telemark 860 deposition controller.

The laser flash lamps were triggered at 10 Hz and the laser could be fired on command by sending a trigger pulse to the laser power supply via a digital delay generator to Q switch the laser for a single pulse. In response to the fire command, an appropriately delayed pulse from the delay generator triggered the camera to start the streak at the required time with respect to the Q-switch trigger.

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J. Appl. Phys., Vol. 88, No. 1, 1 July 2000

Watson, Gifford, and Field

67

FIG. 5. Detonation streak record compared with the column position for fine grain PETN at 76% TMD, using a 3.0 m thick aluminum film, a standoff distance of 144 m, and a laser pulse energy of 157 mJ. The flyer velocity was 5.3 m ns 1: P PETN column; F aluminum film; S fused silica substrate.

B. Streak photography

FIG. 3. Scatter plot of the results of the PETN initiation studies.

F. ESEM

Electron micrographs were taken in an Electroscan E3 ESEM. The samples used were pressed directly into modified stubs and then cleared of loose material in the same way as the charges that were used in the initiation experiments. ESEM is particularly useful for such studies since it can be used to look at insulating materials with no need for depositing a conducting surface layer. ESEM techniques have been used extensively within this laboratory for investigating properties of energetic materials.25
IV. RESULTS A. PETN initiation

Both the fine and coarse grain PETN powders were pressed to a variety of densities and the surfaces of the explosive columns were polished flat. Detonation of the explosive was confirmed from the streak records and the marks left on a copper witness plate. In some cases there was only limited reaction which was characterized by damage to the film and substrate which could not be attributed to the effects of the laser and by some loss of explosive typically 1 mm depth of the column . The results for both explosives are presented in Fig. 3. It can be seen that the fine grain PETN initiates at lower flyer impact velocities and at lower densities than the larger grain material.

The streak photographs showed that the flyer impact produced almost instantaneous initiation of the fine grain PETN. The two streak records shown in Figs. 4 and 5 show detonation velocities of 5.5 km s 1. The time delay between the laser pulse arrival A recorded due to scattering of laser light in the substrate and the outbreak of detonation is primarily due to the finite time taken for the reaction to spread from the center of the column surface where the flyer impacted, to the side of the column where the detonation breakout was observed. The early part of the detonation traces a curved line B in the streak photograph because the detonation originates at the center of the 5 mm diam column where the flyer impacted. The curve is slightly different in the two photographs and is attributed to slightly noncentral flyer impacts on the explosive column. A distance variation between the two impacts, with respect to the camera, of approximately 700 m would explain the discrepancy assuming a constant detonation velocity . The detonation wave C can be seen to continue at a constant velocity along the remainder of the column. The bright emission D at the top of the column was caused by the burning aluminum film left on the substrate. The position of the explosive assembly is shown next to the streak photograph.
C. ESEM microscopy

The ESEM micrographs shown in Figs. 6 and 7 indicate that the fine grain material provides a far more homogeneous target than the coarser powder. The spacing between the fine grains, which is the determining factor in terms of collapsing

FIG. 4. Detonation streak record compared with the column position for fine grain PETN at 74% TMD, using a 3.0 m thick aluminum film, a standoff distance of 120 m, and a laser pulse energy of 101 mJ. The flyer velocity was 4.3 m ns 1: P PETN column; F aluminum film; S fused silica substrate.

FIG. 6. ESEM micrograph of pressed ultrafine PETN. Scale bar: 5

m.

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68

J. Appl. Phys., Vol. 88, No. 1, 1 July 2000

Watson, Gifford, and Field

FIG. 7. ESEM micrograph of pressed sieve 135 PETN.

A further point is that fine grain material will be stronger and less likely to fail by brittle processes. This has been shown by a number of groups both within this laboratory and elsewhere.27–31 Instead plastic failure predominates. Research on PETN and many other explosives has shown that plastic failure is usually by localized shear banding.1,2,32 This we regard as a second major mechanism. However it has yet to be shown that the initiation and propagation of these shear bands is fast enough to be effective in this very short duration shock loading. At present we favor void collapse as an initiation mechanism since it is proven to operate on the time scales involved here. This study has shown that if this type of very thin flyer plate initiation is to be used in devices, it is desirable to have smooth surfaces and a distribution of many small voids. These characteristics are more likely to be found in charges of fine grain explosives.
ACKNOWLEDGMENTS

pore hot spots, is on the order of 0.5–1.0 m. The coarse grain material has a typical grain spacing of around 50 m and so will have larger pores as well as a far smaller surface area to volume ratio, which will impede heat transport from the collapsing gas spaces to the bulk of the grains.
V. CONCLUSIONS

The fine grain PETN, with a particle size of approximately 1 m, was found to be much more sensitive to initiation by laser-driven flyer plate impact than conventional PETN with particle sizes of 106 m. There are a number of possible explanations for this, but some seem more probable than others. The use of thin flyer plates means that the shock pressure is only held for a time period of the order of a nanosecond before the release wave arrives in the form of a rarefaction fan. At least partial energy release must have occurred during this period for initiation to take place. The width of the shock will be only on the order of a few microns. The fine grain material has a smoother surface see Fig. 6 and the shock will encompass several grain layers and a void structure with a large number of micron-sized voids. By contrast the coarser PETN has a rougher surface see Fig. 7 and will be impacted initially only at high points. At no stage will the shock contain complete grains or voids. In both cases the voids will collapse rapidly and produce hot spots by gas heating and jet impact.3–7 These hot spots will be of micron size and therefore large enough to be critical hot spots if the temperatures achieved are 1000 K.5 However the increased distance between the surface and the centers of the grains in the coarse material acts to slow down the rate at which heat can be transferred to the material and raise the temperature of the bulk to levels at which exothermic reaction can take place. Only those regions of the material near the surface region of the grains will be able to undergo reaction prior to the arrival of the release fan. Thus the ultrafine material with its far greater specific surface area will undergo more reaction during the shock transit period. A calculation of the thermal transfer times based on inert spheres26 shows that the dependence on particle size varies as r 2 .

The research was supported by the Engineering and Physical Sciences Research Council EPSRC and DERA Fort Halstead . The equipment was purchased on grants from EPSRC and AWE Aldermaston. M.J.G. is supported on a CASE studentship funded by Orica and EPSRC. Thanks go to P. Royall for his help in using the ESEM.
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