• Journal of the Mineralogical Society of Korea
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• 제26권1호
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• pp.27-34
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• 2013

X-ray powder diffraction is one of the most powerful techniques for qualitative and quantitative analysis of crystalline compounds. Thus, there exist a number of different methods for quantifying mineral mixtures using X-ray diffraction pattern. We present here the use of Rietveld and PONKCS (partial or no known crystal structure) methods for quantification of amorphous and crystallized mineral phases in synthetic mixtures of standard minerals (amorphous silica, quartz, mullite and corundum). Pawley phase model of amorphous silica was successfully built from the pattern of 100 wt% amorphous silica and internal standard-spiked samples by PONKCS approach. The average of absolute bias for quantities of amorphous silica was 1.85 wt%. The larger bias observed for lower quantities of amorphous silica is probably explained by low intensities of diffraction pattern. Averages of absolute bias for minerals were 0.53 wt% for quartz, 0.87 wt% for mullite and 0.57 wt% for corundum, respectively. The PONKCS approach achieved improved quantitative results compared with classical Rietveld method by using an internal standard.

• Journal of Magnetics
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• 제16권1호
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• pp.27-30
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• 2011

Nano-sized manganese ferrite powders and films, $MnFe_2O_4$, were fabricated by the sol-gel method, and the effects of annealing temperature on the crystallographic and magnetic properties were studied by using X-ray diffractometry, field emission scanning electron microscopy, M$\"{o}$ssbauer spectroscopy, and vibrating sample magnetometry. X-ray diffraction spectroscopy of powder samples annealed above 523 K indicated the presence of spinel structure, and the film samples annealed above 773 K also had spinel structure. The particle size increased with the annealing temperature. For the powder samples, the Mossbauer spectra annealed above 573 K could be fitted as the superposition of two Zeeman sextets due to the tetrahedral and octahedral sites of $Fe^{3+}$ ions. Using the M$\"{o}$ssbauer subspectrum area ratio the cation distribution could be written as ($Mn_{0.52}Fe_{0.48}$) $[Mn_{0.48}Fe_{1.52}]$ $O_4$. However the spectrum annealed at 523 K only showed as a doublet due to a superparamagnetic phase. As the annealing temperature was increased, the saturation magnetization and the corecivity of the powder samples increased, as did the coercivity of film samples.

• Korean Journal of Crystallography
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• 제3권2호
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• pp.129-132
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• 1992

The multiplicity factor, which is defined as the number of different planes in a form having identical interplanar spacing and identical intensity, is tabulated here for the eleven Laue groups on the basis of their symmetries.

• Journal of Powder Materials
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• 제3권2호
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• pp.91-96
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• 1996

The effect of vacuum annealing on the oxidation behavior of milled WC-15%Co powder mixture has been studied. A cobalt component in the milled powder mixture was oxidized preferentially above 175$^{\circ}C$ in air. The specimens showed a steady increase in weight at 175$^{\circ}C$ but did constant weight followed by rapid increase in specimen weight at the beginning above 20$0^{\circ}C$. Oxidation of the milled powder mixture was significantly suppressed by vacuum annealing at 30$0^{\circ}C$ for 10 h. Suppression of oxidation by vacuum annealing and different oxidation behaviors of the milled powder mixture between 175$^{\circ}C$ and 20$0^{\circ}C$, were attributed to removal of strain energy stored in the cobalt powder during vacuum annealing or oxidation treatment above 20$0^{\circ}C$. The role of stored strain energy on oxidation of milled WC-15%Co powder mixture was proved by X-ray diffraction method and differential thermal analysis.

• Journal of Powder Materials
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• 제5권4호
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• pp.273-278
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• 1998

$De-NO_x$ transition metals(Cu, Co)/ZSM-5 catalyst was made by mechanical alloying method, and their microstructures and repeated usage-properties were investigated by scanning electron microscopy, transmission electron microscopy and X-ray diffraction. The conversions ability of NO in the catalyst was measured. A part of ZSM-5 in CO/ZSM-5 composite powders was amorphous and the amorphous phase became less stable with increasing Co content. Conversion ability of NO in 10Cu/ZSM-5 powders decreased from 89% to 12% and that in 10Co/ZSM-5 decreased from 22% to 17% by 7 times conversion tests.

• The Korean Journal of Ceramics
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• 제5권4호
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• pp.341-347
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• 1999

An ambiguity on the correct room temperature structure of $Bi_5Ti_3FeO_{15}$ was resolved using a combined Rietveld refinement of neutron and X-ray diffraction. The structure of this compound has been reported to have a space group of F2mm (adopting 2-fold rotation symmetry along the c-axis) or A21am. However, our diffraction, study reveals that some reflections would violate F-centering and confirm that the belong to $A2_1$am. Out refinement with the space group of $A2_1$am converged at $R_p=6.85%, R_wp=9.23%$ and $\chi^2$=1.66 for an isotropic temperature model with 85 variables. The lattice constants are a=5.4677(1) $\AA$, b=5.4396(1) $\AA$, and c=41.2475(8)$\AA$. In structure, Ti/Fe atoms at the oxygen octahedral sites of the perovskite unit are completely disordered, resulting in that these atoms are transparent in neutron diffraction. The octahedra of the perovskite unit are relatively displaced along the a-axis against the Bi atoms, which contribute as a major component to the spontaneous polarization of $Bi_5Ti_3FeO_{15}$.

• Clean Technology
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• 제27권3호
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• pp.240-246
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• 2021

The waste etching solution for chip on film (COF) contained about 3.5% copper, and it was recovered through cementation using iron samples. The effect of cementation with plate, chip, and powder iron samples was investigated. The molar ratio (m/r) of iron to copper was used as a variable in order to increase the recovery rate of copper. As the molar ratio increased, the copper content in the solution rapidly decreased at the beginning of the cementation reaction. Before and after the reaction, the copper content of the solution was determined by Inductively Coupled Plasma (ICP) using copper concentration according to time. After cementation at room temperature for 1 hour, the recovery rate of copper had increased the most in the iron powder sample, having the largest specific surface area of the samples, followed by the chip and plate samples. The recovered copper powder was characterized for its crystalline phase, morphology, and elemental composition by X-ray diffraction (XRD), scanning electron microscopy (SEM), and Energy-dispersive X-ray spectroscopy (EDS), respectively. Copper and unreacted iron were present together in the iron powder samples. The optimum condition for recovering copper was obtained using iron chips with a molar ratio of iron to copper of 4 giving a recovery rate of about 98.4%.

• Journal of Industrial Technology
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• 제41권1호
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• pp.25-30
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• 2021

Hydride-dehydride process for efficient recycling of tantalum (Ta) is used for manufacturer of Ta powder. In case of metal powder, Impurities as like nitride, oxygen, hydrogen is decreased of physical properties. For manufacture of Ta powder, control of theses impurities is important. In this study, to decreased of impurities on Ta powder using HDH process optimize dehydride condition. Dehydration behavior of Ta is depended on temperature, time, and atmosphere. Phase transition of Ta hydride is analyzed by X-ray diffraction (XRD). Concentration of hydrogen is decreased with temperature increased. At high temperature, concentration of hydrogen in Ta is similar according to time increased. Size and morphology of powder is not observed after dehydride. Ta powder, which is less than 20 um, concentration of hydrogen under 800 ppm is obtain.

• Journal of Powder Materials
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• 제6권3호
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• pp.238-245
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• 1999

The preparation of $n-TiO_2$ powder by the Chemical Vapor Synthesis process (CVS) was studied using the liquid metal organic precursor (TTIP). The residence time and the collection methods were considered as main processing variables through the experiments. The CVS equipment consisted of a micropump and a flashvaporizer, a tube furnace and a tubular collection device. The synthesis was performed at $1000^{\circ}C$ with various sets of collection zone. The residence time and the total system pressure were controlled in the range of 3~20 ms and 10 mbar, respectively. Nitrogen adsorption, X-ray diffraction and electron microscopy were used to determine particle size, specific surface area and crystallographic structure. The grain size of the as-prepared $n-TiO_2$ powder was in the range of 2~8 nm for all synthesis parameters and the powder exhibited only little agglomeration. The relationship between particle characteristics and the processing variables is reviewed based on simple growth model.

• Journal of Powder Materials
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• 제21권2호
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• pp.93-96
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• 2014

Cobalt coated tungsten carbide-cobalt composite powder has been prepared through wet chemical reduction method. The cobalt sulfate solution was converted to the cobalt chloride then the cobalt hydroxide. The tungsten carbide powders were added in to the cobalt hydroxide, the cobalt hydroxide was reduced and coated over tungsten carbide powder using hypo-phosphorous acid. Both the cobalt and the tungsten carbide phase peaks were evident in the tungsten carbide-cobalt composite powder by X-ray diffraction. The average particle size measured via scanning electron microscope, particle size analysis was around 380 nm and the thickness of coated cobalt was determined to be 30~40 nm by transmission electron microscopy.