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1

Kamminga, Machteld E., Simon J. Cassidy, Partha P. Jana, Mahmoud Elgaml, Nicola D. Kelly, and Simon J. Clarke. "Intercalates of Bi2Se3 studied in situ by time-resolved powder X-ray diffraction and neutron diffraction." Dalton Transactions 50, no. 33 (2021): 11376–79. http://dx.doi.org/10.1039/d1dt00960e.

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2

O’Hare, Dermot, John S. O. Evans, Andrew Fogg, and Stephen O’Brien. "Time-resolved, in situ X-ray diffraction studies of intercalation in lamellar hosts." Polyhedron 19, no. 3 (February 2000): 297–305. http://dx.doi.org/10.1016/s0277-5387(99)00359-9.

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3

Rau, J. V., V. Rossi Albertini, N. S. Chilingarov, S. Colonna, and U. Anselmi Tamburini. "In situ time-resolved X-ray diffraction study of manganese trifluoride thermal decomposition." Journal of Fluorine Chemistry 108, no. 2 (May 2001): 253–56. http://dx.doi.org/10.1016/s0022-1139(01)00368-2.

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4

Forster, K. M., J. P. Formica, J. T. Richardson, and D. Luss. "Solid-State Reaction Kinetics Determination via in Situ Time-Resolved X-Ray Diffraction." Journal of Solid State Chemistry 108, no. 1 (January 1994): 152–57. http://dx.doi.org/10.1006/jssc.1994.1023.

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5

Orikasa, Yuki, Takehiro Maeda, Yukinori Koyama, Taketoshi Minato, Haruno Murayama, Katsutoshi Fukuda, Hajime Tanida, et al. "Phase Transition Analysis between LiFePO4and FePO4by In-Situ Time-Resolved X-ray Absorption and X-ray Diffraction." Journal of The Electrochemical Society 160, no. 5 (2013): A3061—A3065. http://dx.doi.org/10.1149/2.012305jes.

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6

Vamvakeros, Antonios, Simon D. M. Jacques, Marco Di Michiel, Pierre Senecal, Vesna Middelkoop, Robert J. Cernik, and Andrew M. Beale. "Interlaced X-ray diffraction computed tomography." Journal of Applied Crystallography 49, no. 2 (March 1, 2016): 485–96. http://dx.doi.org/10.1107/s160057671600131x.

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An X-ray diffraction computed tomography data-collection strategy that allows, post experiment, a choice between temporal and spatial resolution is reported. This strategy enables time-resolved studies on comparatively short timescales, or alternatively allows for improved spatial resolution if the system under study, or components within it, appear to be unchanging. The application of the method for studying an Mn–Na–W/SiO2 fixed-bed reactor in situ is demonstrated. Additionally, the opportunities to improve the data-collection strategy further, enabling post-collection tuning between statistical, temporal and spatial resolutions, are discussed. In principle, the interlaced scanning approach can also be applied to other pencil-beam tomographic techniques, like X-ray fluorescence computed tomography, X-ray absorption fine structure computed tomography, pair distribution function computed tomography and tomographic scanning transmission X-ray microscopy.
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7

YONEMURA, Mitsuharu. "In-situ Observation of Weld Solidification using Two-dimensional Time-resolved X-ray Diffraction." JOURNAL OF THE JAPAN WELDING SOCIETY 81, no. 7 (2012): 572–76. http://dx.doi.org/10.2207/jjws.81.572.

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8

Capitán, M. J., N. Thouin, and G. Rostaing. "A high temperature furnace for in situ and time-resolved x-ray diffraction studies." Review of Scientific Instruments 70, no. 5 (May 1999): 2248–52. http://dx.doi.org/10.1063/1.1149747.

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9

Kikuma, Jun, Masamichi Tsunashima, Tetsuji Ishikawa, Shin-Ya Matsuno, Akihiro Ogawa, Kunio Matsui, and Masugu Sato. "In Situ Time-Resolved X-Ray Diffraction of Tobermorite Formation Process Under Autoclave Condition." Journal of the American Ceramic Society 93, no. 9 (April 12, 2010): 2667–74. http://dx.doi.org/10.1111/j.1551-2916.2010.03815.x.

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10

El Osta, Racha, Mark Feyand, Norbert Stock, Franck Millange, and Richard I. Walton. "Crystallisation Kinetics of Metal Organic Frameworks From in situ Time-Resolved X-ray Diffraction." Powder Diffraction 28, S2 (September 2013): S256—S275. http://dx.doi.org/10.1017/s0885715613000997.

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A time-resolved powder diffraction study of the crystallisation of porous metal organic framework materials with the CPO-27 structure ([M2(dhtp)(H2O)2]·8H2O where, dhtp=2,5-dioxoterephthalate) using the energy dispersive X-ray diffraction method is described. Crystallisation under solvothermal conditions is performed between 70 - 110 °C from clear solutions of metal salts (M=Co2+ or Ni2+) and 2,5-dihydroxyterephthalic acid in a mixture of THF-water in sealed reaction vessels, using both conventional and microwave heating. Integration of Bragg peak areas with time provides accurate crystallisation curves, which are modelled using the method of Gualtieri to determine rate constants for nucleation and for growth and then, by Arrhenius analysis, activation energies. Crystallisation is determined to be one-dimensional, consistent with the elongated morphology of the crystals produced in these reactions. With conventional heating the Co-containing CPO-27 crystallises more rapidly than the isostructural Ni-containing analogue and analysis of the kinetic parameters would suggest a complex multi-step crystallisation process. The effect of microwave heating is upon activation energies: the values for both nucleation and for crystal growth are lowered compared to reactions using conventional heating.
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11

Cahill, C. L., L. G. Benning, H. L. Barnes, and J. B. Parise. "In situ time-resolved X-ray diffraction of iron sulfides during hydrothermal pyrite growth." Chemical Geology 167, no. 1-2 (June 2000): 53–63. http://dx.doi.org/10.1016/s0009-2541(99)00199-0.

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12

Wu, Yue, Sebastian Henke, Gregor Kieslich, Inke Schwedler, Miaosen Yang, Duncan A. X. Fraser, and Dermot O'Hare. "Time-Resolved In Situ X-ray Diffraction Reveals Metal-Dependent Metal-Organic Framework Formation." Angewandte Chemie 128, no. 45 (October 11, 2016): 14287–90. http://dx.doi.org/10.1002/ange.201608463.

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13

Wu, Yue, Sebastian Henke, Gregor Kieslich, Inke Schwedler, Miaosen Yang, Duncan A. X. Fraser, and Dermot O'Hare. "Time-Resolved In Situ X-ray Diffraction Reveals Metal-Dependent Metal-Organic Framework Formation." Angewandte Chemie International Edition 55, no. 45 (October 11, 2016): 14081–84. http://dx.doi.org/10.1002/anie.201608463.

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14

Buelens, Lukas C., Vladimir V. Galvita, Hilde Poelman, Christophe Detavernier, and Guy B. Marin. "Kinetics of Multi-Step Redox Processes by Time-Resolved In Situ X-ray Diffraction." Chemie Ingenieur Technik 88, no. 11 (August 10, 2016): 1684–92. http://dx.doi.org/10.1002/cite.201600057.

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15

Rodriguez, José A., Jonathan C. Hanson, Wen Wen, Xianqin Wang, Joaquín L. Brito, Arturo Martínez-Arias, and Marcos Fernández-García. "In-situ characterization of water–gas shift catalysts using time-resolved X-ray diffraction." Catalysis Today 145, no. 3-4 (July 2009): 188–94. http://dx.doi.org/10.1016/j.cattod.2008.11.018.

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16

Moorhouse, Saul J., Yue Wu, Hannah C. Buckley, and Dermot O'Hare. "Time-resolved in situ powder X-ray diffraction reveals the mechanisms of molten salt synthesis." Chemical Communications 52, no. 96 (2016): 13865–68. http://dx.doi.org/10.1039/c6cc08133a.

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We report the first use of high-energy monochromatic in situ X-ray powder diffraction to gain unprecedented insights into the chemical processes occurring during high temperature, lab-scale metal oxide syntheses.
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17

Baggio, Bruna F., and Yvonne Grunder. "In Situ X-Ray Techniques for Electrochemical Interfaces." Annual Review of Analytical Chemistry 14, no. 1 (June 5, 2021): 87–107. http://dx.doi.org/10.1146/annurev-anchem-091020-100631.

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This article reviews progress in the study of materials using X-ray-based techniques from an electrochemistry perspective. We focus on in situ/in operando surface X-ray scattering, X-ray absorption spectroscopy, and the combination of both methods. The background of these techniques together with key concepts is introduced. Key examples of in situ and in operando investigation of liquid–solid and liquid–liquid interfaces are presented. X-ray scattering and spectroscopy have helped to develop an understanding of the underlying atomic and molecular processes associated with electrocatalysis, electrodeposition, and battery materials. We highlight recent developments, including resonant surface diffraction and time-resolved studies.
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18

Haferkamp, Sebastian, Franziska Fischer, Werner Kraus, and Franziska Emmerling. "Mechanochemical Knoevenagel condensation investigated in situ." Beilstein Journal of Organic Chemistry 13 (September 26, 2017): 2010–14. http://dx.doi.org/10.3762/bjoc.13.197.

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The mechanochemical Knoevenagel condensation of malononitrile with p-nitrobenzaldehyde was studied in situ using a tandem approach. X-ray diffraction and Raman spectroscopy were combined to yield time-resolved information on the milling process. Under solvent-free conditions, the reaction leads to a quantitative conversion to p-nitrobenzylidenemalononitrile within 50 minutes. The in situ data indicate that the process is fast and proceeds under a direct conversion. After stopping the milling process, the reaction continues until complete conversion. The continuous and the stopped milling process both result in crystalline products suitable for single crystal X-ray diffraction.
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19

Valério, Adriana, Sérgio L. Morelhão, Alex J. Freitas Cabral, Márcio M. Soares, and Cláudio M. R. Remédios. "X-Ray Dynamical Diffraction in Powder Samples with Time-Dependent Particle Size Distributions." MRS Advances 5, no. 29-30 (December 2, 2019): 1585–91. http://dx.doi.org/10.1557/adv.2019.445.

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ABSTRACTIn situ X-ray diffraction is one of the most useful tools for studying a variety of processes, among which crystallization of nanoparticles where phase purity and size control are desired. Growth kinetics of a single phase can be completely resolved by proper analysis of the diffraction peaks as a function of time. The peak width provides a parameter for monitoring the time evolution of the particle size distribution (PSD), while the peak area (integrated intensity) is directly related to the whole diffracting volume of crystallized material in the sample. However, to precisely describe the growth kinetics in terms of nucleation and coarsening, the correlation between PSD parameters and diffraction peak widths has to be established in each particular study. Corrections in integrated intensity values for physical phenomena such as variation in atomic thermal vibrations and dynamical diffraction effects have also to be considered in certain cases. In this work, a general correlation between PSD median value and diffraction peak width is deduced, and a systematic procedure to resolve time-dependent lognormal PSDs from in situ XRD experiments is described in details. A procedure to correct the integrated intensities for dynamical diffraction effects is proposed. As a practical demonstration, this analytical procedure has been applied to the single-phase crystallization process of bismuth ferrite nanoparticles.
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20

Bugaev, Aram L., Oleg A. Usoltsev, Andrea Lazzarini, Kirill A. Lomachenko, Alexander A. Guda, Riccardo Pellegrini, Michele Carosso, et al. "Time-resolved operando studies of carbon supported Pd nanoparticles under hydrogenation reactions by X-ray diffraction and absorption." Faraday Discussions 208 (2018): 187–205. http://dx.doi.org/10.1039/c7fd00211d.

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21

O'Hare, Dermot, John S. O. Evans, Robin J. Francis, P. Shiv Halasyamani, Poul Norby, and Jonathan Hanson. "Time-resolved, in situ X-ray diffraction studies of the hydrothermal syntheses of microporous materials." Microporous and Mesoporous Materials 21, no. 4-6 (May 1998): 253–62. http://dx.doi.org/10.1016/s1387-1811(98)00009-2.

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22

Hutchins, Peter T., Olivier Leynaud, Luke A. O’Dell, Mark E. Smith, Paul Barnes, and Paul F. McMillan. "Time-Resolved in Situ Synchrotron X-ray Diffraction Studies of Type 1 Silicon Clathrate Formation." Chemistry of Materials 23, no. 23 (December 13, 2011): 5160–67. http://dx.doi.org/10.1021/cm2018136.

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23

O'Brien, Stephen, Robin J. Francis, Andrew Fogg, Dermot O'Hare, Nanae Okazaki, and Kazuyuki Kuroda. "Time-Resolved in Situ X-ray Powder Diffraction Study of the Formation of Mesoporous Silicates." Chemistry of Materials 11, no. 7 (July 1999): 1822–32. http://dx.doi.org/10.1021/cm990044a.

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24

Rau, J. V., V. S. Komlev, A. Generosi, M. Fosca, V. Rossi Albertini, and S. M. Barinov. "In situ time-resolved X-ray diffraction study of octacalcium phosphate transformations under physiological conditions." Journal of Crystal Growth 312, no. 14 (July 2010): 2113–16. http://dx.doi.org/10.1016/j.jcrysgro.2010.03.044.

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25

Jensen, Anders C. S., Mogens Hinge, and Henrik Birkedal. "Calcite nucleation on the surface of PNIPAM–PAAc micelles studied by time resolved in situ PXRD." CrystEngComm 17, no. 36 (2015): 6940–46. http://dx.doi.org/10.1039/c5ce00424a.

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Nanocrystalline calcite is formed under the influence of block copolymers containing thermoresponsive PNIPAM and a mineralization controlling block of poly(acrylic acid) and the nanocrystal formation kinetics studied by in situ X-ray diffraction.
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26

YONEMURA, Mitsuharu, Takahiro OSUKI, Hidenori TERASAKI, Yuichi KOMIZO, Masugu SATO, and Hidenori TOYOKAWA. "In-situ Observation of Microstructure Formation Process of Weld Metals by Time-resolved X-ray Diffraction." Tetsu-to-Hagane 93, no. 2 (2007): 138–44. http://dx.doi.org/10.2355/tetsutohagane.93.138.

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27

Rau, J. V., A. Generosi, D. Ferro, F. Minozzi, B. Paci, V. Rossi Albertini, G. Dolci, and S. M. Barinov. "In situ time-resolved X-ray diffraction study of evolution of nanohydroxyapatite particles in physiological solution." Materials Science and Engineering: C 29, no. 4 (May 2009): 1140–43. http://dx.doi.org/10.1016/j.msec.2008.09.035.

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28

Skjærvø, Susanne Linn, Kristin Høydalsvik Wells, Sanna Sommer, Tuong-Dan Vu, Julian R. Tolchard, Wouter van Beek, Tor Grande, Bo B. Iversen, and Mari-Ann Einarsrud. "Rationalization of Hydrothermal Synthesis of NaNbO3 by Rapid in Situ Time-Resolved Synchrotron X-ray Diffraction." Crystal Growth & Design 18, no. 2 (January 29, 2018): 770–74. http://dx.doi.org/10.1021/acs.cgd.7b01192.

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29

Liu, Hongjun, Ola G. Grendal, Susanne Linn Skjærvø, Antoine R. M. Dalod, Wouter van Beek, Abderrahime Sekkat, Mari-Ann Einarsrud, and David Muñoz-Rojas. "Reaction Pathway of the Hydrothermal Synthesis of AgCuO2 from In Situ Time-Resolved X-ray Diffraction." Crystal Growth & Design 20, no. 7 (April 27, 2020): 4264–72. http://dx.doi.org/10.1021/acs.cgd.9b01516.

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30

Loh, Joanne S. C., Andrew M. Fogg, Helen R. Watling, Gordon M. Parkinson, and Dermot O'Hare. "A kinetic investigation of gibbsite precipitation using in situ time resolved energy dispersive X-ray diffraction." Physical Chemistry Chemical Physics 2, no. 16 (2000): 3597–604. http://dx.doi.org/10.1039/b003050n.

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31

Moorhouse, Saul J., Nenad Vranješ, Andrew Jupe, Michael Drakopoulos, and Dermot O’Hare. "The Oxford-Diamond In Situ Cell for studying chemical reactions using time-resolved X-ray diffraction." Review of Scientific Instruments 83, no. 8 (August 2012): 084101. http://dx.doi.org/10.1063/1.4746382.

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32

Simmance, Kerry, Wouter van Beek, and Gopinathan Sankar. "Time resolved in situ X-ray diffraction study of crystallisation processes of large pore nanoporous aluminophosphate materials." Faraday Discussions 177 (2015): 237–47. http://dx.doi.org/10.1039/c4fd00179f.

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Time resolved high-resolution X-ray powder diffraction was utilized to obtain detailed changes in the crystal structure parameters during the hydrothermal crystallization process of the nanoporous aluminophosphate AlPO-5 (AFI) structure. This in situ study offered not only the influence of metal ions on the onset of crystallization and estimation of the activation energy of the process, but also allowed us to determine in detail the changes in lattice parameters during this process. More importantly the time-resolved study clearly showed the lattice expansion in the divalent metal ions substituted system right from the on-set of crystallization process, compared to the one without any dopant ions, which suggest that an amorphous or poorly crystalline network is formed prior to crystallization that contains the large divalent ions (compared to Al(iii), the substituting element), which is in agreement with the combined XAS/XRD study reported earlier. A mechanism based on this and the earlier study is suggested.
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33

Sharma, Neeraj. "Time-resolved in situ neutron diffraction studies of Li-ion battery materials." Acta Crystallographica Section A Foundations and Advances 70, a1 (August 5, 2014): C353. http://dx.doi.org/10.1107/s2053273314096466.

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Lithium-ion batteries are ubiquitous in society, used in everything from children's toys to mobile electronic devices, providing portable power solutions. There is a continuous drive for the improvement of these batteries to meet the demands of higher power devices and uses. A large proportion of the function of lithium-ion batteries arises from the electrodes, and these are in turn mediated by the atomic-scale perturbations or changes in the crystal structure during an electrochemical process (e.g. battery use). Therefore, a method to both understand battery function and propose ideas to improve their performance is to probe the electrode crystal structure evolution in situ while an electrochemical process is occurring inside a battery. Our work has utilized the benefits of in situ neutron diffraction (e.g. sensitivity towards lithium) to literally track the time-resolved evolution of lithium in electrode materials used in lithium-ion batteries (see Figure 1). With this knowledge we have been able to directly relate electrochemical properties such as capacity and differences in charge/discharge behaviour of a battery to the content and distribution of lithium in the electrode crystal structure. This talk will showcase some of our in situ investigations of materials in lithium-ion batteries, such as LiCoO2, LiFePO4, Li1+yMn2O4, LiNi0.5Mn1.5O4 and Li4Ti5O12/TiO2 electrodes. In addition, selected examples of our work using time-resolved in situ X-ray diffraction to probe other batteries types, such as primary lithium and secondary (rechargeable) sodium-ion batteries will be presented. Using time-resolved diffraction data, a comprehensive atomic-scale picture of battery functionality can be modelled and permutations can be made to the electrodes and electrochemical conditions to optimize battery performance. Therefore, crystallography and electrochemistry can mesh together to solve our energy needs.
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34

Machida, Akihiko, Kensuke Higuchi, Yoshinori Katayama, Kouji Sakaki, Hyunjeong Kim, and Yumiko Nakamura. "A system for time-resolved XRD measurements on hydrogen absorption processes." Acta Crystallographica Section A Foundations and Advances 70, a1 (August 5, 2014): C360. http://dx.doi.org/10.1107/s2053273314096399.

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"To improve performance of hydrogen storage materials, it is essential to understand detailed mechanism of hydrogenation and dehydrogenation reactions. In-situ powder diffraction measurements provide direct information about structural changes accompanying the reactions. We therefore installed a time-resolved x-ray diffraction (XRD) system at a beamline BL22XU at the SPrign-8, a synchrotron radiation facility in Japan. The system was equipped with two area detectors, a flat panel sensor for precise structural analyses and a high speed video camera connected to an x-ray image intensifier for observation of rapid phase changes. Maximum frame rate for the flat panel sensor and high-speed video camera was 2 fps and 125 fps (effective), respectively. A sample cell was connected to a hydrogen supply system. Opening of upstream valve of the sample cell or a change of the pressure at the sample triggered the recording of the diffraction patterns. The pressure of hydrogen gas was limited to 1 MPa. To demonstrate the performance of the system, we have performed time-resolved XRD experiments for LaNi4.5Al0.5. LaNi5 exhibits the significant broadening of the diffraction peaks by hydrogen absorption; however, LaNi4.5Al0.5 shows the no significant broadening. We have succeeded in the measurements of the structural change from the solid solution phase to the hydride phase and have found the formation of the transient intermediate phase on this reaction process. The system is currently used to study several materials. This work was partly supported by New Energy and Industrial Technology Development Organization (NEDO) under ""Advanced Fundamental Research Project on Hydrogen Storage Materials""."
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35

Yonemura, Mitsuharu, Takahiro Osuki, Hidenori Terasaki, Yuichi Komizo, Masugu Sato, and Akiko Kitano. "In-Situ Observation for Weld Solidification in Stainless Steels Using Time-Resolved X-ray Diffraction." MATERIALS TRANSACTIONS 47, no. 2 (2006): 310–16. http://dx.doi.org/10.2320/matertrans.47.310.

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36

Wicker, Scott A., and Edwin H. Walker. "Revisited: Decomposition or Melting? Formation Mechanism Investigation of LiCoO2 via In-Situ Time-Resolved X-ray Diffraction." Inorganic Chemistry 52, no. 4 (January 31, 2013): 1772–79. http://dx.doi.org/10.1021/ic301516a.

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37

Bernard, F., F. Charlot, Ch Gras, V. Gauthier, and E. Gaffet. "In-situ time-resolved X-ray diffraction experiments applied to self-sustained reactions from mechanically activated mixtures." Le Journal de Physique IV 10, PR10 (September 2000): Pr10–89—Pr10–99. http://dx.doi.org/10.1051/jp4:20001011.

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38

Fogg, Andrew M., and Dermot O'Hare. "Study of the Intercalation of Lithium Salt in Gibbsite Using Time-Resolved in Situ X-ray Diffraction." Chemistry of Materials 11, no. 7 (July 1999): 1771–75. http://dx.doi.org/10.1021/cm981151s.

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39

Maruyama, Koji, Hiroyuki Kagi, Toru Inoue, Hiroaki Ohfuji, and Toru Yoshino. "In Situ Observation of Pressure-induced Crystallization from Amorphous Calcium Carbonate by Time-resolved X-ray Diffraction." Chemistry Letters 44, no. 4 (April 5, 2015): 434–36. http://dx.doi.org/10.1246/cl.141062.

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40

Guzmán, Héctor J., Wenqian Xu, Dario Stacchiola, Gerardo Vitale, Carlos E. Scott, José A. Rodríguez, and Pedro Pereira-Almao. "In situ time-resolved X-ray diffraction study of the synthesis of Mo2C with different carburization agents." Canadian Journal of Chemistry 91, no. 7 (July 2013): 573–82. http://dx.doi.org/10.1139/cjc-2012-0516.

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Toluene, n-heptane, and methane were studied as carbon sources during the synthesis of Mo2C. Ammonium heptamolybdate ((NH4)6Mo7O24·4H2O), molybdenum dioxide (MoO2), orthorhombic molybdenum trioxide (α-MoO3), and a low crystallinity molybdenum oxide (MoOx) were employed as metal precursors and their conversion into the carbide phase was followed by time-resolved X-ray diffraction from synchrotron radiation. Thermal treatment was carried out from 298 K up to 1023 K and the evolution of gases analyzed by mass spectrometry. The resulting carbidic phase obtained using methane/H2 was hexagonal β-Mo2C, while in contrast, cubic molybdenum carbide (α-MoC1–x) was obtained when toluene/H2 or n-heptane/H2 were employed, which occurred independently of the original metal precursor. Molybdenum carbide was first detected, on average, at about 923 K. Mass spectrometry results show the formation of CO when methane was used as a carbon source, while methyl radicals and benzene and mainly methyl radicals were detected when toluene and n-heptane were employed, respectively.
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41

Rathouský, Jiří, Günter Schulz-Ekloff, Jiří Had, and Arnošt Zukal. "Time-resolved in situ X-ray diffraction study of MCM-41 structure formation from a homogeneous environment." Physical Chemistry Chemical Physics 1, no. 12 (1999): 3053–57. http://dx.doi.org/10.1039/a901968e.

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42

Landois, Périne, Stéphan Rouziére, Mathieu Pinault, Dominique Porterat, Cristian Mocuta, Erik Elkaim, Martine Mayne-L'Hermite, and Pascale Launois. "Growth of aligned multi-walled carbon nanotubes: First in situ and time-resolved X-ray diffraction analysis." physica status solidi (b) 248, no. 11 (September 1, 2011): 2449–53. http://dx.doi.org/10.1002/pssb.201100201.

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43

Bonaccorso, A. Damiano, Despoina Papargyriou, Aida Fuente Cuesta, Oxana V. Magdysyuk, Stefan Michalik, Thomas Connolley, Julia L. Payne, and John T. S. Irvine. "Time-resolved in-situ x-ray diffraction study of CaO and CaO:Ca3Al2O6 composite catalysts for biodiesel production." Journal of Physics: Energy 3, no. 3 (June 28, 2021): 034014. http://dx.doi.org/10.1088/2515-7655/ac0413.

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44

Taris, Alessandra, Massimiliano Grosso, Mariarosa Brundu, Vincenzo Guida, and Alberto Viani. "Application of combined multivariate techniques for the description of time-resolved powder X-ray diffraction data." Journal of Applied Crystallography 50, no. 2 (March 7, 2017): 451–61. http://dx.doi.org/10.1107/s1600576717001753.

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In this work, multivariate statistical techniques are employed to determine patterns and conversion curves from time-resolved X-ray powder diffraction data. For these purposes, time-window statistical total correlation spectroscopy is introduced for the pattern matching of the crystalline phase and is shown to be effective even in the case of overlapping peaks. When combined with evolving factor analysis and multivariate curve resolution–alternating least squares, this technique allows a definite estimation of patterns and conversion curves. The procedure is applied to in situ synchrotron powder diffraction patterns to monitor the setting reaction of magnesium potassium phosphate ceramic (MKP) from magnesia (MgO) and potassium dihydrogen phosphate. It is shown that the phases involved in the reaction are clearly distinguished and their evolution is correctly described. The conversion curves estimated with the proposed procedure are compared with the ones determined with the peak integration method, leading to an excellent agreement (Pearson's correlation coefficient equal to 0.9995 and 0.9998 for MgO and MKP, respectively). The approach also allows for the detection and description of the evolution of amorphous phases that cannot be described through conventional analysis of powder diffraction data.
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45

Walton, Richard I., Andrew J. Dent, and Simon J. Hibble. "In Situ Investigation of the Thermal Decomposition of Ammonium Tetrathiomolybdate Using Combined Time-Resolved X-ray Absorption Spectroscopy and X-ray Diffraction." Chemistry of Materials 10, no. 11 (November 1998): 3737–45. http://dx.doi.org/10.1021/cm980716h.

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46

Clark, Simon M., John S. O. Evans, Dermot O'Hare, Chris J. Nuttall, and Heng-Vee Wong. "Real-time in situ X-ray diffraction of intercalation reactions." Journal of the Chemical Society, Chemical Communications, no. 7 (1994): 809. http://dx.doi.org/10.1039/c39940000809.

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47

Bednarčík, J., R. Nicula, Karel Saksl, M. Stir, and E. Burkel. "Microstructure Evolution during Thermal Processing : Insight from In-Situ Time-Resolved Synchrotron Radiation Experiments." Materials Science Forum 550 (July 2007): 607–12. http://dx.doi.org/10.4028/www.scientific.net/msf.550.607.

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The magnetic, mechanical or chemical properties of nanocrystalline materials strongly differ from the ones of their coarse-grained counterparts. Moreover, significant changes of the phase diagrams were already evidenced for nanostructured alloys. Thermal processing with or without applied pressure controls the microstructure development at the nanometer scale and thus essentially decides upon the final nanomaterial behaviour and properties. A common route for the synthesis of metallic nanomaterials is the devitrification of amorphous precursors obtained via non-equilibrium processing, e.g. by rapid solidification or high-energy ball-milling. Time-resolved in-situ X-ray diffraction experiments may nowadays be performed at high-brilliance synchrotron radiation sources for a variety of temperature-pressure conditions. The temperature-time evolution of the grain-size distribution and microstrain can be monitored in detail at specimen-relevant scales. Together with local information from electron microscopy and chemical analysis, in-situ X-ray experiments offer a complete set of tools for engineering of the microstructure in nanomaterials. The effect of individual processing steps can be distinguished clearly and further tuned. An example is provided, concerning the high-temperature microstructure development in Co-rich soft magnetic nanostructured alloys.
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48

Rau, Julietta V., Marco Fosca, and Vladimir S. Komlev. "In Situ Time-Resolved Energy Dispersive X-Ray Diffraction Studies of Calcium Phosphate Based Bone Cements." Key Engineering Materials 541 (February 2013): 115–20. http://dx.doi.org/10.4028/www.scientific.net/kem.541.115.

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In situ monitoring of structural changes, taking place upon calcium phosphate bone cements hardening process was carried out by means of the Energy Dispersive X-Ray Diffraction method. Two different cement systems were studied, one of them based on the octacalcium phosphate and another - on the dicalcium phosphate dehydrate. Both systems contained natural biopolymer chitosan and were soaked in Simulated Body Fluid. The obtained experimental results evidence that during the hardening of the cement containing octacalcium phosphate its partial transformation into hydroxyapatite takes place, whereas no significant changes were detected during the hardening process of cement containing the dicalcium phosphate dehydrate.
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49

Tecklenburg, Sabrina, Roberto Colina-Ruiz, Sovanndara Hok, Cynthia Bolme, Eric Galtier, Eduardo Granados, Akel Hashim, et al. "Ultrafast X-ray Diffraction Study of a Shock-Compressed Iron Meteorite above 100 GPa." Minerals 11, no. 6 (May 26, 2021): 567. http://dx.doi.org/10.3390/min11060567.

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Natural kamacite samples (Fe92.5Ni7.5) from a fragment of the Gibeon meteorite were studied as a proxy material for terrestrial cores to examine phase transition kinetics under shock compression for a range of different pressures up to 140 GPa. In situ time-resolved X-ray diffraction (XRD) data were collected of a body-centered cubic (bcc) kamacite section that transforms to the high-pressure hexagonal close-packed (hcp) phase with sub-nanosecond temporal resolution. The coarse-grained crystal of kamacite rapidly transformed to highly oriented crystallites of the hcp phase at maximum compression. The hcp phase persisted for as long as 9.5 ns following shock release. Comparing the c/a ratio with previous static and dynamic work on Fe and Fe-rich Fe-Ni alloys, it was found that some shots exhibit a larger than ideal c/a ratio, up to nearly 1.65. This work represents the first time-resolved laser shock compression structural study of a natural iron meteorite, relevant for understanding the dynamic material properties of metallic planetary bodies during impact events and Earth’s core elasticity.
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50

Norby, P., and J. C. Hanson. "Hydrothermal synthesis of the microporous aluminophosphate CoAPO-5; in situ time-resolved synchrotron X-ray powder diffraction studies." Catalysis Today 39, no. 4 (March 1998): 301–9. http://dx.doi.org/10.1016/s0920-5861(97)00118-1.

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