Jesse Smith High Pressure Collaborative Access Team (HPCAT) Geophysical Laboratory, Carnegie Institution of Washington Rapid, controlled DAC (de)compression.

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