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At least 1,063 records · Page 59

Multimode scanning X-ray diffraction microscopy for diamond anvil cell experiments

We have designed and implemented a new experimental system for fast mapping of crystal structures and other structural features of materials under high pressure at the High Pressure Collaborative Access Team, Sector 16 of the Advanced Photon Source. The system utilizes scanning X-ray diffraction microscopy (SXDM) and is optimized for use with diamond anvil cell devices. In SXDM, the X-ray diffraction (XRD) is collected in a forward scattering geometry from points on a two-dimensional grid by fly-scanning the sample with respect to a micro-focused X-ray beam. The recording of XRD is made during the continuous motion of the sample using a fast (millisecond) X-ray area detector in synchrony with the sample positioners, resulting in a highly efficient data collection for SXDM. A new computer program, X-ray Diffractive Imaging (XDI), has been developed with the SXDM system. The XDI program provides a graphical interface for constructing and displaying the SXDM images in several modes: (1) phase mapping based on structural information, (2) pressure visualization based on the equation of state, (3) microstructural features mapping based on peak shape parameters, and (4) grain size and preferred-orientation based on peak shape parameters. The XDI is a standalone program and can be generally used for displaying SXDM images. Two examples of iron and zirconium samples under high pressure are presented to demonstrate the applications of SXDM. Published under license by AIP Publishing.

47 OTHER INSTRUMENTATION↗

Mean transverse energy of ultrananocrystalline diamond photocathode

Nitrogen incorporated ultrananocrystalline diamond [(N)UNCD] could be an enabling material platform for injector photocathode applications due to its high emissivity. While the quantum efficiency (QE) of UNCD was reported by many groups, no experimental measurements of the intrinsic emittance/mean transverse energy (MTE) have been reported. Here, MTE measurement results for an (N)UNCD photocathode in the photon energy range from 4.41 to 5.26 eV are described. The MTE demonstrates no noticeable dependence on the photon energy, with an average value of 266 meV. This spectral behavior is shown not to be dependent upon physical or chemical surface roughness and inconsistent with low electron effective mass emission from graphitic grain boundaries but may be associated with emission from spatially confined states in the grain boundaries. Lastly, the combined effect of low and constant MTE and high QE, which increases with respect to the excess laser energy, may pave the way for bright UNCD photocathodes for electron injectors.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

An improved setup for radial diffraction experiments at high pressures and high temperatures in a resistive graphite-heated diamond anvil cell

We present an improved setup for the experimental study of deformation of solids at simultaneous high pressures and temperatures by radial x-ray diffraction. This technique employs a graphite resistive heated Mao–Bell type diamond anvil cell for radial x-ray diffraction in combination with a water-cooled vacuum chamber. The new chamber has been developed by the sample environment group at PETRA III and implemented at the Extreme Conditions Beamline P02.2 at PETRA III, DESY (Hamburg, Germany). Here, we discuss applications of the new setup to study deformation of a variety of materials, including ferropericlase, calcium perovskite, bridgmanite, and tantalum carbide, at high-pressure/temperature.

47 OTHER INSTRUMENTATION↗

Direct formation of nitrogen-vacancy centers in nitrogen doped diamond along the trajectories of swift heavy ions

We report depth-resolved photoluminescence measurements of nitrogen-vacancy (NV$^-$) centers formed along the tracks of swift heavy ions in type Ib synthetic single crystal diamonds that had been doped with 100 ppm nitrogen during crystal growth. Analysis of the spectra shows that NV$^-$ centers are formed preferentially within regions where electronic stopping processes dominate and not at the end of the ion range where elastic collisions lead to formation of vacancies and defects. Thermal annealing further increases NV yields after irradiation with SHI preferentially in regions with high vacancy densities. NV centers formed along the tracks of single swift heavy ions can be isolated with lift-out techniques for explorations of color center qubits in quasi 1D registers with average qubit spacing of a few nm and of order 100 color centers per micron along 10 to 30 micron long percolation chains.

72 PHYSICS OF ELEMENTARY PARTICLES AND FIELDS↗

Simultaneous imaging and diffraction in the dynamic diamond anvil cell

The ability to visualize a sample undergoing a pressure-induced phase transition allows for the determination of kinetic parameters, such as the nucleation and growth rates of the high-pressure phase. For samples that are opaque to visible light (such as metallic systems), it is necessary to rely on x-ray imaging methods for sample visualization. Here, we present an experimental platform developed at beamline P02.2 at the PETRA III synchrotron radiation source, which is capable of performing simultaneous x-ray imaging and diffraction of samples that are dynamically compressed in piezo-driven diamond anvil cells. This setup utilizes a partially coherent monochromatic x-ray beam to perform lensless phase contrast imaging, which can be carried out using either a parallel- or focused-beam configuration. The capabilities of this platform are illustrated by experiments on dynamically compressed Ga and Ar. Melting and solidification were identified based on the observation of solid/liquid phase boundaries in the x-ray images and corresponding changes in the x-ray diffraction patterns collected during the transition, with significant edge enhancement observed in the x-ray images collected using the focused-beam. These results highlight the suitability of this technique for a variety of purposes, including melt curve determination.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Space charge limited corrections to the power figure of merit for diamond

An interpretation of the unipolar figure of merit is formulated for wide bandgap (WBG) semiconductors based on the on-state specific resistance (RON,sp) derived from the space charge limited current–voltage relationship (Mott–Gurney square law). The limitations of the traditional Ohmic R ON,sp for WBG semiconductors are discussed, particularly at low doping, while the accuracy of the Mott–Gurney based R ON,sp is confirmed by Silvaco ATLAS drift–diffusion simulations of diamond Schottky pin diodes. The effects of incomplete ionization are considered as well.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Yield strength of CeO 2 measured from static compression in a radial diamond anvil cell

Cerium oxide (ceria, CeO 2 ) is frequently used as a standard in applications such as synchrotron and x-ray free electron lasers for calibrating x-ray wavelengths and offers the potential for understanding the high pressure properties and deformation mechanisms in a wide range of similar face centered cubic (fcc) materials. In this study, the pressure dependence of the strength of ceria was investigated up to 38 GPa using angle dispersive x-ray diffraction in a radial geometry in a diamond anvil cell. In this experiment, the difference in the stress along the axis of compression and perpendicular to the direction of compression can be determined, giving a quantity known as the differential stress. It was found that the differential stress (t), a measure of the lower bound for yield strength, initially increases rapidly from 0.35 ± 0.06 GPa to 2.2 ± 0.4 GPa at pressures of 1.8 and 3.8 GPa, respectively. Above 4 GPa, t increases more slowly to 13.8 ± 2.6 GPa at a pressure of 38 GPa. The changes in the preferred orientation (texture) of CeO 2 with pressure were also measured, allowing for the determination of active deformation mechanisms using an elasto-viscoplastic self-consistent model (EVPSC). It was found that as pressure increased, the [001] direction had a slight preferred orientation along the axis of compression. Our EVPSC model of experimental fiber (cylindrically symmetric) textures and lattice strains were most consistent with dominant slip activity along ${111}$ $\langle$$1\bar10$$\rangle$.

36 MATERIALS SCIENCE↗

Combining femtosecond laser annealing and shallow ion implantation for local color center creation in diamond

A common technique for color center creation in wideband gap semiconductors employs ion implantation and a subsequent thermal annealing. In general, this annealing process is conducted in a vacuum oven. Here, we exploit the annealing based on femtosecond laser pulses. For that purpose, we implant fluorine ions at 54 keV and chlorine ions at 74 keV in diamond and perform micrometer precise annealing using focused femtosecond laser pulses at 800 ± (30) nm with different pulse numbers and repetition rates. In this way, we were able to create shallow spots with color centers of varying brightness.

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Simultaneous measurements of volume, pressure, optical images, and crystal structure with a dynamic diamond anvil cell: A real-time event monitoring system

The dynamic diamond anvil cell (dDAC) technique has attracted great interest because it possibly provides a bridge between static and dynamic compression studies with fast, repeatable, and controllable compression rates. The dDAC can be a particularly useful tool to study the pathways and kinetics of phase transitions under dynamic pressurization if simultaneous measurements of physical quantities are possible as a function of time. We report the development of a real-time event monitoring (RTEM) system with dDAC, which can simultaneously record the volume, pressure, optical image, and structure of materials during dynamic compression runs. In particular, the volume measurement using both Fabry–Pérot interferogram and optical images facilitates the construction of an equation of state (EoS) using the dDAC in a home-laboratory. We also developed an in-line ruby pressure measurement (IRPM) system to be deployed at a synchrotron x-ray facility. This system provides simultaneous measurements of pressure and x-ray diffraction in low and narrow pressure ranges. The EoSs of ice VI obtained from the RTEM and the x-ray diffraction data with the IRPM are consistent with each other. The complementarity of both RTEM and IRPM systems will provide a great opportunity to scrutinize the detailed kinetic pathways of phase transitions using dDAC.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

New dynamic diamond anvil cell for time-resolved radial x-ray diffraction

The dynamic diamond anvil cell (dDAC) is a recently developed experimental platform that has shown promise for studying the behavior of materials at strain rates ranging from intermediate to quasi-static and shock compression regimes. Combining dDAC with time-resolved x-ray diffraction (XRD) in the radial geometry (i.e., with incident x-rays perpendicular to the axis of compression) enables the study of material properties such as strength, texture evolution, and deformation mechanisms. This work describes a radial XRD dDAC setup at beamline P02.2 (Extreme Conditions Beamline) at DESY’s PETRA III synchrotron. Time-resolved radial XRD data are collected for titanium, zirconium, and zircon samples, demonstrating the ability to study the strength and texture of materials at compression rates above 300 GPa/s. In addition, the simultaneous optical imaging of the DAC sample chamber is demonstrated. The ability to conduct simultaneous radial XRD and optical imaging provides the opportunity to characterize plastic strain and deviatoric strain rates in the DAC at intermediate rates, exploring the strength and deformation mechanisms of materials in this regime.

47 OTHER INSTRUMENTATION↗

Magnetometry in a diamond anvil cell using nitrogen vacancy centers in a nanodiamond ensemble

The emerging field of optical magnetometry utilizing negative-charged nitrogen vacancy (NV – ) centers provides a highly sensitive lab bench technique for spatially resolved physical property measurements. Their implementation in high pressure diamond anvil cell (DAC) environments will become common as other techniques are often limited due to the spatial constraints of the sample chamber. Apparatus and techniques are described here permitting for more general use of magnetic field measurements inside a DAC using continuous wave optical detected magnetic resonance in NV – centers in a layer of nanodiamonds. A microstrip antenna delivers a uniform microwave field to the DAC and is compatible with simple metal gaskets, and the sensor layer of deposited nanodiamonds allows for simple determination of the magnetic field magnitude for B in the 1–100 G range. The ferromagnetic transition in iron at 18 GPa is measured with the apparatus, along with its hysteretic response.

75 CONDENSED MATTER PHYSICS, SUPERCONDUCTIVITY AND↗

Enhancement to the conductivity of surface transfer-doped (111) diamond through thermochemical surface etching

The use of a transition metal catalyzed thermochemical etching method for improving the carrier transport properties of the near-surface two-dimensional (2D) hole gas in surface transfer-doped hydrogen-terminated (111) diamond is demonstrated. Using Ni 0.8 Cr 0.2 films deposited and annealed to a temperature of 900 °C, with up to three etch cycles, preferential (111) surface etching produces large terraces exceeding 10 μm in size with a surface microroughness, σ 2 RMS λ, that is two orders of magnitude lower than for the pre-etched (111) surface. Magnetotransport measurements on hydrogen-terminated Hall bars engineered on the pre- and post-etched surfaces and rendered conductive by the adsorbed water layer formed on exposure to ambient conditions demonstrate that this etching causes an improvement in the hole mobility by an order of magnitude, resulting in a measured sheet resistivity of 1.04 kΩ/sq at a temperature of 4.2 K without gating.

42 ENGINEERING↗

Metrology for femtosecond pulsed x-ray heating in diamond anvil cell experiments at the European XFEL: Revisiting the iron phase diagram up to 150 GPa

The development of pulsed intense x-ray sources, such as free electron laser, offers new avenues for high pressure experiments. Here, we study the feasibility and metrology of x-ray heating in diamond anvil cells at the European x-ray free electron laser. This method enables one to volumetrically heat the sample while inhibiting chemical migration and probing the crystallographic structure of the sample throughout the heating with a high repetition rate. We focus our study on iron, whose phase diagram is well established up to 100 GPa, to explore the possibilities and limitations of this technique. We volumetrically heat iron samples at starting pressures ranging from 10 to 138 GPa, using the x-ray beam pulsed at 4.5 MHz in a serial pump-and-probe experimental design. Experimental challenges arise from temperature gradients within the sample, changes in temperature at the 100 ns timescale, the difficulty of direct temperature estimates, the effect of thermal pressure, and the presence of metastable crystallites due to rapid cycles of heating and cooling. Hence, we develop a multi-crystal-like data processing method that allows us to account for sample heterogeneity in probed conditions. We then calibrate our measurements using known physical properties of iron under pressure. Thermal pressure in our experiments increases from 4% of the isochoric prediction at 10 GPa to 23% at 138 GPa, and we show that our data are in agreement with most previous observations of iron in this pressure range. The method can now be implemented at higher pressures and temperatures and on materials with unknown phase diagrams.

Materials science↗

Hyperspectral radiance mapping and chromatic correction for temperature measurement in laser-heated diamond anvil cells

In laser-heated diamond anvil cell (DAC) experiments, the effective heated region typically decreases in size with increasing pressure, leading to steeper thermal gradients. Under these conditions, chromatic aberration in the optical path from sample to detector can significantly create bias in spectro-radiometric temperature measurement. We present a radiance-mapping approach using a hyperspectral camera that records 25 spectral channels spanning 605–875 nm at each pixel in a single exposure, providing spatially and spectrally resolved radiance in each frame. This enables chromatic effects to be recorded and corrected in data processing. We developed a procedure for hyperspectral mapping, involving per-camera calibration, crosstalk removal, measured spectral throughput functions, and optional sub-pixel co-registration to minimize chromatic distortion. The calibrated radiance maps are then used to derive temperature maps of the laser-heated hotspots. For smaller heating spots, the radiance mapping approach reveals chromatic shifts that conventional spectro-radiometric methods cannot quantify. Ambient-pressure heating experiments confirm accurate temperature retrieval. At high pressure, application of the hyperspectral system to a platinum-heating experiment at 12 GPa demonstrates stable temperature reconstruction under steep thermal gradients. Beyond mitigating chromatic aberrations, the ability to diagnose optical artifacts separately from emissivity variations during controlled test experiments or in situ suggests a path toward more rigorous spectral emissivity analysis and improved modeling of thermal transport in laser-heated DAC experiments.

47 OTHER INSTRUMENTATION↗

Anomalous lattice expansion of bcc Ta in helium-loaded diamond anvil cells

Anomalous lattice expansion of bcc Ta is observed in helium-loaded diamond anvil cell (DAC) experiments near 6 GPa and above 400 K, while co-loaded W, Mo, and Au exhibit normal thermal expansion. The Ta volume expansion increases with temperature, reaching ~14% near 650 K before plateauing, and is largely retained after recovery to ambient conditions. Time-resolved measurements at 500 K reveal progressive expansion over several hours, consistent with gradual, thermally activated He incorporation. The largely retained expansion during subsequent cooling and holding at 400 K indicates that the incorporated He is predominantly kinetically trapped. The data reveal two distinct regimes: below ~550 K, modest and spatially uniform expansion consistent with interstitial He trapping at isolated, randomly distributed vacancies; above ~550 K, He-vacancy cluster growth producing dramatically larger expansion, peak broadening, and a core–shell microstructure revealed by micron-resolution X-ray diffraction mapping. These results demonstrate that He is not always a passive pressure medium in DAC experiments and reveal a previously unrecognized regime of He-mediated lattice modification in Ta, complementing conventional ion-implantation studies relevant to nuclear and fusion structural materials.

Diamond anvil cell↗

Diamond Raman laser emitting at 1194, 1419, and 597 nm

A Raman laser based on a synthetic diamond crystal pumped by nanosecond pulses of a 1030-nm Yb : YAG laser and emitting in the IR region at the first and second Stokes wavelengths of 1194 and 1419 nm, respectively, was developed. The conversion efficiency was 34 % with a slope efficiency of 50 % and an average power of 1.1 W at a wavelength of 1194 nm; the average power at 1419 nm was 0.52 W. Frequency doubling of the first Stokes component in a nonlinear BBO crystal resulted in orange (597.3 nm) radiation with a pulse energy of 0.15 mJ, an average power of 0.22 W, and a maximum efficiency of 20 %. (paper)

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗

Optical properties of laser-modified diamond: From visible to microwave range

We have measured the optical properties of a graphitised layer with dc conductivity of 305 Ω{sup −1} cm{sup −1} produced by excimer laser irradiation (KrF, τ = 20 ns, λ = 248 nm) of a polycrystalline diamond surface grown by chemical vapour deposition. Studies have been conducted in a wide range of wavelengths: from far-IR to visible spectral regions. The resulting constants of the Drude model are the basic parameters for calculating the electromagnetic response of diamond/graphite photon elements or metamaterials fabricated using the direct laser writing method. (paper)

71 CLASSICAL AND QUANTUM MECHANICS, GENERAL PHYSIC↗