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CP620, Shock Compression of Condensed Matter - 2001 edited by M. D. Furnish, N. N. Thadhani, and Y. Horie © 2002 American Institute of Physics 0-7354-0068-7/02/$ 19.00 SHOCK INDUCED MELTING OF LEAD (EXPERIMENTAL STUDY) Catherine Mabire, Pierre L. Hereil Centre d Etudes de Gramat - 46500 GRAMAT - FRANCE Abstract. To investigate melting on release of lead, two shock compression measurements have been carried out at 51 GPa. In the first one, a pyrometric measurement has been performed at the Pb/LiF interface. In the second one, the Pb/LiF interface velocity has been recorded using VISAR measurement technique. VISAR and radiance profile are in good agreement and seem to show melting on release of lead. by optical pyrometry, the other with a velocity measurement. The aim of these two shots was to detect melting of lead and also to compare the velocity signal with the color temperature signal. EXPERIMENTS The single-stage powder gun ARION was used to perform two plate impact experiments on lead. The experimental configuration is depicted in figure 1 and the parameters of these two experiments are presented in table 1. Impact velocity and tilt were measured by mean of self-shorting pins located at the periphery of the target. Typically accuracy on impact velocity was ± 1 % and planarity was better than 5 mrad. The impactor disks, buffer plate, target and window all present a 0.01 mm flatness on their two faces and the parallelism difference between the two faces is smaller than 0.02 mm. The face of the lead disk aimed by the pyrometer presents a polished surface with a roughness of 0.01. The window material is characterized by an optical polish. The lead used in these experiments had a purity of 99.9% and a density of 11.346 g/cm3. INTRODUCTION The determination of melting curve under shock compression is very important in shock physics. Several experimental techniques have been used to detect melting under shock conditions: measurement of the release wave on dense impacted materials [l]-[2] and porous materials [3], measurement of the shock temperature by mean of a pyrometer [4]. Recently, a study on tin [5] showed that particle velocity measurements with accurate metrology could display melting on release. However, theoretically, temperature measurement is a more sensitive test of melting than a velocity measurement which provides only pressure/volume information. But, unlike a velocity measurement, temperature measurements of shocked heated metals is still an important unsolved problem of high pressure physics. It would be ideal to obtain temperature and velocity measurements for the same experiment. Unfortunately our experimental device does not allow that. This paper presents two experimental results on lead at shock stresses of about 51 GPa, one with a temperature measurement Table 1. Parameters for the impact experiments on lead Shot impactor buffer plate target window Number A104 A105 Ta (3.03mm) Ta (3.016 mm) Cu (3.024mm) Cu (3.054 mm) Pb LiF (3.788mm) (15.039mm) Pb LiF (3.755 mm) (15.022 mm) 229 impact velocity impact stress interface stress (m/s)______(GPa)______(GPa) 1895 ±4 51.1 ±0.1 30.2 ±0.1 1990 ± 2 54.5 ±0.1 32.1 ±0.1 Interface velocity (m/s) Cu (3 mm Pb (4 mm) _LiF(15rnm) Ta (3 mm). VISAR or PYROMETER self shorting pins (impact velocity and tilt) Space Experimental setup setup FIGURE 1 1 :: Experimental FIGURE g 2000 jL,\J\J\J A B C 1800 1800 1600 1600 650 nm D 1800 1800 850 nm ig g 1600 1 1600 QJ a I 1100 nm HOOnm 1270 nm 1270 nrri 1510 nm 1510 nm 1400 1400 I 1200 "o 1200 U 1000 1000 0.0 0.5 0.5 1.0 1.0 1.5 1.5 Velocity (m/s) Color temperature (K) 2200 2200 2000 2000 Luminance temperature (K) Comparison wave wave diagram diagram // experimental experimental results results FIGURE 22 :: Comparison FIGURE 1400 1400 1200 1200 1000 1000 800 _ 800 L, iA t TX B C N. l^s^^D D o 600 _ 600 5 > 400 2.0 2.0 (µs) Time (ps) : _ 400 200 200 00 A | , , , , i , , , , i , , , , i , , , , 0.0 0.5 1.0 1.5 2.0 0. 0 0.5 1.0 1.5 2. Time (µs) (ps) Interface color color temperatures temperatures measured measured for for shot shot A104 A104 FIGURE 4 : Interface velocity for profile FIGURE 33 :: Interface FIGURE 4 : Interface FIGURE velocity profile measured shot measured A105 for shot A105 In the the first first experiment experiment (shot (shot A104), A104), the the In diagnostic used used was was an an optical optical pyrometer pyrometer [6]. [6]. diagnostic Thermal radiation radiation emitted emitted at at the the Pb/LiF Pb/LiF interface interface Thermal was collected with an optical head then transmitted was collected with an optical head then transmitted to the the pyrometer pyrometer by by optical optical fiber. fiber. The The pyrometer pyrometer is is to designed to to provide provide electrical electrical signals signals proportionnal proportionnal designed to the the collected collected flux flux at at six six wavelengths wavelengths (500 (500 nm, nm, 650 650 to nm, 850 nm, 1100 nm, 1270 nm and 1510 nm). nm, 850 nm, 1100 nm, 1270 nm and 1510 nm). Measured voltages voltages were were converted converted into into flux flux from from Measured calibration realized realized before before experiment experiment with with aa calibration blackbody cavity. cavity. The The flux flux was was then then converted converted into into blackbody color temperature using Planck’s law. The color temperature using Planck's law. The measurement surface surface was was located located at at the the focal focal measurement distance of of the the optical optical device. device. To To avoid avoid possible possible distance parasitic light light radiation, radiation, the the edge edge of of the the window, window, as as parasitic well as a part of its free face, were coated with black well as a part of its free face, were coated with black paint and and aa black black cardboard cardboard tube tube was was put put on on the the paint target up up to to the the optical optical device. device. The The glue glue between between the the target window and and the the lead lead target target was was UV-hardened UV-hardened window LOCTITE 358. The glue thickness was less than than LOCTITE 358. The glue thickness was less 10 µm. This This glue glue remains remains transparent transparent under under shock shock 10 pm. for the the studied studied range range of of stresses stresses and and for temperatures [7]. temperatures [7]. The time-resolved time-resolved color color temperatures temperatures for for 55 The wavelengths is is presented presented in in figure figure 3. 3. The The wavelengths temperature in in lead lead is is too too low low to to obtain obtain an an temperature exploitable signal for the the 500 500 nm nm wavelength. wavelength. The The exploitable signal for five signals signals have have aa first first ramp ramp when when the the shock shock five reaches the Pb/LiF interface. After 0.5 µs, there is aa reaches the Pb/LiF interface. After 0.5 ps, there is change in in slope slope (point (point B). B). This This change change corresponds corresponds change to aa reflected reflected wave wave from from copper copper as the (x, to as shown shown in in the (x, t) diagram of figure 2. The decrease of signal t) diagram of figure 2. The decrease of signal (point (point 230 2200 2200 1.4 3000 3000 1.2 release due to LiF 2500 2500 0.8 1600 0.6 1400 0.4 calculated temperature (hyp. graybody) calculated temperature (hyp. graybody) measured luminance temperature (650 nm) 1200 I ............... calculated calculatedemissivity emissivity(hyp. (hyn. graybody) graybody) 0.0 0.5 0.5 1.0 1.0 1.5 1.5 ^ 2000 calculated calculatedmelting meltingcurve curve. 650 nm 2000 calculated calculated shock shock in in lead lead 850 nm 1100 nm 1270 nm 1510 nm 1500 1500 1000 0.2 measured luminance temperature (650 nm) 1000 1000 Temperature (K) ε = 0.68 ± 0.1 emissivity Temperature (K) 1.0 1800 calculated temperature (hyp. graybody) ^ interface interface Pb/LiF Pb/LiF ca lcu lta ted Hu go nio t T = 1860 ± 50 K 2000 2000 - 500 A & & ^f experimental melting curve [16] experimental melting curve [16] — 0.0 2.0 00 10 10 20 20 30 30 40 40 50 50 60 60 70 70 80 80 Stress Stress (GPa) (GPa) Time Time (µs) (ps) FIGURE 5: FIGURE 5: Calculated Calculated true true temperature temperature and and emissivity emissivity FIGURE FIGURE 6: 6: phase phase diagram diagram of of lead lead C) C) corresponds corresponds to to the the arrival arrival of of the the unloading unloading wave wave at the Pb/LiF interface. During release, at the Pb/LiF interface. During release, we we observe observe an increase of an increase of signal signal (point (point D). D). In the In the second second experiment experiment (shot (shot A105), A105), the the diagnosic used was a VISAR [8]. The acquired diagnosic used was a VISAR [8]. The acquired timetimeresolved velocity profile is resolved velocity profile is displayed displayed in in figure figure 4. 4. The velocity The velocity increase, increase, point point A, A, is is caused caused by by the the arrival compression shock Pb/LiF arrival of of the the compression shock at at the the Pb/LiF interface. The small decrease of velocity, point interface. The small decrease of velocity, point B, B, is is due to the return wave from copper (figure 2). Point due to the return wave from copper (figure 2). Point C C corresponds corresponds to to the the arrival arrival of of the the unloading unloading wave wave at Pb/LiF interface. at the the Pb/LiF interface. As As we we will will see see in in the the next next section, the change change in in slope section, the slope (point (point D) D) is is consistent consistent with the the increase increase of of color color temperature temperature in with in shot shot A104 A104 and may be interpretated as a phase change and may be interpretated as a phase change from from solid to liquid. solid to liquid. ANALYSIS ANALYSIS Shock stresses Shock stresses generated generated in in lead lead targets, targets, indicated in table 1, have been evaluated indicated in table 1, have been evaluated by by the the impedence matching method knowing the equations impedence matching method knowing the equations of state of state of of materials materials [9] [9] and and the the impact impact velocity. velocity. Despite the Despite the difference difference of of impact impact velocities, velocities, these these shock shock stresses stresses are are close, close, so so we we can can consider consider that that velocity and velocity and color color temperature temperature signals signals are are indicative indicative of the release path path in of the same same shock shock -– release in lead. lead. (point A to point C) Compression wave Compression wave (point A to point C) followed followed by by lead. lead. The The shape shape of of the the color color temperature profiles is not so easy to temperature profiles is not so easy to analyse analyse because because we we measured measured thermal thermal radiation radiation emitted emitted by by lead lead through through LiF LiF window window and and not not the the absolute absolute temperature temperature reached reached in in lead. lead. We We observe observe aa ramp ramp instead of a plateau and an increase instead of a plateau and an increase of of color color temperatures temperatures (point (point B) B) instead instead of of the the expected expected decrease. decrease. These These phenomena phenomena have have already already been been observed observed by by Bass Bass [10]. [10]. ItIt isis still still an an unresolved unresolved problem, problem, but but several several explanations explanations can can be be proposed proposed :: 1) a change in optical properties of LiF 1) a change in optical properties of LiF window window [11] [11] ;; 2) 2) aa heterogeneous heterogeneous interface interface temperature temperature [12][12][13] [13] ;; 3) 3) an an emissivity emissivity increase increase caused caused by by damage damage at at the the Pb/LiF Pb/LiF interface interface (because (because of of shock shock and and unloading) unloading) or or by by melting melting of of lead. lead. If If we we consider consider the the Hugoniot Hugoniot melting melting zone zone defined defined by by Lalle Lalle [15] [15] (50 (50 to to 62 62 GPa), GPa), lead lead was was partially partially shock-melted shock-melted in in our our experiments. experiments. So, So, an an emissivity emissivity change change due due to to melting on the release wave (point B) is a plausible melting on the release wave (point B) is a plausible explanation explanation for for the the increase increase of of color color temperature temperature instead of the expected decrease. instead of the expected decrease. True True temperature temperature and and emissivity emissivity have have been been calculated calculated using using the the graybody graybody approximation approximation (figure (figure 5). 5). The The calculated calculated emissivity emissivity value value is is about about 0.68 0.68 on on the plateau. It is less than expected liquid emissivity the plateau. It is less than expected liquid emissivity (about (about 1) 1) but but higher higher than than initial initial values values of of 0.1 0.1 [14]. [14]. This This high high emissivity emissivity is is consistent consistent with with partial partial melting. melting. However, However, in in release, release, there there is is an an unrealisitic unrealisitic true temperature increase and a strong true temperature increase and a strong emissivity emissivity decrease. decrease. These These unrealistic unrealistic values values are are due due to to the the graybody graybody approximation. approximation. We notice velocity profile profile We notice in in figure figure 22 that that the the velocity and interface color temperature profiles present and interface color temperature profiles present singularities The velocity profile singularities at at the the same same time. time. The velocity profile (A-C) is consistent with the compression (A-C) is consistent with the compression path path 231 Release wave (from point C to the end) During the unloading part of the signals, we can notice a strong increase of color temperatures (point D) and a small change in the shape of velocity profile. This color temperature increase cannot be explained by the arrival of a compression wave at the Pb/LiF interface. In release, we know that the absolute temperature in lead is decreasing, so point D corresponds to a strong emissivity increase. We think that this is due to the end of the melting process of lead in release. Melting curve of lead has been determined by means of a laser-heated diamond cell up to 100 GPa [16]. To compare our experimental results with this experimental melting curve, we calculated the stress profile corresponding to our color temperature profiles. Simulation of the experiment have been performed with a 1-D lagrangian code UNIDIM [17]. The behaviour of materials is described by a Mi'e-Griineisen equation of state based on the Hugoniot and the constitutive relation used is perfectly plastic. This calculation does not take into account melting but stress is little changed by melting. We represented the release path follow by lead in the phase diagram using calculated stress and measured color temperatures (figure 6). Hugoniot and melting curve indicated in figure 6 have been calculated using a mixture law between solid and liquid phase of lead [5]. We observe that the temperature increase occurs when the release path moves away from melting curve. It seems to confirm our hypothesis that lead is partially shocked-melted. The release path into LiF window follows the melting curve of lead and is not sufficient to achieve melting. Melting is achieved during the unloading wave from the back of the impactor. The shape of velocity profile is consistent with this explanation. We have already observed the same kind of velocity profile in tin when the Hugoniot point reached under shock was on the melting curve [5]. CONCLUSIONS Comparison between velocity and color temperature profiles may make easier the analysis of temperature profiles. According to our analysis of pyrometric signals, it seems that upon initial shocking, lead is partially melted and remains partially melted upon partial release into LiF window. Complete melting occurs upon release (coming from the impactor), that induces an emissivity increase and an increase of color temperature signals. It would be interesting to do the same experiments at lower shock levels with VISAR and the appropriate pyrometer to display melting on release of lead. ACKNOWLEDGMENT The authors gratefully acknowledge the technical assistance of P. Bouinot. This work was supported by the French Ministry of Defense. REFERENCES 1. 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