Diffraction thermometry and differential thermal analysis

2002 ◽  
Vol 35 (6) ◽  
pp. 664-668 ◽  
Author(s):  
E. H. Kisi ◽  
D. P. Riley

A unit-cell parameter anomaly observed during the precipitation and growth of Ti3SiC2from a Si-substituted TiC phase is interpreted as the release of latent heat. The observations are used to propose a powder diffraction method for conducting differential thermal analysis as part ofin situphase transition studies.

1981 ◽  
Vol 36 (8) ◽  
pp. 917-921 ◽  
Author(s):  
Hans-Otto Cullmann ◽  
Heinz-Walter Hinterkeuser ◽  
Hans-Uwe Schuster

Abstract The ternary compound β-Li2ZnGe was prepared and its structure determined from powder and single crystal data. The compound crystallizes in a modified Na3As type structure, space group Ṗ̇̇̇̇̇̇̇̇̇̇̇̇̇̇3̄m 1 - D33d.The cell parameters are: a = 432.6 pm, c = 1647.0 pm, c/a= 3.83.A phase transition between a-and β-Li2ZnGe was found and the reaction of the elements lithium, zinc and germanium to a-Li2ZnGe was followed by differential thermal analysis. The temperatures and the enthalpies of transition and fusion were determined.


2016 ◽  
Vol 31 (4) ◽  
pp. 292-294 ◽  
Author(s):  
V. D. Zhuravlev ◽  
A. P. Tyutyunnik ◽  
N. I. Lobachevskaya

A polycrystalline sample of Ca4ZrGe3O12 was synthesized using the nitrate–citrate method and heated at 850–1100 °C. Structural refinement based on X-ray powder diffraction data showed that the crystal structure is of the garnet type with a cubic unit-cell parameter [a = 12.71299(3) Å] and the space group Ia$\bar 3$d. The structural formula is presented as Ca3[CaZr]octa[Ge]tetraO12.


2018 ◽  
Vol 64 (6) ◽  
pp. 548
Author(s):  
Gustavo Marroquin ◽  
Gerzon E. Delgado ◽  
Pedro Grima-Gallardo ◽  
Miguel Quintero

The crystal structure of the quaternary compound CuVInSe3 belonging to the system (CuInSe2)1-x(VSe)x with x= ½, was analyzed using X-ray powder diffraction data. This material was synthesized by the melt and anneal method and crystallizes in the tetragonal space group P2c (Nº 112), with unit cell parameters a = 5.7909(4) Å, c = 11.625(1) Å, V = 389.84(5) Å3. The Rietveld refinement of 25 instrumental and structural variables led to Rexp = 6.6 %, Rp = 8.7 %, Rwp = 8.8 % and S = 1.3 for 4501 step intensities and 153 independent reflections. This compound has a normal adamantane structure and is isostructural with CuFeInSe3. The DTA indicates that this compound melts at 1332 K.


2000 ◽  
Vol 64 (2) ◽  
pp. 255-266 ◽  
Author(s):  
J. J. Reece ◽  
S. A. T. Redfern ◽  
M. D. Welch ◽  
C. M. B. Henderson

AbstractThe crystal structure of a manganoan cummingtonite, composition [M4](Na0.13Ca0.41Mg0.46Mn1.00) [M1,2,3](Mg4.87Mn0.13)(Si8O22)(OH)2, (Z = 2), a = 9.5539(2) Å, b = 18.0293(3) Å, c = 5.2999(1) Å, β = 102.614(2)° from Talcville, New York, has been refined at high temperature using in situ neutron powder diffraction. The P21/m to C2/m phase transition, observed as spontaneous strains +ε1 = −ε2, occurs at ˜107°C. Long-range disordering between Mg2+ and Mn2+ on the M(4) and M(2) sites occurs above 550°C. Mn2+ occupies the M(4) and M(2) sites preferring M(4) with a site-preference energy of 24.6±1.5 kJ mol−1. Disordering induces an increase in XMnM2 and decrease in XMnM4 at elevated temperatures. Upon cooling, the ordered states of cation occupancy are ‘frozen in’ and strains in lattice parameters are maintained, suggesting that re-equilibration during cooling has not taken place.


2019 ◽  
Vol 33 (28) ◽  
pp. 1950339 ◽  
Author(s):  
Y. I. Aliyev ◽  
P. R. Khalilzade ◽  
Y. G. Asadov ◽  
T. M. Ilyasli ◽  
F. M. Mammadov ◽  
...  

AgCu[Formula: see text]Fe[Formula: see text]S compounds were synthesized by partial Cu[Formula: see text][Formula: see text][Formula: see text]Fe replacement in the AgCuS crystal at a concentration range of 0[Formula: see text][Formula: see text][Formula: see text]x[Formula: see text][Formula: see text][Formula: see text]0.03. In the differential thermal analysis spectrum obtained at a temperature range of 300 K[Formula: see text][Formula: see text][Formula: see text]T[Formula: see text][Formula: see text][Formula: see text]1300 K, endoeffect corresponding to the structural phase transition in the AgCuS compound was observed at the temperature T[Formula: see text]=[Formula: see text]938 K. It has been determined that this result is also observed in the AgCu[Formula: see text]Fe[Formula: see text]S compound obtained by partial replacement of Cu atoms by Fe atoms. However, in the compound of AgCu[Formula: see text]Fe[Formula: see text]S this effect was observed at higher temperatures. The thermal capacities and enthalpies of phase transitions were calculated for the given compounds.


2011 ◽  
Vol 217-218 ◽  
pp. 163-168 ◽  
Author(s):  
Lin Xin Tong ◽  
Jin Hong Li ◽  
Jian Cao

A series of gels with 3Al2O3•2SiO2 were prepared by Sol-gel method and heated at several temperatures for 2 h to synthesize Ti, Fe-doped mullite. The powers were characterized by differential thermal analysis (DSC-TG) and X-ray powder diffraction (XRD). Phase separation was promoted by doping both TiO2 and Fe2O3; with increasing the amount of dopant ions the formation temperature of Si-Al spinel decreased and the formation temperature of mullite increased by TiO2 doping but decreased by Fe2O3 doping. The formation temperature of pure mullite was about 1250-1350 °C.


2010 ◽  
Vol 649 ◽  
pp. 493-498 ◽  
Author(s):  
Ana Isabel Fernández-Calvo ◽  
Andrea Niklas ◽  
Jacques Lacaze

Both thermal analysis (TA) and differential thermal analysis (DTA) have been used since long to evaluate latent heat release and solid fraction evolution during solidification of metallic alloys. TA makes use of cooling curves recorded under "natural" cooling while DTA consists in recording the temperature difference between the sample temperature and an inert reference during a controlled cooling, i.e. at imposed constant cooling rate. In both cases, the solid fraction evolution is deduced from a calculation of the latent heat release as estimated by means of a heat transfer model. This paper provides a comparison of such evaluations performed on one Al-Si alloy.


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