• Korean Journal of Materials Research
• /
• v.9 no.6
• /
• pp.615-621
• /
• 1999

The new process in order to fabricate of Ni catalyst with high activity by the mechanochemical(MC) method which was combined the mechanical alloying(MA) and the chemical treatment process. The microstructure and characterization of mechanically alloyed Ni-5-wt% Al powder and Ni catalyst gained by alkali leaching were investigated byt he various analysis such as XRD, SEM-EDS, HRTEM and laser particle analyzer. The steady state powder with 1~2$\mu\textrm{m}$ mean particle size was obtained after 30hr milling with the PCA of 2 wt% stearic acid under the condition of grinding stainless steel ball to powder ratio of 60:1 and rotating speed fo 300rpm. According to result of HRTEM diffraction pattern, MA powder of the steady state was nanocrystalline $Al_3$$Ni_2$ intermetallic compound. Ni catalyst was obtained after KOH leaching of the steady state powder was about 20nm nanocrystalline which contained about 8 wt % Al.

• Journal of the Korean Ceramic Society
• /
• v.41 no.1
• /
• pp.86-91
• /
• 2004

$LiCoO_2$ cathode powders with round particle shaped and nano grain sized of 70-300nm were synthesized by a mechanochemical method. The surface of Li-Co precursor prepared by freeze drying method was modified by $K_2SO_4$ coating and ball milling was used for the coating process. The precursor was crystallized to high temperature form of $LiCoO_2$ at $800^{\circ}C$ and the grain growth was inhibited by the $K_2SO_4$ coating effect. The $K_2SO_4$ coating was not decomposed at $800^{\circ}C$ and prevented the contact in the Li-Co precursor particles. The nano-sized $LiCoO_2$ powder had tetragonal phase and it affected the Li diffusion through the surface of particles. It means that the anode materials for hight performance battery should be satisfied not only small particle size but phase contol on the surface of particles. In this study, the powder characteristics and rate capabilities were compared with a commercial powder and the nano-sized $LiCoO_2$ powder fabricated by the mechanochemical method. And the crucial factor which affects on battery performance was also examined.

• Resources Recycling
• /
• v.27 no.4
• /
• pp.57-64
• /
• 2018

Water leaching of tungsten(W) and vanadium(V) was researched from their oxides through mechanochemical (MC) reaction with alkali compounds. Intensive grinding for the mixture of tungsten/vanadium oxide and alkali compounds (NaOH, $Na2CO_3$) was carried out with change of their mixing ratios and grinding duration. Water soluble compounds, $Na_2WO_4$ and $NaVO_3$, were synthesized through MC reaction and their solubilities increased in proportion to the mixing ratio of sodium compound and grinding times. Whereas vanadium leachability was less affected by the mixting ratio and grinding times. The leachabilities of 99.0% were accomplished by a short period of MC treatment, W (30 min.) and V (5 min.). This process enable us to extract W and V from their oxides via a water leaching, and can be applied to the selective recovery of W and V from $DeNO_x$ spent catalysts.

• Bulletin of the Korean Chemical Society
• /
• v.32 no.2
• /
• pp.536-540
• /
• 2011

This study reports the origin of the electrochemical improvement of $LiFePO_4$ when synthesized by wet milling using acetone without conventional carbon coating. The wet milled $LiFePO_4$ delivers 149 $mAhg^{-1}$ at 0.1 C, which is comparable to carbon coated $LiFePO_4$ and approximately 74% higher than that of dry milled $LiFePO_4$, suggesting that the wet milling process can increase the capacity in addition to conventional carbon coating methods. UV spectroscopy, elemental microanalysis, and evolved gas analysis are used to find the root cause of the capacity improvement during the mechanochemical reaction in acetone. The analytical results show that the improvement is attributed to the conductive residual carbon on the surface of the wet milled $LiFePO_4$ particles, which is produced by the reaction of $FeC_2O_4{\cdot}2H_2O$ with acetone during wet milling through oxygen deficiency in the precursor.

• Proceedings of the Korea Association of Crystal Growth Conference
• /
• 1997.10a
• /
• pp.81-85
• /
• 1997

철질화물 및 Mo-Si계 규화물을 합성하기 위하여 실온 메카노케미칼 공정을 적용하였다. 메카노케미칼 처리는 고에너지 유성형 볼밀장치를 사용하였고 용기는 진공배기 후 암모니아 혹은 아르곤 가스로 충전시킨 후 벌밀처리를 행하였다. 분말의 특성평가는 XRD, DTA/DSC, SEM 및 EPMA 등에 의하여 행하였다. 철질화물의 경우 실온에서 최대 23.3 at.%N의 $\varepsilon$상 질화물을 얻을 수 있었다. 또한 Mo-SirP의 경우 100시간 메카노케미칼 처리시킴으로서 MiSi$_2$규화물을 합성할 수 있었으며 얻어진 분말의 결정립은 25cm로 매우 미세한 결정립의 분말재료임이 확인되었다.

• Korean Journal of Materials Research
• /
• v.13 no.1
• /
• pp.24-30
• /
• 2003

The Raney Ni catalyst was fabricated by mechanochemically process(MC process) in the Al-Ni system. Intermetallic compound obtained by mechanical alloying was leached in an alkaline solution. The characteristics of the mechanically alloyed powder and Raney Ni catalyst were analyzed by XRD, ICP-AES and EXAFS. In Al-50wt.%Ni, the metastable intermetallic compound phase close to AlNi phase was obtained by mechanical alloying unlike Al-Ni equilibrium phase diagram. The metastable intermetallic compound was transformed into $Al_3$$Ni_2$phase via the annealing at $750^{\circ}C$. The microstructure of Raney Ni fabricated by MC process was mainly bcc Ni including fcc Ni.

• 한국전기화학회:학술대회논문집
• /
• 2003.07a
• /
• pp.193-197
• /
• 2003

Mixture of $Ni(OH)_2-Mg(OH)_2$ used as the precurs was treated by mechnochemical(MC) and hand grinding process. Carbon nanofibers(CNF) were prepared using CVD process with the above prepared catalyst. CNFs with a uniform diameter were obtained with MC process treated catalyst, and the diameter could be controlled by tuning the grinding time. CNF bundles with close coalescence were produced with MC treated catalyst. After purification of CNFs and loading with Pt, they were used in fuel cell as the cathode catalyst support. The performance with carbon nanofibers prepared using ground mixture was found to be better than that prepared using unground mixture, which is attributed to the homogeneous CNFs with small diameter and specific interaction between Pt and CNFs.

• Bulletin of the Korean Chemical Society
• /
• v.34 no.2
• /
• pp.433-436
• /
• 2013

Carbon-coated $Li_3V_2(PO_4)_3-LiMnPO_4$ composite cathode materials are first reported in this work, prepared by the mechanochemical process with a complex metal oxide as the precursor and sucrose as the carbon source. X-ray diffraction pattern of the composite material indicates that both olivine $LiMnPO_4$ and monoclinic $Li_3V_2(PO_4)_3$ co-exist. We further investigated the electrochemical properties of our $Li_3V_2(PO_4)_3-LiMnPO_4$ composite cathode materials using galvanostatic charging/discharging tests, where our $Li_3V_2(PO_4)_3-LiMnPO_4$ composite electrode materials exhibit the charge/discharge efficiency of 91.9%, while $Li_3V_2(PO_4)_3$ and $LiMnPO_4$ exhibit the efficiency of 87.7 and 86.7% in the first cycle. The composites display unique electrochemical performances in terms of overvoltage and cycle stability, displaying a reduced gap of 141.6 mV between charge and discharge voltage and 95.0% capacity efficiency after $15^{th}$ cycles.

• Journal of the Korean Society for Precision Engineering
• /
• v.22 no.7 s.172
• /
• pp.71-78
• /
• 2005

The purpose of this study is to suggest a hyperfine maskless writing technique by using the nanoindentation and HF wet etching technique. Indents were made on the surface of Pyrex7740 glass by the hyperfine indentation process with a Berkovich diamond indenter, and they were etched in $50\;wr\%$ HF solution. After etching process, convex structure was obtained due to the deformation-induced hillock phenomena. In this study, effects of indentation process parameters (etching time, normal load, loading .ate, hold-time at the maximum load) on the morphologies of the indented surfaces after isotopic etching were investigated from an angle of deformation energies. Finally, sample characters were written to show the possibility of the application.

• Macromolecular Research
• /
• v.13 no.1
• /
• pp.30-38
• /
• 2005

Sulfur-cured gum natural rubber vulcanizates were devulcanized using two different concentrations of diallyl disulfide. The devulcanization process was performed at $110^{\circ}C$ min in an open two-roll cracker-cum-mixing mill. Natural rubber vulcanizates having various sulfur/accelerator ratios were used to study the cleavage of monosulfide, disulfide, and polysulfide bonds. The properties of devulcanized natural rubber increased upon increasing the disulfide concentration and the mechanical properties of the revulcanized natural rubber increased upon decreasing the sulfur content in the original rubber vulcanizates. The scorch time and the maximum state of cure both increased when the ground vulcanizates were treated with higher amounts of disulfide. TGA and DMA were conducted to study the effects of the devulcanization on the thermal stability and the $T_g$ behavior of the vulcanizates. SEM analysis was conducted to study how the failure mechanism was affected by the devulcanization process. It was possible to recover $70-80\%$ of the original gum rubber properties by using this process. From IR spectroscopic analysis, we observed that the oxidation of the main chains did not occur during high-temperature milling.