HP-SR Discussion 28 August 2014

Jesse SmithHPCAT

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

HPCAT Workshop 20141Time-an added dimensionPP(t)

10-3Dynamic CompressionStatic CompressionDAC, LVP100Strain Rate GapIn static high pressure research, time is arbitrary2Time-an added dimension

10-3Dynamic CompressionStatic CompressionDAC, LVP100Strain Rate Gap

Selected scientific challenges from HPCATs 2012 Workshop

Explore non-equilibrium transformations and phase boundariesElucidate dynamics, kinetics, and pathways of phase changesStudy system-dependent nucleation rates and crystal growth3Apparatus and examples16-IDB, the right tool for the jobOptimized beam delivery from source to sampleRemote, precise control of sample pressureHigh-frequency imaging using latest-generation area detectorsHigh-throughput processing of large volume of dataExamplesFast compression and equations of stateRapid decompression and materials synthesisUltrafast (jump) compression for generating high strain rateCyclic (fast) de/compression for kinetics, relaxation, and rheology

4Beam deliverysource

Images courtesy Argonne National Laboratory7 GeVCanted undulator configuration at HPCAT since 2011A high-energy 3rd generation storage ring is crucialE(keV) E2(GeV)5Beam deliveryx-ray opticsIndicesTypical use(111)High flux(220)Nominal(311)High Q

320 mm Kirkpatrick-Baez mirrorsCryo-cooled Si double-crystal monochromatorFWHM < 5 mmIntercept ~0.5 x 0.5 mm2 beam @ 30 keVFocus down to ~4 x 6 mm2 (v x h)You can see these assemblies during the HPCAT Tour on SaturdayPt or Rh stripes6Sample pressure control

7Sample pressure controlplug and play

You can see these apparatus during Saturdays hands-on sessions

Assembly Section ViewDAC cylinderdiamond sample chamberDAC piston60um PZTSpherical washer assyThreaded collarClamping tubeStandard symmetric DAC8Sample pressure controlprecise, automated

Pt

Pt

9Detectorslast piece of the puzzle

100 s2.5 s125 Hz3 kHzFrom commercial IP scanners . . .. . . to hybrid pixel array detectors

15 HzYou can see these detectors during the HPCAT Tour on Saturday10Software

See how this process works during Saturdays hands-on sessionsAutomated peak and unit cell fitting with volume and pressure calculationAutomated image integration using simple macro capability

Simple, easy-to-use software for on-line image visualization11Apparatus and examples16-IDB, the right tool for the jobOptimized beam delivery from source to sampleRemote, precise control of sample pressureHigh-frequency imaging using latest-generation area detectorsHigh-throughput processing of large volume of dataExamplesFast compression and equations of stateRapid decompression and materials synthesisUltrafast (jump) compression for generating high strain rateCyclic (fast) de/compression for kinetics, relaxation, and rheology

12Fast compressionequation of state

Mo+MgOPressure apparatusmembraneLoading500 psi/s (Helium)P0 ~ 80 GPaPf ~ 210 GPaDt ~ 1.3 sCompression rate ~ 100 GPa/sDetectorDectris Pilatus1MExposure period 10 ms (100 Hz)Exposure time7 ms

13Fast compressionequation of state

High-frequency imaging yields acceptable signal-to-background ratioHigh-density data yields extremely robust equation of state

Average compression rate ~100 GPa/sPeak compression rate ~240 GPa/s14Fast compressionthermal EOS

WOW! Its an apple!15Fast compressionthermal EOS

Complete Mbar isotherm in a few secondsExternal heated DAC at HPCAT

16Fast decompressionmaterials synthesis

SiPressure apparatusmembrane + fast release Unloading1500-2000 psi (maximum rate)P0 ~ 20 GPaPf ~ 0 GPaDt ~ tens to hundreds of msDecompression rate ~ 20-2000 GPa/sDetectorDectris Pilatus1MExposure periodarbitraryExposure timearbitrary17Ultrafast (jump) compressionstrain rate

PtMo+MgOPressure apparatusdDACLoading1000 V (minimum rise time)P0 ~ 151 GPaPf ~ 194 GPaDt ~ 1.25 msCompression rate ~ 34 TPa/sDetectorDectris prototype (Eiger 1M)Exposure period 1.25 ms (800 Hz)Exposure time1.23 ms

BeforeAfter (Dt=1.25 ms)18Ultrafast (jump) compressionstrain rate

Strain rate on the order of 101 s-1Even on ms time scale, signal-to-background is useable, no sign of significant peak broadening19Fast, cyclic de/compression

PTime

20Fast, cyclic de/compression

Relaxation of the KCl sample under fast (de)compression Piezo drive FWHM of (200)

Fast compression experiments in radial diffraction geometry:KCl as an exampleRheologyDeformationRelaxation21Current challenges and future prospectsSelected Scientific challenges identified in 2012 Workshop Explore non-equilibrium transformations and phase boundariesElucidate dynamics, kinetics, and pathways of phase changesStudy system-dependent nucleation rates and crystal growthFuture prospectsOrder of magnitude flux increase leading to improved time resolutionReal-time pressure monitoring from x-ray markerClosed-loop dDAC operation for robust and repeatable P cyclingHigher frequency, greater sensitivity area detectors with better E resolutionTechnical challengesDiscrepancy between pressure loading and sample pressureLimitations in pressure range and cyclic repeatability of dDACTime-dependent response of pressure media and/or marker22Contributors and acknowledgmentsThis work was performed at HPCAT (Sector 16), Advanced Photon Source (APS), Argonne National Laboratory. HPCAToperations aresupported by DOE-NNSA under Award No. DE-NA0001974 andDOE-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: Chuanlong Lin, Eric Rod, Stanislav Sinogeikin, Guoyin ShenID-B staff : Yue Meng, Ross Hrubiak, Curtis Kenney-BensonUser 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 TomassinoSoftware Development: Przemek Dera23