• 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.

• 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.

• 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.

• 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.

• 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.

• Journal of the Mineralogical Society of Korea
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• v.18 no.4 s.46
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• pp.259-266
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• 2005

X-ray diffraction (XRD), Electron microprobe analyses (EPMA) and heating experiments were used for mineralogical characterization of natural buserites collected from the Janggun and Dongnam mines. They are closely associated with $7-{\AA}$ phase (usually rancieite) in manganese oxide ores of the supergene oxidation zones of manganese carbonate deposits. Electron microprobe analyses give the average formula $(Ca_{0.78}Mg_{0.64}Mn^{2+}\;_{0.45})Mn^{4+}\;_{8.03}O_{18}\cdot13.2H_{2}O\;and\;(Zn_{0.81}Ca_{0.77}Mg_{0.26})Mn^{4+}\;_{8.00}O_{18}\cdot10.9H_{2}O$ for buserite from the Janggun and the Dongnam mine, respectively. The basal reflection of buserite from the Janggun mine shifts continuously from $9.86\;{\AA}\;at\;40^{\circ}C\;to\;7.60\;{\AA}\;at\;90^{\circ}C$, but the buserite from the Dongnam mine shows tendency of decreasing intensity in the $9.67^{\circ}C$ peak and of increasing intensity in the $7.53\;{\AA}$ peak in the range of $40\∼90^{\circ}C$, showing no gradual shifting of peaks.

• Proceedings of the Korean Powder Metallurgy Institute Conference
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• 2001.11a
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• pp.29-29
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• 2001

열전재료는 열전현상을 가지고 있어 열전발전과 열선냉각이 가능하기 때분에 해저용, 우주용, 군사용의 특수 전원으로 이미 실용화되어있고, 반도체, 레이저 다이오드, 적외선 검출소자 등의 냉각기로 쓰여지고 있어 많은 연구자들이 이들 재료에 대한 연구에 관을 갖고 열전특성을 향상시키기 위하여 많은 연구를 진행하고 있다 이들 열전재료는 사용 온도구역에 따라 3종류로 구분하고 있으며, 실온부근의 저온 영역(20$0^{\circ}C$)이하에서는 $Bi_2Te_3$계 재료, 중온영역(20$0^{\circ}C$~50$0^{\circ}C$)에서sms (Pb,Ge) Te계 재료, 고온영역(50$0^{\circ}C$~lOoo$^{\circ}C$)에서는 Si-Ge계 Fe Si계 재료가 이용되고 있다. 본 연구에서는 실온에서 성능지수가 높은 Bi_2(Te,Se)_3$에 대한 연구를 진행하였다. Bi_2(Te,Se)_3$계 열전재료는 기존의 공법인 Zone melting법을 이용하는 경우 성능지수가 높으나, 단위정이 Rhombohedral 구조파 기저면(basal plane)에 벽개성이 있는 관계로 재료의 적지 않은 손실과 가공상의 어려움이 있다. 또한 사료전체에 걸쳐 화학적으로 균질한 고용체를 얻는 것도 어려운 문제점으보 부각되고 있디 따라서 이와같은 문제점을 보완하기 위하여 용질원자의 편석감소, 고용도의 증가, 균일 고용체 형성, 결정립의 미세화등의 장점이 있는 급속응고법을 본 연구에 응용하였다. 본 연구에서는 위에서와 같은 급속응고의 장점과 대량 가공이 능늪한 연간압출공정을 이용하여 제조된 분말을 성형화 하였다. 특히 열간압출 가공에 있어서 압축다이 각 변화는 재료의 소성유동에 매우 중요한 역하을 하게되며, 이와 갇은 소성유동은 본 재료의 열전특성에 중요한 영향을 미치는 C 면 배양에 중요한 역할을 한 것으 로 기대된다. 이에 본 연구에서는 압출다이 각도 변화에 따른 미세조직변화와 이들 조직이 강도와 열전특성에 미치는 영향을 석하고자 한다. 압출재의 미세조직은 XRD(X Ray Diffraction), SEM(Scanning Electron Microscopy)으로 분석하였으며, 열전특성인 Seebeck계수($\alpha$)와 전기비저항( $\rho$ )은 열전측정장치로, 기계적 강도는 MTS장비를 이용하여 이루어졌다. 또한 압축다이각도 변화에 따른 결정방위 해석은 모노크로미터가 장착된 X RD장비감 이용하여 분석되었다.

• Polymer(Korea)
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• v.31 no.6
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• pp.518-525
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• 2007

The thermomechanical properties and morphologies of nanocomposite fibers of poly(ethylene terephthalate)(PET) incorporating thermally stable organoclays are compared. Dodecyltriphenyl-phosphonium-mica($C_{12}PPh-Mica$) and 1-hexadecane benzimidazole-mica ($C_{16}BIMD-Mica$) were used as reinforcing fillers in the fabrication of PET hybrid fibers. Dispersions of organoclays with PET were studied by using the in-situ polymerization method at various organoclay contents to produce nano-scale composites. The thermo-mechanical properties and morphologies of the PET hybrid fibers were determined using differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), wide angle X-ray diffraction (XRD), electron microscopy (SEM and TEM), and a universal tensile machine (UTM). Transmission electron microscopy (TEM) micrographs show that some of the clay layers are dispersed homogeneously within the polymer matrix on the nano-scale, although some clay particles are agglomerated. We also found that the addition of only a small amount of organoclay is enough to improve the thermal stabilities and mechanical properties of the PET nanocomposite fibers. Even polymers with low organoclay content (<5 wt%) were found to exhibit much higher thermo-mechanical values than pure PET fibers.

• Journal of the Korean Magnetics Society
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• v.14 no.1
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• pp.33-37
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• 2004

Cu$_{0.1}$Fe$_{0.9}$Cr$_2$S$_4$ has been studied with Mossbauer spectroscopy, x-ray diffraction, vibrating sample magnetometer (VSM), and magnetoresistance (MR) measurement. The crystal structure was determined to be a cubic spinel with lattice parameter a$_{0}$=9.9880 $\AA$. The MR measurements show a semiconductor behavior below 110 K and metal behaved above 100 K. The temperature dependence of magnetization of Cu$_{0.1}$Fe$_{0.9}$Cr$_2$S$_4$ was reported. In addition to a large irreversibility between the zero-field-cooling (ZFC) and the field-cooling (FC) magnetization at applied field H=100 Oe, a cusp-like anomaly was observed in both the FC and ZFC curves. It shifted toward the lower temperature region with increasing magnetic field, and then showed convex type maximum at 110 K, under the applied field of 5 kOe. The Mossbauer spectra were measured from 15 K to room temperature. The asymmetric line broadening was observed for the sample Cu$_{0.1}$Fe$_{0.9}$Cr$_2$S$_4$, and it was considered to be dynamic Jahn-Teller relaxation. The charge state of Fe ions was ferrous in character. The unusual reduction of magnetic hyperfine field below 110 K was interpreted in terms of cancellation effect between the mutually opposite orbital current field (H$_{L}$) and Fermi contact field (H$_{C}$).

• Clean Technology
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• v.19 no.3
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• pp.257-263
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• 2013

The zinc phosphate-coated mica (ZP/mica) pigments were prepared using phosphoric acid, zinc nitrate and mica as starting materials, and used as anticorrosive pigments. The scanning electron microscopy (SEM) and x-ray diffraction (XRD) techniques were used to observe the morphology and crystal structure of prepared pigments. The prepared pigments were incorporated into an epoxy binder to prepare coating and the corrosion inhibition performance of the pigments was evaluated using electrochemical impedance spectroscopy (EIS). It was found that the anticorrosive performance of the ZP/mica pigment prepared at $70^{\circ}C$ was the better than that prepared at $20^{\circ}C$. The formation of ZnO, in addition to $Zn_3(PO_4)_2{\cdot}2H_2O$, was observed on ZP/mica pigment prepared at $70^{\circ}C$. The excellent anticorrosive performance of ZP/mica pigment could be ascribed to the synergistic effect with electrochemical anticorrosive mechanism from zinc compounds on mica and barrier anticorrosive mechanism from lamellar mica.