• The Journal of the Petrological Society of Korea
• /
• v.6 no.2
• /
• pp.88-95
• /
• 1997

High pressure X-ray diffraction study was carried out on a polycrystalline graphite to investigate the phase transition(s) at room temperature. Energy dispersive X-ray diffraction method was employed using a Mao-Bell type diamond anvil cell with an Wiggler synchrotron Radiation at the National Synchrotron Light Source. Sodium chloride power was used as the internal pressure sensor for the high pressure determinations as well as the pressure medium for quasihydrostatic pressure environment. Graphite transforms into a hexagonal didose not agree with the previously reported observations and this phase persists when pressure is released down to 0.1 MPa. This result dose not agree with the previously reported observations and this discrepancy would be due to the kinetics in phase transition as well as the uniaxially oriented pressure field in the diamond anvil cell.

• Journal of Ocean Engineering and Technology
• /
• v.8 no.1
• /
• pp.114-122
• /
• 1994

X-ray stress constant, K, was determined for the diffraction line of (211)plane by using Cr-K$\alpha$ radiation. K was -340.87 MPa/deg. Fatigue crack propagation tests of SS41 steel were conducted under stress ratios of 0.1, 0.3 and 0.5. The half-value breadth of X-ray diffraction profile was measured at and beneath the fracture surface. The half-value breadth, B, on the fracture surface was found to increase with increasing $K_max$. The value of B was influenced by stress ratio in SS41 steel. The half-value breadth took the maximum value at the borden of reversed plastic zone, while it approached to the initial (pre-fatigue) value near the boundary of monotonic plastic zone. The maximum depth of the plasticzone was evaluated on the basis of the half-value breadth distribution. The depth $\omega$$_y$ is related to $K_max$by the following equation : $\omega$$_y$ = $\alpha$($K_max$/$\sigma$$_y$$)^2$ where .sigma.$\sigma$$_y$ is the yield strength obtength obtained in tension test .alpha.is 0.136 for SS41 steel.

• Journal of Conservation Science
• /
• v.36 no.1
• /
• pp.1-14
• /
• 2020

This study investigates the crystallinity distribution of ancient silk. Owing to the inherent multi-hierarchical structure of silk protein and the complicated structural changes that occur due to various burial environments, it is challenging but worthwhile to study ancient silk ageing behavior, which is based on the fact that ageing begins with a single fiber and then spreads to a whole fabric. Crystallinity was one of the most effective indicators found to reveal the ageing status of silk. Therefore, a synchrotron radiation-based X-ray diffraction(SR-XRD) method was employed to study the crystallinity distribution of single fibers of ancient silk unearthed from seven archaeological sites in China from historical periods including the warring states, Han dynasty, Song dynasty, and Ming dynasty. In comparison, the conventional X-ray diffraction method, which uses large amounts of samples, was also performed to determine the integral crystallinity of ancient silk. Thermal stability experiments by thermogravimetry(TG) as well as morphology observations by scanning electron microscopy(SEM) and optical microscopy(OM) all confirmed the deterioration of ancient silk. Moreover, the ageing mechanism of ancient silk was proposed with the assistance of an artificial ageing study. The results confirmed the effectiveness of SR-XRD as an ageing indicator, revealing the crystallinity distribution. This research could provide motivation to determine the deterioration status of ancient silk, and would also aid in explaining the fragility of ancient silk due to ageing.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
• /
• v.27 no.12
• /
• pp.797-802
• /
• 2014

In this study, in order to develop the capacitor composition ceramics with the good dielectric properties, $(Ba_{1-x}Ca_x)(Ti_{0.85}Zr_{0.12}Sn_{0.03})O_3$ (abbreviated as BCTZ) ceramics were prepared by the conventional solid-state reaction method. The effects of Ca substitution on the microstructure and dielectric properties was investigated. The X-ray diffraction patterns demonstrated that all the specimens showed perovskite phase, and secondary phases are indicated in the measurement range of X-ray diffraction. Also, all the specimens indicated an rhombohedron phase structure. It was identified from the X-ray diffraction patterns that the secondary phase formed in grain boundaries and then decreased the dielectric properties. For all the specimens, observed one peak was tetragonal cubic phase transition temperature($T_c$), which is located in the vicinity of room temperature.

• Korean Journal of Soil Science and Fertilizer
• /
• v.6 no.4
• /
• pp.253-255
• /
• 1973

Microscopic method was compared with X-ray diflraction analysis for the identification of rockforming minerals using 11 main rock samples in Korea. 1. There was no difference between X-ray diffraction analysis and microscopic one in major minerals, but some accessary minerals. 2. The rock-forming minerals of main rocks presented in this study occured almost in crystalline state so that they could be easily identified by X-ray analysis alone.

• Proceedings of the Korean Vacuum Society Conference
• /
• 2000.02a
• /
• pp.167-167
• /
• 2000

전지 재료의 충방전 과정 연구에는 X-선 분말회절(x-ray powder diffraction techniques)과 중성자회절을 많이 사용하였다. 하지만 이러한 분석기술은 long-range order의 구조에 관한 정보를 제공하는데 유용하지만 atomic scale의 구조에 관한 정보를 얻기에는 한계가 있다. Li 전지에서의 전기화학적 반응에서는 cathode 물질에 포함된 전이금속의 산화, 환원 반응에 의한 Li 이온의 intercalation (charge process)과 deintercalation (discharge process) 현상이 일어난다. 이러한 충방전 과정은 알려지지 않은 다양한 형태의 위상 변화를 동반하게 되는데 x-선 이나 중성자를 이용한 powder diffraction techniques 로는 단지 정성적인 결정학적 정보를 얻을 수 있다. 따라서 최근에 원자 단위의 local structure에 관한 정보와 electrochemical state에 관한 정보를 동시에 얻을 수 있는 X-ray Absorption Fine Structure (XAFS) 분석기술을 Li 전지분석에 활용하기 시작하였다. XAFS는 하나의 x-ray 흡수원자에 대해서 주변원자들의 원자구조에 관한 정보와 구성 원소의 electrochemical state에 관한 정보를 얻을 수 있는 분석방법이다. X-ray Induced Electron Emission Spectroscopy (XIEES)는 x-ray에 의해서 방출된 전자를 검출하여 스펙트럼을 얻는 기능을 함축적으로 나타낸 것으로, x-ray를 물질 표면에 조사하여 발생하는 광전자, Auger 전자, 이차전자 등을 전자검출기(Channel Electron Multiplier: CEM)로 검출하는 기능과, 시료를 투과한 x-ray와 시료에서 발생하는 형광 x-ray를 비례계수기로 검출하는 기능을 가지고 있다. 이러한 검출 능력을 바탕으로 EXAFS, XANES, Standing Wave Technique, Elemental Composition Analysis, DXRD, Total Reflection Technique 등을 이용하여 물질을 구성하고 있는 원소의 성분, 미세원자구조, 전자구조에 관한 정보를 얻을 수 있는 새로운 spectrometer이다. 본 연구에서는 자체 개발한 XIEES의 XAFS 기능을 이용하여 여러 가지 방법으로 제조한 LiMn2-xO4와 LiMnO2, MnO2에서 Mn K-absorption edge에 대한 chemical state 변화를 측정하였다. Absorption edge에서 chemical shift를 측정하기 위해서는 방사광 가속기 수준의 에너지 분해능(~0.3eV)이 필요하다. 이번 연구에서는 SiO2(3140) monochromator를 사용하고 여기에 맞는 적절한 parameter를 적용하여 x-ray 에너지 분해능을 포항방사광가속기 수준으로 개선하였다. XIEES에서 얻은 스펙트럼과 포항방사광가속기에서 얻은 스펙트럼을 비교하였다. Chemical shift가 일어나는 경향은 두 실험 결과가 잘 일치하였다.

• Korean Journal of Crystallography
• /
• v.8 no.1
• /
• pp.20-25
• /
• 1997

Two experimental methods have been developed for high resolution measurement of x-ray scattering. The methods used were (1) an x-ray double crystal diffraction (DCD) spectrometer set-up and (2) an x-ray triple crystal diffraction (TCD) spectrometer set-up. With the DCD arrangement of Si(511)-sample(hkl), rocking curves have been plotted for Si (333), Si(004) and GaAs(004). Also, with the TCD arrangement of Si(111)-Si(111)-Si(511)-sample(hkl) including monolithic monocro-collimator and $K_{\alpha1}$ selector, rocking curves have been plotted for Si(333), Si(004) and GaAs(004). The results of FWHM by DCD and TCD set-up have been compared each other and discussed. The reflection topographs (004) and (115) in an $In_{0.037}Ga_{0.0963}As/GaAs$ sample have been obtained by DCD set-up.

• Korean Journal of Mineralogy and Petrology
• /
• v.34 no.4
• /
• pp.227-239
• /
• 2021

A practical and effective method of X-ray powder diffraction analysis was investigated for quantitative analysis of the mineral content of natural samples. Sample mounting experiments were conducted to select the best randomly oriented powder sample mount. A comparative experiment was also made between a reference intensity ratio (RIR) method, which compares a single peak intensity with standard material, and the Rietveld method, which calculates a full X-ray diffraction pattern, to search for the effective method of mineral quantification. In addition, samples containing amorphous minerals were quantitatively analyzed by the Rietveld method and the efficiency was reviewed. As a result of the study, the optimal random orientation could be reached by the side mounting method. The Rietveld method using the full pattern of X-ray diffraction was more suitable for mineral quantitative analysis, rather than the RIR method using a specific peak. However, either method could depend on the analyst's experience in addition to analytical technique. Moreover, amorphous minerals can be quantitatively analyzed by the Rietveld method, and the analysis results make the geological analysis possible.

• Journal of Welding and Joining
• /
• v.20 no.2
• /
• pp.50-58
• /
• 2002

Residual stress is generated in the structures as a result of irregular elastic-plastic deformation during fabrication processes such as welding, heat treatment, and mechanical processing. There are several factors attributed to the origin of residual stresses, tensile or compressive. The stresses can be determined by destructive ways or nondestructive ways using X-ray or neutron diffraction. Although X-ray diffraction is a well established technique, it is practically limited to near-surface stresses. Neutrons penetrate easily into most materials and neutron diffraction permits non-destructive evaluation of lattice strain within the bulk of large specimens because the radiation is more deeply penetrating for metallic engineering components. This paper presented application of neutron diffraction technique to the residual stress measurement using 20 mm thick welded stainless steel plate($100{\times}100 \textrm{mm}^2$)

• Korean Journal of Materials Research
• /
• v.11 no.8
• /
• pp.661-665
• /
• 2001

The mechanical alloying (MA) effect in $\sigma$-VFe intermetallic compound was studied by neutron and X-ray diffraction. The structure of MA $\sigma$-VFe powders were characterized by the X- ray diffraction with Cu- $K\alpha$ radiation and neutron diffraction with monochromatic neutrons of $1.835\AA$ using a high resolution powder diffractometer (HRPD). Mechanical alloying of $\sigma$-VFe compound gives rise to a dramatic structural change. After 60 hours of MA, the Fe-Fe distribution of the $\sigma$- phase VFe tetragonal structure with 30 atoms in a unit cell is found to change into that of the $\sigma$-(V,Fe) solid solution with bcc structure, which is a stable phase at elevated temperature above $1200^{\circ}C$. A comparison of X-ray diffraction data for the $\alpha$-phase has been also made with the corresponding neutron diffraction data. The (101) and (111) diffraction peaks of the $\sigma$-phase was clearly observed only in neutron diffraction pattern, which is believed to be a characteristic feature due to the chemical atomic ordering of $\sigma$- VFe phase.