• Korean Journal of Materials Research
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• v.33 no.6
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• pp.242-250
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• 2023

Titanium, which has excellent strength and toughness characteristics, is increasingly used in the aerospace field. Among the titanium alloys used for body parts, more than 80 % are Ti-6Al-4V alloys with a tensile strength of 931 MPa. The spark plasma sintering (SPS) method is used for solidification molding of powder manufactured by the mechanical milling (MM) method, by sintering at low temperature for a short time. This sintering method avoids coarsening of the fine crystal grains or dispersed particles of the MM powder. To improve the mechanical properties of pure titanium without adding alloying elements, stearic acid was added to pure titanium powder as a process control agent (PCA), and MM treatment was performed. The properties of the MM powder and SPS material produced by solidifying the powder were investigated by hardness measurement, X-ray diffraction, density measurement and structure observation. The processing deformation of the pure titanium powder depends on the amount of stearic acid added and the MM treatment time. TiN was also generated in powder treated by MM 8 h with 0.50 g of added stearic acid, and the hardness of the powder was higher than that of Ti-6Al-4V alloy when treated with MM for 8 h. When the MM-treated powder was solidified in the SPS equipment, TiC was formed by the solid phase reaction. The SPS material prepared as a powder treated with MM 8 h by adding 0.50 g of stearic acid also formed TiN and exhibited the highest hardness of Hv1253.

• Journal of Powder Materials
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• v.31 no.2
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• pp.132-136
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• 2024

This study investigated the effects of revolution speed and ball size in planetary milling on the microstructure and dehydrogenation behavior of TiH₂ powder. The particle size analysis showed that the large particles present in the raw powder were effectively refined as the revolution speed increased, and when milled at 500 rpm, the median particle size was 1.47 ㎛. Milling with a mixture of balls of two or three sizes was more effective in refining the raw powder than milling with balls of a single size. A mixture of 3 mm and 5 mm diameter balls was the optimal condition for particle refinement, and the measured median particle size was 0.71 ㎛. The dependence of particle size on revolution speed and ball size was explained by changes in input energy and the number of contact points of the balls. In the milled powder, the endothermic peak measured using differential thermal analysis was observed at a relatively low temperature. This finding was interpreted as the activation of a dehydrogenation reaction, mainly due to the increase in the specific surface area and the concentration of lattice defects.

• Journal of Powder Materials
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• v.31 no.4
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• pp.324-328
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• 2024

This study analyzed the influence of ball size and process control agents on the refinement and dehydrogenation behavior of TiH₂ powder. Powders milled using ZrO₂ balls with diameters of 0.1 mm, 0.3 mm, and 0.3+0.5+1 mm exhibited a bimodal particle size distribution, of which the first mode had the smallest size of 0.23 ㎛ for the 0.3 mm balls. Using ethanol and/or stearic acid as process control agents was effective in particle refinement. Thermogravimetric analysis showed that dehydrogenation of the milled powder started at a relatively low temperature compared to the raw powder, which is interpreted to have resulted from a decrease in particle size and an increase in defects. The dehydrogenation kinetics of the TiH₂ powder were evaluated by the magnitude of peak shift with heating rates using thermogravimetric analysis. The activation energy of the dehydrogenation reaction, calculated from the slope of the Kissinger plot, was measured to be 228.6 kJ/mol for the raw powder and 194.5 kJ/mol for the milled powder. TEM analysis revealed that both the milled and dehydrogenated powders showed an angular shape with a size of about 200 nm.

• Proceedings of the Materials Research Society of Korea Conference
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• 2010.05a
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• pp.26.2-26.2
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• 2010

최근에는 차세대 조명용 후보광원인 고출력 백색 LED를 개발하기 위한 경쟁이 치열하며, 이를 위해 업체가 고심하고 있는 가장 큰 문제 중의 하나가 칩에서 발생하는 열을 어떻게 관리하는가 하는 방열의 문제이다. 따라서, LED의 가장 큰 특징인 장수명을 손해보지 않기 위해서는 칩에서 발생되고 있는 열을 외부에 확산시키기 위한 기술 개발이 필수적이다. 다양한 방열소재 중 W-Cu 복합재는 W의 낮은 열팽창계수와 Cu의 높은 열전도도로 인해 방열소재로써 유망한 소재로 주목받고 있으나, 우수한 열적 특성을 발현하기 위해서는 고치밀화를 갖는 W-Cu 복합재 제조가 우선적으로 필요하다. W-Cu 복합체는 일반적으로 액상소결법을 통해 균일한 미세조직을 얻을 수 있으나, 열팽창계수를 낮추기 위해 Cu 함량이 적어지게 되면 치밀화가 어려우며 이를 해결하기 위해 나노입자를 갖는 분말을 이용하고자 하는 연구가 많이 진행되고 있다. 본 연구에서는 W과 Cu 산화물을 이용하는 것이 구성성분끼리의 편석이 발생하지 않으며, 소결성도 우수하여 양산화에 가장 접근한 방법으로 알려져 있다. 그러나, 지금까지의 얻어진 W-Cu 복합체의 경우, 분말상태에서의 얻어진 나노입자가 승온시에 마이크로 크기로 과도한 입자성장이 일어나기 때문에 소결 후에도 나노크기를 유지하기 어려울 뿐만 아니라, 구성상끼리의 응집체가 형성된다. 본 연구에서는 액상소결후에 W 입자가 Cu 기지내에 균일하게 분산되는 동시에 나노크기의 입자를 가지는 고분산 W-Cu 소결체를 얻고자 하였다. 이를 위해 금속산화물 분말의 분쇄를 위해 효과적인 방법으로 알려진 습식상태에서의 고에너지 볼밀링을 통하여 혼합된 텅스텐과 구리 산화물 분말의 수소환원공정을 통해 얻어진 100nm 이하의 입자를 가지는 W-20wt%Cu 나노복합분말을 출발분말로 사용하였다. W-20wt%Cu 나노복합분말의 성형체를 $1050^{\circ}C-1250^{\circ}C$의 온도범위에서 소결거동을 조사하였다. 그 결과, $1100^{\circ}C$ 온도에서 이론밀도에 가까운 소결밀도를 나타내었으며, 이는 기존에 비해 $100^{\circ}C$ 정도 치밀화 온도를 낮추는 결과이다. 소결체의 미세구조 관찰결과, 소결 후 약 200nm의 텅스텐 입자가 Cu내에 균일하게 분산되어 있었다. 제조된 W-Cu 시편에 대해서는 LED 응용성을 조사하기 위해 열전도도와 열팽창계수 등을 평가하였다.

• Journal of the Korean Magnetics Society
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• v.22 no.3
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• pp.85-90
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• 2012

Oxidation of the $Nd_2Fe_{14}B$ compound crystal and its effect on the coercivity of the fine $Nd_2Fe_{14}B$ crystal particles were investigated. Oxidation kinetics of the $Nd_2Fe_{14}B$ compound crystal was investigated using an excessively grown $Nd_2Fe_{14}B$ grains in the $Nd_{15}Fe_{77}B_8$ alloy ingot. Oxidation of the $Nd_2Fe_{14}B$ compound crystal occurred by dissociation of the phase into multi-phase mixture of ${\alpha}$-Fe, $Fe_3B$, and Nd oxides. Oxidation rate of the $Nd_2Fe_{14}B$ compound crystal showed no dependence on the crystallographic direction. The oxidation reaction was modeled according to simple linear relationship. Activation energy for the oxidation of $Nd_2Fe_{14}B$ compound crystal was calculated to be approximately 26.8 kJ/mol. Fine $Nd_2Fe_{14}B$ crystal particles in near single domain size was prepared by ball milling of the HDDR-treated $Nd_{15}Fe_{77}B_8$ alloy, and these particles were used for investigating the effect of oxidation on the coercvity. The near single domain size $Nd_2Fe_{14}B$ crystal particles (${\fallingdotseq}0.3\;{\mu}m$) had high coercivity over 9 kOe. However, the coercivity was radically reduced as the temperature increased in air (<2 kOe at $200^{\circ}C$). This radical coercivity reduction was attributed to the soft magnetic phases, ${\alpha}$-Fe and $Fe_3B$, which were formed on the surface of the fine particles due to the oxidation.

• Journal of Nuclear Fuel Cycle and Waste Technology(JNFCWT)
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• v.15 no.4
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• pp.343-353
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• 2017

Processing and equipment were tailored for engineering scale fabrication of $UO_2$ porous pellets, a feed material for the electrolytic reduction process in the PRIDE (PyRoprocessing Integrated DEmonstration) facility at KAERI (Korea Atomic Energy Research Institute). The starting materials, $UO_2$ powder and pre-milled surrogate oxide powders, were proportioned to simulate the chemical composition of spent fuel (so-called Simfuel). The Simfuel powders were homogenized by mixing, compacted into a pellet shape, and finally heat treated using a tumbling mixer, rotary press, and sintering furnace. After sintering at $1450^{\circ}C$ for 24 h in $4%\;H_2-Ar$, the average bulk density of the $UO_2$ Simfuel pellets was $6.89g{\cdot}cm^{-3}$, which meets the standard of the following electrolytic reduction process. In addition, the results of a microstructural analysis demonstrated that the sintered Simfuel $UO_2$ porous pellets accurately simulate the properties of spent fuel in terms of the formation of second phases. These results provide essential information for the massive fabrication of $UO_2$ porous pellets for engineering scale pyroprocessing research.

• Korean Chemical Engineering Research
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• v.43 no.4
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• pp.517-524
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• 2005

Barium titanate ($BaTiO_3$) particles were prepared by spray pyrolysis from spray solution containing organic additives. The effects of the type and amount of organic precursors on the crystal structure and morphology of the $BaTiO_3$ particles were investigated. It was found that the morphology of $BaTiO_3$ particles before and after calcination depended on the type of organic additives such as citric acid, ethylene glycol and polyethylene glycol. Among these organic additives, citric acid was the most effective to prepare $BaTiO_3$ particles with nano-structured morphology consisting with uniform size nanometer particles after calcination. It was also found that the phase transformability of the metastable cubic phase to the tetragonal one during calcination could be improved by increasing the content of citric acid in the spray solution. As a result, $BaTiO_3$ particles prepared from spray solution containing high concentration of citric acid had good tetragonality, uniform and fine size, and high BET surface area after calcination. $BaTiO_3$ particles prepared by spray pyrolysis had nanometer size and uniform morphology after simple ball milling process.