• 산업기술연구
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• 제19권
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• pp.107-113
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• 1999

The microstructural evolution during mechanical alloying of elemental Fe and Si powders, average composition $Fe_{30}Si_{70}$ and $Fe_{50}Si_{50}$, has been investigated by X-ray diffraction (XRD), Scanning electron microscopy (SEM) and Differential scanning calorimetry (DSC). Mechanical alloying was performed by using a SPEX 8000 Mixer/Mill under argon atmosphere with/without hexane as a process control agent (PCA). In the presence of PCA, the milling process was dominated by fracture resulting in the decrease in particle size to about $1{\mu}m$. The structural development with milling time depended on the average composition of starting powders. The mixture of $Fe_{50}Si_{50}$ and $Fe_{30}Si_{70}$ resulted in the formation of FeSi(${\varepsilon}$ - phase) and $FeSi_2$(${\beta}$ - phase), respectively. In the case of $Fe_{33.3}Si_{66.7}$, a mixture and $FeSi_2({\beta})$ was formed. These results were discussed by considering the thermodynamics and kinetics concerning the milling process.

• 한국분말야금학회:학술대회논문집
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• 한국분말야금학회 2006년도 Extended Abstracts of 2006 POWDER METALLURGY World Congress Part2
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• pp.829-830
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• 2006

Recent research at Harbin Institute of Technology on the synthesis of nanocrystalline and untrafine grained materials by mechanical alloying/milling is reviewed. Examples of the materials include aluminum alloy, copper alloy, magnesium-based hydrogen storage material, and $Nd_2Fe_{14}B/{\alpha}-Fe$ magnetic nanocomposite. Details of the processes of mechanical alloying and consolidation of the mechanically alloyed nanocrystalline powder materials are presented. The microstructure characteristics and properties of the synthesized materials are addressed.

• 한국분말재료학회지
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• 제17권1호
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• pp.36-43
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• 2010

In present work, amorphous TiCuNi powders were fabricated by mechanical alloying process. Amorphization and crystallization behaviors of the TiCuNi powders during high-energy ball milling and subsequent microstructure changes were studied by X-ray diffraction and transmission electron microscope. TEM samples were prepared by the focused ion beam technique. The morphology of powders prepared with different milling times was observed by field-emission scanning electron microscope and optical microscope. The powders developed a fine, layered, homogeneous structure with milling times. The crystallization behavior showed that glass transition, $T_g$, onset crystallization, $T_x$, and super cooled liquid range ${\Delta}T=T_x-T_g$ were 628, 755 and 127K, respectively. The as-prepared amorphous TiCuNi powders were consolidated by spark plasma sintering process. Full densified TiCuNi samples were successfully produced by the spark plasma sintering process. Crystallization of the MA powders happened during sintering at 733K.

• 한국분말재료학회지
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• 제30권6호
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• pp.478-483
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• 2023

High-entropy alloys (HEAs) are characterized by having five or more main elements and forming simple solids without forming intermetallic compounds, owing to the high entropy effect. HEAs with these characteristics are being researched as structural materials for extreme environments. Conventional refractory alloys have excellent high-temperature strength and stability; however, problems occur when they are used extensively in a high-temperature environment, leading to reduced fatigue properties due to oxidation or a limited service life. In contrast, refractory entropy alloys, which provide refractory properties to entropy alloys, can address these issues and improve the high-temperature stability of the alloy through phase control when designed based on existing refractory alloy elements. Refractory high-entropy alloys require sufficient milling time while in the process of mechanical alloying because of the brittleness of the added elements. Consequently, the high-energy milling process must be optimized because of the possibility of contamination of the alloyed powder during prolonged milling. In this study, we investigated the high-temperature oxidation behavior of refractory high-entropy alloys while optimizing the milling time.

• 대한전기학회:학술대회논문집
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• 대한전기학회 1996년도 추계학술대회 논문집 학회본부
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• pp.464-467
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• 1996

The microstructural evolution during mechanical alloying of Nb and Sn powders, of average composition Nb3Sn, has been investigated by X-ray diffraction(XRD) and scanning electron microscopy(SEM). Observations by SEM showed a progressive change of milling time. From the XRD studies, the structural development with milling time depends on the ball size for a given powder/ball ratio. Using a larger ball of 9.5mm diameter, the elemental powders initially alloy mechanically to form an A15 structure phase, and then amorphised with continued milling. However, in case of milling with a smaller ball of 3.968mm diameter, an amorphous phase is first formed. These results can be understood by considering the dependence of the milling energy on the ball size. The homogeneous stoichiometric $Nb_3Sn$ phase could be easily obtained by heat treatment of a supersaturated solid solution produced by MA. Heat treatment of an amorphous phase formed by MA resulted in the mixture of the $Nb_3Sn$ and $Nb_6Sn_5$ phases.

• 한국분말재료학회지
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• 제6권2호
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• pp.145-151
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• 1999

Nickel silicides ($Ni_5$Si$_2$, Ni$_2$Si and NiSi) have been synthesized by mechanical alloying (MA) of Ni-27.9at.9at%Si, Ni-33.3at% and Ni-50.0at% powder mixtures, respectively. From in situ thermal analysis, eash citical milling period for the formation of the three phases was observed to be 40.2, 34.9 and 57.5 min, at which there was a rapid increase in temperature. This indicates that rapid, self-propagating high-temperature synthesis (SHS) reactions were observed to produce the three phases during room-temperature high-energy ball milling of elemental powders. Each Ni silicide, Ni and Si, however, coexisted for an extended milling time even after the critical milling period. The powders mechanically alloyed after the critical period showed the rapid increase in microhardness. The Hv values were found to be higher than 1000kgf/mm$^2$. The formation of nickel silicides by mechanical alloying and the relevant reaction rates appeared to be influenced by the critical milling period and the heat of formation of the products involved ($Ni_5$Si$_2$$\rightarrow$-43.1kJ/mol.at., Ni$_2$Si$\rightarrow$-47.6kJ/mol.at., NiSi$\rightarrow$-42.4kJ/mol.at).

• Nuclear Engineering and Technology
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• 제46권6호
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• pp.857-862
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• 2014

Mechanical alloying under various gas atmospheres such as Ar, an Ar-$H_2$ mixture, and He gases were carried out, and its effects on the powder properties, microstructure and mechanical properties of ODS ferritic steels were investigated. Hot isostatic pressing and hot rolling processes were employed to consolidate the ODS steel plates. While the mechanical alloyed powder in He had a high oxygen concentration, a milling in Ar showed fine particle diameters with comparably low oxygen concentration. The microstructural observation revealed that low oxygen concentration contributed to the formation of fine grains and homogeneous oxide particle distribution by the Y-Ti-O complex oxides. A milling in Ar was sufficient to lower the oxygen concentration, and this led a high tensile strength and fracture elongation at a high temperature. It is concluded that the mechanical alloying atmosphere affects oxygen concentration as well as powder particle properties. This leads to a homogeneous grain and oxide particle distribution with excellent creep strength at high temperature.

• Nuclear Engineering and Technology
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• 제53권8호
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• pp.2582-2590
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• 2021

The high-energy milling is one of the most extended techniques to produce Oxide dispersion strengthened (ODS) powder steels for nuclear applications. The consequences of the high energy mill process on the final powders can be measured by means of deformation level, size, morphology and alloying degree. In this work, an ODS ferritic steel, Fe-14Cr-5Al-3W-0.4Ti-0.25Y₂O₃-0.6Zr, was fabricated using two different mechanical alloying (MA) conditions (M_std and M_act) and subsequently consolidated by Spark Plasma Sintering (SPS). Milling conditions were set to evidence the effectivity of milling by changing the revolutions per minute (rpm) and dwell milling time. Differences on the particle size distribution as well as on the stored plastic deformation were observed, determining the consolidation ability of the material and the achieved microstructure. Since recrystallization depends on the plastic deformation degree, the composition of each particle and the promoted oxide dispersion, a dual grain size distribution was attained after SPS consolidation. M_act showed the highest areas of ultrafine regions when the material is consolidated at 1100 ℃. Microhardness and small punch tests were used to evaluate the material under room temperature and up to 500 ℃. The produced materials have attained remarkable mechanical properties under high temperature conditions.

• 한국분말재료학회지
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• 제6권2호
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• pp.178-185
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• 1999

MoSi$_2$-TiC composite powders were fabricated by in-situ reaction through mechanical alloying. Also the monolithic MoSi$_2$ as well as TiC were synthesiced by mechanical alloying for comparison. An abrupt increase of vial surface temperature was detected due to a sudden reaction between elemental powders during milling. The reaction time for synthesis of composite powders decreased with increasing the content of (Ti+C) powder. It was found that a significant decrease of Ti grain size was observed with increasing the milling time. And the synthesis reaction of MoSi$_2$-TiC composite powders were largely dependent on the reaction between Ti and C powders.

• 한국분말재료학회지
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• 제6권1호
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• pp.27-35
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• 1999

A study was made on the fabrication of nanostructured Fe-Co powders by mechanical alloying and their magnetic properties. Microstrural development during the process of MA was inverstigated by means of X-ray diffraction, differential thermal analyzer, scanning electron microscopy and transmission electron microscopy. The magnetic properties of NS Fe-Co powders were evaluated through the measurements of the saturation magnetization $(M_s)$ as well as the coercivity $(H_c)$. The average grain size calculated from line braodening in XRD peak was about 10nm or less and confirmed by TEM. In this experiment, two different milling methods (cycle opertion and conventional milling) were used. Cycle operation had an advantage over the conventional milling method in that more refined powders can be obtained. Solid state alloying of the components was confirmed from both the change of the saturation magnetization and the change of lattice parameter with Co contentration. Maxium $M_s$ was obtained at the composition of 30at.%Co. Relatively high coercivities of 10~150e were obtained for the compositions investigated, and this seems to be due to the high amount of internal strain introduced during milling.