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

1. Fast (de)compression capabilities and first experimental results at HPCATHPCAT Workshop 2014 Jesse Smith HPCAT

2. 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

3. 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

4. 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

5. 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

6. 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

7. Sample pressure control

8. 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

9. Sample pressure control—precise, automated P P t t

10. 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

11. 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

12. 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

13. 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

14. 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

15. Fast compression—thermal EOS WOW! It’s an apple!

16. Fast compression—thermal EOS Complete Mbar isotherm in a few seconds External heated DAC at HPCAT

17. 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

18. 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)

19. 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

20. Fast, cyclic de/compression P Time

21. 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)

22. 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

23. 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.