Millisecond time-resolved synchrotron radiation X-ray diffraction and high-pressure rapid compression device and its application

At a Glance

Metadata	Details
Publication Date	2022-01-01
Journal	Acta Physica Sinica
Authors	Bihan Wang, Bing Li, Xuqiang Liu, Hao Wang, Sheng Jiang
Citations	1
Analysis	Full AI Review Included

Executive Summary

This analysis summarizes the development and performance of a millisecond time-resolved X-ray Diffraction (XRD) system integrated with a Dynamic Diamond Anvil Cell (dDAC) at the SSRF BL15U1 beamline, designed for non-equilibrium materials science.

Ultra-High Pressure Capability: The system successfully achieved pressures exceeding 300 GPa (up to 359 GPa) using 20 µm culets, pushing the limits of DAC technology for ultra-high pressure research (e.g., Rhenium EOS).
Extreme Compression Rate: Utilizing a piezoelectric actuator, the dDAC achieved rapid compression rates up to 13 TPa/s, bridging the experimental gap between static DAC and nanosecond shockwave experiments.
High-Speed Diagnostics: Time-resolved XRD is performed using a Pilatus 3X 900 K detector, providing a high frame rate of 500 Hz and a time resolution of 2 ms (1 ms exposure, 1 ms readout) for continuous structural monitoring.
Dual Actuation System: Two primary loading methods are implemented: gas membrane control (for high pressure range and controlled, slower rates, ~400 GPa/s) and piezoelectric actuation (for ultra-fast, high strain-rate experiments).
Non-Equilibrium Kinetics: The integrated system enables in-situ observation of structural phase transition kinetics (e.g., Ge phase transitions) and the formation of high-pressure metastable phases during rapid compression and decompression.
Micro-Focus Beam: The BL15U1 beamline provides a high-flux, monochromatic X-ray beam focused down to 2 µm x 2 µm, essential for obtaining usable diffraction signals from the minute DAC sample volume within milliseconds.

Technical Specifications

The following table details the key performance parameters and specifications of the dDAC and time-resolved XRD setup at SSRF BL15U1.

Parameter	Value	Unit	Context
Maximum Pressure Achieved	359	GPa	Piezo-driven dDAC (20 µm culet, Rhenium sample)
Maximum Compression Rate	13	TPa/s	Piezoelectric actuation (Single/Double barrel design)
Gas Membrane Compression Rate	~400	GPa/s	Gas-driven dDAC (Controlled rate)
XRD Detector Model	Pilatus 3X 900 K	N/A	High-frequency area detector
Time Resolution (Frame Rate)	2 (500 Hz)	ms	Exposure and readout time per frame
X-ray Energy Range	5-20	keV	Tunable monochromatic beam (Si(111) DCM)
Energy Resolution (∆E/E)	~1.5 x 10^-4	N/A	Monochromatic beam quality
Focused Spot Size	2 x 2	µm	Kirkpatrick-Baez (K-B) mirror system
Flux Density (at 20 keV)	~10¹⁰	photons/µm²/s	Required for millisecond data acquisition
Piezo Controller	PICA E-481.00	N/A	High-power controller (0-1100 V output)
Gas Controller	PACE 5000	N/A	Pressure range up to 3000 psi
DAC Culet Size (Ultra-high P)	20, 30	µm	Used in dynamic compression tests

Key Methodologies

The dynamic high-pressure experiments rely on the precise synchronization of rapid compression and high-speed X-ray data acquisition.

Micro-Focus Beam Delivery: The X-ray beam is conditioned using white beam slits (S1), a double crystal monochromator (DCM), and K-B mirrors to deliver a high-flux, 2 µm x 2 µm monochromatic spot onto the sample chamber.
Initial Static Loading: The DAC is pre-loaded to a starting pressure (P₀) using manual screws or controlled by the gas membrane pressure (0-30 psi pre-pressure required for the membrane).
dDAC Integration: The DAC is mounted within a customized steel assembly can, integrated with either the gas membrane system (PACE 5000 controller) or the piezoelectric stack system (PICA controller).
Actuator Control:
- Piezoelectric: Voltage waveforms (e.g., trapezoidal or triangular, 0-1000 V) are applied to the piezo stack to control the rapid extension/compression rate (up to 13 TPa/s).
- Gas Membrane: Controlled gas flow rate (up to 3000 psi) is used to inflate the membrane, pushing the DAC piston for dynamic loading (up to 400 GPa/s).
Synchronization and Acquisition: The Pilatus 3X 900 K detector is triggered to begin continuous data acquisition (500 Hz). Immediately following, the dDAC actuator is triggered to initiate the rapid compression event, ensuring the entire dynamic process is captured within the continuous recording window (up to tens of thousands of frames).
In-situ Pressure Calibration: Pressure is determined in real-time by fitting the diffraction peaks of a known material (e.g., Rhenium or NaCl) and applying its established Equation of State (EOS).
Data Analysis Pipeline: High-volume 2D diffraction data are rapidly processed via batch azimuthal integration (using tools like Dioptas) to generate 1D I-2θ patterns, which are then stacked (XRD time stacking diagram) to visualize structural evolution and kinetics over the millisecond timescale.

Commercial Applications

The ability to probe material structure under extreme, non-equilibrium conditions at high strain rates is critical for several advanced engineering and scientific fields.

Aerospace and Defense (Shock Physics):
- Characterizing the structural response and phase transition pathways of materials (metals, ceramics) subjected to high-strain-rate loading, relevant for modeling impact resistance and energetic material performance.
- Validating constitutive models used in hydrocodes and finite element analysis for dynamic events.
Advanced Materials Synthesis:
- Developing novel metastable materials (e.g., high-pressure phases of Ge or Si) that can only be formed or quenched under specific rapid compression/decompression pathways.
- Optimizing synthesis parameters for high P-T chemical reactions that occur rapidly or involve reactants that degrade quickly (e.g., H₂O or H₂ reacting with DAC components).
Geophysical Modeling and Energy Storage:
- Refining the Equations of State (EOS) for deep Earth and planetary materials (e.g., periclase, alloys) under dynamic compression, improving models of planetary interiors.
- Studying the dynamic behavior of materials relevant to high-density energy storage under rapid cycling conditions.
Fundamental Engineering Research:
- Investigating stress relaxation, strain-rate dependence, and kinetic barriers in polycrystalline materials, informing the design of high-strength alloys and composites.
- Rapidly acquiring P-V-T data points for materials, significantly accelerating the mapping of complex phase diagrams.

View Original Abstract

Non-equilibrium transition dynamics under high pressure depends on temperature, pressure and (de)compression rate. The studies require combination of time-resolved probe and rapid compression device on different time scales. Here we report the time-resolved X-ray diffraction (XRD) and dynamic diamond anvil cell (dDAC) system, which were recently developed at the BL15U1 beamline of Shanghai Synchrotron Radiation Facility (SSRF). There are two rapid loading methods for dDAC. One uses membrane control and the other is piezoelectric actuator driven dDAC. Both methods can dynamically compress the DAC sample chamber up to 300 GPa on millisecond scale (20 μm culet is used), and the time-resolved XRD data are obtained correspondingly. A new type of piezoelectric ceramic dDAC is designed with single-side drive or double-side drive, which allows us to realize extremely high pressure (above 300 GPa) with a fast compression rate of 13 TPa/s. During the rapid compression process, the X-ray diffraction spectra are collected continuously and simultaneously. The XRD detector is Pilatus 3X 900K, which has 2-ms resolution with 500 kHz frame rate. The millisecond time-resolved XRD and high pressure rapid compression system developed at BL15U1 of SSRF enrich the high-pressure experimental methods and enable the beamline to carry out ultra-high pressure experiments, non-equilibrium phase transition and relevant scientific researches.

Tech Support

Original Source

DOI: https://doi.org/10.7498/aps.71.20212360