Diffraction studies of cubic phase stability in undoped zirconia thin films

2000 ◽  
Vol 15 (2) ◽  
pp. 369-376 ◽  
Author(s):  
S. C. Moulzolf ◽  
R. J. Lad

Pure stoichiometric ZrO2 films were deposited on amorphous silica substrates by electron beam evaporation of Zr in the presence of an electron cyclotron resonance oxygen plasma. Grain size, strain, and texture were analyzed by x-ray diffraction and reflection high-energy electron diffraction. Films grown at room temperature are polycrystalline and exist in the cubic phase. Growth at elevated temperatures produces coexisting cubic and monoclinic phases and shows a maximum critical grain size of ??~10 nm for stabilization of the cubic phase. Pole figure analysis indicates a preferred cubic [200] fiber axis for room-temperature growth and dual monoclinic {111} and in-plane textures for films grown at 400 °C. Postdeposition annealing experiments confirm the existence of a critical grain size and suggest mechanisms for grain growth.

MRS Advances ◽  
2020 ◽  
Vol 5 (29-30) ◽  
pp. 1529-1535 ◽  
Author(s):  
Rijie Zhao ◽  
Jianrong Gao ◽  
Yang Ren

AbstractMelting, solidification and solid-state transformation of the intermetallic Ni3Sn compound were investigated in situ using synchrotron high-energy X-ray diffraction. It was observed that the compound undergoes a hexagonal to cubic transition before melting. In solidification, a disordered cubic phase crystallizes from the liquid at a large undercooling but it is reordered prior to bulk solidification. In melting and solidification, forced or natural flows are active bringing about significant changes of crystal orientations. These in situ observations provided insights into phase transformations of Ni3Sn at elevated temperatures and their roles in formation of metastable microstructure consisting of coarse grains and subgrains.


2012 ◽  
Vol 626 ◽  
pp. 913-917
Author(s):  
W.S. Yeo ◽  
Z. Nur Amirah ◽  
H.S.C. Metselaar ◽  
T.H. Ong

The allotropic phase transformation of cobalt powder prepared by high-energy ball milling was investigated as a function of milling time. Measurement of crystallite size and micro-strain in the powder systems milled for different times were conducted by X-ray diffractometry. The X-ray diffraction (XRD) peaks were analyzed using the Pearson VII profile function in conjunction with Rietveld method. X-ray diffraction line broadening revealed that allotropic transformation between face-centred-cubic phase (fcc) and hexagonal close-packed phase (hcp) in cobalt is grain size dependent and also on the accumulation of structure defects. The results showed that the phase formation of cobalt depends on the mill intensity that influences of both the grain size and the accumulation of structure defects. However, this theory alone is not adequate to explain the effects in this work. It was found that the total surface energy (Ω) theory satisfactorily explains the phase transformation behavior of cobalt. The smaller value of surface energy (Ω) of the fcc crystal than the hcp phase when size decreases may alter the qualitative aspects of the phase formation.


Crystals ◽  
2021 ◽  
Vol 12 (1) ◽  
pp. 35
Author(s):  
Blanca Yamile Rosas ◽  
Alvaro A. Instan ◽  
Karuna Kara Mishra ◽  
S. Nagabhusan Achary ◽  
Ram S. Katiyar

The compound 0.9[KNbO3]-0.1[(BaNi1/2Nb1/2O3−δ] (KBNNO), a robust eco-friendly (lead-free) ferroelectric perovskite, has diverse applications in electronic and photonic devices. In this work, we report the dielectric, ferroelectric, and structural phase transitions behavior in the KBNNO compound using dielectric, X-ray diffraction, and Raman studies at ambient and as a function of temperature. Analyses of X-ray diffraction (XRD) data at room temperature (rtp) revealed the orthorhombic phase (sp. Gr. Amm2) of the compound with a minor secondary NiO cubic phase (sp. Gr. Fm3m). A direct optical band gap Eg of 1.66 eV was estimated at rtp from the UV–Vis reflectance spectrum analysis. Observation of non-saturated electric polarization loops were attributed to leakage current effects pertaining to oxygen vacancies in the compound. Magnetization studies showed ferromagnetism at room temperature (300 K) in this material. XRD studies on KBNNO at elevated temperatures revealed orthorhombic-to-tetragonal and tetragonal-to-cubic phase transitions at 523 and 713 K, respectively. Temperature-dependent dielectric response, being leaky, did not reveal any phase transition. Electrical conductivity data as a function of temperature obeyed Jonscher power law and satisfied the correlated barrier-hopping model, indicating dominance of the hopping conduction mechanism. Temperature-dependent Raman spectroscopic studies over a wide range of temperature (82–673 K) inferred the rhombohedral-to-orthorhombic and orthorhombic-to-tetragonal phase transitions at ~260, and 533 K, respectively. Several Raman bands were found to disappear, while a few Raman modes such as at 225, 270, 289, and 831 cm−1 exhibited discontinuity across the phase transitions at ~260 and 533 K.


2000 ◽  
Vol 639 ◽  
Author(s):  
Ryuhei Kimura ◽  
Kiyoshi Takahashi ◽  
H. T. Grahn

ABSTRACTAn investigation of the growth mechanism for RF-plasma assisted molecular beam epitaxy of cubic GaN films using a nitrided AlGaAs buffer layer was carried out by in-situ reflection high energy electron diffraction (RHEED) and high resolution X-ray diffraction (HRXRD). It was found that hexagonal GaN nuclei grow on (1, 1, 1) facets during nitridation of the AlGaAs buffer layer, but a highly pure, cubic-phase GaN epilayer was grown on the nitrided AlGaAs buffer layer.


2010 ◽  
Vol 654-656 ◽  
pp. 1106-1109
Author(s):  
Ya Qiong He ◽  
Chang Hui Mao ◽  
Jian Yang

Nanocrystalline Fe-Co alloy powders, which were prepared by high-energy mechanical milling, were nitrided under the mixing gas of NH3/H2 in the temperature range from 380°C to 510°C. X-ray diffraction (XRD) was used to analyze the grain size and reaction during the processing. The magnetic properties of the nitrided powders were measured by Vibrating Sample Magnetometer (VSM). The results show that with the appearance of Fe4N phase after nitride treatment, and the grain-size of FeCo phase decreases with the increase of nitridation temperature between 380°C to 450°C.The saturation magnetization of nitrided alloy powder treated at 480°C is about 18% higher than that of the initial Fe-Co alloy powder, accompanied by the reduction of the coercivity. Transmission electron microscope (TEM) was used, attempting to further analyze the effect of Fe4N phase on microstructure and magnetic properties of the powder mixtures.


2011 ◽  
Vol 479 ◽  
pp. 54-61 ◽  
Author(s):  
Fei Wang ◽  
Ya Ping Wang

Microstructure evolution of high energy milled Al-50wt%Si alloy during heat treatment at different temperature was studied. Scanning electron microscope (SEM) and X-ray diffraction (XRD) results show that the size of the alloy powders decreased with increasing milling time. The observable coarsening of Si particles was not seen below 730°C in the high energy milled alloy, whereas, for the alloy prepared by mixed Al and Si powders, the grain growth occurred at 660°C. The activation energy for the grain growth of Si particles in the high energy milled alloy was determined as about 244 kJ/mol by the differential scanning calorimetry (DSC) data analysis. The size of Si particles in the hot pressed Al-50wt%Si alloy prepared by high energy milled powders was 5-30 m at 700°C, which was significantly reduced compared to that of the original Si powders. Thermal diffusivity of the hot pressed Al-50wt%Si alloy was 55 mm2/s at room temperature which was obtained by laser method.


2006 ◽  
Vol 524-525 ◽  
pp. 619-624 ◽  
Author(s):  
Mark R. Terner ◽  
Peter Hedström ◽  
Jonathan Almer ◽  
J. Ilavsky ◽  
Magnus Odén

Residual stresses and microstructural changes during phase separation in Ti33Al67N coatings were examined using microfocused high energy x-rays from a synchrotron source. The transmission geometry allowed simultaneous acquisition of x-ray diffraction data over 360° and revealed that the decomposition at elevated temperatures occurred anisotropically, initiating preferentially along the film plane. The as-deposited compressive residual stress in the film plane first relaxed with annealing, before dramatically increasing concurrently with the initial stage of phase separation where metastable, nm-scale c-AlN platelets precipitated along the film direction. These findings were further supported from SAXS analyses.


1995 ◽  
Vol 403 ◽  
Author(s):  
D. V. Dimitrov ◽  
A. S. Murthy ◽  
G. C. Hadjipanayis ◽  
C. P. SWANN

AbstractFe-O and Co-O films were prepared by DC magnetron sputtering in a mixture of Ar and O2 gases. By varying the oxygen to argon ratio, oxide films with stoichiometry FeO, Fe3O4, α-Fe2O3, CoO and Co3O4 were produced. TEM studies showed that the Fe – oxide films were polycrystalline consisting of small almost spherical grains, about 10 nm in size. Co-O films had different microstructure with grain size and shape dependent on the amount of oxygen. X-ray diffraction studies showed that the grains in Fe-O films were randomly oriented in contrast to Co-O films in which a <111> texture was observed. Pure FeO and α-Fe2O3 films were found to be superparamagnetic at room temperature but strongly ferromagnetic at low temperatures in contrast to the antiferromagnetic nature of bulk samples. A very large shift in the hysteresis loop, about 3800 Oe, was observed in field cooled Co-CoO films indicating the presence of a large unidirectional exchange anisotropy.


2006 ◽  
Vol 301 ◽  
pp. 177-180 ◽  
Author(s):  
Yuichiro Kuroki ◽  
Tomoichiro Okamoto ◽  
Masasuke Takata

Copper aluminum disulfide (CuAlS2) powders were synthesized in an evacuated ampoule at elevated temperatures. X-ray diffraction analysis revealed that the powders heated at temperatures higher than 800oC were single-phase CuAlS2. In the cathodoluminescence (CL) spectra measured at room temperature, the powders heated at temperatures higher than 600oC exhibited a visible emission peak at approximately 1.8 eV and a distinct ultraviolet emission peak at 3.45 eV. The powder heated at 700oC showed the maximum intensity of ultraviolet emission which is considered to be associated with excitons.


Author(s):  
Alexander M. Antipin ◽  
Olga A. Alekseeva ◽  
Natalia I. Sorokina ◽  
Alexandra N. Kuskova ◽  
Michail Yu. Presniakov ◽  
...  

The La2Mo2O9(LM) and Pr2Mo2O9(PM) single crystals are studied using precision X-ray diffraction and high-resolution transmission microscopy at room temperature. The crystal structures are determined in the space groupP213. La and Pr atoms, as well as Mo1 and O1 atoms, are located in the vicinity of the threefold axes rather than on the axes as in the high-temperature cubic phase. In both structures studied, the O2 and O3 positions are partially occupied. The coexistence of different configurations of the Mo coordination environment facilitates the oxygen-ion migration in the structure. Based on the X-ray data, the activation energies of O atoms are calculated and the migration paths of oxygen ions in the structures are analysed. The conductivity of PM crystals is close to that of LM crystals. The O2 and O3 atoms are the main contributors to the ion conductivity of LM and PM.


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