High pressure <i>in situ</i> x-ray absorption spectroscopy cell for studying simultaneously the liquid phase and the solid/liquid interface

Grunwaldt, Jan‐Dierk; Ramin, Michael; Rohr, Markus; Michailovski, Alexej; Patzke, Greta R.; Baiker, Alfons

doi:10.1063/1.1914787

Cited by 69 publications

(57 citation statements)

References 49 publications

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“…Window materials that have been used are Be and diamond. Grunwaldt et al recently reported a high-pressure XAFS cell with Be/PEEK ͓poly-͑etherether ketone͔͒ windows that could withstand 25 MPa and 500 K. 20 However, as mentioned above, Be is a poor window material because of its toxicity and tendency to form an oxide. Diamond as a window material is thermally and physically stable but prohibitively expensive.…”

Section: Strategy For the Design Of An In Situ Xafs Cellmentioning

confidence: 99%

Design of a high-temperature and high-pressure liquid flow cell for x-ray absorption fine structure measurements under catalytic reaction conditions

Kawai

Chun

Asakura

et al. 2008

Review of Scientific Instruments

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The design and performance of a new high-pressure and high-temperature cell for measurement of x-ray absorption fine structure ͑XAFS͒ spectra of solid catalysts working in a flowing liquid are presented. The cell has flat, high-purity sintered cubic boron nitride ͑c-BN͒ windows which can tolerate high temperature ͑900 K͒ and high pressure ͑10 MPa͒. The c-BN is a new material which has the highest tensile strength, second only to diamond, and is also chemically and thermally stable. The use of the cell is demonstrated for measurements of PtPd/ Al 2 O 3 and Ni 2 P / SiO 2 hydrodesulfurization catalysts at reaction conditions. A technique called delta ͑⌬͒, involving determining the difference between XAFS spectra of the sample at reaction conditions and the bare sample, is introduced.

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Section: Strategy For the Design Of An In Situ Xafs Cellmentioning

confidence: 99%

Design of a high-temperature and high-pressure liquid flow cell for x-ray absorption fine structure measurements under catalytic reaction conditions

Kawai

Chun

Asakura

et al. 2008

Review of Scientific Instruments

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“…Extended Xray absorption fine structure (EXAFS) experiments investigating processes in combination with UV-vis and/or IR [8][9][10][11][12][13] have been applied to investigate in situ catalytic processes at both ambient and high pressures and for both gas-solid and liquid-solid systems. However, some concepts have to be clarified regarding the best combination of techniques and, in particular, the evaluation of cost/benefit and the real advantages of the use of both IR and X-ray synchrotron radiation sources for simultaneous time-resolved experiments has to be performed and discussed.…”

Section: Scientific Opportunitiesmentioning

confidence: 99%

Time Resolved IR and X-Ray Simultaneous Spectroscopy: New Opportunities for the Analysis of Fast Chemical-Physical Phenomena in Materials Science

Marcelli

Hampai

et al. 2009

Acta Phys. Pol. A

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New powerful sources and advanced analytical techniques have been considered in the last decade to face up the continuously increasing scientific demands, in particular, in materials science. As an example, nanoscience and nanotechnology researches are characterized by ultimate spatial resolution, fast and ultrafast time--resolved analysis, but the complexity of the investigated phenomena requires new analytical capabilities and new experimental techniques were introduced in the research arena. The availability all over the world of brilliant synchrotron radiation sources offers incredible opportunities. Many challenging experiments were made possible by these sources and understanding of many complex dynamical problems was obtained. Nevertheless, a strong demand of new analytical approaches, mainly based on concurrent and possibly simultaneous time-resolved experimental techniques, is emerging. Pioneering time resolved experiments combining X-ray and infrared radiation with a conventional source were performed more than a decade ago. Nowadays, many beamlines at third generation synchrotron radiation facilities are equipped with conventional sources to allow complementary techniques and the strategy of a concurrent analysis is mandatory in the investigation of many phenomena in frontier multidisciplinary researches. Moreover, new opportunities will be available by means of concurrent spectroscopic experiments investigating complex phenomena on a short timescale, from the sub-second to the microsecond time domain. We will present and discuss researches where the combination of IR and X-ray simultaneous experiments may return unique information on complex dynamical processes and phase transitions occurring in materials science. Finally, we will briefly describe the conceptual layout of a synchrotron radiation beamline to perform concurrent IR and X-ray experiments.

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“…For this purpose, a special in situ-EXAFS cell was used (see Supporting Information). [38] The EXAFS technique is ideally suited to monitor both crystalline and amorphous solid intermediates as well as species in solution, whereas all crystalline components can be fully characterized in terms of the complementary EDXRD method.…”

mentioning

confidence: 99%

Studying the Solvothermal Formation of MoO₃ Fibers by Complementary In Situ EXAFS/EDXRD Techniques

et al. 2005

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The reliable and straightforward fabrication of nanoparticles is essential for developing future nanotechnology. [1][2][3][4][5] Nanoscale transition-metal oxides provide a wide spectrum of important properties, [6,7] and their functionalization and alignment is greatly facilitated by anisotropic morphologies. [8] Among the transition-metal oxides, MoO 3 is the focus of much attention owing to its numerous applications, for example, in catalysis [9][10][11] or sensor technology. [12,13] We have recently developed a solvothermal procedure that provides a convenient access to highly anisotropic nanoscale MoO 3 fibers. [14,15] The solvothermal process [16] is famous for its unique control facilities regarding the particle size of the material produced. [17,18] Its major drawback, however, is that the predictive and rational preparation of a desired solid remains a major preparative challenge-especially if the morphology of the product is to be tuned as well. This problem is because of the tremendous impact of the synthetic parameters on the course of the reaction. Thus, the development of solvothermal nanomaterials syntheses may require considerable "trial and error" work. The elucidation of solvothermal reaction mechanisms is therefore vital for devising more predictive strategies so that the resulting materials can be optimized for commercial purposes. As solvothermal reactions are usually performed in thick-walled reaction containers, sophisticated in situ techniques employing high-intensity synchrotron radiation are required for their direct monitoring. [19][20][21][22] Generally, the development of high-pressure, in situ spectroscopic approaches is a challenging topic of chemistry and materials science. [23] Orientating kinetic studies may also be performed by quenching hydrothermal reactions, but this information is only valid if the recovered material is not affected by any irreversible changes upon cooling and isolation. Among the multitude of solvothermally generated materials, special emphasis has been placed upon the in situ study of zeolites, [24][25][26] open-framework compounds, [27,28] silicate minerals, [29,30] and sulfide-based systems. [22,31] For the transitionmetal oxides, the main focus has been on ternary compounds of industrial interest (e. g. bismuth molybdates [32] or BaTiO 3[33] ), whereas considerably fewer binary oxides (such as ZrO 2 [34] ) have been investigated by solvothermal in situ methods. Very little mechanistic information is available on their solvothermal transformation into nanomaterials.Herein, we report the first comprehensive in situ study on the growth of MoO 3 fibers by complementary EDXRD (energy dispersive X-ray diffraction) and XANES/EXAFS (X-ray absorption near edge structure/extended X-ray absorption fine structure) techniques. While XRD allows the long-range order to be monitored, XANES/EXAFS provides information on the short-range order. [35][36][37] This information is indispensable for describing the solvothermal crystallization of nanostructured matter, because ...

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High pressure in situ x-ray absorption spectroscopy cell for studying simultaneously the liquid phase and the solid/liquid interface

Cited by 69 publications

References 49 publications

Design of a high-temperature and high-pressure liquid flow cell for x-ray absorption fine structure measurements under catalytic reaction conditions

Design of a high-temperature and high-pressure liquid flow cell for x-ray absorption fine structure measurements under catalytic reaction conditions

Time Resolved IR and X-Ray Simultaneous Spectroscopy: New Opportunities for the Analysis of Fast Chemical-Physical Phenomena in Materials Science

Studying the Solvothermal Formation of MoO₃ Fibers by Complementary In Situ EXAFS/EDXRD Techniques

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High pressure in situ x-ray absorption spectroscopy cell for studying simultaneously the liquid phase and the solid/liquid interface

Cited by 69 publications

References 49 publications

Design of a high-temperature and high-pressure liquid flow cell for x-ray absorption fine structure measurements under catalytic reaction conditions

Design of a high-temperature and high-pressure liquid flow cell for x-ray absorption fine structure measurements under catalytic reaction conditions

Time Resolved IR and X-Ray Simultaneous Spectroscopy: New Opportunities for the Analysis of Fast Chemical-Physical Phenomena in Materials Science

Studying the Solvothermal Formation of MoO3 Fibers by Complementary In Situ EXAFS/EDXRD Techniques

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Studying the Solvothermal Formation of MoO₃ Fibers by Complementary In Situ EXAFS/EDXRD Techniques