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

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Cyclic Oxidation Behavior of Vacuum Plasma Sprayed NiCoCrAlY Overlay Coatings (진공 플라즈마 용사법을 통해 형성된 NiCoCrAlY 오버레이 코팅의 반복 산화 거동)

  • Yoo, Yeon Woo;Nam, Uk Hee;Park, Hunkwan;Park, Youngjin;Lee, Sunghun;Byon, Eungsun
    • Journal of Surface Science and Engineering
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    • v.52 no.6
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    • pp.283-288
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    • 2019
  • MCrAlY overaly coatings are used as oxidation barrier coatings to prevent degradation of the underlying substrate in high temperature and oxidizing environment of the hot section of gas turbines. Therefore, oxidation resistance in high temperature is important property of MCrAlY coatings. Also, coefficients of thermal expansion (CTE) of MCrAlY have middle value of that of Ni-based superalloys and oxides, which have the effect of preventing the delamination of the surface oxides. Cyclic oxidation test is one of the most useful methods for evaluating the high temperature durability of coatings used in gas turbines. In this study, NiCoCrAlY overlay coatings were formed on Inconel 792(IN 792) substrates by vacuum plasma spraying process. Vacuum plasma sprayed NiCoCrAlY coatings and IN 792 susbstrates were exposed to 1000℃ one-hour cyclic oxidation environment. NiCoCrAlY coatings showed lower weight gain in short-term oxidation. In long-term oxidation, IN 792 substrates showed higher weight loss due to delamination of surface oxide but NiCoCrAlY coatings showed lower weight loss. X-ray diffraction (XRD) analysis showed α-Al2O3 and NiCr2O4 was formed during the cyclic oxidation test. Through cross-section observation using scanning electron microscopy (SEM) and electron back scatter diffraction (EBSD) analysis, thermally grown oxide (TGO) layer composed of α-Al2O3 and NiCr2O4 was formed and the thickness of TGO increased during 1000℃ cyclic oxidation test. β phase in upper side of NiCoCrAlY coating was depleted due to oxidation of Al and outer beta depletion zone thickness also increased as the cyclic oxidation time increased.

Dry reforming of Propane to Syngas over Ni-CeO2/γ-Al2O3 Catalysts in a Packed-bed Plasma Reactor (충전층 플라즈마 반응기에서 Ni-CeO2/γ-Al2O3 촉매를 이용한 프로페인-합성 가스 건식 개질)

  • Sultana, Lamia;Rahman, Md. Shahinur;Sudhakaran, M.S.P.;Hossain, Md. Mokter;Mok, Young Sun
    • Clean Technology
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    • v.25 no.1
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    • pp.81-90
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    • 2019
  • A dielectric barrier discharge (DBD) plasma reactor packed with $Ni-CeO_2/{\gamma}-Al_2O_3$ catalyst was used for the dry ($CO_2$) reforming of propane (DRP) to improve the production of syngas (a mixture of $H_2$ and CO) and the catalyst stability. The plasma-catalytic DRP was carried out with either thermally or plasma-reduced $Ni-CeO_2/{\gamma}-Al_2O_3$ catalyst at a $C_3H_8/CO_2$ ratio of 1/3 and a total feed gas flow rate of $300mL\;min^{-1}$. The catalytic activities associated with the DRP were evaluated in the range of $500{\sim}600^{\circ}C$. Following the calcination in ambient air, the ${\gamma}-Al_2O_3$ impregnated with the precursor solution ($Ni(NO_3)_2$ and $Ce(NO_3)_2$) was subjected to reduction in an $H_2/Ar$ atmosphere to prepare $Ni-CeO_2/{\gamma}-Al_2O_3$ catalyst. The characteristics of the catalysts were examined using X-ray diffraction (XRD), transmission electron microscopy (TEM), field emission scanning electron microscopy (FE-SEM), energy dispersive X-ray spectrometry (EDS), temperature programmed reduction ($H_2-TPR$), temperature programmed desorption ($H_2-TPD$, $CO_2-TPD$), temperature programmed oxidation (TPO), and Raman spectroscopy. The investigation revealed that the plasma-reduced $Ni-CeO_2/{\gamma}-Al_2O_3$ catalyst exhibited superior catalytic activity for the production of syngas, compared to the thermally reduced catalyst. Besides, the plasma-reduced $Ni-CeO_2/{\gamma}-Al_2O_3$ catalyst was found to show long-term catalytic stability with respect to coke resistance that is main concern regarding the DRP process.

Mineralogical, Micro-textural, and Geochemical Characteristics for the Carbonate Rocks of the Lower Makgol Formation in Seokgaejae Section (석개재 지역 하부 막골층 탄산염암의 광물조성, 미세구조 및 지화학적 특성)

  • Park, Chaewon;Kim, Ha;Song, Yungoo
    • Economic and Environmental Geology
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    • v.51 no.4
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    • pp.323-343
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    • 2018
  • This study defines the mineralogical, micro-textural and geochemical characteristics for the carbonate rocks and discusses the fluids that have affected the depositional environment of the Lower Makgol Formation in Seokgaejae section. Based on analysis of X-ray Diffraction (XRD), Scanning Electron Microscope-Energy Dispersive X-ray Spectrometry (SEM-EDS), Electron Probe Micro Analyzer-Wavelength Dispersive X-ray Spectrometry (EPMA-WDS) and Laser Ablation-Inductively Coupled Plasma-Mass Spectrometry (LA-ICP-MS), carbonate miorofacies in the basal and the lower members of the Makgol Formation are distinguished and classified into four types. Type 1 dolomite (xenotopic interlocking texture) and Type 2 dolomite (idiotopic interlocking texture) have relatively high Mg/Ca ratio, flat REE pattern, low Fe and Mn. Extensively interlocking textures in these dolomites indicate constant supply of Mg ion from hypersaline brine. Type 3 and Type 4 dolomite (scattered and loosely-aggregated texture) have relatively moderate Mg/Ca ratio, MREE enriched pattern, low to high Fe and Mn. These partial dolomitization indicate limited supply of Mg ion under the influx of meteoric water with seawater. Also, the evidence of Fe-bearing minerals, recrystallization and relatively high Fe and Mn in Type 4 indicates the influence of secondary diagenetic fluids under suboxic conditions. Integrating geochemical data with mineralogical and micro-textural evidence, the discrepancy between the basal and the lower members of the Makgol Formation indicates different sedimentary environment. It suggest that hypersaline brine have an influence on the basal member, while mixing meteoric water with seawater have an effect on the lower member of the Makgol Formation.

Mineralogical and Geochemical Characteristics of the Precipitates in Acid Mine Drainage of the Heungjin-Taemaek Coal Mine (흥진태맥 석탄광 산성광산배수 침전물의 광물학적 및 지구화학적 특성)

  • Shin, Ji-Hwan;Park, Ji-Yeon;Kim, Yeongkyoo
    • Economic and Environmental Geology
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    • v.54 no.2
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    • pp.299-308
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    • 2021
  • Fe(II) released from mining activities is precipitated as various Fe(III)-oxyhydroxides when exposed to an oxidizing environment including mine drainage. Ferrihydrite, one of the representative precipitated Fe(III) minerals, is easy to adsorb heavy metals and other pollutants due to the large specific surface area caused by very low crystallinity. Ferrihydrite is transformed to thermodynamically more stable goethite in the natural environment. Hence, information on the transformation of ferrihydrite to goethite and the related mobility of heavy metals in the acid mine drainage is important to predict the behaviors of those elements during ferrihydrite to goethite transition. The behaviors of heavy metals during the transformation of ferrihydrite to goethite were investigated for core samples collected from an AMD treatment system in the Heungjin-Taemaek coal mine by using X-ray diffraction (XRD), chemical analysis, and statistical analysis. XRD results showed that ferrihydrite gradually transformed to goethite from the top to the bottom of the core samples. Chemical analysis showed that the relative concentration of As was significantly high in the core samples compared with that in the drainage, indicating that As was likely to be adsorbed strongly on or coprecipitated with iron oxyhydroxide. Correlation analysis also indicated that As can be easily removed from mine drainage during iron mineral precipitation due to its high affinity to Fe. The concentration ratio of As, Cd, Co, Ni, and Zn to Fe generally decreased with depth in the core samples, suggesting that mineral transformation can increase those concentrations in the drainage. In contrast, the concentration ratio of Cr to Fe increased with depth, which can be explained by the chemical bond of iron oxide and chromate, and surface charge of ferrihydrite and goethite.

Methylene Blue Photodegradation Properties of Anatase/brookite Hybrid TiO2 Photocatalyst Prepared with Different Acid Catalysts (산 촉매에 따른 아나타제/브루카이트 혼성형 TiO2 광촉매의 메틸렌블루 광분해특성)

  • Yun, Seok-Min;Kim, Jinhoon;Jeong, Euigyung;Im, Ji Sun;Lee, Young-Seak
    • Applied Chemistry for Engineering
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    • v.22 no.1
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    • pp.21-25
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    • 2011
  • In this study, anatase/brookite hybrid $TiO_2$ was prepared using different acid catalysts and microwave to improve photodegradation of organic pollutants. The methylene blue photodegradation properties of the prepared photocatalysts with different particle/crystal size and brookite fractions were investigated. Surface characteristics and particle sizes of anatase/brookite hybrid $TiO_2$ were evaluated using scanning electron microscopy (SEM) and laser diffraction particle size analyzer, respectively and crystal structures were investigated with X-ray diffraction (XRD). Methylene blue photodegradation properties were evaluated with UV-vis spectrophotometer. Anatase and anatase/brookite hybrid $TiO_2$ had less than 500 nm size of clusters and the average particle size of $6.66{\sim}6.85{\mu}m$, suggesting that types of acid catalysts did not affect the size. XRD of the prepared $TiO_2$ showed that the photocatalysts had anatase/brookite hybrid crystal structure and applying microwave did not change their crystal structure. Photodegradation of methylene blue with the prepared photocatalyst did not increased proportionally to the fraction of brookite and the crystal size and decreased when brookite fraction and the crystal size increased further. Anatase/brookite hybrid $TiO_2$ with brookite fraction of 9.4% and crystal size of 4.53 nm shows the best photodegradation activity of methylene blue.

The Effect of the Crystalline Phase of Zirconia for the Dehydration of Iso-propanol (이소프로판올의 탈수반응에서 지르코니아 촉매의 결정상에 따른 영향)

  • Sim, Hye-In;Park, Jung-Hyun;Cho, Jun Hee;Ahn, Ji-Hye;Choi, Min-Seok;Shin, Chae-Ho
    • Korean Chemical Engineering Research
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    • v.51 no.2
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    • pp.208-213
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    • 2013
  • Zirconium hydroxide was synthesized by varying the aging time of the zirconyl chloride octahydrate at $100^{\circ}C$ in aqueous solution and the resulting hydroxides were calcined at $700^{\circ}C$ for 6 h to obtain the crystalline $ZrO_2$. The materials used in this study were characterized by differential thermal analysis (DTA), X-ray diffraction (XRD), $N_2$-sorption, transmission electron microscopy (TEM), $NH_3$ temperature-programmed desorption ($NH_3$-TPD), $CO_2$-TPD and iso-propanol TPD analyses to correlate with catalytic activity for the dehydration of iso-propanol. The pure tetragonal $ZrO_2$ phase was obtained after 24 h aging of zirconium hydroxide and successive calcination at $700^{\circ}C$. The increase of aging time showed the production of smaller particle size $ZrO_2$ resulting that the higher specific surface area and total pore volume. $NH_3$-TPD results revealed that the relative acidity of the catalysts increased along with the increase of aging time. On the other hand, the results of $CO_2$-TPD showed the reverse trend of $NH_3$-TPD results. The best catalytic activity for the dehydration of iso-propanol to propylene was shown over $ZrO_2$ catalyst aged for 168 h which had the highest $S_{BET}$ ($178\;m^2\;g^{-1}$). The catalytic activity could be correlated with high surface area, relative acidity and easy desorption of iso-propanol.

Wear Behaviors of WC-CoCr and WC-CrC-Ni Coatings Sprayed by HVOF (고속화염 용사법으로 제조된 WC-CoCr 코팅과 WC-CrC-Ni 코팅의 내마모 거동)

  • Lee, Seoung Soo
    • Journal of the Korea Academia-Industrial cooperation Society
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    • v.21 no.6
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    • pp.204-211
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    • 2020
  • The high-velocity oxy-fuel (HVOF) thermal spraying coating technique has been considered a promising replacement for traditional electrolytic hard chrome plating (EHC), which caused environmental pollution and lung cancer due to toxic Cr6+. In this paper, two types of cermet coatings were prepared by HVOF spraying: WC-CoCr and WC-CrC-Ni coatings. The produced coatings were analyzed extensively in terms of the micro-hardness, porosity, crystalline phase and microstructure using a hardness tester, optical microscopy, X-ray diffraction, and scanning electron microscopy (including energy dispersed spectroscopy (EDS)), respectively. The wear and friction behaviors of the coatings were evaluated comparatively by reciprocating sliding wear tests at 25 ℃, 250 ℃, and 450 ℃. The results revealed correlations among the microstructures, metallic binder matrixes, porosities, and wear performance of the coatings. For example, WC-CoCr coatings showed better sliding wear resistance than WC-CrC-Ni coatings, regardless of the test temperature due to the more homogeneous microstructure, Co-rich, Cr-rich metallic binder matrix, and lower porosity.

Enhanced critical current density of in situ processed MgB2 bulk superconductors with MgB4 additions

  • Kim, S.H.;Kang, W.N.;Jun, B.H.;Lee, Y.J.;Kim, C.J.
    • Progress in Superconductivity and Cryogenics
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    • v.19 no.1
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    • pp.36-41
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    • 2017
  • The effects of $MgB_4$ addition on the superconducting properties and the microstructure of in situ processed $MgB_2$ bulk superconductors were studied. $MgB_4$ powder of 1-20 wt.% was mixed with (Mg + 2B) powder and then pressed into pellets. The pellets of (Mg + 2B + $xMgB_4$) were heat-treated at $650^{\circ}C$ for 1 h in flowing argon. The powder X-ray diffraction (XRD) analysis for the heat-treated samples showed that the major formed phase in all samples was $MgB_2$ and the minor phases were $MgB_4$ and MgO. The full width at half maximum (FWHM) values showed that the grain size of $MgB_2$ decreased as the amount of $MgB_4$ addition increased. $MgB_4$ particles included in a $MgB_2$ matrix is considered to suppress the grain growth of $MgB_2$. The onset temperatures ($T_{c,onset}$) of $MgB_2$ with $MgB_4$ addition (0-10 wt.%) was between 37-38 K. The 20 wt.% $MgB_4$ addition slightly reduced the $T_{c,onset}$ of $MgB_2$ to 36.5 K. This result indicates that $MgB_4$ addition did not influence the superconducting transition temperature ($T_c$) of $MgB_2$ significantly. On the other hand, the small additions of 1-5 wt.% $MgB_4$ increased the critical current density ($J_c$) of $MgB_2$. The $J_c$ enhancement by $MgB_4$ addition is attributed not only to the grain size refinement but also to the possible flux pinning of $MgB_4$ particles dispersed in a $MgB_2$ matrix.

A Study on the Low Temperature Epitaxial Growth of $CoSi_2$ Layer by Multitarget Bias cosputter Deposition and Phase Sequence (Multitarget Bias Cosputter증착에 의한 $CoSi_2$층의 저온정합성장 및 상전이에 관한 연구)

  • Park, Sang-Uk;Choe, Jeong-Dong;Gwak, Jun-Seop;Ji, Eung-Jun;Baek, Hong-Gu
    • Korean Journal of Materials Research
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    • v.4 no.1
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    • pp.9-23
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    • 1994
  • Epitaxial $CoSi_2$ layer has been grown on NaCl(100) substrate at low deposition temperature($200^{\circ}C$) by multitarget bias cosputter deposition(MBCD). The phase sequence and crystallinity of deposited silicide as a function of deposition temperature and substrate bias voltage were studied by X-ray diffraction(XRD) and transmission electron microscopy(TEM) analysis. Crystalline Si was grown at $200^{\circ}C$ by metal induced crystallization(M1C) and self bias effect. In addition to, the MIC was analyzed both theoretically and experimentally. The observed phase sequence was $Co_2Si \to CoSi \to Cosi_2$ and was in good agreement with that predicted by effective heat of formation rule. The phase sequence, the CoSi(l11) preferred orientation, and the crystallinity had stronger dependence on the substrate bias voltage than the deposition temperature due to the collisional cascade mixing, the in-situ cleaning, and the increase in the number of nucleation sites by ion bombardment of growing surface. Grain growth induced by ion bombardment was observed with increasing substrate bias voltage at $200^{\circ}C$ and was interpreted with ion bombardment dissociation model. The parameters of $E_{Ar}\;and \alpha(V_s)$ were chosen to properly quantify the ion bombardment effect on the variation in crystallinty at $200^{\circ}C$ with increasing substrate bias voltage using Langmuir probe.

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Dielectric properties of $0.6Pb(Sc_{1/2}Ta_{1/2})O_3-0.4PbTiO_3$ ceramics prepared by the molten salt synthesis method (용융염 합성법에 의해 제조된 $0.6Pb(Sc_{1/2}Ta_{1/2})O_3-0.4PbTiO_3$ 세라믹스의 유전성)

  • Park, Kyung-Bong;Kim, Tae-Huei;Kwon, Seung-Hyup;Lim, Dong-Ju
    • Journal of the Korean Crystal Growth and Crystal Technology
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    • v.17 no.2
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    • pp.69-74
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    • 2007
  • [ $0.6Pb(Sc_{1/2}Ta_{1/2})O_3-0.4PbTiO_3$ ] (hereafter PSTT) ceramics were prepared by the molten salt synthesis (MSS) method using KCI as a flux. Formation of perovskite phase was investigated by a differential thermal analysis (DTA) and X-ray diffraction (XRD) analysis in the temperature range from $600^{\circ}C$ to $850^{\circ}C$. A 92% perovskite phase was synthesized at $750^{\circ}C$ for 2 hrs using the MSS method, while 82% perovskite phase was synthesized at $850^{\circ}C$ for 4ks using the calcining of mixed oxide (CMO) method. This result could be due to the improvement in reactivity of $Sc_2O_3$ by melting of KCI. The MSS specimen sintered at $1,100^{\circ}C$ for 4hrs showed a dielectric constant of 11,200, a remnant polarization of $13.5{\mu}C/cm^2$ and a coercive field of 10.198 kV/cm, which was discussed in view of the microstructure.