• 한국분말재료학회지
• /
• 제28권6호
• /
• pp.497-501
• /
• 2021

Cobalt (Co) is mainly used to prepare cathode materials for lithium-ion batteries (LIBs) and binder metals for WC-Co hard metals. Developing an effective method for recovering Co from WC-Co waste sludge is of immense significance. In this study, Co is extracted from waste cemented carbide soft scrap via mechanochemical milling. The leaching ratio of Co reaches approximately 93%, and the leached solution, from which impurities except nickel are removed by pH titration, exhibits a purity of approximately 97%. The titrated aqueous Co salts are precipitated using oxalic acid and hydroxide precipitation, and the effects of the precipitating agent (oxalic acid and hydroxide) on the cobalt microstructure are investigated. It is confirmed that the type of Co compound and the crystal growth direction change according to the precipitation method, both of which affect the microstructure of the cobalt powders. This novel mechanochemical process is of significant importance for the recovery of Co from waste WC-Co hard metal. The recycled Co can be applied as a cemented carbide binder or a cathode material for lithium secondary batteries.

• 한국세라믹학회지
• /
• 제48권5호
• /
• pp.454-457
• /
• 2011

We report the preparation of nanocrystalline cobalt ferrite, $CoFe_2O_4$, particles using recycled $Co_3O_4$ and their surface coating with silica using micro emulsion method. Firstly, the $Co_3O_4$ powders were separated from waste cemented carbide with acid-base chemical treatment. The cobalt ferrite nanoparticles with the size 10 nm are prepared by thermal decomposition method using recycled $Co_3O_4$. $SiO_2$ was coated onto the $CoFe_2O_4$ particles by the micro-emulsion method. The $SiO_2$-coated $CoFe_2O_4$ particles were studied their physical properties and characterized by X-ray diffraction (XRD), high resolution-transmission electron microscopy (TEM) analysis and CIE Lab value.

• The Korean Journal of Ceramics
• /
• 제5권4호
• /
• pp.395-399
• /
• 1999

MgO/metal nanocomposite powder mixtures were prepared by solution chemical processes to obtain suitable structure for ceramic/metal nanocomposites. Nickel or cobalt nitrate, as a source of metal dispersion, was dissolved into alcohol and mixed with magnesia powder. After calcined in air, these powders were reduced by hydrogen. Densified nanocomposites were successively obtained by Pulse Electric Current Sintering (PECS) process. The dispersed metal partical size depended on temperature and time in calcination and reduction processes. The phase analyses in the synthesized powders as a functioni of temperature were tracked using a dynamic high temperature X-ray diffractioni (HTXRD) system. Phase and crystallite size analyses were done using X-ray diffractioni and TEM. The MgO/metal nanocomposites were successfully fabricated, and ferromagnetic responses with enhanced coercive force were also investigated for these composites.

• Korean Chemical Engineering Research
• /
• 제55권6호
• /
• pp.861-867
• /
• 2017

니켈 함량이 높은 리튬이차전지용 NCA 양극소재의 용량 및 수명특성을 향상시키기 위하여 붕소와 코발트를 상업용 $Li_{1.06}Ni_{0.91}Co_{0.08}Al_{0.01}O_2$ (NCA)에 도핑하여 리튬이차전지의 양극소재로 사용하였다. 상업용 NCA 양극소재는 약 $5{\mu}m$와 $12{\mu}m$ 크기의 2차 입자들이 혼합되어 있고 붕소와 코발트 도핑후 입자크기는 조금 감소되었다. 붕소와 코발트를 도핑한 NCA-B와 NCA-Co의 초기 방전용량은 각각 214 mAh/g과 200 mAh/g으로 도핑하지 않은 NCA에 비해 높게 나타났으며, 특히 NCA-Co는 20번째의 방전용량이 157 mAh/g으로 가장 우수한 방전용량특성을 나타내었다. 이는 코발트를 도핑함으로써 c축 방향으로의 결정이 성장되어 리튬이온의 확산이 용이하기 때문이다.

• 한국결정성장학회지
• /
• 제12권2호
• /
• pp.87-90
• /
• 2002

$LiCoO_{2}$ powders were synthesized at various temperatures using lithium hydroxide and cobalt hydroxide as precursors prepared by precipitation process and freeze-drying. In this study, the$LiCoO_{2}$ samples were synthesized via a solid state reaction with various LiOH concentration between 10 % and 30 % excess. And $LiCoO_{2}$powders were calcined at 600~$800^{\circ}C$ in a short time. Measurements of XRD and SEM were performed to characterize the properties of the prepared materials. The effect of amount of Li ions on the structural change in powder has been examined using the XRD analysis. For the not added excess of LiOH, CoOOH phase presented in the XRD pattern of $LiCoO_{2}$ due to loss of Li ions during firing. The morphology and particle size of the powders were examined using SEM. The obtained powders are high temperature-$LiCoO_{2}$HT-LiCoO$_{2}$) and homogeneous with the range of grain size in the order of hundreds of nanometers. The effects of variation of LiOH concentration on the structural change in powder were investigated using the Rietveld analysis. As an analysis result, c/a is constant by 4.99 on all occasions. Finally, the structure of HT-$LiCoO_{2}$ was simulated by the commercial software $Creius^{2}$(Molecular Simulations, Inc.) from the results of Rietveld analysis.

• 한국재료학회지
• /
• 제22권6호
• /
• pp.316-320
• /
• 2012

$Co_3O_4$, $Al_2O_3$ and $Co_3O_4$/$Al_2O_3$ mesoporous powders were prepared by a sol-gel method with starting matierals of aluminum isopropoxide and cobalt (II) nitrate. A P123 template is employed as an active organic additive for improving the specific surface area of the mixed oxide by forming surfactant micelles. A transition metal cobalt oxide supported on alumina with and without P123 was tested to find the most active and selective conditions as a heterogeneous catalyst in the reaction of styrene epoxidation. A bBlock copolymer-P123 template was added to the staring materials to control physical and chemical properties. The properties of $Co_3O_4$/$Al_2O_3$ powder with and without P123 were characterized using an X-ray diffractometer (XRD), a Field-Emission Scanning Electron Microscope (FE-SEM), a Bruner-Emmertt-Teller (BET) surface analyzer, and $^{27}Al$ MAS NMR spectroscopy. Powders with and without P123 were compared in catalytic tests. The catalytic activity and selectivity were monitored by GC/MS, $^1H$, and $^{13}C$-NMR spectroscopy. The performance for the reaction of epoxidation of styrene was observed to be in the following order: [$Co_3O_4$/$Al_2O_3$ with P123-1173 K > $Co_3O_4$/$Al_2O_3$ with P123-973 K > $Co_3O_4$-973 K>$Co_3O_4$/$Al_2O_3$-973 K > $Co_3O_4$/$Al_2O_3$ with P123-1473 K > $Al_2O_3$-973 K]. The existence of ${\gamma}$-alumina and the nature of the surface morphology are related to catalytic activity.

• 한국재료학회:학술대회논문집
• /
• 한국재료학회 2011년도 춘계학술발표대회
• /
• pp.58.1-58.1
• /
• 2011

WC-Co and other similar cemented carbides have been widely used as hard materials in industrial cutting tools and as mould metals; and a number of techniques have been applied to improve its microstructural characteristics, hardness and ear resistance. Cobalt is used primarily to facilitate liquid phase sintering and acts as a matrix, i.e. a cementing phase between WC grains. A uniform distribution of metal phase in a ceramic is beneficial for improved mechanical properties of the composite. WC-Co, starting from initial powders, is vastly used for a variety of machining, cutting, drilling, and other applications because of its unique combination of high strength, high hardness, high toughness, and moderate modulus of elasticity, especially with fine grained WC and finely distributed cobalt. In this study, that started with two different compositions of initial powders, WC-7.5wt%Co and WC-12wt%Co with initial powder size being 1~3 ${\mu}m$, magnetic pulsed compaction followed by subsequent vacuum sintering were carried out to produce consolidated preforms. Magnetic Pulsed Compaction (MPC), a very short duration (~600 ${\mu}s$), high pressure (~4 Gpa), high-density preform molding method was used with varied pressure between 0.5 and 3.0 Gpa, in order to reach an initial high density that would help improve the sintering behavior. For both compositions and varied MPC pressure, before and after sintering, changes in microstructural behavior and mechanical properties were analyzed. With proper combination of MPC pressure and sintering, samples were obtained with better mechanical properties, densification and microstructural behavior, and considerably improved than other conventional processes.

• 한국분말재료학회지
• /
• 제16권5호
• /
• pp.310-315
• /
• 2009

Ultra-fine TiC/Co composite powder was synthesized by the carbothermal reduction process without wet chemical processing. The starting powder was prepared by milling of titanium dioxide and cobalt oxalate powders followed by subsequent calcination to have a target composition of TiC-15 wt.%Co. The prepared oxide powder was mixed again with carbon black, and this mixture was then heat-treated under flowing argon atmosphere. The changes in the phase, mass and particle size of the mixture during heat treatment were investigated using XRD, TG-DTA and SEM. The synthesized oxide powder after heat treatment at 700$^{\circ}C$ has a mixed phase of TiO$_2$ and CoTiO$_3$ phases. This composite oxide powder was carbothermally reduced to TiC/Co composite powder by the solid carbon. The synthesized TiC/Co composite powder at 1300$^{\circ}C$ for 9 hours has particle size of under about 0.4 $\mu$m.

• Korean Chemical Engineering Research
• /
• 제50권6호
• /
• pp.1008-1014
• /
• 2012

국내의 경우 배출되는 이산화탄소의 양은 연간 6억톤 이상으로 대기로의 방출을 막기 위해 이 중 일부를 포집하여 저장을 하여야 하나, 아직 적당한 저장소를 발견하지 못한 상태이다. 따라서 포집된 이산화탄소의 일부를 다시 유용한 탄소원으로 전환하여 사용하고자 하는 연구가 많이 진행되고 있다. 본 연구의 목적은 안정한 이산화탄소를 보다 적은 에너지원을 사용하여 유용한 탄소자원을 만드는데 있다. 이를 위해 환원가스와 금속계 산화물(활성화제)이 필요하다. 따라서 환원가스는 수소를 사용하였고, 활성화제로는 코발트계 페라이트를 사용하였다. 활성화제는 제법에 따라 물성에 대한 차이가 있을 것으로 판단하여 고상법과 수열합성법을 이용해 제조된 분말을 사용하여 각각 이산화탄소 분해 특성 연구를 수행하였다. 이산화탄소의 분해 특성을 관찰하기 위해 TPR/TPO와 TGA 장치를 사용하였다. TPR/TPO를 이용한 $CO_2$에 의한 흡착분해 곡선면적을 측정한 결과 고상법으로 제조된 활성화제 중 CoO의 함량이 5와 10 wt%일때 우수한 성능을 나타내었다. 마찬가지로 TGA를 이용한 실험결과에서도 고상법에 의해 제조된 시료가 수소에 의한 흡착환원이 29.0 wt% 발생하였고, $CO_2$에 의한 산화량도 27.5 wt%로 가장 높게 나타났다. 그리고 $CO_2$의 분해효율이 95%로 우수한 이산화탄소 전환 특성을 나타내었다.

• 한국분말재료학회지
• /
• 제22권5호
• /
• pp.350-355
• /
• 2015

Perforated polygonal cobalt oxide ($Co_3O_4$) is synthesized using electrospinning and a hydrothermal method followed by the removal of a carbon nanofiber (CNF) template. To investigate their formation mechanism, thermogravimetric analysis, field-emission scanning electron microscopy, transmission electron microscopy, X-ray diffraction, and X-ray photoelectron spectroscopy are examined. To obtain the optimum condition of perforated polygonal $Co_3O_4$, we prepare three different weight ratios of the Co precursor and the CNF template: sample A (Co precursor:CNF template- 10:1), sample B (Co precursor:CNF template-3.2:1), and sample C (Co precursor:CNF template-2:1). Among them, sample A exhibits the perforated polygonal $Co_3O_4$ with a thin carbon layer (5.7-6.2 nm) owing to the removal of CNF template. However, sample B and sample C synthesized perforated round $Co_3O_4$ and destroyed $Co_3O_4$ powders, respectively, due to a decreased amount of Co precursor. The increased amount of the CNF template prevents the formation of polygonal $Co_3O_4$. For sample A, the optimized weight ratio of the Co precursor and CNF template may be related to the successful formation of perforated polygonal $Co_3O_4$. Thus, perforated polygonal $Co_3O_4$ can be applied to electrode materials of energy storage devices such as lithium ion batteries, supercapacitors, and fuel cells.