High Temperature XRD Studies of Selected Carbonate Minerals

1984 ◽  
Vol 28 ◽  
pp. 331-338 ◽  
Author(s):  
S. S. Iyengar ◽  
P. Engler ◽  
M. W. Santana ◽  
E. R. Wong
Keyword(s):  
High Temperature ◽  
Thermal Behavior ◽  
Reaction Products ◽  
X Ray Diffraction ◽  
In Situ Xrd ◽  
Natural Minerals ◽  
High Temperature Xrd ◽  
Analytical Reagent ◽  
Thermal Analysis Techniques

Thermal analysts have exploited the sensitivity of carbonate mineral decomposition to furnace atmosphere as a diagnostic tool for identifying and quantifying these minerals in mixtures and solid solutions (1-3). However, thermal analysis techniques alone cannot reveal information about the reaction products after each thermal event. In-situ high temperature x-ray diffraction is one technique that can identify these products. Using this technique, Kissinger et al. (4) identified the reaction products of the thermal decomposition of reagent grade FeCO3 (siderite) and MgCO3 (magnesite). However, the thermal behavior of analytical reagent grade carbonates differs from natural minerals (1). Milodowski and Morgan (5) used in-situ XRD to investigate the thermal behavior of the dolomite-ankerite series.

Characterization of a Diamond Ground Y-TZP and Reversion of the Tetragonal to Monoclinic Transformation

2017 ◽  
Vol 42 (4) ◽  
pp. 407-417 ◽  
Author(s):  
LM Candido ◽  
LMG Fais ◽  
EB Ferreira ◽  
SG Antonio ◽  
LAP Pinelli
Keyword(s):  
High Temperature ◽  
Crystalline Phase ◽  
Monoclinic Phase ◽  
Volume Fraction ◽  
Monoclinic Zirconia ◽  
X Ray Diffraction ◽  
High Temperature Xrd ◽  
M Phase ◽  
Wet Ground

SUMMARY Purpose: To characterize the surface of an yttria-stabilized zirconia (Y-TZP) ceramic after diamond grinding in terms of its crystalline phase, morphology, mean roughness (Ra), and wettability as well as to determine a thermal treatment to reverse the resulting tetragonal to monoclinic (t-m) transformation. Methods and Materials: Y-TZP specimens were distributed into different groups according to the actions (or no action) of grinding and irrigation. Grinding was accomplished using a diamond stone at a low speed. The samples were characterized by x-ray diffraction (XRD), scanning electron microscopy, goniometry, and profilometry. In situ high-temperature XRD was used to determine an annealing temperature to reverse the t-m transformation. Ra was submitted to the Kruskal-Wallis test, followed by the Dunn test (α=0.05). The volume fraction of the monoclinic phase and contact angle were submitted to one-way analysis of variance, followed by the Tukey test (α=0.05). Results: Monoclinic zirconia was observed on the surface of samples after dry and wet grinding with a diamond stone. The volume fraction of the monoclinic phase was smaller on the dry ground samples (3.6%±0.3%) than on the wet ground samples (5.6%±0.3%). High-temperature XRD showed reversion of the t-m phase transformation, which started at 700°C and completed at 800°C in a conventional oven. Conclusions: Grinding with a diamond stone partially transformed the crystalline phase on the surface of a Y-TZP ceramic from tetragonal to monoclinic zirconia while simultaneously increasing the surface roughness and wettability. The t-m transformation could be reversed by heat treatment at 800°C or 900°C for 60 minutes or 1000°C for 30 minutes.

Observation of a Collapsing Layer Structure in Mg/Al Layered Double Hydroxides with Interlayer Hydrogen Phosphate by High Temperature In Situ X-Ray Diffraction with Synchrotoron Radiation

2011 ◽  
Vol 700 ◽  
pp. 67-70
Author(s):  
Akihiro Shimamura ◽  
Linus Perander ◽  
Eiji Kanezaki ◽  
Mark Ian Jones ◽  
James B. Metson
Keyword(s):  
High Temperature ◽  
Thermal Behavior ◽  
Layered Double Hydroxides ◽  
Layer Structure ◽  
Ex Situ ◽  
X Ray Diffraction ◽  
Hydrogen Phosphate ◽  
X Ray ◽  
Double Hydroxides

The collapsing layer structure of hydrogen phosphate intercalated Mg/Al-layered double hydroxides (LDH-HPO4) was investigated by high temperature in-situ X-ray diffraction with synchrotron radiation (in-situ XRD). The thermal behavior of the layer structure of LDH-HPO4 showed the same behavior in both in-situ and ex-situ XRD up until 109 °C as previously reported. The basal spacing of LDH-HPO4 continuously decreases above this temperature and finally the layer structure of LDH-HPO4 collapses. Another diffraction peak, d110, which gives a lattice constant a0, decreases at 62 °C, keeps constant to 120°C, increases up to 176°C and again keeps constant until the layer collapse. In this study, the different thermal behavior is observed between two reflections by in-situ XRD measurement, which explains the mechanism of the collapse of the layer structure in LDH-HPO4.

Hydrocalumite and Its Polymer Derivatives. 1. Reversible Thermal Behavior of Friedel's Salt: A Direct Observation by Means of High-Temperature in Situ Powder X-ray Diffraction

2003 ◽  
Vol 15 (23) ◽  
pp. 4361-4368 ◽  
Author(s):  
Laetitia Vieille ◽  
Isabelle Rousselot ◽  
Fabrice Leroux ◽  
Jean-Pierre Besse ◽  
Christine Taviot-Guého
Keyword(s):  
High Temperature ◽  
Thermal Behavior ◽  
Direct Observation ◽  
X Ray Diffraction ◽  
X Ray ◽  
Friedel’S Salt

A Low-High Temperature Camera for In-Situ X-Ray Diffraction Studies of Catalysts

1983 ◽  
Vol 27 ◽  
pp. 285-291
Author(s):  
J. Pielaszek ◽  
J.B. Cohen
Keyword(s):  
High Temperature ◽  
Porous Silica ◽  
X Ray Diffraction ◽  
X Ray ◽  
Controlled Atmospheres ◽  
Research Areas ◽  
High Temperature Xrd ◽  
Different Temperatures ◽  
Porous Silica Glass

X-Ray diffraction studies of substances under controlled atmospheres and at different temperatures are of great importance in many research areas. This is especially true in the area of catalysis, where the correlation of structural and catalytic properties is needed. The camera described here was made for this purpose although any sample in the powdered form can be studied as well. Many catalysts are in the form of highly dispersed metal deposited on a granulated support. The content of metal may vary from a few tenths to several percent. In a camera used by Janko and Borodzinski a small amount of catalyst was spread out on a porous silica glass sample holder which then was placed in a high temperature XRD camera with flowing gas of controlled composition.

scholarly journals In-Situ X-ray Diffraction Measurement for Pure Niobium Metal in High Temperature Hydrogen Atmosphere

2006 ◽  
Vol 70 (6) ◽  
pp. 467-472 ◽  
Author(s):  
Tomonori Nambu ◽  
Nobue Shimizu ◽  
Hisakazu Ezaki ◽  
Hiroshi Yukawa ◽  
Masahiko Morinaga ◽  
...  
Keyword(s):  
High Temperature ◽  
Hydrogen Atmosphere ◽  
Diffraction Measurement ◽  
X Ray Diffraction ◽  
X Ray ◽  
Pure Niobium

In Situ XRD Study of Zirconia Phase Transformation Produced from Chemical and Mineral Processes

2016 ◽  
Vol 840 ◽  
pp. 375-380
Author(s):  
Meor Yusoff Meor Sulaiman ◽  
Khaironie Mohamed Takip ◽  
Ahmad Khairulikram Zahari
Keyword(s):  
High Temperature ◽  
Heating Temperature ◽  
Tetragonal Zirconia ◽  
Amorphous Structure ◽  
High Temperature Phase ◽  
Temperature Phase ◽  
Zirconyl Chloride ◽  
High Temperature Xrd ◽  
Temperature Phase Transition

The high temperature phase transition of zirconia produced from commercial zirconyl chloride chemical was compared with that produced from a Malaysian zircon mineral. Zirconyl chloride was produced from zircon by using the hydrothermal fusion method. Initial XRD diffractogram of these samples at room temperature show that they are of amorphous structure. High temperature XRD studies was then performed on these samples; heated up to 1500°C. The XRD diffractograms shows that the crystalline structure of tetragonal zirconia was first observed and the monoclinic zirconia becomes more visible at higher heating temperature.

In Situ X-Ray Diffraction Studies of Crystallization Growth Behavior in ZnO-Bi2O3-B2O3 Glass as a Route to Functional Optical Devices

MRS Advances ◽  
2018 ◽  
Vol 3 (11) ◽  
pp. 563-567 ◽  
Author(s):  
Quentin Altemose ◽  
Katrina Raichle ◽  
Brittani Schnable ◽  
Casey Schwarz ◽  
Myungkoo Kang ◽  
...  
Keyword(s):  
Heat Treatment ◽  
Glass Ceramics ◽  
Treatment Temperature ◽  
Crystal Phase ◽  
X Ray Diffraction ◽  
X Ray ◽  
In Situ Xrd ◽  
Dsc Measurements ◽  
Transmission Window

ABSTRACTTransparent optical ZnO–Bi2O3–B2O3 (ZBB) glass-ceramics were created by the melt quenching technique. In this work, a melt of the glass containing stoichiometric ratios of Zn/Bi/B and As was studied. Differential scanning calorimeter (DSC) measurements was used to measure the thermal behavior. VIS/NIR transmission measurements were used to determine the transmission window. X-ray diffraction (XRD) was used to determine crystal phase. In this study, we explore new techniques and report a detailed study of in-situ XRD of the ZBB composition in order to correlate nucleation temperature, heat treatment temperature, and heat treatment duration with induced crystal phase.

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