J O U R N A L DE PHYSIQUE

Colloque C8, suppliment au n O l l , Tome 45, novembre 1984 page C8-83

EXPERIMENTS A T H I G H TEMPERATURE AND PRESSURE LASER H E A T I N G THROUGH THE DIAMOND C E L L

R . J e a n l o z and D . L .

Heinz

Department of Geology and Geophysics, U n i v e r s i t y of California, Berkeley, CaZifornia 94720, U.S.A.

R6sum6 - I1 e s t p o s s i b l e d e r 6 a l i s e r d e s e x p g r i e n c e s q u a n t i t a t i v e s 5 haut e s p r e s s i o n s e t t e m p g r a t u r e s s t a t i q u e s , e n c h a u f f a n t l ' i n t g r i e u r d'une c e l l u l e 5 enclumes d e diarrant A l ' a i d e d ' u n l a s e r c o n t i n u . Des ~ e m p 6 r a t u r e s d e 1500 2 5000K o n t 6 t 6 a t t e i n t e s d a n s t o u t e l a gamme d e p r e s s i o n s : 10 a 100 GPa. Le c h a u f f a g e e s t o b t e n u en f o c a l i s a n t l e f a i s c e a u d ' u n l a s c r Nd: YAG e t l e s t e m p g r a t u r e s s o n t d k t e r m i n g e s p a r r a d i o m 6 t r i e a v c c une p r g c i s i o n d ' e n v i r o n 200K. Le p r o f i l d e t e m p g r a t u r e d e l a zone chauff 6 c p a r l e l a s e r e s t dgterming p a r un f i l t r a g e s p a t i a l , o b t e n u p a r b a l a y a g e d'une f e n t e . Dans c e s c o n d i t i o n s l e s t e m p 6 r a t u r e s d e f u s i o n s o n t d g t e r m i n c e s s o i t p a r l a mesure d e l a t e m p 6 r a t u r e o b s e r v g e 2 l ' i n t e r face liquide-solide, s o i t 2 p a r t i r de l a tempgrature correspondant 2 l ' a p p a r i t i o n d e l a phase v i t r e u s e l o r s q u e l ' o n augmente p r o g r e s s i v e m e n t l a puissance de chauffage. A b s t r a c t -Quantitative experiments a r e possible a t sustained high p r e s s u r e s and temperatures by means of CW-laser heating through t h e diamond-anvil cell. Temperatures of 1500 t o 5000 K have been reached throughout t h e 10 t o 100 GPa p r e s s u r e range. Heating is achieved by a focused Nd: YAG laser beam, a n d t e m p e r a t u r e s a r e determined radiometrically with a n accuracy of about 200 K. The variation of t e m p e r a t u r e across t h e laser-heated spot is derived by means of spatial Altering with a slit t h a t can be scanned. In this way, t h e melting temp e r a t u r e c a n be determined either from t h e temperature observed a t t h e liquid-solid interface or from t h e peak temperature a t which glass is first produced with increasing laser power.

IN TROD UCTION
Two of t h e most important advantages of t h e diamond-anvil cell for high-pressure research derive from t h e strength of diamond a n d i t s transparency across a broad range of t h e electromagnetic spectrum. Thus, n o t only is i t possible t o achieve ultrahigh static pressures of 100 GPa o r more, b u t t h e ability to observe t h e sample in situ and probe it with electromagnetic radiation while a t pressure is a n especially important feature of t h e diamond cell. In t h e present case. we use this transparency t o c a r r y o u t quantitative experiments a t simultaneously high pressures a n d temperatures. CW laser radiation which is absorbed by t h e sample. b u t not by t h e diamond anvils. is used to achieve temperatures of several thousand Kelvin. By t h e same token, one can observe t h e thermal radiation emitted from t h e hot sample located between t h e diamonds; t h e blackbody-like radiation makes it possible t o determine t h e sample temperature a t high pressures. High temperature experiments a t elevated pressures a r e of interest for studies of phase equilibria, a s well a s for t h e synthesis of high-pressure phases t h a t can often be quenched and examined a t r o o m t e m p e r a t u r e a n d pressure. Melting is among t h e most important transitions t h a t c a n be examined, b u t high-pressure reactions t h a t would be kinetically impeded a t low temperatures a r e also of interest. As temperatures of 5000 K o r more can be achieved a t pressures of 10-100 GPa, t h i s experimental technique is also of direct geophysical interest for studying materials a t t h e conditions of t h e Earth's interior (Fig. 1). Indeed, beginning with t h e pioneering work of Ming and Bassett / I / , most of t h e research with laser-heated diamond cells h a s been carried out by t h e geophysical community. To date. however, this work has been more exploratory than quantitative: temperature in t h e diamond cell h a s been roughly estimated by means of optical pyrometry. and little has been done t o control t h e temperature o r t o derive quantitative phase equilibria from s u c h experiments. Article published online by EDP Sciences and available at http://dx.doi.org/10.1051/jphyscol:1984817

JOURNAL DE PHYSIQUE

P,T Range of Diamond-Cell Experiments

PRESSURE (GPa)

Fig. 1 - Pressure-temperature range t h a t is accessible in diamond-cell experiments a s compared with t h e range of estimated temperatures (geotherms) in t h e lower mantle and outer core of t h e Earth. Current estimates of t h e melting curves of iron and mantle silicates a r e also shown. The highest pressures so f a r achieved with t h e diamond cell a r e a t room temperature, but external heating and cooling (for cryogenic experiments) allow temperatures below about 1000 K to be reached. With laser heating, t e m p e r a t u r e s exceeding 2000 t o 4000 K have been reached a t pressures up to 100 GPa.

W describe here a spectroradiometric technique t h a t is currently being developed in order e to quantify the high-pressure laser heating experiments. Although many of t h e results a r e of a preliminary nature, our major conclusion is t h a t it is possible to carry out phase equilibrium studies throughout t h e pressure-temperature regime illustrated in Figure 1. The details of our c u r r e n t techniques, and some of t h e problems t h a t remain unsolved, a r e summarized in t h e following sections.

EXPERIMENTAL TECHNIQUES
The n a t u r e of laser heating a t t h e sample in t h e diamond cell is qualitatively summarized in Figure 2. Typical dimensions a r e a sample thickness and diameter of 5 to 20 p m and 50 t o 250 p m , respectively, with the sample being contained by a metal gasket between t h e diamond anvils. The highest temperatures a r e achieved in t h e focal spot, which is of dimension 10 t o 50 p m depending on t h e focusing optics used (see below). Because of their high thermal conductivity and large size, relative to t h e sample, t h e diamonds a c t essentially as infinite h e a t sinks. Thus. large t e m p e r a t u r e variations a p p e a r due to conduction both in t h e vertical (2) and radial ( T ) dimensions; and t h e gaussian intensity distribution across t h e focal spot also contributes to t h e radial temperature dependence (Fig. 2). The temperature variations with position present a major technical difficulty in making quantitative measurements. In particular, t h e spatial t e m p e r a t u r e Aeld must be determined in order to carry out phase equilibrium experiments. There is a n important chemical advantage, however, in t h e fact t h a t t h e hot, reactive p a r t of t h e sample is only in contact with cold material of t h e same composition (cold sample material). Problems of contamination a r e minimized, and t h e diamond anvils a r e protected from damage caused by reactions with t h e sample. This f a c t illustrates t h e importance of properly focusing t h e laser a t t h e middle of t h e sample thickness in order t o achieve high temperatures. Our complete laser heating system is schematically illustrated in Figure 3. The 1064 nm radiation from a Nd:YAG laser with 100 W (multimode) C power is used t o h e a t t h e sample W between t h e diamond anvils. A mode-selecting a p e r t u r e is used t o isolate t h e focusable TEMOOmode. which carries a maximum power of 25 t o 30 W a t t h e sample.

Fig. 2 - Cross section illustrating a sample being laser h e a t e d within t h e diamond cell. The Nd:YAG laser beam is focused within the sample, which is contained by a metal gasket between t h e diamond anvils. Typical dimensions a r e given. and t h e radial ( T ) a n d vertical (2) dependence of temperature in t h e sample is schematically illustrated.

'\

LOWER DIAMOND

TEMPERATURE

Dlchro~c Mirror

Wavelength

Fig. 3 - Summary of t h e laser heating system used in t h e p r e s e n t experiments. The beam from a CW Nd:YAG laser (TEMOOmode) is Focused into t h e high-pressure diamond cell by m e a n s of a microscope system containing a dichroic mirror. The dichroic mirror reflects t h e laser beam but transmits t h e thermal radiation emitted from t h e sample a t visible wavelengths (wavy lines). The spectrum of t h e thermal radiation is determined by a monochromator located above t h e dichroic mirror; from this s p e c t r u m t h e emissivity and temp e r a t u r e of t h e sample a r e determined. Also, t h e fluctuations in laser power and sample t e m p e r a t u r e a r e monitored a s a function of time.

The focusing is achieved with a beam expander (optional) a n d a long working-distance objective: typically we use a Leitz UM 20 objective (0.33 numerical aperture), which yields a beam waist of about 10 prn (or 50 p n ) a t t h e sample when using (or not using) a 6X beam expander. The laser power c a n be varied by changing t h e power a t t h e pump lamps. For a given experiment, however, we use a polarizer- a t t e n u a t o r system located right a f t e r t h e beam expander in o r d e r t o change t h e laser power t h a t is received a t t h e sample. By changing t h e power outside t h e laser cavity in this way, t h e r e is n o change in mode-structure o r focal level of t h e laser beam. The efficiency of this a t t e n u a t o r is such t h a t between 5 W (minimum) and 23 W (maximum) reach t h e sample a t peak laser power.

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The microscope system which focuses the laser beam is also used to observe t h e sample in the diamond cell. Visual observation (direct o r with a closed circuit television) is important for reproducibly focusing the laser in t h e sample and for monitoring changes in t h e sample a t high pressures a n d temperatures. The thermal radiation from t h e sample passes through t h e "hot mirror" (high-pass dichroic Alter) t h a t reflects t h e laser beam through the objective. This thermal radiation is focused onto t h e entrance slit of a holographic-grating monochromator (12 nm/rnm dispersion and 833 p m slit widths) with a silicon detector. Extra dichroic filters a r e placed in front of t h e entrance slit in order t o assure t h a t none of t h e primary (1064 nm) laser radiation enters the monochromator. Also, a low-pass (IR transmitting) filter located a t t h e polarizer-attenuator prevents any of t h e pump-lamp radiation from contaminating t h e sample spectra. As a result, even with maximum laser power almost n o surface is radiation is observed through t h e spectrometer when a reflective ( n ~ n a b s o r b i n ~ ) placed in t h e sample area. The s p e c t r a l response of this system, which is summarized in Figure 4, illustrates t h e exclusion of radiation a t 1064 nm. The s t r u c t u r e in t h e response curve is caused mainly by t h e multilayer dichroic filters t h a t a r e used a s well a s by t h e detector response. As is evident, however, this system which is maximized for visible wavelengths is ideal for measuring t h e thermal radiation of samples a t about 1500 to 5000 K. At lower temperatures, t h e light intensity is often too low to obtain a reliable spectrum (especially for samples of low emissivity). At higher temperatures, t h e limitation derives more from o u r d a t a reduction technique, a s described below, t h a n from fundamental optical constraints. The d e t e c t o r o u t p u t is amplified. and smoothed as a function of time (100 to 220 pF capacitors give smoothing time constants of order 1 to 2 sec.), before being r e a d by a HewlettPackard 9826 minicomputer which is used t o process t h e s p e c t r a l data. In o r d e r t o scan over a full s p e c t r u m 4 t o 8 minutes a r e usually required, b u t it is often possible to determine t h e t e m p e r a t u r e more rapidly. Speciflcally, only a fraction of t h e s p e c t r u m need be collected if t h e sample emissivity varies little with wavelength (ie., t h e greybody model applies), a s is often t h e case. Thus, temperature can be reliably measured with this system in less than one minute. Nevertheless, sufficient time is available for characterizing t h e s p e c t r u m of t h e thermal radiation, a s continuous heating experiments lasting well over one h o u r have been successfully accomplished in t h e diamond cell.

WAVELENGTH (nm)

Fig. 4 - Spectral response of t h e present radiometer system is compared with t h e laser wavelength (arrow a t 1064 nm) and t h e thermal emission from blackbodies (Planck functions) a t 2000 K, 3000 K and 4000 K. The system response (intensity in a r b i t r a r y units) includes t h e effects of Alters. dichroic mirrors, lenses and the detector; changes in ordersorting a r e shown by short vertical lines. l'here is additionally a scale factor ranging over 10 for t h e system response. The Wien approximation to t h e Planck function is shown for illustrative purposes (see text).

liters

DATA REDUCTION AND SYSTEM CALIBRATION

The thermal emission from t h e Laser-heated sample is analyzed in terms of the greybody model which relates spectral intensity. I(A), t o emissivity. e, and temperature. 7?

with A, h, k and c being wavelength, Planck's constant, Boltzmann's constant a n d t h e velocity of light, respectively. In o r d e r to t e s t t h e greybody assumption t h a t & is independent of wavelength it is convenient to use Wien's linearized approximation t o the Planck function (1). Thus. deflning a normalized intensity

a n d a normalized frequency

which a r e both observable, Wien's relation c a n be expressed a s a linear equation in

'I'-I:

(3) The problem with using (3) a s an approximation t o (1) is t h a t it is only valid a t relatively low temperatures. As is evident from Figure 4, however, t h e Wien equation accurately reproduces t h e Planck relation for t h e p r e s e n t experimental conditions up to temperatures of about 5000 K. The advantage, on t h e o t h e r hand, of reducing t h e data in terms of (3) is t h a t it is easy to t e s t for t h e validity of t h e greybody model (i.e.. check t h a t r is independent of A by checking t h e linearity of J versus I. ), a n d uncertainties in t h e spectral measurements c a n ? be directly propagated to t h e corresponding uncertainties in T and c. Starting with this analysis, high-temperature d a t a c a n be iteratively reduced t o correct for t h e difference between t h e Wien and Planck functions. if necessary. The spectroradiometer system is calibrated with respect to a standard tungsten-fllament lamp of spectral emittance which is known absolutely. To date, however, we have not calibrated t h e emissivities absolutely in t h e laser-heating experiments a t pressure. The reason is t h a t t h e surface a r e a of emittance in t h e diamond cell must be accurately measured in every experiment; this is possible (using optical techniques / 2 / ) but dimcult. Still, emissivities a r e typically determined to a factor of 2 to 5, and what is most important is t h a t t h e relative wavelength dependence of E is accurately measured. Also, t h e main concern h a s been in measuring t e m p e r a t u r e and, a s is evident from (3). this is independent of how well t.he absolute emissivity is known. As a check on t h e accuracy of t h e spectral temperature determinations during laser heating, t h e zero-pressure melting of several metals has been examined between 1500 a n d 5000 K. High-purity metal wires were heated in a n argon atmosphere to prevent oxidation. The temperature was measured a s in experiments with t h e diamond cell. The main difference with t h e high-pressure experiments is t h a t a much larger region is uniformly melted ( 100 pm characteristic dimension) because of t h e absence of t h e diamond h e a t sinks.

J = lne

- WT-'

The melting temperature was bracketed in a c r u d e b u t unambiguous way by t h e direct observation (or lack thereof) of flowage and formation of a bead of melt. As is evident from Figure 5, t h e present results a r e consistent with t h e known melting temperatures in all cases b u t t h a t of tungsten, which exhibits a 5 p e r c e n t discrepancy. Although Larger t h a n t h e estimated error on the t e m p e r a t u r e determination (derived from t h e spectral fit to t h e greybody function), a n accuracy of 5 percent is plausible for t h e present experiments. It should be noted, however, t h a t s u r f a c e tension might obscure t h e occurrence of liquid flow and result in an overestimate of t h e melting temperature, a s observed. Another difficulty worth mentioning is t h a t because of t h e nonlinearity of t h e laser-sample coupling it is not always possible to achieve temperatures n e a r t h e melting point in both t h e solid and liquid phases (cf. iron and zirconium).

FLUCTUATfONS IN LASER POWER

One important cause of uncertainties in t h e p r e s e n t experiments is t h a t t h e laser output fluctuates by a few percent a s a function of time. These fluctuations a r e monitored by means or a silicon detector on the back (high reflectance) mirror of the laser: there is sufficient light leakage t o continuously monitor t h e power (Fig. 3). As a result of the laser-

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Fig. 5 - Melting of four metals under t h e laser beam a t zero pressure. The difference between t h e radiometrically measured temperature and the known melting temperature (T,. given a t t h e bottom) is plotted for Fe, Zr, M and W. Open symbols refer to t h e direct observation of o flow whereas closed symbols indicate t h a t the sample appeared solid. In all cases t h e metal was in a s t r e a m of Ar.

intensity fluctuations, sample temperatures vary by about 200 K. This value is of similar magnitude a s the discrepancies observed in t h e zero-pressure melting experiments. W e partly surmount t h e problems caused by temperature fluctuations by means of the temporal smoothing t h a t is applied to t h e spectrometer output. It is clear, however, t h a t f u r t h e r improvements a r e possible. Among o t h e r solutions, t h e laser o u t p u t could be smoothed with a feedback system or t h e spectrum could be collected much more rapidly by mcans of a detector array. From a different perspective, t h e laser-intensity fluctuations can actually be advantageous. For a sample t h a t is passively absorbing t h e laser radiation, one would expect. t h e temperat u r e fluctuations to correlate with the changes in laser intensity (due t o h e a t flow a loss of high-frequency components and a slight phase shift would be expected, a s is schematically shown in Fig. 3). In contrast, the occurrence of reactions (in particular. melting) in the sample would be expected t o result in a loss of correlation between the t e m p e r a t u r e and t h e laser intensity. That is, kinetics and t h e latent h e a t (which a c t s a s a n e x t r a h e a t sink) prevent t h e sample temperature from closely following t h e changes in energy deposition by t h e l a s e r beam. These expectations a r e born out by laser-heating experiments in t h e diamond cell (Fig. 6). A refractory compound such as AIZOg is solid a t elevated temperatures, and it exhibits a close correlation between laser intensky and sample t e m p e r a t u r e (monitored here by the intensity of thermal radiation a t 600 n m wavelength). The dominant oscillations a r e of a few Hz in frequency, a n d t h e effects of thermal conduction a r e clearly evident (phase shift and loss of high frequency components in t h e temperature fluctuatiorls). The result for a sample t h a t is partially molten u n d e r t h e laser beam is markedly different (Fig. 6). In this case. t h e correlation between laser intensity and sample temperature is poor. Qualitatively, this effect is analogous to what is observed in Differential Scanning Calorimetry experiments. Thus, although more work is required t o develop this technique, t h e correlation of laser a n d temperature fluctuations could provide a powerful tool for t h e in situ determination of high-temperature reactions, a n d specifically melting, in t h e diamond cell.

Fig. 6 - Oscilloscope traces illustrating t h e fluctuations in sample temperature associated with fluctuations in laser output (see Fig. 3). In e a c h of t h e four r u n s the upper and Lower traces correspond respectively to t h e laser power and sample temperature as functions of time. Durations for each run a r e 1 and 2 seconds. a s indicated; laser intensity and sample temperature a r e in arbitrary units. The t r a c e s a r e well correlated in t h e two runs with A1 O3 (upper half) and poorly correlated in t h e two r u n s with (Mg Fee, ) Si04 (oli,ne s t a r g n g material; lower half). These experiments were carried out a?'%5 to$& GPa pressure in t h e diamond cell, and a few p e r c e n t P t were mixed in with t h e AL2O3 in order to absorb t h e laser beam.

Fig. 7 - Axial view in transmitted white light of four glass blobs crea .ed by laser heating in t h e diamond cell a t 30 GPa pressure. The starting material was Mgo Feo lSiOQ which was converted t o t h e high-pressure perovskite phase by laser heating &? ppr$ssures above 25 CPa. The largest glass blob (top) is 18 p m in diameter.

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MELTING EXPERIMENTS AND THE SPATIAL VARIATION OF TEMPERATURE

An alternative and more definitive proof t h a t samples a r e melted in the diamond cell is t h e formation of glass on quenching (turning off the laser). In this case, it is advantageous t o work with silicates o r oxides t h a t a r e good glass formers. An example is illustrated in Figure 7, in which t h e starting material is t h e high-pressure perovskite phase of pyroxene; this was synthesized in situ a t a b o u t 30 GPa from starting material of composition Mg.o,88 Fe 12Si03. Aside from its glass-forming ability this perovskite is of interest because it 1s c o n s i t e r e d t o be t h e dominant mineral of t h e earth's lower mantle/3/. Indeed silicate perovskite, which is stable only above a b o u t 20 GPa, is probably t h e single most abundant mineral within o u r planet. Four glass blobs a r e evident in t h e microphotograph, t h e largest being formed a t t h e highest laser power. With decreasing power t h e quenched blobs become smaller, a n d a t low power n o glass is observed. Thus, a t low power t h e peak temperature in t h e diamond cell is below t h e melting point of t h e sample (Fig. 8). With increasing laser power, both the average and peak temperatures a r e observed t o increase, and once t h e peak temperature intersects t h e melting point a small amount of glass is formed on quenching. With higher laser power, a larger region is melted and therefore a larger amount of glass is observed. Based on Figure 8, two approaches a r e suggested for determining t h e melting t e m p e r a t u r e of samples in t h e diamond cell. On t h e one hand, if t h e peak temperature is determined for t h e r u n in which glass is A r s t observed with increasing laser power, this brackets t h e melting temperature from below. On t h e o t h e r hand, t h e melting point can also be determined a t higher laser power by measuring t h e temperature a t the location of the glass-crystal interface. This is more difficult, but more satisfactory, than the preceding technique because it involves a direct measurement of t h e coexistence temperature between melt a n d solid; t h a t is, t h e experiment is inherently reversed. In either case, it is evident t h a t t h e temperature variation across t h e sample (Figs. 2 a n d 8) must be directly measured for quantitative phase-equilibrium studies to be possible. As a flrst c u t t o this problem wc t r e a t t h e laser heated spot as a disc source of light, with temp e r a t u r e varying a s a function 07 radial distance from t h e c e n t e r of t h e spot. Hence t h e temperature fleld can be directly measured by means of a movable slit which is placed directly on, a n d oriented perpendicular to, t h e e n t r a n c e slit of t h e monochromator (Fig. 9).

glass

Distance

INCREASING LASER POWER

Fig. 8 - Schematic illustration of t h e temperature a s a function of radial distance across t h e laser-heated spot. At low laser power t h e peak temperature is below the melting point of t h e z m p l e . Tm (left panel). With increasing laser power t h e average temperature, TaV, increases a n d t h e peak t e m p e r a t u r e intersects t h e melting temperature (middle panel). At this point glass is formed on quenching if t h e sample material is a glass former. At higher laser power, a larger region is melted a n d h e n c e a larger amount of glass is found after t h e laser is turned ofl (right panel).

MONOCHROMATOR SLIT 8 3 3 ~
(stotionory)

25pm

SAMPLING SLIT (moveable)

Fig. 9 - A vertical sampling slit can be translated across the image of the sample which is focused a t t h e stationary, horizontal e n t r a n c e slit of t h e monochromator. By scanning t h e slit horizontally across the image of t h e laser-heated spot it is possible to determine the spatial variation of temperature in the sample. The sampling slit is 10 t o 25 p m wide, t h e monochromator slit is 833 p m wide and t h e laser-heated region is typically 250 p m in diameter.
'

This sampling slit blocks out all but a thin strip of t h e sample image which is focused a t t h e e n t r a n c e slit. W use sampling slits of 10 and 25 p m dimension which can be moved with a e precision of 1 p m . As t h e magnification of t h e sample image is approximately 5x a t t h e slit. a spatial averaging (projected slit width) and positioning of 2 to 5 p m and 200 nm respectively, is achieved across the temperature field in t h e sample. Because of t h e vertical (on-axis) variation of temperature (Fig. 2), t h e disc approximation used here must always result in an underestimate of t h e peak temperature. Nevertheless, this gives a relatively good estimate of t h e spatial variation of temperature. The slitsampling across a disc is a n exarnple of a tomographic problem, with the invcrsior~given by T a n Abel transform /4/. Therefore, t h e spectral intensity as a function of radial distar~ce, , is calculated from t h e spectral intensity t h a t is measured a s a function of slit position, z:

Combining (4) with (1) or ( 3 ) provides a n estimate of t h e position-dependerit temperature and emissivity: T(T) and E ( 7 ) . The result of one such scan for a laser heating experiment on magnesium silicate perovskite in t h e diamond cell is shown in Figure 10. This figure illustrates sorrie of the difficulties t h a t must still be resolved, a s well providing concrete results from t h e present technique. The 7(r)curve was constrained by t h e d a t a between 5 a n d 25 p m radial dist.ance and by the average temperature (measured over t h e whole field of view) of 4100 (i200) K. Near t h e c e n t e r of t h e hot spot the results were extremely unstable because of t h e fluctuations in light intensity a s a function of time. That is, t h e size of t h e molten region fluctuates in response t o t h e fluctuations in laser intensity. Because of its small dimension (6 p m diameter, based on the size of t h e quenched glass). fluctuations of only I to 2 p m in t h e size of t h e molten region drastically alIect t,he amount. of thermal radiation t h a t is emitted from t h e central area. Beyond t h e 50 p m beam-waist diameter t h e t e m p e r a t u r e drops of! and. for t h e optical configuration used in this run, the decreasing light intensity produces large uncertainties in t h e temperature determinations a t T > 20 p m . W believe t h a t t h e minimum in f l ~near 10 e ) prn radial distance may be due t o t h e laser being slightly defocused. W have found t h a t it is e critical to reproducibly focus t h e laser in t h e middle of t h e sample thickness (F'ig. 2) in order to get reproducible profiles. Because of variation in t h e thicknesses of diamond anvils and in t h e index of refraction of diamond a s a function of pressure. t h e laser focusing must be carefully checked in each experiment. One way t h a t this can be accomplished is by fir~dir~g

J O U R N A L DE PHYSIQUE

Radial Distance (,urn)

Fig. 10 - Profile of t e m p e r a t u r e a s a function of radial distance from the c e n t e r of t h e laserheated spot for a sample of silicate perovskite a t 35 GPa in t h e diamond cell. The average ternperaturc across t h e h o t regions is 4100 K a n d the beam-waist diameter is 50 p m in this experiment. The t e m p e r a t u r e distribution. T(T), satisfies the average temperature a s well a s temperature points derived by inversion (see text). Error bars show the estimated uncertainties and open symbols have uncertainties well over 100 percent. Upon turning off t h e laser, a glass region 5 p m in diameter was quenched, and t h e corresponding t e m p e r a t u r e a t the solid- liquid interface is found to be near 3000 K.

the focal position t h a t produces t h e narrowest temperature distribution, corresponding t o the smallest beam waist in t h c sample. According t o Figure 10, t h e liquid-crystal interface is a t about 3000 K for t h e silicate perovskite a t 35 GPa. This value is in accord with t h e peak temperature a t which glass first appears with increasing laser power. Interestingly, the melting t e m p e r a t u r e of t.his perovskite a p p e a r s t o be c o n s t a n t a t a b o u t 3000 K between 30 and 60 GPa pressurc, a n d this may have important geophysical ramifications /5/. The main conclusion from this work, however, is t h a t continuous laser heating car1 be used t o achieve t e m p e r a t u r e s of several thousand Kelvin a t pressures of 10 to 100 GPa in the diamond cell. Average temperature, a n d both the spatial and temporal variation of t e m p e r a t u r e in t h e sample can be monitored by spectroradiometry. Thus, phase-equilibrium experiments a r e possible a t high pressures a n d t e m p e r a t u r e over time scales of minutes t o hours.

ACKNOWLEDGEMENTS
Work supported by t h e U.S. National Science Foundation, NASA and the A.P. Sloan Foundation.

REFERENCES
/ I / . MING. L.C.. and BASSETT, W.A.. Rev. Sci:Instrum., 45, (1974) 1115-1118. / 2 / . SCOTT, C. and JEANLOZ, R., Rev. Sci. Instrum, 55, (1984) 558-562.

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JEANLOZ, R., and THOMPSON, A.B., Rev. Geophys. Space Phys., 21, (1983) 51-74. DEANS. S.R.. The Radon Transform a n d Some of Its Applications, J. Wiley and Sons, New York (1983). HEINZ. D.L.. a n d JEANLOZ. R.. US-Japan Conference on Partial Melting. Proceedings. Eugene. Oregon. USA. (September 1984).