An in-situ heater for the XAS beamline (12-ID) in Australia

Johannessen, Bernt; Hussain, Zakria; East, Daniel; Gibson, Mark

doi:10.1088/1742-6596/430/1/012119

Cited by 3 publications

(6 citation statements)

References 11 publications

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“…X-ray absorption near edge structure (XANES) spectra were collected at the U L 3 -edge on beamline 12 at the Australian Synchrotron . 2.7 mg of α-SrUO 4 was mixed thoroughly with 4.4 mg of BN, and the uniform mixture was loaded into a 2 mm diameter quartz capillary (∼6 mm in length) and placed into a water cooled Linkam TS1500 heating stage operating in an argon atmosphere . The measurements were performed in transmission mode using argon-filled ionization chambers at temperatures between room temperature and 900 °C.…”

Section: Methodsmentioning

confidence: 99%

“…23 2.7 mg of α-SrUO 4 was mixed thoroughly with 4.4 mg of BN, and the uniform mixture was loaded into a 2 mm diameter quartz capillary (∼6 mm in length) and placed into a water cooled Linkam TS1500 heating stage operating in an argon atmosphere. 24 The measurements were performed in transmission mode using argonfilled ionization chambers at temperatures between room temperature and 900 °C. The heating rate was set at 30 °C/min, and the sample was given at least 10 min of soak time before each measurement.…”

Section: ■ Experimental Sectionmentioning

confidence: 99%

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Nonstoichiometry in Strontium Uranium Oxide: Understanding the Rhombohedral–Orthorhombic Transition in SrUO₄

et al. 2016

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In situ neutron and synchrotron X-ray diffraction studies demonstrate that SrUO4 acts as an oxygen transfer agent, forming oxygen vacancies under both oxidizing and reducing conditions. Two polymorphs of SrUO4 are stable at room temperature, and the transformation between these is observed to be associated with thermally regulated diffusion of oxygen ions, with partial reduction of the U(6+) playing a role in both the formation of oxygen deficient α-SrUO4-δ and its subsequent transformation to stoichiometric β-SrUO4. This is supported by ab initio calculations using density functional theory calculations. The oxygen vacancies play a critical role in the first order transition that SrUO4 undergoes near 830 °C. The changes in the oxidation states and U geometry associated with the structural phase transition have been characterized using X-ray absorption spectroscopy, synchrotron X-ray diffraction, and neutron diffraction.

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Section: Methodsmentioning

confidence: 99%

Section: ■ Experimental Sectionmentioning

confidence: 99%

Nonstoichiometry in Strontium Uranium Oxide: Understanding the Rhombohedral–Orthorhombic Transition in SrUO₄

et al. 2016

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“…[46] In addition to the electrocatalytic reactions, the in situ XAFS spectra are also used for detecting the electronic structure catalysts during heterogeneous catalysis, such as the preferential oxidation of CO in hydrogen (PROX) reaction (Figure 5b). [48] Prof. Lu and co-workers investigated the electronic structure of isolated Fe(OH) x on Pt/SiO 2 under realistic reaction conditions by in situ XAFS (Figure 5c-f). [49] In this case the catalyst was first pressed into a sample pellet and was then loaded into a homemade quartz reaction cell, where Kapton foil was used as the X-ray window material.…”

Section: In Situ Techniquesmentioning

confidence: 99%

Section: Analytical Spectroscopy For Sacsmentioning

confidence: 99%

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Emerging Applications of Synchrotron Radiation X‐Ray Techniques in Single Atomic Catalysts

Song

Davis

et al. 2022

Small Methods

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spectral range, linearly polarized light, and high collimation. At present, several different typical characterization methods of synchronizing radiation are developed, including X-ray diffraction (XRD), smallangle X-ray scattering (SAXS), X-ray biological macromolecular structure analysis, X-ray absorption spectrum fine structure (XAFS), X-ray magnetic circular dichroism (XMCD) technique, X-ray fluorescence analysis (XRF), X-ray imaging technique, vacuum ultraviolet photoionization mass spectrometry technology, photoelectric emission technology, angle-resolved photoelectron spectroscopy (ARPES), etc. [2,3] The application of synchrotron radiation theory and experimental technique has promoted the development of physics, chemistry, biology, materials, environmental science, and other research areas. Many important scientific and technological advances have been completed on the interdisciplinary platform of synchrotron radiation devices. [4,5] For example, Ramakrishnan, Steitz and Yonath successfully mapped the 3D positions of ribosome atoms using synchrotron radiation X-ray protein crystallography when studying the structure and function of ribosomes, and they won the Nobel prize in chemistry in 2009. Shi et al. from Tsinghua University have made use of synchrotron radiation X-ray crystallography and biological macromolecular structure analysis techniques to develop a series of advances in the study of apoptosis and transport proteins. [6,7] In addition, synchrotron radiation also plays an irreplaceable role in the development of advanced Single atom catalysts (SACs) can achieve a maximum atom utilization efficiency of 100%, which provides significantly increased active sites compared with traditional catalysts during catalytic reactions. Synchrotron radiation technology is an important characterization method for identifying singleatom catalysts. Several types of internal information, such as the coordination number, bond length and electronic structure of metals, can all be analyzed. This review will focus on the introduction of synchrotron radiation techniques and their applications in SACs. First, the fundamentals of synchrotron radiation and the corresponding techniques applied in characterization of SACs will be briefly introduced, such as X-ray absorption near edge spectroscopy and extended X-ray absorption fine structure spectroscopy and in situ techniques. The detailed information obtained from synchrotron radiation X-ray characterization is described through four routes: 1) the local environment of a specific atom; 2) the oxidation state of SACs; 3) electronic structures at different orbitals; and 4) the in situ structure modification during catalytic reaction. In addition, a systematic summary of synchrotron radiation X-ray characterization on different types of SACs (noble metals and transition metals) will be discussed.The ORCID identification number(s) for the author(s) of this article can be found under https://doi.org/10.1002/smtd.202201078.

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In situ high temperature powder x-ray diffraction technique using a sapphire single-crystal flat cell

Kobayashi,

Kawaguchi,

Yamada

2023

Review of Scientific Instruments

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Understanding the behaviors of materials in their operating and manufacturing environments is essential not only in the scientific field, but also in the context of designing industrial materials for target applications. In this study, we developed a high-temperature x-ray diffraction (XRD) system, using a small microscope heating stage at the BL02B2 beamline in SPring-8. Newly designed sample cells composed of sapphire single crystals were employed to perform XRD experiments using powdered samples at high temperatures and under oxidization/reduction gas atmospheres, with a short sample exchange time. More specifically, XRD experiments were conducted under vacuum, air, inert gas (maximum temperature: ∼1400 °C), and reduction gas flow conditions (maximum temperature: ∼900 °C). In addition, to monitor the changes in the exhausted gas composition during the chemical reactions, the developed heating system was combined with in situ gas-analysis tools (a remote gas-pressure control system, gas chromatograph, and mass spectrometer), which allowed analysis of the gas-adsorption/desorption and solid–gas reaction processes. Several heating experiments, such as the observation of the reduction of Fe oxides, phase transitions of ZrO2 and BaCO3, and synthesis of BaZrO3, demonstrated the validity and usefulness of this system.

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An in-situ heater for the XAS beamline (12-ID) in Australia

Cited by 3 publications

References 11 publications

Nonstoichiometry in Strontium Uranium Oxide: Understanding the Rhombohedral–Orthorhombic Transition in SrUO₄

Nonstoichiometry in Strontium Uranium Oxide: Understanding the Rhombohedral–Orthorhombic Transition in SrUO₄

Emerging Applications of Synchrotron Radiation X‐Ray Techniques in Single Atomic Catalysts

In situ high temperature powder x-ray diffraction technique using a sapphire single-crystal flat cell

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An in-situ heater for the XAS beamline (12-ID) in Australia

Cited by 3 publications

References 11 publications

Nonstoichiometry in Strontium Uranium Oxide: Understanding the Rhombohedral–Orthorhombic Transition in SrUO4

Nonstoichiometry in Strontium Uranium Oxide: Understanding the Rhombohedral–Orthorhombic Transition in SrUO4

Emerging Applications of Synchrotron Radiation X‐Ray Techniques in Single Atomic Catalysts

In situ high temperature powder x-ray diffraction technique using a sapphire single-crystal flat cell

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Product

Resources

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Nonstoichiometry in Strontium Uranium Oxide: Understanding the Rhombohedral–Orthorhombic Transition in SrUO₄

Nonstoichiometry in Strontium Uranium Oxide: Understanding the Rhombohedral–Orthorhombic Transition in SrUO₄