• Proceedings of the Korean Society of Precision Engineering Conference
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• 2004.10a
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• pp.442-446
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• 2004

Reducing the particle size of drug materials down to submicron is an important matter in pharmaceutical industry. Cryogenic milling technology is one of the mechanical milling processes, which is mostly utilized in refining grain size of metal and ceramics at extremely low temperature environment. This technique has not been readily studied in application to medical and biotechnology. This paper, therefore, describes the application of cryogenic milling process to reduce particle size of Ibuprofen. The shape and size of the Ibuprofen particle before and after the cryogenic ball milling process were analyzed. XRD analysis was performed to examine a change in crystallinity of Ibuprofen by the cryogenic ball milling process. The results showed that the size of Ibuprofen particles was reduced to 1/10 or less of its initial size. The results also showed that the degree of crystallinity of Ibuprofen was slightly reduced after cryogenic ball milling with nitrogen

• Journal of the Korean Society for Precision Engineering
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• v.27 no.7
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• pp.49-54
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• 2010

The cryogenic ball milling was performed on carbon nanotubes (CNTs) at an extremely low temperature to increase the dispersion of CNTs. The effects of milling speed and time on the deagglomeration and structural changes of CNTs were studied. FESEM was used to analyze the dispersion and the change of particle size before and after milling process. Transmission electron microscopic (TEM) analysis was also investigated the effect of cryogenic ball milling on the morphological characteristics of CNTs. The structural changes by the cryogenic ball milling process were further confirmed by x-ray diffraction (XRD) and Raman spectroscopic analysis. The results showed that the agglomeration of CNTs was significantly reduced and amorphous structure was observed at high milling speed. However, the milling time has no great effect on the dispersion property and structural change of CNTs compared with milling speed.

• Journal of the Korean Society for Precision Engineering
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• v.21 no.11
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• pp.195-199
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• 2004

For the present study, the cryogenic ball milling process was applied to make Ibuprofen microsized. The cryogenic ball milling was performed at low temperature of about -18$0^{\circ}C$ for 6 hours. The particle size distribution was determined before and after the cryogenic process. X-ray diffraction (XRD) measurement was made to determine the effect of cryogenic process on the crystallinity of Ibuprofen. The results showed that the size of Ibuproffn was reduced about 10 times by the cryogenic process. The degree of crystallinity of Ibuproffn was slightly reduced by the cryogenic process.

• Transactions of the Korean Society of Mechanical Engineers A
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• v.29 no.7 s.238
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• pp.1022-1027
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• 2005

In this study, ball milling process was applied to reduce the particle size of bio-material down to submicron size. The material used was Ibuprofen. The ball milling was performed at low temperature of about $-180^{\circ}C$. The effect of processing conditions (milling time, milling speed) on the particle size was determined. The results showed that the degree of crystallite of Ibuprofen was slightly reduced by the ball milling process. The results also showed that the size of Ibuprofen was significantly reduced by the ball milling process. The effect of milling time was significant within the milling time of six hours while it was small thereafter.

• Progress in Superconductivity and Cryogenics
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• v.19 no.2
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• pp.19-24
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• 2017

Cryogenic milling which is a combined process of low-temperature treatment and mechanical milling was applied to fabricate high critical current density $(J_c)MgB_2$ bulk superconductors. Liquid nitrogen was used as a coolant, and no solvent or lubricant was used. Spherical Mg ($6-12{\mu}m$, 99.9 % purity) and plate-like B powder (${\sim}1{\mu}m$, 97 % purity) were milled simultaneously for various time periods (0, 2, 4, 6 h) at a rotating speed of 500 rpm using $ZrO_2$ balls. The (Mg+2B) powders milled were pressed into pellets and heat-treated at $700^{\circ}C$ for 1 h in flowing argon. The use of cryomilled powders as raw materials promoted the formation reaction of superconducting $MgB_2$, reduced the grain size of $MgB_2$, and suppressed the formation of impurity MgO. The superconducting critical temperature ($T_c$) of $MgB_2$ was not influenced as the milling time (t) increased up to 6 h. Meanwhile, the critical current density ($J_c$) of $MgB_2$ increased significantly when t increased to 4 h. When t increased further to 6 h, however, $J_c$ decreased. The $J_c$ enhancement of $MgB_2$ by cryogenic milling is attributed to the formation of the fine grain $MgB_2$ and a suppression of the MgO formation.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.23 no.2
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• pp.108-113
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• 2013

Chalcopyrite material $CuInSe_2$ (CIS) is known to be a very prominent absorber layer for high efficiency thin film solar cells. Current interest in the photovoltaic industry is to identify and develop more suitable materials and processes for the fabrication of efficient and cost-effective solar cells. Various processes have been being tried for making a low cost CIS absorber layer, this study obtained the CIS nanoparticles using commercial powder of 6 mm pieces for low cost CIS absorber layer by high frequency ball milling and cryogenic milling. And the CIS absorber layer was prepared by paste coating using milled-CIS nanoparticles in glove box under inert atmosphere. The chalcopyrite $CuInSe_2$ thin films were successfully made after selenization at the substrate temperature of $550^{\circ}C$ in 30 min, CIS solar cell of Al/ZnO/CdS/CIS/Mo structure prepared under various deposition process such as evaporation, sputtering and chemical vapor deposition respectively. Finally, we achieved CIS nanoparticles solar cell of electric efficient 1.74 % of Voc 29 mV, Jsc 35 $mA/cm^2$ FF 17.2 %. The CIS nanoparticles-based absorber layers were characterized by using EDS, XRD and HRSEM.

• Proceedings of the Korean Society of Precision Engineering Conference
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• 2004.05a
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• pp.158-158
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• 2004

본 연구에서는 이부프로펜(Ibuprofen)분말을 마이크론(Micron) 크기의 입자로 만들기 위하여 극저온 볼 밀링 공정(Cryogenic Ball Milling Process)을 사용하였다. 극저온 볼 밀링 공정은 약 -18$0^{\circ}C$의 질소 분위기에서 6시간 동안 실행되어 졌다 이부프로펜 분말 형상의 변화는 SEM(Scanning Electronic Microscope)촬영을 통하여 관찰하였으며, 분말의 입자 크기와 분포는 입도 분석기(Particle Size Analysis)를 사용하여 극저온 볼 밀링 공정 전ㆍ후의 변화를 관찰하였다(중략)

• Journal of the Korean Society for Heat Treatment
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• v.26 no.6
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• pp.279-287
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• 2013

Oxide Dispersion Strengthened (ODS) Fe with $Al_2O_3$ dispersoid was successfully produced by reactive milling with a mixture of Fe, $Fe_3O_4$ (Magnetite), $Fe_2O_3$ (Hematite) and Al reactants at cryogenic temperature. The milled powders were consolidated by Vacuum Hot Press (HP) at 1323 K, and the consolidated materials were characterized by Transmission Electron Microscopy (TEM), Scanning Transmission Electron Microscopy (STEM), and Energy Dispersive Spectroscopy (EDS); the yield strength and the hardness of the consolidated materials were determined by compressive test and Vickers hardness test at room temperature. The grain size of the materials was estimated by X-ray Diffraction technique using the scherrer's formula. The TEM observations showed that the microstructure was comprised with a mixture of nanocrystalline Fe matrix and $Al_2O_3$ nano-dispersoids with a bimodal size distribution; the 0.2% off-set yield strength of the materials was as high as $758{\pm}29$ MPa and the Vickers hardness was $358{\pm}2$. The effect of the cryogenic milling and addition of extra Fe powder was discussed on the suppression of MSR (Mechanically induced Self-sustaining Reaction) for the desired microstructural evolution of ODS alloys.

• Journal of the Korean Society for Heat Treatment
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• v.25 no.3
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• pp.138-145
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• 2012

An ${\alpha}$-Ferrite (Fe) powder dispersed with 4 vol.% of $Al_2O_3$ was successfully produced by a simple miling at 210 K with a mixture of $Fe_2O_3$, Fe and Al ingredient powders, followed by 2 step high temperature consolidation: Hot Pressing (HP) at 1323 K and then Hot Isostatic Pressing at 1423 K. The microstructure of the consolidated material was characterized by standard metallographic techniques such as XRD (X-ray Diffraction), TEM and STEM-EDS. The results of STEM-EDS analysis showed that the HIPed materials comprised a mixture of pure Fe matrix with a grain size of ~20 nm and $Al_2O_3$ with a bimodal size distribution of extremely fine (~5 nm) and medium size dispersoids (~20 nm). The mechanical properties of the consolidated materials were characterized by compressive test and micro Vickers hardness test at room temperature. The results showed that the yield strength of the ODS (Oxide Dispersion Strengthened) Fe alloy are as much as $674{\pm}39$ MPa and the improvement of the yield strength is attributed to the presence of the fine $Al_2O_3$ dispersoid.

• Journal of Powder Materials
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• v.28 no.5
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• pp.389-395
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• 2021

Oxide dispersion-strengthened (ODS) steel has excellent high-temperature properties, corrosion resistance, and oxidation resistance, and is expected to be applicable in various fields. Recently, various studies on mechanical alloying (MA) have been conducted for the dispersion of oxide particles in ODS steel with a high number density. In this study, ODS steel is manufactured by introducing a complex milling process in which planetary ball milling, cryogenic ball milling, and drum ball milling are sequentially performed, and the microstructure and high-temperature mechanical properties of the ODS steel are investigated. The microstructure observation revealed that the structure is stretched in the extrusion direction, even after the heat treatment. In addition, transmission electron microscopy (TEM) analysis confirmed the presence of oxide particles in the range of 5 to 10 nm. As a result of the room-temperature and high-temperature compression tests, the yield strengths were measured as 1430, 1388, 418, and 163 MPa at 25, 500, 700, and 900℃, respectively. Based on these results, the correlation between the microstructure and mechanical properties of ODS steel manufactured using the composite milling process is also discussed.