• Title/Summary/Keyword: Ball milling process

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Evaluations of Microstructure and Hydrogenation Properties on $Mg_2NiH_x$ ($Mg_2NiH_x$ 수소저장합금의 미세결정구조 및 수소화 특성평가)

  • Seok, Song;Shin, Kyung;Kweon, Soon-Yong;Ur, Soon-Chul;Lee, Young-Geun;Hong, Tae-Whan
    • Transactions of the Korean hydrogen and new energy society
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    • v.16 no.3
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    • pp.238-243
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    • 2005
  • Mg and Mg-based alloys are most important hydrogen storage materials. It is a lightweight and low-cost materials with high hydrogen storage capacity. However, the formation of hydride at high temperature, the deterioration effect, the hydriding and dehydriding kinetics are bad factor for application. In this study, Mg and Ni have been produced by hydrogen induced mechanical alloying(HIMA) process. The raw materials, Mg(purity 99.9%) chip and Ni(purity 99.95%) chip was prepared by using a planetary ball mill apparatus(FRITSCH pulverisette 5). The balls to chips mass ratio(BCR) are 30:1. The hydrogen pressure induced 2.0MPa and milling times were 12, 24, 48, 72, 96 hours with a rotating speed of 200rpm. X-ray diffraction(XRD) analysis was made to characterize the crystallite size and misfit strain. The crystallite size measured by laser particle size analysis(PSA). Microstructure changes were investigated by scanning electron microscopy(SEM) and the transmission electron microscopy(TEM). The hydrogen storage properties were evaluated by using an Sivert's type automatic pressure-composition-therm(PCT) apparatus.

The Study on Peak Disappearance of Minor Phase and Formation of ${Al_3}Ti$ in Mechanically Alloyed Al-Ti Samples (기계적 합금화한 Al-Ti 시료에서 미소상 피이크의 소멸현상과 ${Al_3}Ti$ 형성에 관한 연구)

  • Kim, Jin-Gon;Kim, Hye-Seong;Kim, Byeong-Hui
    • Korean Journal of Materials Research
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    • v.11 no.12
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    • pp.1035-1041
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    • 2001
  • The refining process and solubility of Ti in Al matrix during mechanical alloying (MA) were investigated by using X-ray diffraction (XRD), transmission electron microscopy (TEM) as functions of alloy composition, milling time and ball to powder ratio (BPR). Mechanical alloyed samples were annealed for investigating their stability and the formation behavior of$Al_3Ti$in the temperature range from$200{\circ}C$to$600{\circ}C$. It is observed from present experimental that disappearance of Ti peaks in mechanically alloyed Al-10wt%Ti is not simply attributable to the dissolution of Ti into Al, but associated mainly with extreme refining and/or heavy straining of Ti particles The annealing of the mechanically alloyed Al-Ti powders show differences in aluminide formation behavior when Ti content in Al is equal to or less than l0wt% and higher than l5wt%Ti. When Ti-content in Al is equal to or less than l0wt%, the MA powders transform directly to a global equilibrium state forming $DO_{22}- type\;Al_3$Ti above$400{\circ}C$. In the Al-Ti samples with equal to or higher than l5wt%Ti, transitional phases of cubic$Al_3Ti$and tetragonal $Al_{24}Ti_8$ are formed above$400{\circ}C$. They are stable only below$500{\circ}C$, and, $DO_{22}-type\;Al_3Ti$ becomes dominant aluminide at temperature higher than$ 600{\circ}C$.

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Electrochemical Characteristics of Silicon/Carbon Composites with CNT for Anode Material (CNT를 첨가한 Silicon/Carbon 음극소재의 전기화학적 특성)

  • Jung, Min zy;Park, Ji Yong;Lee, Jong Dae
    • Korean Chemical Engineering Research
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    • v.54 no.1
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    • pp.16-21
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    • 2016
  • Silicon/Carbon/CNT composites as anode materials for lithium-ion batteries were synthesized to overcome the large volume change during lithium alloying-de alloying process and low electrical conductivity. Silicon/Carbon/CNT composites were prepared by the fabrication processes including the synthesis of SBA-15, magnesiothermic reduction of SBA-15 to obtain Si/MgO by ball milling, carbonization of phenolic resin with CNT and HCl etching. The prepared Silicon/Carbon/CNT composites were analysed by XRD, SEM, BET and EDS. In this study, the electrochemical effect of CNT content to improve the capacity and cycle performance was investigated by charge/discharge, cycle, cyclic voltammetry and impedance tests. The coin cell using Silicon/Carbon/CNT composite (Si:CNT=93:7 in weight) in the electrolyte of $LiPF_6$ dissolved in organic solvents (EC:DMC:EMC=1:1:1 vol%) has better capacity (1718 mAh/g) than those of other composition coin cells. The cycle performance of coin cell was improved as CNT content was increased. It is found that the coin cell (Si:CNT=89:11 in weight) has best capacity retension (83%) after 2nd cycle.

Hydrothermal Synthesis of Vanadium (IV) Dioxide and its Thermochromic Property (바나듐(IV) 이산화물의 수열합성 및 이의 열변색 특성)

  • Lee, Hun Dong;Son, Dae Hee;Lee, Won Ki;Jin, Young Eup;Lee, Gun-Dae;Park, Seong Soo
    • Applied Chemistry for Engineering
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    • v.26 no.4
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    • pp.427-431
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    • 2015
  • In this study, vanadium dioxide ($VO_2$) powder well known as a thermochromic material was prepared from $V_2O_5$ powder and oxalic acid dihydrate by hydrothermal and calcination process at various conditions. The chemical bonding and crystal structures in addition to thermal property of samples were determined using FE-SEM, XRD, XPS, and DSC. Also, spectroscopic and thermochromic properties of film samples were analyzed by UV-Vis-NIR spectroscopy after the thin film was prepared from the sol dispersed with the size of below 50 nm by the ball-milling of powder sample. With increasing the calcination temperature, the phase transition temperature of samples increased from $40^{\circ}C$ to $70^{\circ}C$ due to the increase of particle size.

A study on the fabrication technology of ceramic interconnect for the SOFC by wet process (습식법을 이용한 고체산화물 연료전지용 세라믹 연결재 제조 특성연구)

  • 이길용;김종희;송락현;백동현;정두환;신동열
    • Proceedings of the Materials Research Society of Korea Conference
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    • 2003.03a
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    • pp.200-200
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    • 2003
  • 고체산화물 연료전지(SOFC)에서 사용되는 연결재의 주 기능은 각 단위 셀의 연료극과 다음 셀의 공기극을 전기적으로 연결하여, 공기와 사용연료의 분리역할을 하기 위하여 사용된다. SOFC용 연결재는 다른 구성요소 소재보다, 높은 전자 전도성, 낮은 이온전도성, 우수한 기계 적강도가 요구되며, SOFC는 고온에서 작동되기 때문에, 상온에서 작동온도까지 다른 요소 소재들과 유사한 열팽창계수와 물리, 화학적으로 안정성이 요구된다. 현재 연결재 제조기술은 EVD, CVD, plasma spraying, tape casting 등 다양하게 연구되고 있으며, 본 연구는 세라믹 연결재 증착방법 중 저렴한 비용으로 대량 생산이 용이한 습식법(dip coaling)을 적용하여, 연료극 지지체식 flat-tube형 고체산화물 연료전지의 지지체를 위해 세라믹 연결재를 제조하고, 그 특성을 연구하였다. 세라믹 연결재로써 선정한 합성조성은 LaCr $O_3$에 Ca이 치환 고용된 L $a_{0.6}$C $a_{0.41}$Cr $O_3$으로 pechini법으로 합성하였다. 합성된 조성은 100$0^{\circ}C$에서 5시간 하소후 가속 Ball Milling하여 0.5$\mu\textrm{m}$의 평균입자크기를 얻을 수 있었다. XRD 상분석결과 perovskite상 (L $a_{1-x}$ Ca/x/Cr $O_3$)과 CaCr $O_4$를 얻을 수 있었다. slurry를 제조하여 막의 밀착성을 증진시키기 위해 sand blasting시킨 flat tube지지체에 진공펌프를 이용하여 소재내부와 외부의 압력차로 dip coating한 후, 140$0^{\circ}C$로 소결 하였다. coating 결과 박리현상은 없었으나, 표면과 단면의 SEM분석결과 다소 porous한 박막층이 형성되었으며, Ca이온이 지지체로 permeation되는 현상이 발생하였다. 이와 같은 결과로부터 보다 치밀한 박막생성을 위해, slurry 제조조건을 변화시켰으며, Ca이온의 migration을 막기 위해 barrier layer를 이용하였다 완전 소결된 지지체는 가스투과도와 전기전도도측정을 통하여 특성을 평가하였다.였다.다.

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Effect of Freezing and Sintering Condition of CuO-SnO2/Camphene Slurries on the Pore Structure of Porous Cu-Sn (CuO-SnO2/camphene 슬러리의 동결 및 소결조건이 Cu-Sn 다공체의 기공구조에 미치는 영향)

  • Kim, Joo-Hyung;Oh, Sung-Tag;Hyun, Chang-Yong
    • Journal of Powder Materials
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    • v.23 no.1
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    • pp.49-53
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    • 2016
  • The present study demonstrates the effect of freezing conditions on the pore structure of porous Cu-10 wt.% Sn prepared by freeze drying of $CuO-SnO_2$/camphene slurry. Mixtures of CuO and $SnO_2$ powders are prepared by ball milling for 10 h. Camphene slurries with 10 vol.% of $CuO-SnO_2$ are unidirectionally frozen in a mold maintained at a temperature of $-30^{\circ}C$ for 1 and 24 h, respectively. Pores are generated by the sublimation of camphene at room temperature. After hydrogen reduction and sintering at $650^{\circ}C$ for 2 h, the green body of the $CuO-SnO_2$ is completely converted into porous Cu-Sn alloy. Microstructural observation reveals that the sintered samples have large pores which are aligned parallel to the camphene growth direction. The size of the large pores increases from 150 to $300{\mu}m$ with an increase in the holding time. Also, the internal walls of the large pores contain relatively small pores whose size increases with the holding time. The change in pore structure is explained by the growth behavior of the camphene crystals and rearrangement of the solid particles during the freezing process.

Estimation of a Lattice Parameter of Sintered Ni-W Alloy Rods by a Neutron Diffraction Method (중성자 회절법에 의한 Ni-W 합금 소결체의 격자상수 측정)

  • Kim, Chan-Joong;Kim, Min-Woon;Park, Soon-Dong;Jun, Byung-Hyuk;Jang, Serk-Won;Seong, Baek-Seok
    • Journal of Powder Materials
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    • v.15 no.3
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    • pp.239-243
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    • 2008
  • Ni-W(1-5 at.%) alloy rods were made by powder metallurgy process including powder mixing, compacting and subsequent sintering. Ni and W powder of appropriate compositions were mixed by a ball milling and isostatically pressed in a rubber mold into a rod. The compacted rods were sintered at $1000^{\circ}C-1150^{\circ}C$ at a reduced atmosphere for densification. The lattice parameters of Ni-W alloys were estimated by a high resolution neutron powder diffractometer. All sintered rods were found to have a face centered cubic structure without any impurity phase, but the diffraction peak locations were linearly shifted with increasing W content. The lattice parameter of a pure Ni rod was $3.5238{\AA}$ which is consistent with the value reported in JCPDS data. The lattice parameter of N-W alloy rods increased by $0.004{\AA}$ for 1 atomic % of W, which indicates the formation of a Ni-W solid solution due to the substitution of nickel atoms by tungsten atoms of larger size.

Size Control of Nd-Fe-B Precursor Particles Prepared by Spray Drying and Its Effect on the Magnetic Properties of Nd-Fe-B Alloy Powders after Reduction-Diffusion (분무건조된 Nd-Fe-B 전구체 입자의 크기조절 및 환원-확산 후 자기 특성에 미치는 영향)

  • Baek, Youn-Kyoung;Seo, Young-Taek;Lee, Jung-Goo;Kim, Dong Su;Bae, Dong Sik;Choi, Chul-Jin
    • Journal of Powder Materials
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    • v.20 no.5
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    • pp.359-365
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    • 2013
  • In this study, we fabricated $Nd_2Fe_{14}B$ hard magnetic powders with various sizes via spray drying combined with reduction-diffusion process. Spray drying is widely used to produce nearly spherical particles that are relatively homogeneous. Thus, the precursor particles were prepared by spray drying using the aqueous solution containing Nd salts, Fe salts and boric acid with the target stoichiometric composition of $Nd_2Fe_{14}B$. The mean particle sizes of the spray-dried powders are in the range from one to seven micrometer, which are adjusted by controlling the concentrations of precursor solutions. After debinding the as-prepared precursor particles, ball milling was also conducted to control the particle sizes of Nd-Fe-B oxide powders. The resulting particles with different sizes were subjected to subsequent treatments including hydrogen reduction, Ca reduction and washing for CaO removal. The size effect of Nd-Fe-B oxide particles on the formation of $Nd_2Fe_{14}B$ phase and magnetic properties was investigated.

Preparation of Sintered ATZ by Sol-Gel Process and Properties (졸-겔법에 의한 알루미나 강화 지르코니아 소결체의 제조 및 특성)

  • Han, Kyoung Ran;Park, Sun Jin;Hong, Kug-Sun;Jun, Hyung Woo
    • Analytical Science and Technology
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    • v.6 no.2
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    • pp.225-229
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    • 1993
  • ATZ was prepared by adding an alumina sol equivalent to 2wt% as $Al_2O_3$ to an aqueous slurry of alumina (AKP-30) and zirconia (TZ-2Y or TZ-0Y) in the range of 10-30ATZ, followed by gelation, calcination, and sintereing between $1450^{\circ}C{\sim}1550^{\circ}C$ for 2h. They showed excellent microstructure with alumina grains of <$0.5{\mu}m$ and>99% of the theoretical density. Fracture toughness of ${\sim}8MPa{\cdot}m^{1/2}$ was observed around 20ATZ which was higher than $6MPa{\cdot}m^{1/2}$ obtainable by ball-milling.

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Classification of Chemical Warfare Agents Using Thick Film Gas Sensor Array (후막 센서 어레이를 이용한 화학 작용제 분류)

  • Kwak Jun-Hyuk;Choi Nak-Jin;Bahn Tae-Hyun;Lim Yeon-Tae;Kim Jae-Chang;Huh Jeung-Soo;Lee Duk-Dong
    • Journal of the Korea Institute of Military Science and Technology
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    • v.7 no.2 s.17
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    • pp.81-87
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    • 2004
  • Semiconductor thick film gas sensors based on tin oxide are fabricated and their gas response characteristics are examined for four simulant gases of chemical warfare agent (CWA)s. The sensing materials are prepared in three different sets. 1) The Pt or Pd $(1,\;2,\;3\;wt.\%)$ as catalyst is impregnated in the base material of $SnO_2$ by impregnation method.2) $Al_2O_3\;(0,\;4,\;12,\;20\;wt.\%),\;In_2O_3\;(1,\;2,\;3\;wt.\%),\;WO_3\;(1,\;2,\;3\;wt.\%),\;TiO_2\;(3,\;5,\;10\;wt.\%)$ or $SiO_2\;(3,\;5,\;10\;wt.\%)$ is added to $SnO_2$ by physical ball milling process. 3) ZnO $(1,\;2,\;3,\;4,\;5\;wt.\%)$ or $ZrO_2\;(1,\;3,\;5\;wt.\%)$ is added to $SnO_2$ by co-precipitation method. Surface morphology, particle size, and specific surface area of fabricated sensing films are performed by the SEM, XRD and BET respectively. Response characteristics are examined for simulant gases with temperature in the range 200 to $400^{\circ}C$, with different gas concentrations. These sensors have high sensitivities more than $50\%$ at 500ppb concentration for test gases and also have shown good repetition tests. Four sensing materials are selected with good sensitivity and stability and are fabricated as a sensor array A sensor array Identities among the four simulant gases through the principal component analysis (PCA). High sensitivity is acquired by using the semiconductor thick film gas sensors and four CWA gases are classified by using a sensor array through PCA.