• Title/Summary/Keyword: XRD analysis

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Structural and thermal analysis of electrochemically Li intercalated synthetic graphite (전기 화학적으로 리튬이 층간 삽입된 인조흑연의 구조와 열적 특성 분석)

  • Oh, Won-Chun
    • Analytical Science and Technology
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    • v.14 no.3
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    • pp.197-202
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    • 2001
  • The characteristics of the electrochemically Li intercalated synthetic graphite were determined from the studies with XRD method, DSC and solid $^7Li-NMR$ spectrophotometric analysis. From the results of X-ray diffraction method, it was found that the compounds in the stage 1 structure were predominantly formed. The enthalpy and entropy changes of the compounds can be obtained from the differential scanning calorimetric analysis results. From these results, it was found that exothermic and endothermic reactions of lithium intercalated into synthetic graphite are related to thermal stability of lithium ion between carbon graphene layers. From the $^7Li-NMR$ data, scientific observation found that bands are shift toward higher frequencies with increasing lithium concentration because non-occupied electron shells of Li increased in charge carrier density. Line widths of the Li intercalated synthetic graphite compounds decreased slowly because of non-homogeneous local magnetic order and the random electron spin direction for substituted Li.

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Nb-carbonitride Analysis Techniques in Nb-steels (강 중 Nb계 탄질화 석출물 정량분석 기술)

  • Lee, J.J.;Jung, S.W.;Yoo, K.S.
    • Analytical Science and Technology
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    • v.7 no.4
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    • pp.493-504
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    • 1994
  • The morphology and structure of precipitates of formed in Nb steels were investigated using SEM, TEM and XRD. The quantitative analysis of the precipitates was performed by ICP-AES. The potentiostatic etching method was employed as an extraction method using 10% AA-methanol and 15% Na-citrate electrolytes. The two selected potentials relative to SCE(Standard Calomel Electrode), -100mV in 10% AA-methanol solution and -250mV in 15% Na-citrate solution were found to be effective for the extraction. XRD analysis showed that composition of Nb carbonitride in Nb-steel(0.01% C-0.7% Nb-0.004N) was $NbC_{0.65}N_{0.2}$.

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Confinement effectiveness of Timoshenko and Euler Bernoulli theories on buckling of microfilaments

  • Taj, Muhammad;Khadimallah, Mohamed A.;Hussain, Muzamal;Mahmood, Shaid;Safeer, Muhammad;Al Naim, Abdullah F.;Ahmad, Manzoor
    • Advances in concrete construction
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    • v.11 no.1
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    • pp.81-88
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    • 2021
  • Rice Husk Ash (RHA) geopolymer paste activated by sodium aluminate were characterized by X-ray diffractogram (XRD), scanning electron microscope (SEM), energy dispersion X-Ray analysis (EDAX)and fourier transform infrared spectroscopy (FTIR). Five series of RHA geopolymer specimens were prepared by varying the Si/Al ratio as 1.5, 2.0, 2.5, 3.0 and 3.5. The paper focuses on the correlation of microstructure with hardened state parameters like bulk density, apparent porosity, sorptivity, water absorption and compressive strength. XRD analysis peaks indicates quartz, cristobalite and gibbsite for raw RHA and new peaks corresponding to Zeolite A in geopolymer specimens. In general, SEM micrographs show interconnected pores and loosely packed geopolymer matrix except for specimens made with Si/Al of 2.0 which exhibited comparatively better matrix. Incorporation of Al from sodium aluminate were confirmed with the stretching and bending vibration of Si-O-Si and O-Si-O observations from the FTIR analysis of geopolymer specimen. The dense microstructure of SA2.0 correlate into better performance in terms of 28 days maximum compressive strength of 16.96 MPa and minimum for porosity, absorption and sorptivity among the specimens. However, due to the higher water demand to make the paste workable, the value of porosity, absorption and sorptivity were reportedly higher as compared with other geopolymer systems. Correlation regression equations were proposed to validate the interrelation between physical parameters and mechanical strength. RHA geopolymer shows comparatively lower compressive strength as compared to Fly ash geopolymer.

Effect of Sintering Condition on Tensile Strength of Fe-based Non-equiatomic High Entropy Alloy (철계 비동일분율 고엔트로피 합금의 인장 강도에 미치는 소결 조건 영향)

  • Seo, Namhyuk;Jeon, Junhyub;Kim, Gwanghun;Park, Jungbin;Son, Seung Bae;Lee, Seok-Jae
    • Journal of Powder Materials
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    • v.28 no.3
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    • pp.221-226
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    • 2021
  • We fabricate the non-equiatomic high-entropy alloy (NE-HEA) Fe49.5Mn30Co10Cr10C0.5 (at.%) using spark plasma sintering under various sintering conditions. Each elemental pure powder is milled by high-energy ball milling to prepare NE-HEA powder. The microstructure and mechanical properties of the sintered samples are investigated using various methods. We use the X-ray diffraction (XRD) method to investigate the microstructural characteristics. Quantitative phase analysis is performed by direct comparison of the XRD results. A tensile test is used to compare the mechanical properties of small samples. Next, electron backscatter diffraction analysis is performed to analyze the phase fraction, and the results are compared to those of XRD analysis. By combining different sintering durations and temperature conditions, we attempt to identify suitable spark plasma sintering conditions that yield mechanical properties comparable with previously reported values. The samples sintered at 900 and 1000℃ with no holding time have a tensile strength of over 1000 MPa.

Estimation of cremation temperature on Baekje human bones from Seoul Seokchon-dong Ancient Tomb No.1 using XRD and FT-IR analysis (XRD와 FT-IR을 이용한 백제시대 옛사람 뼈의 화장(火葬) 온도 추정 - 서울 석촌동 고분군 1호 매장의례부 출토 옛사람 뼈를 중심으로 -)

  • YU, Jia;PARK, Serin;SHIN, Jiyoung
    • Korean Journal of Heritage: History & Science
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    • v.54 no.3
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    • pp.228-241
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    • 2021
  • Cremated archaeological bones provide crucial information to unravel the details of ancient cremation events and funeral culture. The research on cremated bones to date has been mainly focused on extracting archaeological information in Korea. Recently, the techniques of physical anthropology have been applied to obtain biological information and cremation temperatures for individuals. This study analyzed human remains excavated from Seoul Seokchon-dong Ancient Tombs and determined whether there were human cremations as well as the estimated cremation temperatures. There was no trace of fire in the pits where cremated bones were found; therefore, it is assumed that they were deposited with the artifacts. In this study, four samples were selected according to the surface color of the bones, and X-ray diffraction analysis (XRD) and Fourier-transformed infrared spectroscopy (FT-IR) were used for analysis. All four of the Seokchon-dong cremated bones were found, based on the crystallization index of X-ray diffraction analysis, to have experienced cremation above the temperature of 700℃. Infrared spectroscopy results indicated that the four bones from Seokchon-dong were cremated at temperatures above 700℃ and below 1,000℃. IR peaks were observed at 700℃, whereas no changes were found when bones experienced more than 1000℃. We assume that the cremated people in the Seokchon-dong Tombs were people of high-status because cremation at such a high temperature at that period required much effort. Here we present significant evidence of the cremation status and temperature of archaeological human bones on the basis of XRD and FT-IR, allowing for the restoration of the cremation events and funeral culture in archaeological sites.

X-ray diffraction analysis of the effect of ball milling time on crystallinity of milled polyacrylonitrile-based carbon fiber

  • Lee, Sang-Hye;Kang, Dong-Su;Lee, Sang-Min;Roh, Jae-Seung
    • Carbon letters
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    • v.26
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    • pp.11-17
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    • 2018
  • Milled carbon fiber (mCF) was prepared by a ball milling process, and X-ray diffraction (XRD) diffractograms were obtained by a $2{\theta}$ continuous scanning analysis to study mCF crystallinity as a function of milling time. The raw material for the mCF was polyacrylonitrile-based carbon fiber (T700). As the milling time increased, the mean particle size of the mCF consistently decreased, reaching $1.826{\mu}m$ at a milling time of 18 h. The XRD analysis showed that, as the milling time increased, the fraction of the crystalline carbon decreased, while the fraction of the amorphous carbon increased. The (002) peak became asymmetric before and after milling as the left side of the peak showed an increasingly gentle slope. For analysis, the asymmetric (002) peak was deconvoluted into two peaks, less-developed crystalline carbon (LDCC) and more-developed crystalline carbon. In both peaks, Lc decreased and $d_{002}$ increased, but no significant change was observed after 6 h of milling time. In addition, the fraction of LDCC increased. As the milling continued, the mCF became more amorphous, possibly due to damage to the crystal lattices by the milling.

Physical and Chemical Weathering Indices for Biotite Granite and Granitic Weathered Soil in Gyeongju

  • Ban, Jae-Doo;Moon, Seong-Woo;Lee, Seong-Won;Lee, Joo-Gong;Seo, Yong-Seok
    • The Journal of Engineering Geology
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    • v.27 no.4
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    • pp.451-462
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    • 2017
  • Physical weathering caused by external forces and chemical weathering caused by the decomposition or alteration of constituent materials are the two factors that dominate the mechanical properties of rocks. In this study, a field investigation was undertaken to identify the physical and chemical weathering characteristics of the biotite granite and granitic weathered soils in Gyeongju, South Korea. Samples were collected according to their grade of weathering and subjected to modal analysis, XRD analysis, XRF analysis, physical property tests, particle size distribution tests, and slake durability tests. Modal and XRD analysis identified these rocks as biotite granite; secondary alteration minerals were not observed. Physical property tests and particle size distribution analyses indicate an average porosity of 41.28% and a sand content of > 90 wt.%. These values are somewhat higher than those of granites in general. The results of the slake durability test and XRF analyses show that the physical and chemical weathering indices of the samples vary with the degree of weathering.

Effect of Mechanical Alloying Atmosphere on Formation of AlN (AlN의 형성에 미치는 기계적 합금화 분위기의 영향)

  • Yu Seung-Hoon;Lee Young Sung;Shin Kwang-Seon
    • Journal of Powder Materials
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    • v.12 no.3
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    • pp.214-219
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    • 2005
  • In order to investigate the formation of AlN, mechanical alloying was carried out in $N_2$ and $NH_3$ atmosphere. Differential thermal analysis (DTA), x-ray diffraction (XRD) and chemical analysis were carried out to examine the formation behavior of aluminum nitrides. No diffraction pattern of AlN was observed in XRD analysis of the as-milled powders in $NH_3\;or\;N_2$ atmosphere. However, DTA and chemical analysis indicated that the precursors for AlN were formed in the Al powders milled in $NH_3$ atmosphere. The AlN precursors transformed to AlN after heat treatment at and above $600^{\circ}C$. It was considered that the reaction between Al and $NH_3$ was possible by the formation of fresh Al surface during mechanical alloying of Al powders.

Differential Thermal Analysis and Quantum Chemical Consideration for Catalytic Stability of Ion Exchanged Faujasite Type Zeolite 1. Ni2+-Faujasite계 (이온교환된 Faujasite형 제올라이트의 촉매적 안정성에 대한 시차열분석 및 양자화학적 고찰; 1. Ni2+-Faujasite계)

  • Kim, Myung-Chul;Kim, Jong-Taik
    • Applied Chemistry for Engineering
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    • v.4 no.1
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    • pp.75-81
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    • 1993
  • The thermochemical stability of $Ni^{2+}-faujasite$ was studied by differential thermal analysis(DTA), thermal gravitational analysis(TGA), X-ray diffraction analysis(XRD) and quantum chemical calculations. Dehydration of $Ni^{2+}-faujasite$ was observed at 373-773K. A CNDO/2 calculations have been applied on cluster models for the representative T sites in faujasite to get total energy and wiberg bond orders. It has proved that the decrease of zeolitic crystallinity is directly related to the weakening of Al-O bonds in framework.

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Transesterification of Jatropha Oil over Ceria-Impregnated ZSM-5 for the Production of Bio-Diesel

  • Bhagiyalakshmi, Margandan;Vinoba, Mari;Grace, Andrews Nirmala
    • Bulletin of the Korean Chemical Society
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    • v.34 no.10
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    • pp.3059-3064
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    • 2013
  • In this study transesterification of Triglycerides (TG) from Jatropha curcas oil (JCO) with methanol for production of biodiesel was investigated over cerium impregnated ZSM-5 catalysts. NaZSM-5 was synthesized in an alkaline medium and impregnated with cerium oxide by wet method using cerium nitrate as a source for cerium. They were characterized by X-ray diffraction (XRD), Thermogravimeteric analysis (TGA), $CO_2$-temperature programmed desorption, and $N_2$ adsorption/desorption analysis. XRD analysis showed decrease in intensity of the patterns with the increase in the ceria loading but crystallization of ceria to larger size is an evident for 10 and 15% loading. The optimal yield of transesterification process was found to be 90% under the following conditions: oil to methanol molar ratio: 1:12; temperature: $60^{\circ}C$; time: 1 h; catalyst: 5 wt %. Here the yield of fatty acid methyl ester (FAME) was calculated through $^1H$ NMR analysis. The investigation on catalyst loading, temperature, time and reusability illustrated that these ceria impregnated NaZSM-5's were found to be selective, recyclable and could yield biodiesel at low temperature with low methanol to oil ratio due to the presence of both Lewis and Bronsted basicity. Hence, from the above study it is concluded that ceria impregnated ZSM-5 could be recognized as a potential catalysts for biodiesel production in industrial processes.