Modulated Structures in PbHfO3 Crystals at High-Pressure-High-Temperature Conditions

2018 ◽  
Vol 386 ◽  
pp. 149-155 ◽  
Author(s):  
Maria Knjazeva ◽  
Yurii Bronwald ◽  
Daria Andronikova ◽  
Georgiy Lityagin ◽  
Alexey Bosak ◽  
...  
Keyword(s):  
Intermediate Phase ◽  
Temperature Phase ◽  
X Ray Diffraction ◽  
Simultaneous Application ◽  
Intermediate Phases ◽  
High Pressure High Temperature ◽  
Modulated Structures ◽  
Higher Temperature ◽  
Lower Temperature ◽  
Oxygen Framework

Lead hafnate single crystals were characterized using single crystal x-ray diffraction under simultaneous application of hydrostatic pressure and high temperatures. The information on the structure of two intermediate phases, situated between antiferroelectric and paraelectric phases in the pressure-temperature phase diagram, has been obtained. The lower-temperature intermediate phase is characterized by incommensurate displacive modulations in Pb sublattice. The higher-temperature intermediate phase is characterized by oxygen framework distortion, primarily in the form of anti-phase tilts of the oxygen octahedra, which is also present in the lower-temperature intermediate phase.

Differences and similarities among hypoxanthinium nitrate hydrate structures

2019 ◽  
Vol 75 (8) ◽  
pp. 1036-1044 ◽  
Author(s):  
Małgorzata Katarzyna Cabaj ◽  
Roman Gajda ◽  
Anna Hoser ◽  
Anna Makal ◽  
Paulina Maria Dominiak
Keyword(s):  
Room Temperature ◽  
Temperature Phase ◽  
X Ray Diffraction ◽  
Acta Cryst ◽  
X Ray ◽  
Nitrate Hydrate ◽  
Different Temperatures ◽  
Lower Temperature ◽  
Low Temperature Phase ◽  
Nitrate Anions

Crystals of hypoxanthinium (6-oxo-1H,7H-purin-9-ium) nitrate hydrates were investigated by means of X-ray diffraction at different temperatures. The data for hypoxanthinium nitrate monohydrate (C5H5N4O+·NO3 −·H2O, Hx1) were collected at 20, 105 and 285 K. The room-temperature phase was reported previously [Schmalle et al. (1990). Acta Cryst. C46, 340–342] and the low-temperature phase has not been investigated yet. The structure underwent a phase transition, which resulted in a change of space group from Pmnb to P21/n at lower temperature and subsequently in nonmerohedral twinning. The structure of hypoxanthinium dinitrate trihydrate (H3O+·C5H5N4O+·2NO3 −·2H2O, Hx2) was determined at 20 and 100 K, and also has not been reported previously. The Hx2 structure consists of two types of layers: the `hypoxanthinium nitrate monohydrate' layers (HX) observed in Hx1 and layers of Zundel complex H3O+·H2O interacting with nitrate anions (OX). The crystal can be considered as a solid solution of two salts, i.e. hypoxanthinium nitrate monohydrate, C5H5N4O+·NO3 −·H2O, and oxonium nitrate monohydrate, H3O+(H2O)·NO3 −.

Large-scale and facile fabrication of PbSe nanostructures by selenization of a Pb sheet

2015 ◽  
Vol 08 (05) ◽  
pp. 1550063 ◽  
Author(s):  
Sara Hoomi ◽  
Ramin Yousefi ◽  
Farid Jamali-Sheini ◽  
Abdolhossein Sáaedi ◽  
Mohsen Cheraghizade ◽  
...  
Keyword(s):  
Large Scale ◽  
Chemical Vapor ◽  
Infrared Region ◽  
Photoelectron Spectra ◽  
X Ray Diffraction ◽  
X Ray ◽  
Facile Fabrication ◽  
Higher Temperature ◽  
Set Up ◽  
Lower Temperature

PbSe nanostructures were synthesized by selenization of lead sheets in a chemical vapor deposition (CVD) set-up under a selenium ambiance. The lead sheets were placed in the different temperature zones, between 300°C and 450°C. Field emission scanning electron microscope (FESEM) images showed that, PbSe nanostructures grown on the lead sheets with different morphologies. PbSe nanostructures with flakes shape were grown on the lead sheets that were placed in the lower temperature, while PbSe nanocubes and nanorods, which were grown on the nanocubes, were grown on the lead sheets in the higher temperature. The phase and composition of the product were identified by X-ray diffraction (XRD) pattern and X-ray photoelectron spectra (XPS). The XRD and XPS results showed that, the PbSe phase was started to form after 350°C and completed at 450°C. However, the XPS results showed that the Se concentration was different in the samples. In addition, Raman measurements confirmed the XRD and XPS results and indicated three Raman active modes, which belonged to PbSe phase for the nanostructures. The optical properties of the products were characterized by UV–Vis. The optical characterization results showed a band gap for the PbSe nanostructures in the infrared region.

Effect of Aging Treatment on Damping Capacity in Mncunife Alloy

2012 ◽  
Vol 246-247 ◽  
pp. 1158-1162
Author(s):  
Xu Fu ◽  
Ning Li ◽  
Yu Hua Wen ◽  
Jing Teng ◽  
Ying Zhang
Keyword(s):  
Electron Microscope ◽  
Aging Treatment ◽  
Damping Capacity ◽  
Torsion Pendulum ◽  
X Ray Diffraction ◽  
X Ray ◽  
Transmission Electron ◽  
Higher Temperature ◽  
Lower Temperature ◽  
The Relationship

M2052 alloys with various aging treatments are obtained in order to investigate the relationship between aging treatment and damping capacity by the torsion pendulum, X-Ray Diffraction (XRD) and Transmission Electron Microscope (TEM) methods. The results show that M2052 can obtain high damping capacity (δ>0.2) when aged at a range from 400°C to 450°C, and the damping capacity after aged at a lower temperature is higher than that aged at a higher temperature for the maximum values. TEM and XRD results show that fcc-fct transformation occurs after aging treatment. The volumes of fct structures are one of reason to affect the damping capacity in M2052 alloy. The better understanding aging treatment could promote the applications of M2052 alloy.

Ab initio structure determination and Rietveld refinement of a high-temperature phase of zirconium hydrogen phosphate and a new polymorph of zirconium pyrophosphate from in situ temperature-resolved powder diffraction data

2000 ◽  
Vol 56 (4) ◽  
pp. 618-625 ◽  
Author(s):  
Anne Marie Krogh Andersen ◽  
Poul Norby
Keyword(s):  
Powder Diffraction ◽  
Diffraction Data ◽  
Intermediate Phase ◽  
Temperature Phase ◽  
Powder Diffraction Data ◽  
Hydrogen Phosphate ◽  
Intermediate Phases ◽  
Zirconium Pyrophosphate ◽  
Phosphate Groups

The collected in situ temperature-resolved synchrotron powder data revealed that the transformation of the recently reported three-dimensional τ-Zr(HPO4)2 to cubic ZrP2O7 goes through two intermediate phases. The first intermediate phase, ρ-Zr(HPO4)2, is formed in a reversible phase transition at 598 K, which involves both rearrangement and disordering of the hydrogen phosphate groups of τ-Zr(HPO4)2. At 688 K condensation of the hydrogen phosphate groups leads to the formation of the second intermediate, a new polymorph of zirconium pyrophosphate (β-ZrP2O7). Heating above 973 K results in the gradual transformation of β-ZrP2O7 to cubic zirconium pyrophosphate (α-ZrP2O7). The crystal structures of the two intermediate phases were solved from the in situ powder diffraction data using direct methods and refined using the Rietveld method. Both phases are orthorhombic, space group Pnnm and Z = 2. The lattice parameters for the two phases are: ρ-Zr(HPO4)2: a = 8.1935 (2), b = 7.7090 (2), c = 5.4080 (1) Å; β-ZrP2O7: a = 8.3127 (5), b = 6.6389 (4), c = 5.3407 (3) Å. The formation mechanism for the new zirconium pyrophosphate polymorph, β-ZrP2O7, is discussed in relation to structurally restricted soft chemistry.

Reaction Mechanism of LiFePO4/C Cathode Materials Synthesized by Carbothermal Reduction Method

2010 ◽  
Vol 178 ◽  
pp. 248-253 ◽  
Author(s):  
Li Min Gao ◽  
Guang Chuan Liang ◽  
Li Wang ◽  
Xiao Ke Zhi ◽  
Xiao Fei Jie
Keyword(s):  
Carbothermal Reduction ◽  
Reduction Method ◽  
Intermediate Phase ◽  
Raw Materials ◽  
X Ray Diffraction ◽  
Thermo Gravimetric ◽  
X Ray ◽  
Reducing Atmosphere ◽  
Carbothermal Reduction Method ◽  
Lower Temperature

LiFePO4/C powders were synthesized by carbothermal reduction method using Li2CO3 (A.R), FePO4 (A.R) and glucose as raw materials. In this paper, the carbothermal reaction courses were characterized by Thermo-gravimetric (TG)/Differential Thermal Analysis (DTA), X-ray diffraction (XRD) and Fourier transform infrared (FTIR). It was found that the different synthesis temperatures and the different reducing atmosphere in systems could lead to different reactions, resulting in different final products and a direct impact on material performance. At around 350 °C LiFePO4 is directly formed without intermediate phase. In lower temperature of 400-500 °C, the sample included a certain amount of Li3PO4 and Fe2O3 impurity phases. When calcination temperature rose to 550 °C, the sample could be pure LiFePO4 phase.

The occurrence of iron silicides in a fulgurite: Implications for fulgurite genesis

2020 ◽  
Vol 58 (1) ◽  
pp. 115-123
Author(s):  
Christopher J. Stefano ◽  
Stephen A. Hackney ◽  
Anthony R. Kampf
Keyword(s):  
Lake Michigan ◽  
Rapid Quenching ◽  
Lightning Strike ◽  
Temperature Phase ◽  
X Ray Diffraction ◽  
Scattered Electron ◽  
Iron Silicides ◽  
Natural Glass ◽  
Lower Temperature ◽  
Spherical Droplets

ABSTRACT Rapidly formed eutectic textures are observed in Fe silicides in a fulgurite from Michigan. The 14 cm-diameter fulgurite was formed in sandy glacial till in 2014 near Houghton Lake, Michigan. Spherical droplets of iron silicides up to ∼200 μm in diameter were found in the natural glass. Back-scattered electron images of some droplets show a eutectic intergrowth texture of two iron silicides with individual crystals up to ∼1 μm in maximum dimension. X-ray diffraction study showed the specimens to be an intergrowth of naquite (FeSi) and linzhiite (FeSi2) or naquite and xifengite (Fe5Si3). Droplets also contain minor native silicon, Fe-Ti silicides, and/or other Ti- rich phases which were discovered during TEM observations. It is important to note that the lower-temperature phase luobusaite (Fe3Si7) was not observed in any droplets, indicating rapid quenching of the fulgurite, consistent with a natural origin during a lightning strike as opposed to an artificial origin, e.g., resulting from a downed power line.

An investigation into the temperature phase transitions of synthesized materials with Al- and Mg-doped lithium manganese oxide spinels by in situ powder X-ray diffraction

2016 ◽  
Vol 32 (1) ◽  
pp. 23-30
Author(s):  
C. D. Snyders ◽  
E. E. Ferg ◽  
D. Billing
Keyword(s):  
Phase Transitions ◽  
Intermediate Phase ◽  
Phase Changes ◽  
Synthesis Process ◽  
Temperature Phase ◽  
Gravimetric Analysis ◽  
Spinel Oxide ◽  
X Ray Diffraction ◽  
X Ray

Three spinel materials were prepared and characterized by in situ powder X-ray diffraction (PXRD) techniques to track their phase changes that occurred in the typical batch synthesis process from a sol–gel mixture to the final crystalline spinel oxide. The materials were also characterized by thermal gravimetric analysis, whereby the materials decomposition mechanisms that were observed as the precursor, was gradually heated to the final oxide. The results showed that all the materials achieved their total weight loss at about 400 °C. The in situ PXRD analysis showed the progression of the phase transitions where certain of the materials changed from a crystalline precursor to an amorphous intermediate phase and finally to the spinel cathode oxide (Li1.03Mg0.2Mn1.77O4). For other materials, the precursor would start as an amorphous phase and upon heating, convert into an impure intermediate phase (Mn2O3) before forming the final spinel oxide (Li1.03Mn1.97O4). On the other hand, the LiAl0.4Mn1.6O4 would start with an amorphous precursor, with no intermediate phases and immediately formed the final spinel oxide phase. The in situ PXRD study also showed the increases in the materials respective lattice parameters of the crystalline unit cells upon heating and the significant increases in their crystallite sizes when heated above 600 °C.

scholarly journals Magnetic charge and ordering in kagome spin ice

2012 ◽  
Vol 370 (1981) ◽  
pp. 5718-5737 ◽  
Author(s):  
Gia-Wei Chern ◽  
Oleg Tchernyshyov
Keyword(s):  
Intermediate Phase ◽  
Numerical Study ◽  
Magnetic Ordering ◽  
Charge Order ◽  
Spin Correlation ◽  
Temperature Phase ◽  
Spin Ice ◽  
Universality Classes ◽  
Lower Temperature ◽  
Two Stages

We present a numerical study of magnetic ordering in spin ice on kagome, a two-dimensional lattice of corner-sharing triangles. The magnet has six ground states and the ordering occurs in two stages, as one might expect for a six-state clock model. In spin ice with short-range interactions up to second neighbours, there is an intermediate critical phase separated from the paramagnetic and ordered phases by Kosterlitz–Thouless (KT) transitions. In dipolar spin ice, the intermediate phase has long-range order of staggered magnetic charges. The high- and low-temperature phase transitions are of the Ising and 3-state Potts universality classes, respectively. Freeze-out of defects in the charge order produce a very large spin correlation length in the intermediate phase. As a result of that, the lower-temperature transition appears to be of the KT type.

TEM studies of the ThMn12–type and Th2Zn17–type phases in the Nd-Fe-Ti system

2013 ◽  
Vol 19 (S4) ◽  
pp. 129-130
Author(s):  
D. Nunes ◽  
A.P. Gonçalves ◽  
P.A. Carvalho
Keyword(s):  
Permanent Magnets ◽  
Experimental Studies ◽  
Temperature Phase ◽  
X Ray Diffraction ◽  
Transmission Electron ◽  
Elemental Analyses ◽  
Second Phases ◽  
Two Phases ◽  
Lower Temperature ◽  
Rare Earth Intermetallic Compounds

Rare-earth intermetallic compounds with high Fe concentrations and adopting the ThMn12–type and Th2Zn17-type structures have attracted considerable attention in the field of permanent magnets. A large number of experimental studies has been done on these compounds, which are usually measured on alloys structurally characterized only by powder X-ray diffraction (XRD). However, the materials are often multiphasic and their quenched or annealed microstructures evidence homogenization ranges, second phases (resulting from segregation) and on-going phase transformations that may not be easily detectable by XRD. Additional microstructural studies on these systems are therefore required.Among the Fe-based systems, the ThMn12–type and Th2Zn17–type structures usually require stabilization by a third element, such as Ti. In the present work Nd:11Fe:Ti has been prepared by melting Nd, Fe and Ti in an arc furnace followed by subsequent splat-quenching and/or annealing treatments. The resulting materials have been characterized by XRD, scanning and transmission electron microscopy coupled with energy dispersive spectroscopy.The results have shown that the presence of α-Fe(Ti) could not be avoided during the solidification of the Nd:11Fe:Ti alloy. Furthermore, the microstructure morphologies and elemental analyses showed that at moderate cooling rates a secondary crystallization phase of Th2Zn17–type appeared in the Nd:11Fe:Ti alloy as result of a peritectic reaction. This lower temperature phase was however not detected in the splat-quenched material, where the high cooling rate route suppressed its crystallization. Nevertheless during a subsequent heat-treatment at 800 ºC the following decomposition took place: NdFe11Ti → Nd2(Fe,Ti)17 + α-Fe(Ti) + Fe2Ti. This reaction had already been proposed by Jang and Stadelmaier, who suggested that the NdFe11Ti compound is unstable at temperatures below 1000 °C. The current study shows that this transformation results in the fine lamellar intergrowth of the Th2Zn17-type phase in ThMn12-type grains, displaying random distribution of planar defects (Figure 1). The reciprocal space of the combined parent and intergrown phases has been mapped through a series of 3-D microdiffraction experiments (Figure 2). This allowed to establish that the preferred orientation relation between the two phases is (020)1:12//(003)2:17 and [100]1:12//[110]2:17, with the invariant plane sitting at 1:12//(333)2:17 planes.The work was supported by the Portuguese Science Foundation through the CTM/48617/2002, PEst-OE/CTM-UI0084/2011 and CFMC-PEst-OE/FIS/UI0261/2011 grants.

Sign in / Sign up

Export Citation Format

Share Document