Fast de compression capabilities and first experimental results at hpcat hpcat workshop 2014
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Fast (de)compression capabilities and first experimental results at HPCAT HPCAT Workshop 2014. Jesse Smith HPCAT. Time-an added dimension. In static high pressure research, time is arbitrary. P(t). P. Strain Rate Gap. Dynamic Compression. Static Compression. 10 -3. 10 0. DAC, LVP.

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Fast (de)compression capabilities and first experimental results at HPCAT HPCAT Workshop 2014

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Fast de compression capabilities and first experimental results at hpcat hpcat workshop 2014

Fast (de)compression capabilities and first experimental results at HPCATHPCAT Workshop 2014

Jesse Smith

HPCAT


Fast de compression capabilities and first experimental results at hpcat hpcat workshop 2014

Time-an added dimension

In static high pressure research, time is arbitrary

P(t)

P

Strain Rate Gap

Dynamic Compression

Static Compression

10-3

100

DAC, LVP


Fast de compression capabilities and first experimental results at hpcat hpcat workshop 2014

Time-an added dimension

  • 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

Strain Rate Gap

Dynamic Compression

Static Compression

10-3

100

DAC, LVP


Fast de compression capabilities and first experimental results at hpcat hpcat workshop 2014

Apparatus and examples

16-IDB, the right tool for the job

  • Optimized beam delivery from source to sample

  • Remote, precise control of sample pressure

  • High-frequency imaging using latest-generation area detectors

  • High-throughput processing of large volume of data

Examples

  • Fast compression and equations of state

  • Rapid decompression and materials synthesis

  • Ultrafast (jump) compression for generating high strain rate

  • Cyclic (fast) de/compression for kinetics, relaxation, and rheology


Fast de compression capabilities and first experimental results at hpcat hpcat workshop 2014

Beam delivery—source

A high-energy 3rd generation storage ring is crucial

7 GeV

E(keV) ∝E2(GeV)

Canted undulator configuration at HPCAT since 2011

Images courtesy Argonne National Laboratory


Fast de compression capabilities and first experimental results at hpcat hpcat workshop 2014

Beam delivery—x-ray optics

Cryo-cooled Si double-crystal monochromator

320 mm Kirkpatrick-Baez mirrors

Pt or Rh stripes

FWHM < 5 mm

  • Intercept ~0.5 x 0.5 mm2 beam @ 30 keV

  • Focus down to ~4 x 6 mm2 (v x h)

  • You can see these assemblies during the HPCAT Tour on Saturday


Fast de compression capabilities and first experimental results at hpcat hpcat workshop 2014

Sample pressure control


Fast de compression capabilities and first experimental results at hpcat hpcat workshop 2014

Sample pressure control—plug and play

Spherical washer assy

60um PZT

Clamping tube

“Standard” symmetric DAC

Threaded collar

DAC piston

diamond sample chamber

DAC cylinder

Assembly Section View

  • You can see these apparatus during Saturday’s hands-on sessions


Fast de compression capabilities and first experimental results at hpcat hpcat workshop 2014

Sample pressure control—precise, automated

P

P

t

t


Fast de compression capabilities and first experimental results at hpcat hpcat workshop 2014

Detectors—last piece of the puzzle

From commercial IP scanners . . .

100 s

. . . to hybrid pixel array detectors

2.5 s

15 Hz

125 Hz

3 kHz

  • You can see these detectors during the HPCAT Tour on Saturday


Fast de compression capabilities and first experimental results at hpcat hpcat workshop 2014

Software

Automated peak and unit cell fitting with volume and pressure calculation

Simple, easy-to-use software for on-line image visualization

Automated image integration using simple macro capability

  • See how this process works during Saturday’s hands-on sessions


Fast de compression capabilities and first experimental results at hpcat hpcat workshop 2014

Apparatus and examples

16-IDB, the right tool for the job

  • Optimized beam delivery from source to sample

  • Remote, precise control of sample pressure

  • High-frequency imaging using latest-generation area detectors

  • High-throughput processing of large volume of data

Examples

  • Fast compression and equations of state

  • Rapid decompression and materials synthesis

  • Ultrafast (jump) compression for generating high strain rate

  • Cyclic (fast) de/compression for kinetics, relaxation, and rheology


Fast de compression capabilities and first experimental results at hpcat hpcat workshop 2014

Fast compression—equation of state

Mo+MgO

Pressure apparatus—membrane

Loading—500 psi/s (Helium)

P0 ~ 80 GPa

Pf ~ 210 GPa

Dt ~ 1.3 s

Compression rate ~ 100 GPa/s

Detector—DectrisPilatus1M

Exposure period– 10 ms (100 Hz)

Exposure time—7 ms


Fast de compression capabilities and first experimental results at hpcat hpcat workshop 2014

Fast compression—equation of state

High-frequency imaging yields acceptable signal-to-background ratio

Average compression rate ~100 GPa/s

Peak compression rate ~240 GPa/s

High-density data yields extremely robust equation of state


Fast de compression capabilities and first experimental results at hpcat hpcat workshop 2014

Fast compression—thermal EOS

WOW! It’s an apple!


Fast de compression capabilities and first experimental results at hpcat hpcat workshop 2014

Fast compression—thermal EOS

Complete Mbar isotherm in a few seconds

External heated DAC at HPCAT


Fast de compression capabilities and first experimental results at hpcat hpcat workshop 2014

Fast decompression—materials synthesis

Si

Pressure apparatus—membrane + fast release

Unloading—1500-2000 psi (maximum rate)

P0 ~ 20 GPa

Pf ~ 0 GPa

Dt ~ tens to hundreds of ms

Decompression rate ~ 20-2000 GPa/s

Detector—DectrisPilatus1M

Exposure period–arbitrary

Exposure time—arbitrary


Fast de compression capabilities and first experimental results at hpcat hpcat workshop 2014

Ultrafast (jump) compression—strain rate

Mo+MgO

Pressure apparatus—dDAC

Loading—1000 V (minimum rise time)

P0 ~ 151 GPa

Pf ~ 194 GPa

Dt ~ 1.25 ms

Compression rate ~ 34 TPa/s

Detector—Dectris prototype (Eiger 1M)

Exposure period– 1.25 ms (800 Hz)

Exposure time—1.23 ms

Before

P

t

After (Dt=1.25 ms)


Fast de compression capabilities and first experimental results at hpcat hpcat workshop 2014

Ultrafast (jump) 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


Fast de compression capabilities and first experimental results at hpcat hpcat workshop 2014

Fast, cyclic de/compression

P

Time


Fast de compression capabilities and first experimental results at hpcat hpcat workshop 2014

Fast, cyclic de/compression

Relaxation of the KCl sample under fast (de)compression

Fast compression experiments in radial diffraction geometry:

KCl as an example

Rheology

Deformation

Relaxation

Piezo drive FWHM of (200)


Fast de compression capabilities and first experimental results at hpcat hpcat workshop 2014

Current challenges and future prospects

Selected Scientific challenges identified in 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

Technical challenges

  • Discrepancy between pressure loading and sample pressure

  • Limitations in pressure range and cyclic repeatability of dDAC

  • Time-dependent response of pressure media and/or marker

Future prospects

  • Order of magnitude flux increase leading to improved time resolution

  • Real-time pressure monitoring from x-ray marker

  • Closed-loop dDAC operation for robust and repeatable P cycling

  • Higher frequency, greater sensitivity area detectors with better E resolution


Fast de compression capabilities and first experimental results at hpcat hpcat workshop 2014

Contributors and acknowledgments

P(t) development: Chuanlong Lin, Eric Rod, Stanislav Sinogeikin, Guoyin Shen

ID-B staff : Yue Meng, Ross Hrubiak, Curtis Kenney-Benson

Software Development: Przemek Dera

User Collaboration (partial list): Jodie Bradby and Bianca Haberl; NenadVelisavljevic, Dana Dattlebaum, and Raja Chellappa; Hyunchae Cynn and ZsoltJenei;Choong-ShikYoo and Dane Tomassino

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.


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