Time-resolved X-ray Diffraction Research Articles

Metastable water at several compression rates and its freezing kinetics into ice VII

Water can be dynamically over-compressed well into the stability field of ice VII. Whether water then transforms into ice VII, vitreous ice or a metastable novel crystalline phase remained uncertain. We report here the freezing of over-compressed water to ice VII by time-resolved X-ray diffraction. Quasi-isothermal dynamic compression paths are achieved using a dynamic-piezo-Diamond-Anvil-Cell, with programmable pressure rise time from 0.1 ms to 100 ms. By combining the present data set with those obtained on various ns-dynamical platforms, a complete evolution of the solidification pressure of metastable water versus the compression rate is rationalized within the classical nucleation theory framework. Also, when crystallization into ice VII occurs in between 1.6 GPa and 2.0 GPa, that is in the stability field of ice VI, a structural evolution over few ms is then observed into a mixture of ice VI and ice VII that seems to resolve apparent contradictions between previous results.

Developing time-resolved x-ray diffraction diagnostics at the National Ignition Facility (invited).

As part of a program to measure phase transition timescales in materials under dynamic compression, we have designed new x-ray imaging diagnostics to record multiple x-ray diffraction measurements during a single laser-driven experiment. Our design places several ns-gated hybrid CMOS (hCMOS) sensors within a few cm of a laser-driven target. The sensors must be protected from an extremely harsh environment, including debris, electromagnetic pulses, and unconverted laser light. Another key challenge is reducing the x-ray background relative to the faint diffraction signal. Building on the success of our predecessor (Target Diffraction In Situ), we implemented a staged approach to platform development. First, we built a demonstration diagnostic (Gated Diffraction Development Diagnostic) with two hCMOS sensors to confirm we could adequately protect them from the harsh environment and also acquire acceptable diffraction data. This allowed the team to quickly assess the risks and address the most significant challenges. We also collected scientifically useful data during development. Leveraging what we learned, we recently developed a much more ambitious instrument (Flexible Imaging Diffraction Diagnostic for Laser Experiments) that can field up to eight hCMOS sensors in a flexible geometry and participate in back-to-back shots at the National Ignition Facility (NIF). The design also allows for future iterations, such as faster hCMOS sensors and an embedded x-ray streak camera. The enhanced capabilities of the new instrument required a much more complex design, and the unexpected issues encountered on the first few shots at NIF remind us that complexity has consequences. Our progress in addressing these challenges is described herein, as is our current focus on improving data quality by reducing x-ray background and quantifying the uncertainties of our diffraction measurements.

Combustion synthesis of the (Ti,Zr)B2-(Zr,Ti)C eutectic composites: Structure formation and properties

The macrokinetic characteristics of combustion of the quaternary Ti-Zr-B-C mixture as well as the mechanism and stages of phase formation for the synthesis products were investigated. The mechanical and thermophysical properties of the hot-pressed boride/carbide ceramics with eutectic composition (Ti,Zr)B2-43%at.(Zr,Ti)C were measured. Preliminary mechanical alloying (MA) of the (Zr + Ti) mixture was shown to yield Ti/Zr granules having a laminar structure and consisting of alternating layers of titanium, zirconium, and (Zr,Ti)ss solid solution. The method used to prepare reaction mixtures and the initial temperature T0 increased within the range of 20–370 °C have virtually no effect on combustion temperature, which is 2260–2400 °C, while higher T0 increases the combustion rate by a factor of 1.5–2. The use of MA Ti/Zr granules reduces the combustion rate as well as the specific heat release amount and the heat release rate. Time-resolved X-ray diffraction data showed that binary carbides (Zr1-xTix)C and diborides (Ti1-yZry)B2 of variable stoichiometry are formed in the combustion wave of the Ti-Zr-B-C reaction mixtures within less than 0.25 s. The carbide and diboride phases are formed simultaneously; the use of MA Ti/Zr granules in the reaction mixtures reduces the content of solid solutions of variable stoichiometry among the reaction products. The ceramics fabricated using a combination of combustion synthesis and hot pressing have a dense and homogeneous structure that consist of bonded grains of the diboride (Ti0.80Zr0.20)B2 and carbide (Zr0.83Ti0.17)C phases having the following properties: density, 5.3 g/cm3; hardness, 22.9 GPa; fracture toughness, 4.7 MPa m0.5; heat capacity, 0.52 J/(g·K); thermal diffusivity, 11.67 mm2/s; and thermal conductivity, 33.28 W/(m·K).

Dynamical decoding of the competition between charge density waves in a kagome superconductor

The kagome superconductor CsV3Sb5 hosts a variety of charge density wave (CDW) phases, which play a fundamental role in the formation of other exotic electronic instabilities. However, identifying the precise structure of these CDW phases and their intricate relationships remain the subject of intense debate, due to the lack of static probes that can distinguish the CDW phases with identical spatial periodicity. Here, we unveil the out-of-equilibrium competition between two coexisting 2 × 2 × 2 CDWs in CsV3Sb5 harnessing time-resolved X-ray diffraction. By analyzing the light-induced changes in the intensity of CDW superlattice peaks, we demonstrate the presence of both phases, each displaying a significantly different amount of melting upon excitation. The anomalous light-induced sharpening of peak width further shows that the phase that is more resistant to photo-excitation exhibits an increase in domain size at the expense of the other, thereby showcasing a hallmark of phase competition. Our results not only shed light on the interplay between the multiple CDW phases in CsV3Sb5, but also establish a non-equilibrium framework for comprehending complex phase relationships that are challenging to disentangle using static techniques.

Ice formation and its elimination in cryopreservation of oocytes

Damage from ice and potential toxicity of ice-inhibiting cryoprotective agents (CPAs) are key issues in assisted reproduction of humans, domestic and research animals, and endangered species using cryopreserved oocytes and embryos. The nature of ice formed in bovine oocytes (similar in size to oocytes of humans and most other mammals) after rapid cooling and during rapid warming was examined using synchrotron-based time-resolved x-ray diffraction. Using cooling rates, warming rates and CPA concentrations of current practice, oocytes show no ice after cooling but always develop large ice fractions—consistent with crystallization of most free water—during warming, so most ice-related damage must occur during warming. The detailed behavior of ice at warming depended on the nature of ice formed during cooling. Increasing cooling rates allows oocytes soaked as in current practice to remain essentially ice free during both cooling and warming. Much larger convective warming rates are demonstrated and will allow routine ice-free cryopreservation with smaller CPA concentrations. These results clarify the roles of cooling, warming, and CPA concentration in generating ice in oocytes and establish the structure and grain size of ice formed. Ice formation can be eliminated as a factor affecting post-warming oocyte viability and development in many species, improving outcomes and allowing other deleterious effects of the cryopreservation cycle to be independently studied.

A Time-Domain Perspective on the Structural and Electronic Response in Epitaxial Ferroelectric Thin Films on Silicon.

This operando study of epitaxial ferroelectric Pb(Zr0.48Ti0.52)O3 capacitors on silicon substrates studies their structural response via synchrotron-based time-resolved X-ray diffraction during hysteresis-loop measurements in the 2-200 kHz range. At high frequencies, the polarization hysteresis loop is rounded and the classical butterfly-like strain hysteresis acquires a flat dumbbell shape. We explain these observations from a time-domain perspective: The polarization and structural motion within the unit cell are coupled to the strain by the piezoelectric effect and limited by domain wall velocity. The solution of this coupled oscillator system is derived experimentally from the simultaneously measured electronic and structural data. The driving stress σFE(t) is calculated as the product of the measured voltage U(t) and polarization P(t). Unlike the electrical variables, σFE(t) and η(t) of the ferroelectric oscillate at twice the frequency of the applied electrical field. We model the measured frequency-dependent phase shift between η(t) and σFE(t).

Development of a laser-driven shock compression platform for time-resolved XRD experiments at the ID09 beamline of the European Synchrotron Radiation Facility

ABSTRACT We present a newly developed laser-driven shock compression platform at the ID09 beamline of the European Synchrotron Radiation Facility (ESRF). This platform combines a custom high-power EKSPLA laser with ESRF's high-energy X-ray pulses to perform in situ, time-resolved X-ray diffraction (XRD) measurements in materials under well characterized, moderate pressure (up to 1 Mbar) and short-duration shock waves. Its purpose is to serve as a shock driver to study materials under dynamic pressure, focusing on phase transitions in condensed matter. We provide a detailed description of this platform's design and functionalities, along with preliminary experimental results obtained from iron and tin samples subjected to shock compression. These results not only demonstrate the platform's ability to acquire high-quality X-ray diffraction data but also highlight its potential for advancing research in material science and high-energy-density physics.

Water Solvent Reorganization upon Ultrafast Resonant Stimulated X-ray Raman Excitation of a Metalloporphyrin Dimer.

We propose an X-ray Raman pump-X-ray diffraction probe scheme to follow solvation dynamics upon charge migration in a solute molecule. The X-ray Raman pump selectively prepares a valence electronic wavepacket in the solute, while the probe provides information about the entire molecular ensemble. A combination of molecular dynamics and ab initio quantum chemistry simulations is applied to a Zn-Ni porphyrin dimer in water. Using time-resolved X-ray diffraction and pair distribution functions, we extracted solvation shell dynamics.

Understanding charge transfer dynamics in blended positive electrodes for Li-ion batteries

This paper investigates the electrochemical behavior of binary blend electrodes comprising equivalent amounts of lithium-ion battery active materials, namely LiNi0.5Mn0.3Co0.2O2 (NMC), LiMn2O4 (LMO), LiFe0.35Mn0.65PO4 (LFMP) and LiFePO4 (LFP)), with a focus on decoupled electrochemical testing and operando X-ray diffraction (XRD). All possible 50:50 blend combinations were studied and the distribution of current between blend components was followed during continuous and pulsed charge and discharge processes. The results demonstrate the significant impact of the voltage profiles of individual materials on the current distribution, with the effective C-rate of each component varying throughout the State of Charge (SoC). Pulsed decoupled electrochemical testing reveals the exchange of charge between blend components during relaxation, showcasing the "buffer effect", which has also been captured through time-resolved operando XRD experiments in real blends carefully considering beam-induced effects. The directionality and magnitude of the charge transfer were found to depend on the nature of the components and the cell SoC, being also influenced by temperature. These dependencies can be rationalized considering both thermodynamics (voltage profile) and reaction kinetics of the blend constituents. These findings contribute to advancing the understanding of internal dynamics in blended electrodes, offering valuable insights for the rational design of blends to meet the diverse operational demands of lithium-ion batteries.

Functional protein dynamics in a crystal.

Proteins are molecular machines and to understand how they work, we need to understand how they move. New pump-probe time-resolved X-ray diffraction methods open up ways to initiate and observe protein motions with atomistic detail in crystals on biologically relevant timescales. However, practical limitations of these experiments demands parallel development of effective molecular dynamics approaches to accelerate progress and extract meaning. Here, we establish robust and accurate methods for simulating dynamics in protein crystals, a nontrivial process requiring careful attention to equilibration, environmental composition, and choice of force fields. With more than seven milliseconds of sampling of a single chain, we identify critical factors controlling agreement between simulation and experiments and show that simulated motions recapitulate ligand-induced conformational changes. This work enables a virtuous cycle between simulation and experiments for visualizing and understanding the basic functional motions of proteins.

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

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

Zeta Potential and Size Analysis of Zeolitic Imidazolate Framework-8 Nanocrystals Prepared by Surfactant-Assisted Synthesis.

The crystal nucleation and growth mechanism of monodispersed metal-organic framework nanoparticles were studied using time-resolved light dynamic, electrokinetic, and powder X-ray diffraction methods. We confirmed that zeolitic imidazolate framework-8 (ZIF-8) nanocrystals follow a nonclassical crystal growth pathway, where a fast nucleation occurs with dense liquid clusters or nanocrystals forming spontaneously when two precursors are mixed. We also explored the zeta potential and solvodynamic size changes of ZIF-8 prepared by a surfactant-assisted synthesis. Three modulators, including 1-methylimidazole (1-mIm), tris(hydroxymethyl)aminomethane (THAM), and (1-hexadecyl)trimethylammonium bromide (CTAB), were studied. We found that 1-mIm dramatically increases the rate of nucleation of ZIF-8. With an increasing amount of 1-mIm, which functions as a coordination modulator, the size increases, and the zeta potential of ZIF-8 decreases. Whereas THAM, as both a coordination and a deprotonation modulator, increases the size and zeta potential of ZIF-8 simultaneously, CTAB, as a long alkyl cationic surfactant, mainly adsorbs on the surface of ZIF-8, and the zeta potential of the formed ZIF-8 is controlled by the amount of CTAB in solution compared with its critical micelle concentration. Overall, we reveal that the modulator type and concentration can be used to control the size and zeta potential of the dispersed ZIF-8 nanocrystals in a colloid system. The experiments also enable identification of the nucleation and crystal growth processes of ZIF-8. The findings will be applicable to other nanocrystals in colloid systems, which are used for heterogeneous catalysis and guest molecular loadings.

Dehydration kinetics of nanoconfined water in beryl probed by high temperature single crystal synchrotron X-ray diffraction

Understanding changes in material properties through external stimuli plays a key role in validating the expected performance of materials and engineering material properties in a controlled manner. Here, we introduce a fundamental protocol to deduce dehydration reactions kinetics of water confined in nanopore channels, with the cyclosilicate beryl as the scaffold of interest, using time-resolved synchrotron X-ray diffraction (SXRD), in the temperature interval of 298–1038 K. The temperature-dependent intensity (I)\\documentclass[12pt]{minimal} \\usepackage{amsmath} \\usepackage{wasysym} \\usepackage{amsfonts} \\usepackage{amssymb} \\usepackage{amsbsy} \\usepackage{mathrsfs} \\usepackage{upgreek} \\setlength{\\oddsidemargin}{-69pt} \\begin{document}$$(I)$$\\end{document} of the strongest reflection (112) was used as the crystallite variable. An estimation of an isobaric thermal crystallite coefficient, k\\documentclass[12pt]{minimal} \\usepackage{amsmath} \\usepackage{wasysym} \\usepackage{amsfonts} \\usepackage{amssymb} \\usepackage{amsbsy} \\usepackage{mathrsfs} \\usepackage{upgreek} \\setlength{\\oddsidemargin}{-69pt} \\begin{document}$$k$$\\end{document}, analogous with the isobaric thermal expansion coefficient, established the rate of relative crystallization as a function of temperature, ∂I∂T\\documentclass[12pt]{minimal} \\usepackage{amsmath} \\usepackage{wasysym} \\usepackage{amsfonts} \\usepackage{amssymb} \\usepackage{amsbsy} \\usepackage{mathrsfs} \\usepackage{upgreek} \\setlength{\\oddsidemargin}{-69pt} \\begin{document}$$\\frac{\\partial I}{\\partial T}$$\\end{document}. A plot of lnk\\documentclass[12pt]{minimal} \\usepackage{amsmath} \\usepackage{wasysym} \\usepackage{amsfonts} \\usepackage{amssymb} \\usepackage{amsbsy} \\usepackage{mathrsfs} \\usepackage{upgreek} \\setlength{\\oddsidemargin}{-69pt} \\begin{document}$$lnk$$\\end{document} and 1T\\documentclass[12pt]{minimal} \\usepackage{amsmath} \\usepackage{wasysym} \\usepackage{amsfonts} \\usepackage{amssymb} \\usepackage{amsbsy} \\usepackage{mathrsfs} \\usepackage{upgreek} \\setlength{\\oddsidemargin}{-69pt} \\begin{document}$$\\frac{1}{T}$$\\end{document} gives rise to two kinetic steps, indicating a slow dehydration stage up to ~ 700 K and a fast dehydration stage up to the investigated temperature 1038 K. The crystal structure of beryl determined up to 1038 K, in temperature increment as small as 10 K, indicates the presence of channel ions Na and Fe and a gradual decrease of water upon heating.

Phase Formation during the Synthesis of the MAB Phase from Mo-Al-B Mixtures in the Thermal Explosion Mode.

This work focused on the production of the MoAlB MAB phase through self-propagating, high-temperature synthesis in the thermal explosion mode. The influence of the method of a Mo-Al-B-powder reaction mixture preparation on the combustion temperature, mechanism, and stages of the MAB phase formation in the combustion process was investigated. The combustion temperatures of the mixtures obtained in the rotary ball mill and high-speed planetary ball mill were 1234 and 992 °C, respectively. The formation of intermediate compounds Mo3Al8 and α-MoB in the combustion front, along with MoAlB, was established using the time-resolved X-ray diffraction method. In the case of the mixture prepared in a ball mill, the primary interaction in the combustion front occurred through the Al melt, and in the case of using a planetary mill, solid-phase reactions played an important role. The mechanical activation of the mixture in a planetary mill also accelerated the processes of phase formation. The method of a reaction mixture preparation has virtually no effect on the MoAlB MAB phase content in combustion products (92-94%), but it does affect their structure. The synthesis products have a lamellar structure composed of MAB grains with a thickness of ~0.4 μm and a length of ~2-10 μm.

Bioactive glass–ceramics containing fluorapatite, xonotlite, cuspidine and wollastonite form apatite faster than their corresponding glasses

Crystallisation of bioactive glasses has been claimed to negatively affect the ion release from bioactive glasses. Here, we compare ion release and mineralisation in Tris–HCl buffer solution for a series of glass–ceramics and their parent glasses in the system SiO2–CaO–P2O5–CaF2. Time-resolved X-ray diffraction analysis of glass–ceramic degradation, including quantification of crystal fractions by full pattern refinement, show that the glass–ceramics precipitated apatite faster than the corresponding glasses, in agreement with faster ion release from the glass–ceramics. Imaging by transmission electron microscopy and X-ray nano-computed tomography suggest that this accelerated degradation may be caused by the presence of nano-sized channels along the internal crystal/glassy matrix interfaces. In addition, the presence of crystalline fluorapatite in the glass–ceramics facilitated apatite nucleation and crystallisation during immersion. These results suggest that the popular view of bioactive glass crystallisation being a disadvantage for degradation, apatite formation and, subsequently, bioactivity may depend on the actual system study and, thus, has to be reconsidered.

Investigation of the mechanical work during ultrasonic fatigue loading using pulsed time-resolved X-ray diffraction.

In the energy production and transportation industries, numerous metallic structures may be subjected to at least several billions of cycles, i.e. loaded in the very high cycle fatigue domain (VHCF). Therefore, to design structures in the VHCF domain, a reliable methodology is necessary. One useful quantity to characterize plastic activity at the microscopic scale and fatigue damage evolution is the mechanical work supplied to a material. However, the estimation of this mechanical work in a metal during ultrasonic fatigue tests remains challenging. This paper aims to present an innovative methodology to quantify this. An experimental procedure was developed to estimate the mechanical work from stress and total strain evolution measurements during one loading cycle with a time accuracy of about 50 ns. This was achieved by conducting time-resolved X-ray diffraction coupled to strain gauge measurements at a synchrotron facility working in pulsed mode (single-bunch mode).

Time-resolved X-ray diffraction diagnostic development for the National Ignition Facility.

We present the development of an experimental platform that can collect four frames of x-ray diffraction data along a single line of sight during laser-driven, dynamic-compression experiments at the National Ignition Facility. The platform is comprised of a diagnostic imager built around ultrafast sensors with a 2-ns integration time, a custom target assembly that serves also to shield the imager, and a 10-ns duration, quasi-monochromatic x-ray source produced by laser-generated plasma. We demonstrate the performance with diffraction data for Pb ramp compressed to 150GPa and illuminated by a Ge x-ray source that produces ∼7 × 1011, 10.25-keV photons/ns at the 400μm diameter sample.

A modular table-top setup for ultrafast x-ray diffraction.

We present a table-top setup for femtosecond time-resolved x-ray diffraction based on a Cu Kα (8.05keV) laser driven plasma x-ray source. Due to its modular design, it provides high accessibility to its individual components (e.g., x-ray optics and sample environment). The Kα-yield of the source is optimized using a pre-pulse scheme. A magnifying multilayer x-ray mirror with Montel-Helios geometry is used to collect the emitted radiation, resulting in a quasi-collimated flux of more than 105 Cu Kα photons/pulse impinging on the sample under investigation at a repetition rate of 10Hz. A gas ionization chamber detector is placed right after the x-ray mirror and used for the normalization of the diffraction signals, enabling the measurement of relative signal changes of less than 1% even at the given low repetition rate. Time-resolved diffraction experiments on laser-excited epitaxial Bi films serve as an example to demonstrate the capabilities of the setup. The setup can also be used for Debye-Scherrer type measurements on poly-crystalline samples.

Probing the Effect of Environments on the Stability of Ni2P Nanoparticle Electrocatalysts

Ni2P has been shown to be an effective catalyst for the hydrogen evolution reaction (HER), making it a promising replacement for Pt which is the current state of the art HER catalyst.1,2 H2 is a clean-energy critical fuel and chemical highlighted by the US Department of Energy’s “Hydrogen Shot,” which seeks to reduce “the cost of carbon-neutral hydrogen by 80% to $1 per 1 kg in 1 decade, highlighting the key role of hydrogen in implementing carbon-neutral solutions.”3 Ni2P is also a good or promising catalyst for other reactions, such as alcohol oxidation, hydrodesulfurization,4,5 nitrate reduction, and oxygen evolution reaction.6 However, Ni2P and other TMPs are susceptible to oxidation, which can lead to catalyst degradation and loss in certain conditions.7,8 Stability is an important part of catalysis, especially for achieving the goals of the Hydrogen Shot. Therefore, it is important to understand complex degradation mechanisms in order to better understand structure-activity relationships in these materials. In the present work, in situ Ni K-edge X-ray absorption spectroscopy (XAS) and ex situ P Kα and Kβ X-ray emission spectroscopy (XES) couple together to understand the degradation of Ni2P and show the effects of electrolyte pH, ligands, and air on Ni2P nanoparticles.5 nm Ni2P nanoparticles were synthesized by heating NiCl2 and tris(diethylamino)phosphine in oleylamine. The nanoparticles were drop cast onto carbon fiber paper electrodes and Si wafers or Au-coated wafers for P Kα and Kβ XES. Oleylamine ligands are removed by thermal annealing. Electrochemical experiments were conducted with a three-electrode cell using carbon fiber paper or Au-coated wafers deposited with Ni2P nanoparticles as working electrode, Ag/AgCl calibrated to the H2 redox couple as reference electrode, and graphite rod as counter electrode. P Kα and Kβ XES experiments were conducted inside a N2 glovebox to prevent unintentional air oxidation. Transmission-mode Ni K-edge XAS was conducted on a benchtop spectrometer.Upon exposure to air, as-synthesized Ni2P nanoparticles were studied via P Kα and Kβ XES. Results showed that the phosphide species converted to phosphate with analysis of intermediates well fit by a simple two-phase mixture. Phosphide:phosphate ratios were quantified using linear combination analysis, providing a powerful tool to analyze P speciation on various samples in an inert environment and with minimal loss of material, both advantages of this system over 31P magic angle spinning solid state nuclear magnetic resonance spectroscopy and X-ray photoelectron spectroscopy. Continued work looks at analyzing the effects of the ligand environment on the stability of nanoparticles in electrolytes spanning from acidic to basic pH. We hypothesize that ligands will significantly stabilize the nanoparticles against corrosion and that without ligands Ni2P readily converts to a nickel phosphate species upon exposure to electrolyte.References(1) Popczun, E. J.; McKone, J. R.; Read, C. G.; Biacchi, A. J.; Wiltrout, A. M.; Lewis, N. S.; Schaak, R. E. Nanostructured Nickel Phosphide as an Electrocatalyst for the Hydrogen Evolution Reaction. J. Am. Chem. Soc. 2013, 135 (25), 9267–9270. https://doi.org/10.1021/ja403440e.(2) Liu, P.; Rodriguez, J. A. Catalysts for Hydrogen Evolution from the [NiFe] Hydrogenase to the Ni2P(001) Surface: The Importance of Ensemble Effect. J. Am. Chem. Soc. 2005, 127 (42), 14871–14878. https://doi.org/10.1021/ja0540019.(3) Bullock, M.; More, K. Basic Energy Sciences Roundtable: Foundational Science for Carbon-Neutral Hydrogen Technologies (Report); DOESC Office of Basic Energy Sciences, 2022. https://doi.org/10.2172/1834317.(4) Layan Savithra, G. H.; Muthuswamy, E.; Bowker, R. H.; Carrillo, B. A.; Bussell, M. E.; Brock, S. L. Rational Design of Nickel Phosphide Hydrodesulfurization Catalysts: Controlling Particle Size and Preventing Sintering. Chem. Mater. 2013, 25 (6), 825–833. https://doi.org/10.1021/cm302680j.(5) Rodriguez, J. A.; Kim, J.-Y.; Hanson, J. C.; Sawhill, S. J.; Bussell, M. E. Physical and Chemical Properties of MoP, Ni2P, and MoNiP Hydrodesulfurization Catalysts: Time-Resolved X-Ray Diffraction, Density Functional, and Hydrodesulfurization Activity Studies. J. Phys. Chem. B 2003, 107 (26), 6276–6285. https://doi.org/10.1021/jp022639q.(6) Menezes, P. W.; Indra, A.; Das, C.; Walter, C.; Göbel, C.; Gutkin, V.; Schmeiβer, D.; Driess, M. Uncovering the Nature of Active Species of Nickel Phosphide Catalysts in High-Performance Electrochemical Overall Water Splitting. ACS Catal. 2017, 7 (1), 103–109. https://doi.org/10.1021/acscatal.6b02666.(7) Ha, D.-H.; Han, B.; Risch, M.; Giordano, L.; Yao, K. P. C.; Karayaylali, P.; Shao-Horn, Y. Activity and Stability of Cobalt Phosphides for Hydrogen Evolution upon Water Splitting. Nano Energy 2016, 29, 37–45. https://doi.org/10.1016/j.nanoen.2016.04.034.(8) Parra-Puerto, A.; Ng, K. L.; Fahy, K.; Goode, A. E.; Ryan, M. P.; Kucernak, A. Supported Transition Metal Phosphides: Activity Survey for HER, ORR, OER, and Corrosion Resistance in Acid and Alkaline Electrolytes. ACS Catal. 2019, 11515–11529. https://doi.org/10.1021/acscatal.9b03359.

Bayesian Framework for Analyzing Adsorption Processes Observed via Time-Resolved X-ray Diffraction

Bayesian Framework for Analyzing Adsorption Processes Observed via Time-Resolved X-ray Diffraction