Phase Evolution of Thermally Treated Amorphous Tricalcium Phosphate Nanoparticles

2008 ◽  
Vol 396-398 ◽  
pp. 595-598 ◽  
Author(s):  
Nicola Döbelin ◽  
Tobias J. Brunner ◽  
Wendelin J. Stark ◽  
Manuel Eggimann ◽  
Martin Fisch ◽  
...  
Keyword(s):  
Tricalcium Phosphate ◽  
Elevated Temperatures ◽  
Particle Growth ◽  
Phase Evolution ◽  
Flame Spray ◽  
Crystallite Growth ◽  
X Ray ◽  
Heat Treated ◽  
Flame Spray Synthesis

X-ray amorphous tricalcium-phosphate nanoparticles (ATCP) produced by flame spray synthesis were heat-treated at temperatures between 500 and 1000 °C and analyzed in situ by X-ray powder diffraction. The main phase occurring after crystallisation at 525 °C was α-TCP, minor phases were identified as β-TCP and hydroxyapatite. More elevated temperatures induced crystallite growth and the transformation of α-TCP into β-TCP. Above 900 °C no α-TCP was traceable anymore. α’-TCP was not observed in the experiment. This study shows that nanoparticulate α-TCP can be obtained by thermal treatment of an amorphous TCP nanoparticle in a temperature range where sintering effects such as particle growth and densification are moderate or nearly negligible.

An in situ microtomography apparatus with a laboratory x-ray source for elevated temperatures of up to 1000 °C

2021 ◽  
Vol 92 (3) ◽  
pp. 033704
Author(s):  
Rongqi Zhu ◽  
Zhaoliang Qu ◽  
Shuo Yang ◽  
Daining Fang
Keyword(s):  
Elevated Temperatures ◽  
X Ray

Thermal stability and miscibility of co-evaporated methyl ammonium lead halide (MAPbX3, X = I, Br, Cl) thin films analysed by in situ X-ray diffraction

2018 ◽  
Vol 6 (24) ◽  
pp. 11496-11506 ◽  
Author(s):  
Paul Pistor ◽  
Thomas Burwig ◽  
Carlo Brzuska ◽  
Björn Weber ◽  
Wolfgang Fränzel
Keyword(s):  
Thin Films ◽  
Thermal Stability ◽  
Thermal Treatment ◽  
Phase Evolution ◽  
X Ray Diffraction ◽  
Crystalline Phases ◽  
X Ray ◽  
Subsequent Thermal Treatment ◽  
Lead Halide

We present the identification of crystalline phases by in situ X-ray diffraction during growth and monitor the phase evolution during subsequent thermal treatment of CH3NH3PbX3 (X = I, Br, Cl) perovskite thin films.

scholarly journals Mechanistic insight of KBiQ2 (Q = S, Se) using panoramic synthesis towards synthesis-by-design

2021 ◽  
Author(s):  
Rebecca McClain ◽  
Christos D. Malliakas ◽  
Jiahong Shen ◽  
Jiangang He ◽  
Chris Wolverton ◽  
...  
Keyword(s):  
Crystalline Phase ◽  
Phase Evolution ◽  
X Ray Diffraction ◽  
Panoramic View ◽  
X Ray ◽  
Mechanistic Insight

This work uses in situ powder X-ray diffraction studies to observe crystalline phase evolution over the course of multiple K-Bi-Q (Q = S, Se) reactions, thereby constructing a “panoramic” view of each reaction from beginning to end.

scholarly journals Catalytic Behaviour of Flame-Made CuO-CeO2 Nanocatalysts in Efficient CO Oxidation

Catalysts ◽  
2019 ◽  
Vol 9 (3) ◽  
pp. 256 ◽  
Author(s):  
Feng Zhao ◽  
Shuangde Li ◽  
Xiaofeng Wu ◽  
Renliang Yue ◽  
Weiman Li ◽  
...  
Keyword(s):  
Electron Microscopy ◽  
Water Vapor ◽  
Co Oxidation ◽  
Photoelectron Spectroscopy ◽  
Co Adsorption ◽  
Synergistic Interaction ◽  
Flame Spray ◽  
Oxidation Activity ◽  
X Ray

CuO-CeO2 nanocatalysts with varying CuO contents (1, 5, 9, 14 and 17 wt %) were prepared by one-step flame spray pyrolysis (FSP) and applied to CO oxidation. The influences of CuO content on the as-prepared catalysts were systematically characterized by X-ray diffraction (XRD), N2 adsorption-desorption at −196 °C, field emission scanning electron microscopy (FESEM), high-resolution transmission electron microscopy (HRTEM), Raman spectroscopy, X-ray photoelectron spectroscopy (XPS), and hydrogen-temperature programmed reduction (H2-TPR). A superior CO oxidation activity was observed for the 14 wt % CuO-CeO2 catalyst, with 90% CO conversion at 98 °C at space velocity (60,000 mL × g−1 × h−1), which was attributed to abundant surface defects (lattice distortion, Ce3+, and oxygen vacancies) and high reducibility supported by strong synergistic interaction. In addition, the catalyst also displayed excellent stability and resistance to water vapor. Significantly, in situ diffuse reflectance infrared Fourier transform spectroscopy (in situ DRIFTS) showed that in the CO catalytic oxidation process, the strong synergistic interaction led readily to dehydroxylation and CO adsorption on Cu+ at low temperature. Furthermore, in the feed of water vapor, although there was an adverse effect on the access of CO adsorption, there was also a positive effect on the formation of fewer carbon intermediates. All these results showed the potential of highly active and water vapor-resistive CuO-CeO2 catalysts prepared by FSP.

Transformation of ferrihydrite to hematite: anin situinvestigation on the kinetics and mechanisms

2008 ◽  
Vol 72 (1) ◽  
pp. 217-220 ◽  
Author(s):  
H. P. Vu ◽  
S. Shaw ◽  
L. G. Benning
Keyword(s):  
High Resolution ◽  
Growth Mechanism ◽  
Elevated Temperatures ◽  
X Ray Diffraction ◽  
Electron Microscopic ◽  
Time Resolved ◽  
X Ray ◽  
Resolution Electron ◽  
Stage Process

AbstractThe kinetics and mechanisms of the transformation of 2-line ferrihydrite (FH) to hematite (HM), in the presence of Pb at elevated temperatures and high pH condition, were elucidated using synchrotron-based,in situenergy dispersive X-ray diffraction (EDXRD). The time-resolved diffraction data indicated that HM crystallization occurred via a two-stage process. Based on the EDXRD data, combined with high-resolution electron microscopic images, an aqueous-aided 2D growth mechanism is proposed for both HM crystallization stages.

Controlled Environment Specimen Transfer

2014 ◽  
Vol 20 (4) ◽  
pp. 1038-1045 ◽  
Author(s):  
Christian D. Damsgaard ◽  
Henny Zandbergen ◽  
Thomas W. Hansen ◽  
Ib Chorkendorff ◽  
Jakob B. Wagner
Keyword(s):  
Electron Microscope ◽  
Transmission Electron Microscope ◽  
Elevated Temperatures ◽  
Controlled Environment ◽  
Ambient Atmosphere ◽  
Air Exposure ◽  
X Ray ◽  
Environmental Transmission ◽  
Transmission Electron

AbstractSpecimen transfer under controlled environment conditions, such as temperature, pressure, and gas composition, is necessary to conduct successive complementary in situ characterization of materials sensitive to ambient conditions. The in situ transfer concept is introduced by linking an environmental transmission electron microscope to an in situ X-ray diffractometer through a dedicated transmission electron microscope specimen transfer holder, capable of sealing the specimen in a gaseous environment at elevated temperatures. Two catalyst material systems have been investigated; Cu/ZnO/Al2O3 catalyst for methanol synthesis and a Co/Al2O3 catalyst for Fischer–Tropsch synthesis. Both systems are sensitive to ambient atmosphere as they will oxidize after relatively short air exposure. The Cu/ZnO/Al2O3 catalyst, was reduced in the in situ X-ray diffractometer set-up, and subsequently, successfully transferred in a reactive environment to the environmental transmission electron microscope where further analysis on the local scale were conducted. The Co/Al2O3 catalyst was reduced in the environmental microscope and successfully kept reduced outside the microscope in a reactive environment. The in situ transfer holder facilitates complimentary in situ experiments of the same specimen without changing the specimen state during transfer.

Hydroxyapatite Scaffolds Produced by Hydrothermal Deposition of Monetite on Polyurethane Sponges Substrates

2011 ◽  
Vol 493-494 ◽  
pp. 820-825 ◽  
Author(s):  
Fernanda Danielle Mishima ◽  
Luis Henrique Leme Louro ◽  
Felipe Nobre Moura ◽  
Luciano Andrade Gobbo ◽  
Marcelo Henrique Prado da Silva
Keyword(s):  
Electron Microscopy ◽  
Aqueous Solution ◽  
Tricalcium Phosphate ◽  
Porous Scaffolds ◽  
New Bone Formation ◽  
Total Conversion ◽  
X Ray ◽  
Heat Treated ◽  
Wide Range ◽  
Scanning Electron

Hydroxyapatite scaffolds have been being produced by a wide range of processes. The optimun material to be used as bone graft has to be partially resorbable, with resorption rates similar to new bone formation ones. The samples must have porosity compatible with tissue ingrowth. Hydroxyapatite and tricalcium phosphate ceramics are good choices for designing such materials. In the present study, polymeric sponges were coated with hydroxyapatite and sintered. The method consists of coating polyurethane sponges substrates in an aqueous solution rich in phosphate (PO4)3-and calcium (Ca)2+ions. The solution is composed by 0.5M Ca(OH)2, 0.3M H3PO4and 1M CH3CHCO2HOH (lactic acid) at pH of 3.7. The sponges were immersed in a beaker with the solution and heated up to 80°C to precipitate monetite on the sponge. Continuous and adherent coatings were formed on the surface of sponges interconections. These coatings were characterised by X-ray diffractometry and the only identified phase was monetite. The substrates were converted to hydroxyapatite in an alkali solution.The total conversion from monetite to hydroxyapatite was confirmed by XRD analyses. The struts were heat treated in order to eliminate the organic sponge and sinter the scaffolds. After sintering, hydroxyapatite and tricalcium phosphate were identified on the struts. Optical microscopy revealed the morphology of the struts, while scanning electron microscopy (SEM) showed the precipitates morphology. The method showed to be efficient in the production of porous scaffolds.

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