• 한국광물학회지
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• 제31권3호
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• pp.161-172
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• 2018

멀티 앤빌 프레스(multi-anvil press)는 일반적으로 5-25 GPa의 압력범위와 ${\sim}2,300^{\circ}C$의 온도범위를 구현할 수 있는 고압 기기로, 지구과학에서는 상부맨틀-맨틀전이대까지의 지구 구성물질의 구조를 연구하는 데 도움이 된다. 본 연구에서는 광물의 상전이를 이용한 멀티 앤빌 프레스에 대한 압력-부하 보정(pressure-load calibration) 과정을 소개하고, 시료실(sample chamber) 내에 존재할 수 있는 온도구배에 대해서 논의하였다. 압력-부하 보정은 14/8 G2, 14/8 step, 14/8 HT 조립세트(assembly set)와 18/12 조립세트에 대해 1,100톤 멀티 앤빌 프레스를 이용하여 수행했다. 초기 물질로 석영, 규회석구조의 $CaGeO_3$, 포르스테라이트를 사용했고, 고압상의 동정은 XRD 분석을 통해 수행하였다. 광물의 상전이를 통해 $1,200^{\circ}C$에서 시료에 가해지는 압력을 유추할 수 있었으며, ${\alpha}$-석영에서 코에사이트로의 상전이는 3.1 GPa, 석류석 구조의 $CaGeO_3$에서 페로브스카이트 구조의 $CaGeO_3$로의 상전이는 5.9 GPa, 코에사이트에서 스티쇼바이트로의 상전이는 9.2 GPa, 포르스테라이트에서 와즐리아이트로의 상전이는 13.6 GPa의 압력 확인에 이용했다. XRD 결과로 획득한 압력-부하 보정 곡선은 기존에 보고된 유사한 기기의 압력-부하 보정 곡선에 비해 동일 압력을 구현하기 위해 50톤 가량의 유압이 더 필요한 것으로 확인됐다. 이러한 차이는 시료실의 크기 및 조립세트의 압력 매체(pressure medium)와 이차앤빌 사이의 마찰력으로부터 기인한 유압 손실에 의한 것으로 생각된다. 또한 본 연구에서는 14/8 HT 조립세트에서의 시료실 내의 온도구배를 확인했다. 특히 열전대(thermocouple)의 위치 변화에 따라 시료실 높이에 평행한 방향으로 약 ${\sim}200^{\circ}C/mm$에 해당하는 온도구배가 존재한다. 본 연구로부터 구한 멀티 앤빌 프레스의 압력-부하 보정 곡선과 시료실 내의 온도구배 값은 앞으로 맨틀 내에서의 다양한 비정질 및 결정질의 지구물질에 대한 원자 구조의 변화와 그에 따른 물성 변화를 설명하는 데 적용할 수 있다.

• 한국광물학회지
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• 제26권1호
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• pp.35-44
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• 2013

유사 올리빈 구조를 가지는 탄소코팅 합성 $Li^+Fe^{2+}(PO_4)^{3-}$ 분말시료에 대한 상온-고압실험을 대칭 다이아몬드 앤빌기기를 이용하여 35.0 GPa까지 시행하였다. $LiFePO_4$의 압축 데이터를 이용하여 계산된 체적탄성률은 $130.1{\pm}10.3$ GPa이다. 18 GPa 이상의 압력에서 d = 3.386 ${\AA}$ 위치에 새로운 피크가 관찰되고 35 GPa에서는 d = 2.854 ${\AA}$에 또 다른 피크가 관찰되고 있으나 주 결정구조는 사방정계인 것으로 판단된다. 압력에 대한 단위 포 부피의 압축은 M1($Li^+O_6$)의 수축이 두드러지고 M2($Fe^{2+}O_6$)와 사면체($PO_4$)의 수축은 상대적으로 작은 것으로 나타났다.

• 대한전자공학회:학술대회논문집
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• 대한전자공학회 2001년도 The 6th International Symposium of East Asian Resources Recycling Technology
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• pp.610-615
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• 2001

Over 800 thousand tons per year (TPY) agricultural biowastes, such as sugar cane bagasse, sugarcane leaf, rice straw, rice husk and corn leaf, are produced in Taiwan. These biomasses are the major types of agricultural wastes and are abundantly available. However, these biowastes cause disposal and landfill problems. Ossification ashes of the agricultural biowastes containing 70-95 % amorphous silica would make the utilization system of agricultural biowaste ashes become highly economically and environmentally attractive. Experimentally, high crystallinity (99%$^{+}$) zeolites ZSM-5 and ZSM-48 synthesized from the reaction mixtures containing a silica source from ashes of these biowastes gasification were investigated. Tetrapropylammonium bromide (TPABr) and 1,6-diamino-hexane (C$_{6}$ DN) were used as structure-directing agents in syntheses of ZSM-5 and ZSM-48, respectively. X-ray powder diffraction (XRD) and scanning electron microscopy/energy dispersive spectroscopy (SEM/EDX) data indicated that ZSM-5 or ZSM-48 with a high crystallinity can be obtained within 48 hours of crystallization in the high pressure (15-20 atm) autoclave at 393-473 K. The Si/Al ratios of synthetic zeolite products were determined by X-ray fluorescence (XRF) and induced couple plasma/mass spectroscopy (ICP/MS). It was observed that the ZSM-5 crystals a.e composed of hexagonal rod-shaped crystals with typically 8-13 пm in size by SEM. In addition, ZSM-48 crystalline materials are composed of spherical aggregates of needle-shaped or rod-like crystals with typically 2-3 пm in diameter and 6-8 пm in length.h.

• 한국진공학회:학술대회논문집
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• 한국진공학회 2012년도 제42회 동계 정기 학술대회 초록집
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• pp.245-245
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• 2012

Syntheses of oxide supported metal catalysts by wet-chemical routes have been well known for their use in heterogeneous catalysis. However, uniform deposition of metal nanoparticles with controlled size and shape on the support with high reproducibility is still a challenge for catalyst preparation. Among various synthesis methods, arc plasma deposition (APD) of metal nanoparticles or thin films on oxide supports has received great interest recently, due to its high reproducibility and large-scale production, and used for their application in catalysis. In this work, Au and Pt nanoparticles with size of 1-2 nm have been deposited on titania powder by APD. The size of metal nanoparticles was controlled by number of shots of metal deposition and APD conditions. These catalytic materials were characterized by x-ray diffraction (XRD), inductively coupled plasma (ICP-AES), CO-chemisorption and transmission electron microscopy (TEM). Catalytic activity of the materials was measured by CO oxidation using oxygen, as a model reaction, in a micro-flow reactor at atmospheric pressure. We found that Au/$TiO_2$ is reactive, showing 100% conversion at $110^{\circ}C$, while Pt/$TiO_2$ shows 100% conversion at $200^{\circ}C$. High activity of metal nanoparticles suggests that APD can be used for large scale synthesis of active nanocatalysts. We will discuss the effect of the structure and metal-oxide interactions of the catalysts on catalytic activity.

• 한국수소및신에너지학회논문집
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• 제25권1호
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• pp.19-27
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• 2014

Mg hydride has a high hydrogen capacity (7.6%), at high temperature, and is a lightweight and low cost material, thus it a promising hydrogen storage material. However, its high operation temperature and very slow reaction kinetics are obstacles to practical application. In order to overcome these disadvantages of Mg hydride, graphene powder was added to it. The addition of graphene has been shown to reduce the operating temperature of dehydrogenation. Moreover, in this report the environmental aspects of $MgH_x$-Graphene composites are investigated by means of the environmental life cycle assessment (LCA) method. $MgH_x$-Graphene mixture was prepared by hydrogen induced mechanical alloy (HIMA). The synthesized powder was characterized by XRD(X-ray Diffraction). The hydrogenation behaviors were evaluated by using a Sievert's type automatic PCT apparatus. Such evaluation of Materials also conducted in the LCA. From the result of P-C-T(Pressure-Composition-Temperature) curves, the $MgH_x$-3wt.% graphene composite was evaluated as having a 5.86wt.% maximum hydrogen storage capacity, at 523K. From absorption kinetic testing, the $MgH_x$-7wt.% graphene composite was evaluated as having a maximum 6.94wt.%/ms hydrogen absorption rate, at 573K. Environment evaluation results for the $MgH_x$-graphene composites and other materials indicated environmental impact from the electric power used and from the materials themselves.

• 한국재료학회지
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• 제24권1호
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• pp.53-59
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• 2014

The corrosion resistance of submerged entry nozzle (SEN) materials were investigated for high-class steel manufacturing. Composite samples were fabricated by mixing $ZrO_2$, $Al_2O_3$, MgO, mullite, spinel, and carbon. The raw materials were mixed with attrition milling, compacted in a uniaxial pressure of 200MPa and calcined at $1000^{\circ}C$ for 3 h in $N_2$ atmosphere. The bulk density and apparent porosity of the calcined samples were measured by the liquid displacement method in water using Archimedes's principle. The corrosion resistance of the samples were measured by cup test with mold powder at $1550^{\circ}C$ for 2 h. The microstructure and elemental analysis of samples were observed by scanning electron microscopy (SEM), energy dispersive spectrum (EDS), and X-ray diffraction pattern (XRD). The XRD result shows that the starting raw materials were crystalline phase. The microstructure of fabricated specimen was investigated before and after corrosion tests at $1000^{\circ}C$ and $1550^{\circ}C$ for 2h. $ZrO_2$-C composite showed good resistance in the slag corrosion test. Among the composite oxide materials, $ZrO_2-Al_2O_3$-C and $ZrO_2$-MgO-C showed better resistance than $ZrO_2$-C in the slag corrosion test. The diameter variation index of $ZrO_2$-C refractory was 16.1 at $1000^{\circ}C$ for 2 h. The diameter variation index of the $ZrO_2-Al_2O_3$-C refractory was larger than that of the $ZrO_2$-C refractory at $1550^{\circ}C$ for 2 h.

• Bulletin of the Korean Chemical Society
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• 제17권9호
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• pp.794-798
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• 1996

Solid solutions of the nonstoichiometric Dy1-xSrxCoO3-y system with the compositions of x=0.00, 0.25, 0.50, 0.75, and 1.00 have been synthesized by the solid state reaction at 1000 ℃ under atmospheric air pressure. The crystallographic structures of the solid solutions are analyzed by the powder X-ray diffraction patterns at room temperature. The analyses assign the compositions of x=0.00 and 0.25 to the orthorhombic system with space group of Pbnm/D2h16, the compositions of x=0.50 and 0.75 to the tetragonal system like a typical SrCoO2.86, and the composition of x=l.00 or SrCoO2.50 to the brownmillerite type system with space group of I**a. The reduced lattice volumes increase with x value due to the larger radius of Sr2+ ion than that of Dy3+ ion. The mole ratio of Co4+ ion to total Co ion with mixed valence state between Co3+ and Co4+ ions at B sites or τ value has been determined by an iodometric titration. All the samples except for the DyCoO3 compound show the mixed valnce state and thus the composition of x=0.50 has the maximum τ value in the system. The oxygen vacancies increasing with x value are randomly distributed over the crystal lattice except for the composition of x=l.00 which have the ordering of the oxygen vacancies. The nonstoichiometric chemical formulas of the Dy1-xSrxCo3+1-τCo4+τO3-(x-τ)/2 system are formulated from the x, τ, and y values. The electrical conductivity in the temperature range of 100 to 900 K increases with τ value linearly because of positive holes of the Co4+ ions in π* band as a conducting carrier. The activation energy of the x=0.50 as Ea=0.17 eV is minimum among other compouds. Broad and high order transition due to the overlap between σ* and π* bands broadened by the thermal activation is observed near 1000 K and shows a low temperature-semiconducting behavior. Magnetic properties following the Currie-Weiss law show the low to high spin transition in the cobaltate perovskite. Especially, the composition of x=0.75 presents weak ferromagnetic behavior due to the Co3+-O2--Co4+ indirect superexchange interaction.