• Title/Summary/Keyword: X-ray diffraction analysis(XRD)

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Preparation of Ultra Fine Ammonium Perchlorate Crystals (초미세 크기의 과염소산암모늄 결정체 제조)

  • 김준형;임유진
    • Journal of the Korean Society of Propulsion Engineers
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    • v.8 no.1
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    • pp.1-7
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    • 2004
  • The precipitation of ultra fine ammonium perchlorate(UFAP) crystals from the N-methyl pyrrolidone(NMP) solutions of ammonium perchlorate(AP) was studied. The characteristics of the precipitated crystals were investigated by means of scanning electron micrograph(SEM), X-ray diffraction(XRD), and thermogravimetric analysis(TGA). When chloroform, methylene chloride and toluene were the precipitants, the product crystals had a mean particle size less than 2$\mu\textrm{m}$. The crystallographical property and thermal decomposition behavior of the prepared UFAP were almost the same as those of the commercial AP.

Effect of Basal-plane Stacking Faults on X-ray Diffraction of Non-polar (1120) a-plane GaN Films Grown on (1102) r-plane Sapphire Substrates

  • Kim, Ji Hoon;Hwang, Sung-Min;Baik, Kwang Hyeon;Park, Jung Ho
    • JSTS:Journal of Semiconductor Technology and Science
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    • v.14 no.5
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    • pp.557-565
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    • 2014
  • We report the effect of basal-plane stacking faults (BSFs) on X-ray diffraction (XRD) of non-polar (11$\underline{2}$0) a-plane GaN films with different $SiN_x$ interlayers. Complete $SiN_x$ coverage and increased three-dimensional (3D) to two-dimensional (2D) transition stages substantially reduce BSF density. It was revealed that the Si-doping profile in the Si-doped GaN layer was unaffected by the introduction of a $SiN_x$ interlayer. The smallest in-plane anisotropy of the (11$\underline{2}$0) XRD ${\omega}$-scan widths was found in the sample with multiple $SiN_x$ layers, and this finding can be attributed to the relatively isotropic GaN mosaic resulting from the increase in the 3D-2D growth step. Williamson-Hall (WH) analysis of the (h0$\underline{h}$0) series of diffractions was employed to determine the c-axis lateral coherence length (LCL) and to estimate the mosaic tilt. The c-axis LCLs obtained from WH analyses of the present study's representative a-plane GaN samples were well correlated with the BSF-related results from both the off-axis XRD ${\omega}$-scan and transmission electron microscopy (TEM). Based on WH and TEM analyses, the trends in BSF densities were very similar, even though the BSF densities extracted from LCLs indicated that the values were reduced by a factor of about twenty.

On the Crystalline Structures of Iron Oxides formed During Removal Process of Iron in Water (수중의 철 제거 시 생기는 산화철의 결정구조에 관한 연구)

  • Cho, Bong-Yeon
    • KSCE Journal of Civil and Environmental Engineering Research
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    • v.26 no.1B
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    • pp.107-111
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    • 2006
  • The samples collected from two reactors are analyzed by X-ray diffraction and M$\ddot{o}$ssbauer spectroscopy in this study. It is concluded that the iron oxide crystal attached on anthracite media which possesses catalytic ability is identified to be Ferrihydrite, regardless of the value of pH from the analysis of the iron oxide. Iron oxide in Batch reactor is identified to be Microcrystalline goethite.

Analysis of the Change in Microstructures of Nano Copper Powders During the Hydrogen Reduction using X-ray Diffraction Patterns and Transmission Electron Microscope, and the Mechanical Property of Compacted Powders (X-선 회절 패턴 측정과 투과 전자 현미경을 이용한 구리 나노분말의 수소 환원 처리 시 발생하는 미세조직 변화 및 치밀화 시편의 물성 분석)

  • Ahn, Dong-Hyun;Lee, Dong Jun;Kim, Wooyeol;Park, Lee Ju;Kim, Hyoung Seop
    • Journal of Powder Materials
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    • v.21 no.3
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    • pp.207-214
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    • 2014
  • In this study, nano-scale copper powders were reduction treated in a hydrogen atmosphere at the relatively high temperature of $350^{\circ}C$ in order to eliminate surface oxide layers, which are the main obstacles for fabricating a nano/ultrafine grained bulk parts from the nano-scale powders. The changes in composition and microstructure before and after the hydrogen reduction treatment were evaluated by analyzing X-ray diffraction (XRD) line profile patterns using the convolutional multiple whole profile (CMWP) procedure. In order to confirm the result from the XRD line profile analysis, transmitted electron microscope observations were performed on the specimen of the hydrogen reduction treated powders fabricated using a focused ion beam process. A quasi-statically compacted specimen from the nano-scale powders was produced and Vickers micro-hardness was measured to verify the potential of the powders as the basis for a bulk nano/ultrafine grained material. Although the bonding between particles and the growth in size of the particles occurred, crystallites retained their nano-scale size evaluated using the XRD results. The hardness results demonstrate the usefulness of the powders for a nano/ultrafine grained material, once a good consolidation of powders is achieved.

A Preliminary Study on the Fire Safety Testing Method for Fire-resistance Paints Using an X-ray Analysis Method (X-선 분석법을 이용한 내화도료의 화재안전성 평가 방법에 관한 기초연구)

  • Shim, Ji-Hun;Cho, Nam-Wook;Kim, Kang-Woo
    • Fire Science and Engineering
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    • v.28 no.5
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    • pp.58-63
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    • 2014
  • Fire-resistance paints are supposed to become intumescent and diminish heat transfer along the steel frames in case of a fire. If unsatisfactory fire-resistance paints which do not satisfy their standard specification are used, it may result in a severe disaster. Because satisfactory fire-resistance paints are hardly discriminated from the unsatisfactory ones by a simple visual inspection, more reliable and convenient onsite evaluation methods are necessary. Here we report the preliminary study result on the fire safety testing method for fire-resistance paints using an X-ray analysis method. It was found that the existence and quantity of effective constituents in fire-resistance paints can be detected by the X-ray analysis method. X-ray fluorescence (XRF) analyses showed that P and Cl elements are much more enriched in fire-resistance paints, compared to normal paints. X-ray diffraction (XRD) analyses showed that ammonium polyphosphate is present as the main crystalline material in fire-resistance paints, but absent in normal paints. The X-ray analysis method is expected to be used for the onsite inspection of fire-resistance paints with the upcoming availability of portable XRF and XRD instruments.

Preparation and characterization of magnetic nanoparticles with two kinds of core/shell structures (핵/껍질 구조를 가진 두 종류의 자기 나노입자의 제조와 특성비교)

  • 고영재;손인호;김영국;동성용;이근진;박규섭
    • Journal of the Korean Vacuum Society
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    • v.10 no.1
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    • pp.87-92
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    • 2001
  • Magnetic Fe-Co(C) nanocapsules and Fe-Co nanoparticles were prepared by arc-discharge in two kinds of atmospheres, i.e. methane and a mixture of ($H_2$+Ar), respectively. Characterization and magnetic properties of this two kinds of ultrafine particles were investigated systematically by means of X-ray diffraction, Mssbauer spectroscopy, X-ray photoelectron spectroscopy, transmission electron microscopy, energy disperse spectroscopy analysis, chemical analysis, oxygen determination and magnetization measurement. Effects of carbon element, decomposed from a methane atmosphere in carbon arc process, on phase structures, magnetic states and surface characterization were studied in comparison to that of Ar element. Two ultrafine particles showed a little difference in the weight ratio of (Fe/co) and the size for Fe-Co nanoparticles was about two times bigger than Fe-Co(C) nanocapsules. The saturation magnetization of Fe-Co (C) nanocapsules was about 8% higher than that of Fe-Co nanoparticles while their phase constitutions were similar. Although no carbon could be detected by XRD measurement because of extremely thin shells on the surfaces of the cores, it is still believed that they are carbon and oxygen layers.

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Formation of Si Nanodot by Using SiNx Thin Films (SiNx 박막을 이용한 Si Nanodot의 형성)

  • Lee, Jang Woo;Park, Ik Hyun;Shin, Byul;Chung, Chee Won
    • Applied Chemistry for Engineering
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    • v.16 no.6
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    • pp.768-771
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    • 2005
  • The deposition of silicon nitride ($SiN_x$) thin films was carried out on $SiO_2/Si$ substrate at room temperature by reactive dc magnetron sputtering. The analysis of deposited $SiN_x$ films using x-ray photoelectron spectroscopy indicated that the composition of $SiN_x$ films was Si-rich. The deposited $SiN_x$ thin films were annealed by varying annealing temperature and time. X-ray diffraction (XRD) analysis was performed in order to examine the crystallization of Si in $SiN_x$ thin films. The optical and electrical properties of $SiN_x$ thin films were measured for the observation of Si nanodot. As a result, we observed the XRD peaks that might be the Si crystals. As the annealing time and annealing temperature increased, the photoluminescence intensity of $SiN_x$ films gradually increased. The capacitance-voltage characteristics of $SiN_x$ film measured before and after annealing indicated that the trap effect of electrons or holes occurred due to the existence Si nanodots in the $SiN_x$ thin films.

Synthesis and Characterization of CdSe/graphene Nanocomposites and their Catalytic Reusability Studies under Visible Light Radiation

  • Ali, Asghar;Oh, Won-Chun
    • Journal of the Korean Ceramic Society
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    • v.52 no.6
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    • pp.502-507
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    • 2015
  • We examined the photo catalytic activity and catalytic recyclability of CdSe/graphene nanocomposites fabricated via modified hydrothermal technique. The prepared composites were characterized by X-ray diffraction (XRD), scanning electron microscopy (SEM) with energy dispersive X-ray (EDX), transmission electron microscopy (TEM), Raman spectroscopic analysis, and X-ray photoelectron spectroscopy (XPS). The photocatalytic behavior was investigated through decomposition of RBB as a standard dye under visible light radiation. Our results indicate that there is significant potential for graphene based semiconductor hybrids materials to be used as photocatalysts under visible light irradiation for the degradation of organic dyes from industry effluents.

Characterization of few-layered reduced graphene oxide (rGO) for standardization (소수의 층을 갖는 환원 graphene oxide(rGO) 표준화를 위한 물성분석)

  • Ahn, Hae Jun;Huh, Seung Hun;Jee, Youngho;Lee, Byeong Woo
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.32 no.6
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    • pp.239-245
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    • 2022
  • Reduced graphene oxide (rGO) has attracted many attention and applications due to its excellent electrochemical ability. Therefore, standardization of rGO through structural and thermal analysis facilitates quality improvement and management, enabling users to increase efficiency and reduce relevant costs. For rGO and graphene-related materials, it is very important to determine the number of layers and define the resulting difference in physical properties. In this study, 3~4 layers of rGO-1 and 9~10 layers of rGO-2 were obtained from graphene oxide (GO) through a hydrazine reduction process. For the prepared rGOs, X-ray diffraction (XRD) pattern obtained a diffraction peak at 2θ≈25° related to (002) reflection was used to calculate the layer numbers by determining interlayer distance and FWHM value. To reduce the angular uncertainty, XRD data analysis was performed with angle correction using standard reference materials for X-ray powder diffraction analysis. Precise interlayer distance and number of layers were determined using OriginLab and open-source XRD diffraction analysis programs using the angle-corrected diffraction data. TG-DSC thermal analysis was performed to further standardize the physical properties of rGO samples.

Layered Metal Hydroxides Containing Calcium and Their Structural Analysis

  • Kim, Tae-Hyun;Heo, Il;Paek, Seung-Min;Park, Chung-Berm;Choi, Ae-Jin;Lee, Sung-Han;Choy, Jin-Ho;Oh, Jae-Min
    • Bulletin of the Korean Chemical Society
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    • v.33 no.6
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    • pp.1845-1850
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    • 2012
  • Layered metal hydroxides (LMHs) containing calcium were synthesized by coprecipitation in solution having two different trivalent metal ions, iron and aluminum. Two mixed metal solutions ($Ca^{2+}/Al^{3+}$ and $Ca^{2+}/Fe^{3+}$ = 2/1) were added to sodium hydroxide solution and the final pH was adjusted to ~11.5 and ~13 for CaAl-and CaFe-LMHs. Powder X-ray diffraction (XRD) for the two LMH samples showed well developed ($00l$) diffractions indicating 2-dimensional crystal structure of the synthesized LMHs. Rietveld refinement of the X-ray diffraction pattern, the local structure analysis through X-ray absorption spectroscopy, and thermal analysis also confirmed that the synthesized precipitates show typical structure of LMHs. The chemical formulae, $Ca_{2.04}Al_1(OH)_6(NO_3){\cdot}5.25H_2O$ and $Ca_{2.01}Fe_1(OH)_6(NO_3){\cdot}4.75H_2O$ were determined by inductively coupled plasma-atomic emission spectroscopy (ICP-AES). Particle morphology and thermal behavior for the synthesized LMHs were examined by field emission scanning electron microscopy and thermogravimetricdifferential scanning calorimetry.