jesse smith high pressure collaborative access team (hpcat) geophysical laboratory, carnegie...
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Jesse SmithHigh Pressure Collaborative Access Team (HPCAT)
Geophysical Laboratory, Carnegie Institution of Washington
Rapid, controlled DAC (de)compressionThe fundamental time-resolved approach
in static high pressure research
2015 IUCr High Pressure Workshop
Time – a (relatively) new DAC direction
2015 IUCr High-Pressure Workshop
PP(t)In static high pressure research, time is arbitrary
Selected scientific challenges from HPCAT’s 2012 Workshop
• Explore non-equilibrium transformations and phase boundaries• Elucidate dynamics, kinetics, and pathways of phase changes• Study system-dependent nucleation rates and crystal growth
Link to workshop report: https://hpcat.carnegiescience.edu/article/advances-matter-under-extreme-conditions-report-hpcat-workshop-october-10-12-2012
A few (of several) instances of P(t)
2015 IUCr High-Pressure Workshop
Overview
2015 IUCr High-Pressure Workshop
Critical experimental components• Source – optimized beam delivery from source to sample• Pressure control – remote, programmable, precise control• Detectors – short exposure, short readout, high frequency• Software – high throughput processing of lots of data
Examples, samples (apparatus)• Fast equation of state of Mo (membrane)• Ramp P↘ looking for metastable phase(s) of Ge (decompression membrane)• Measuring ultrahigh (DAC) strain rates in Mo (dDAC)• Synthesis of pure, amorphous Si (pneumatic rapid release box)
Source – Advanced Photon Source
2015 IUCr High-Pressure Workshop
7 GeV
A high-energy 3rd generation storage ring is crucial
E(keV) ∝ E2(GeV)
Sector 16 of the Advanced Photon SourceArgonne National Laboratory
Images courtesy Argonne National Laboratory
HPCAT – four dedicated HP beamlines
2015 IUCr High-Pressure Workshop
ID-DSpectroscopy
XES,IXS – 1eVNRIXS – 2meV
ID-BMicro-diffraction
Laser heatingCryostat
BM-BWhite LauePEC
BM-DMicro-diffractionXANES
Split in space14-42 keV
5-36 keV
Sector 16Bending magnet beamlines
Sector 16Canted undulator beamlines
Pressure control – traditional apparatus
2015 IUCr High-Pressure Workshop
Pressure control – contemporary control
2015 IUCr High-Pressure Workshop
P
t
P
t
2015 IUCr High-Pressure Workshop
Detectors – characterization in real time
100 s
2.5 s
125 Hz
3 kHz
From commercial IP scanners . . .
. . . to hybrid pixel array detectors
15 Hz
Software – must be semi-automated
2015 IUCr High-Pressure Workshop
Automated peak and unit cell fitting with volume and
pressure calculation
Simple yet powerful software for on-line image visualization, integration, and analysis
Dipotas – C. Prescher
GSE_shell – P. Dera
Overview
2015 IUCr High-Pressure Workshop
Critical experimental components• Source – optimized beam delivery from source to sample• Pressure control – remote, programmable, precise control• Detectors – short exposure, short readout, high frequency• Software – high throughput processing of lots of data
Examples, samples, and apparatus• Fast equation of state of Mo (membrane)• Ramp P↘ looking for metastable phase(s) of Ge (decompression membrane)• Measuring ultrahigh (DAC) strain rates in Mo (dDAC)• Synthesis of pure, amorphous Si (pneumatic rapid release box)
Rapid compression (pneumatic)
2015 IUCr High-Pressure Workshop
Mo + MgOPressure apparatus—membraneLoading—500 psi/s (He)P0 ~ 80 GPaPf ~ 210 GPaDt ~ 1.3 sCompression rate ~ 100 GPa/sDetector—DECTRIS PILATUS 1M-FExposure period– 10 ms (100 Hz)Exposure time—7 ms
2015 IUCr High-Pressure Workshop
Rapid compression – equation of state
High-frequency imaging yields acceptable signal-
to-background ratio
High-density data yields extremely robust equation of state
Average compression rate ~100 GPa/s
Peak compression rate ~240 GPa/s
Ramp decompression (pneumatic)
2015 IUCr High-Pressure Workshop
Jodie Bradby and Bianca Haberl
Development of double-sided membrane assembly for rapid, controlled sample decompression
Sinogeikin et al., RSI 86, 072209 (2015)
Ramp decompression – metastable Ge phases
2015 IUCr High-Pressure Workshop
Unloading (s)3100390700.3
Haberl et al., PRB 89, 144111 (2014)
Formation of R8 germanium on decompression appears to be time-
independent (at least over four orders), and requires hydrostatic conditions
Haberl et al., PRB 89, 144111 (2014)
2015 IUCr High-Pressure Workshop
Ultrafast (step) compression (dDAC)
10-3
Dynamic CompressionStatic Compression
DAC, LVP
100
Strain Rate Gap
Sinogeikin et al., RSI 86, 072209 (2015)
2015 IUCr High-Pressure Workshop
Ultrafast (step) compression – strain rate
P
t
Mo + MgOPressure apparatus—dDACLoading—1000 V (minimum rise time)P0 ~ 151 GPaPf ~ 194 GPaDt ~ 1.25 msCompression rate ~ 34 TPa/sDetector—DECTRIS EIGER 1M (prototype)Exposure period– 1.25 ms (800 Hz)Exposure time—1.23 ms
Before
After (Dt=1.25 ms)
2015 IUCr High-Pressure Workshop
Ultrafast (step) compression—strain rate
Strain rate* on the order of 101 s-1
Even on ms time scale, signal-to-background is useable, no sign of significant peak broadening
*based on aMo
Step decompression (pneumatic quick release)
2015 IUCr High-Pressure Workshop
Control Area
Experimental Hutch
Chuanlong Lin
Step decompression – amorphous Si synthesis
2015 IUCr High-Pressure Workshop
SiPressure apparatus—membrane + fast release Unloading—1500-2000 psi (maximum rate)P0 ~ 20 GPaPf ~ 0 GPaDt ~ tens to hundreds of msDecompression rate ~ 20-2000 GPa/sDetector – DECTRIS PILATUS 1M-FExposure period–arbitraryExposure time—arbitrary
Summary
2015 IUCr High-Pressure Workshop
We can leverage P(t) to:
• Address scientific questions in several contexts
• Improve experimental precision and accuracy
• Access intermediate strain rates
• Maintain static high pressure conditions after rapid DP
• Monitor crystal structure before, during, and after DP event
• Complement the mature fields of static and dynamic HP research
Rapid DAC (de)compression and x-ray diffraction . . . . . . A new frontier in extreme conditions crystallography
Contributors and acknowledgments
This work was performed at HPCAT (Sector 16), Advanced Photon Source (APS), Argonne National Laboratory. HPCAT operations are supported by DOE-NNSA under Award No. DE-NA0001974 and DOE-BES under Award No. DE-FG02-99ER45775, with partial instrumentation funding by NSF. The Advanced Photon Source is a U.S. Department of Energy (DOE) Office of Science User Facility operated for the DOE Office of Science by Argonne National Laboratory under Contract No. DE-AC02-06CH11357.
P(t) development at HPCAT: Stanislav Sinogeikin, Chuanlong Lin, Eric Rod, Ligang Bai, Guoyin ShenSee Smith et al., Rev. Sci. Instrum. 86, 072208 (2015) and Sinogeikin et al., Rev. Sci. Instrum. 86, 072209 (2015),
User Collaboration (partial list): Jodie Bradby and Bianca Haberl; Nenad Velisavljevic, Dana Dattlebaum, and Raja Chellappa; Hyunchae Cynn and Zsolt Jenei; Choong-Shik Yoo and Dane Tomassino
Software Development: Przemek Dera
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