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1
GSECARS, University of Chicago, Chicago
Dynamics of Crystallization and Melting under PressureVitali Prakapenka
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LVP
DAC
R.Wenk, 2005
•Most of what we know about the structure of the Earth's deep interior comes from the study of seismic wave velocities
•In order to interpret such measurements in terms of mineralogical/compositional models of the Earth's interior, data on the physical and chemical properties of minerals at high pressures and temperatures are essential
•Knowledge of thermodynamics, phase equilibria, crystal chemistry, crystallography, rheology, diffusion and heat transport are required to characterize the structure and dynamics of the Earth's deep interior
The world’s deepest borehole in Sakhalin is 12,345 m (40,502 ft)
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At pressures above 225 gigapascals andtemperatures over 3400 kelvin, Fe0.9Ni0.1 adoptsa body-centered cubic structure
Science 316, 1880 (2007), Times Cited: 53
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6 8 10 12 14
5 6 7 8 9 10 11 12 13 14 15
molten Ge
~1280K
Inte
nsity
, a.u
.
2Θ, degrees
1280K 1150K 1050K RT
MgOGe II
Ge, 19 GPa
0 5 10 15 20 25 30 35 40
400
800
1200
1600
2000 Voronin Ge-I Ge-I/Ge-II Ge-II melt
Tem
pera
ture
, K
Pressure, GPa
Ge-I Ge-II
Liquid
Prakapenka et al., High Pressure Research, 2008 , 28:3,225
High P-T phase diagram of Germanium
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hot spot in the confined space
10 microns
Diamond anvil
Diamond anvil
Pressure medium
Sample
Laser
X-ray
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Fe : SiO2, 38 GPa,
30 µm
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Carbon transport in diamond anvil cells
Prakapenka et al, High Temperatures High Pressures, 2003/2004, volume 35/36, pages 237-249
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Dewaele et al, PRL, 2010
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RT
1400K
1520K
1900K
1700K
T quenched
Fe:C(d) + NaCl, 1:1, P ~ 92 GPa
^ diamond
Fe3C
Fe7C3
Prakapenka et al, 2011
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SEM images of FeO sample after laser heating
Leonid Dubrovinsky, BGI
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11
10 15 20
10 15 20
10 15 20
10 15 20
10 15 20
10 15 20
101 hcp
101 hcp
111 fcc
MeltT ~ 3250 K
10 15 20
10 15 20
Melting of Fe-Ni alloy at 60 GPa
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12
Ice VII, 7 GPa, Tm ~ 600K
(110)
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13
HT RT
Ice VII, 7 GPa, Tm ~ 600K
Laser heating
RT, starting
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14
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15
60 s, 100 mm, 3 p/s
(110)
Laser effect?
Ice VII, 7 GPa, Tm ~ 600K
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16
Pt foil: melting at ambient pressure with double sided laser heating
2100 K 1900 K
solid Pt fluid
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Grain boundary misorientation maps of electron back scattered diffraction
Kim et al, METALS AND MATERIALS International, Vol. 8, No. 1 (2002), pp. 7~13
Images of electron back scattered diffraction at 1000”C and 0.5/sec under various strains; (a) 10%, (b) 50% and (c) 500%
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Dynamic recrystallization
http://www.ndt-ed.org
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•Chemistry •Sample diffusion•Crystallization
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fs ps ns µs ms s min
Atomicvibrations
Dislocation nucleation
recrystallization
Thermally activated reaction dynamics
Phase Transformation diffusion
Static experiment
o phase transition kineticso structural dynamics & deformation o chemical reaction dynamicso transport properties (diffusion)o electronic properties
Probing fundamental ultrafast processes
High P-T-B-εLaserDynamic load
XESInelastic scattering
SAXSSynchrotron
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Finite-element calculations of the temperature profiles in the DAC cavity
8 ns pulse width
Goncharov, JSR, 2009
CW
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0.16 0.20 0.24 0.28 0.32 0.36 0.400.0
0.3
0.6
Inte
nsity
, a.u
.
Time, ms
up to 50 kHz
Pulse laser heating
1 μs
Goncharov, Prakapenka et al, Rev. Sci. Instrum. 81, 113902 (2010)
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Prakapenka et al., High Pressure Research, 2008 , 28:3,225
Optical schema of the on-line, flat top, double-sided laser heating system at GSECARS
500 – 10,000 K
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Standard Operating Mode, top-up102 mA in 24 singlets (single bunches) with a nominal current of 4.25 mA and a spacing of 153 nanoseconds between 40 ps singlets.
Special Operating Mode - hybrid fill, top-upTotal current is 102 mA. A single bunch containing 16 mA isolated from the remaining bunches by symmetrical 1.594 microseconds gaps. The remaining current is distributed in 8 group of 7 consecutive bunches with a maximum of 11 mA per group. The total length of the bunch train is 500 ns.
Synchrotron24 singlets
4.25 mA153 ns
T=3.672 µs
Synchrotronhybrid fill
500 ns, 88 mA
65 ps, 16 mA
1.594 µsT=3.672 µs
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Pt, 69 GPa
200 ns delay
600 ns delay
0 ns delay
Pilatus, 10000 pls600 ns width
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2Θ, degree
Detector window: 0.6 usScan step: 0.2 usCeO2, 105 pulses, 37 keV
0.2 µs
Synchrotronhybrid fill
500 ns, 88 mA
16 mA
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-0.4 0.0 0.4 0.8 1.2 1.6
0
20
40
60
80
100
120Co
unts
, a.u
Delay, microseconds
Synchrotronhybrid fill
500 ns, 88 mA
16 mA
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9
100
200
300
Inte
nsity
, a.u
.
Two theta, degree
HT RT
Synchrotronhybrid fill
500 ns, 88 mA
16 mALaser
-2 -1 0 1 2 3 4 5 6 7
0
2
4
Inte
nsity
, a.u
.
Time, µs
detector laser
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Wavelength (nm)
560 580 600 620 640 660
Rel
ativ
e In
tens
ity
1316(5) K
2741(6) KMeasurements
Planck fit
The time-resolved radiometric measurements of temperature
accumulation times: 0.1-10 s500 ns temporal resolution
Goncharov, Prakapenka et al, Rev. Sci. Instrum. 81, 113902 (2010)
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9 10 11
50
(200
)
Inte
nsity
, a.u
2Θ, degree
300 K 2600 K 3600 K(1
11) Ir, 40 GPa
2600 K300 K 3600 K
Pulsed laser heating Ir at 40 GPa
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TwoTheta (degree)
4 6 8 10 12 14 16
Inte
nsity
(arb
. uni
ts)
0
1
2
3
4 2400 K 3000 K 3350 K 3600 K
• Melting can be detected by observing a diffuse diffraction ring
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dspace/aIr
0.3 0.4 0.5 0.6 0.7 0.8 0.9
Inte
nsity
(arb
. uni
ts)
IrN2 at 42 GPa- this work IrN2 at 0 GPa -Crowhurst et al., 2007
IrIr Ir Ir
• Chemical reactivity is very fast in pulsed heating experiments• New possibilities for studying of chemical reactions
IrN2
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6 8 10 12 14 16 18
40
80
120In
ensi
ty, a
.u
2Θ, degree
pulse mode, 0.2s continius, 10s
Compare XRD for CeO2 collected with PILATUS detector for different exposure time:
continues 10s (divided by 50) and 0.2s averaged over 105pls, 2us window
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5 10 150.00
0.01
0.02
0.03
0.04In
tens
ity, a
.u.
2Θ, degree
10 pls
Detector window: 2 us or ~12 single bunches or ~2x105 photons
Standard Operating Mode, top-up: 102 mA in 24 singlets (single bunches) with a nominal current of 4.25 mA and a spacing of 153 nanoseconds between 40 ps singlets
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5 10 150.0
0.1
0.2
0.3
0.4In
tens
ity, a
.u.
2Θ, degree
10 pls 100 pls
Detector window: 2 us or ~12 single bunches or ~2x105 photons
Standard Operating Mode, top-up: 102 mA in 24 singlets (single bunches) with a nominal current of 4.25 mA and a spacing of 153 nanoseconds between 40 ps singlets
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5 10 150
10
20
30
40In
tens
ity, a
.u.
2Θ, degree
10 pls 100 pls 10000 pls
Detector window: 2 us or ~12 single bunches or ~2x105 photons
Standard Operating Mode, top-up: 102 mA in 24 singlets (single bunches) with a nominal current of 4.25 mA and a spacing of 153 nanoseconds between 40 ps singlets
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MAR-CCDReadout time: 3.5 sDynamic range: 16 bitsSize: Ø165 mmPixel size: 79 um
PILATUS 100KReadout time: 2.7 msDynamic range: 20 bitsSize: ~84x33 mm2
Pixel size: 172 um
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Dynamic x-ray probe optimization:
Synchrotronhybrid fill
500 ns, 88 mA
65 ps, 16 mA
1.594 µsT=3.672 µs
< 1 µs:
Synchrotron24 singlets
4.25 mA153 ns
T=3.672 µs2 -100 µs:
Detector: larger area, higher efficiency above 30 keV
Sample: thick, high Z, single crystal
General:
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Probing fundamental ultrafast processes
o high temperature EOSo phase transition kineticso structural dynamics & deformation o chemical reaction dynamicso transport properties (e.g., diffusion)o electronic properties
Pulse laser heating and optical spectroscopy combined with time-resolved x-ray probe
Reliable experimental conditions at higher then static T and P
CIW :A. GoncharovV. Struzhkin
GSECARS: Mark Rivers, Steve Sutton, Yanbin Wang, Peter Eng, Matt Newville, Przemek Dera, Nancy Lazarz, Fred Sopron
ESRF :I. Kantor