• Korean Journal of Materials Research
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• v.15 no.3
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• pp.166-171
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• 2005

Fe-6Al-9Si(N) alloy powders were synthesized by hybrid process of chemical nitrification and mechanical milling. The nitriding treatment on Fe-6Al-9Si alloy powders formed $\gamma'-Fe_4N$ phase on the powders surface. The nitriding-treated powders were pulverized by horizontal high-energy ball milling machine. The longer ball milling time tended to reduce the size of alloy powders. In ball milling for 36h, extremely fine powders with about $7\~9wt\%$ nitrogen were obtained. Through X-ray diffraction analysis on the powders, it was found out that the longer milling time caused a disappearance of the crystallinity of $\alpha-Fe$ in the powders. TEM study confirmed that the powders is comprised of a few tens nano-meter sized crystals, including $\alpha-Fe$ phase with partially $\gamma'-Fe_4N$ phase. Hysteresis curves of the synthesized powders measured by VSM revealed lower saturation magnetization and higher coercivity, which seemed to be attributed to nitrogen-impregnation and severe residual stress developed during the high energy milling. Microstructure observation on the powder annealed at 873 K for 1 h showed 10 to 20 nm sized $\alpha-Fe$ crystal. Such a enhanced crystallinity significantly increased the magnetization and decreased the coercivity, which was attributed to not only the crystallinity but also residual stress relaxation.

• Transactions of the Korean hydrogen and new energy society
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• v.10 no.4
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• pp.225-232
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• 1999

The $Mg_2Ni$ hydrogen storage alloys which have much higher theoretical discharge capacity than $AB_5$ and $AB_2$ type alloys were synthesized by mechanical alloying with some additives and subjected to the electrochemical measurements. Two different processes were employed to the synthesis of $Mg_2Ni$ alloys with using the high energy ball mill SPEX 8000. One was only ball milling, 12 hrs, the Mg and Ni powders for 12 hrs with additives such as $AB_5$, Ni, Co and Cu powders. In the other process the Mg and Ni powders were ball milled for 1 hr first and then heat treated at $300{\sim}400^{\circ}C$ for 1 hr to get $Mg_2Ni$ alloy, and finally the $Mg_2Ni$ alloy powders were ball milled with the additives for 12 hrs. The alloy powders prepared were compacted at room temperature under $7.64tons/cm^2$ into disk type electrodes for the electrochemical measurements. The experimntal results showed that the electrodes prepared with the heat treated alloy powders had a higher discharge capacities than those without heat treatment. The addition of Ni caused an increase of the discharge capacity and the addition of Co improved the cycling characteristics. The electrode prepared by ball milling of $Mg_2Ni$ and 10wt% Ni powders has showed the highest discharge capacity, 546mAh/g.alloy, which was 55% of the theoretical capacity.

• Korean Journal of Materials Research
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• v.14 no.5
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• pp.305-309
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• 2004

Mechanical alloying (MA) of Ti-25.0～37.5at%Si powders was carried out in a high-energy ball mill, and in situ thermal analysis was also made during MA. In order to classify the synthesis behavior of the powders with respect to at%Si, the synthesis behavior during MA was investigated by in situ thermal analysis and X-ray diffraction (XRD). In situ thermal analysis curves and XRD patterns of Ti-25.0～26.1at%Si powders showed that there were no peaks during MA, indicating $Ti_{5}$ $Si_3$ was synthesised by a slow reaction of solid state diffusion. Those of Ti-27.1～37.5at%Si powders, however, showed that there were exothermic peaks during MA, indicating $_Ti{5}$ $Si_3$ and$ Ti_3$Si phase formation by a rapid exothermic reaction of self-propagating high-temperature synthesis (SHS). For Ti-27.1～37.5at%Si powders, the critical milling times for SHS decreased from 38.1 to 18.5 min and the temperature rise, ΔT (= peak temperature - onset temperature) increased form $19.5^{\circ}C$ to $26.7^{\circ}C$ as at%Si increased. The critical composition of Si for SHS reaction was found to be 27.1at% and the critical value of the negative heat of formation of Ti-27.1at%Si to be -1.32 kJ/g.

• Korean Journal of Materials Research
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• v.14 no.5
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• pp.310-314
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• 2004

Mechanical alloying (MA) of Ti-50.0～66.7at%Si powders was carried out in a high-energy ball mill, and in situ thermal analysis was also made during MA. In order to classify the synthesis behavior of the powders with respect to at%Si, the synthesis behavior during MA was investigated by in situ thermal analysis and X-ray diffraction (XRD). In situ thermal analysis curves and XRD patterns of Ti-50.0～59.6at%Si powders showed that there were exothermic peaks during MA, indicating TiSi, $TiS_2$, and $Ti_{5}$ $Si_4$ phase formation by a rapid exothermic reaction of self-propagating high-temperature synthesis (SHS). Those of Ti-59.8～66.7 at%Si powders, however, showed that there were no peaks during MA, indicating any Ti silicide was not synthesised until MA 240 min. For Ti-50.0～59.6at%Si powders, the critical milling times for SHS increased from 34.5 min to 89.5 min and the temperature rise, $\Delta$T (=peak temperature-onset temperature) decreased form $26.2^{\circ}C$ to $17.1^{\circ}C$ as at%Si increased. The critical composition of Si for SHS reaction was found to be 59.6at% and the critical value of the negative heat of formation of Ti-59.6at%Si to be -1.48 kJ/g.

• Journal of Powder Materials
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• v.22 no.5
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• pp.356-361
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• 2015

Fe-30 wt% TiC composite powders are fabricated by in situ reaction synthesis after planetary ball milling of (Fe, $TiH_2$, Carbon) powder mixture. Two sintering methods of a pressureless sintering and a spark-plasma sintering are tested to densify the Fe-30 wt% TiC composite powder compacts. Pressureless sintering is performed at 1100, 1200 and $1300^{\circ}C$ for 1-3 hours in a tube furnace under flowing argon gas atmosphere. Spark-plasma sintering is carried out under the following condition: sintering temperature of $1050^{\circ}C$, soaking time of 10 min, sintering pressure of 50 MPa, heating rate of $50^{\circ}C/min$, and in a vacuum of 0.1 Pa. The curves of shrinkage and its derivative (shrinkage rate) are obtained from the data stored automatically during sintering process. The densification behaviors are investigated from the observation of fracture surface and cross-section of the sintered compacts. The pressureless-sintered powder compacts are not densified even after sintering at $1300^{\circ}C$ for 3 h, which shows a relative denstiy of 66.9%. Spark-plasma sintering at $1050^{\circ}C$ for 10 min exhibits nearly full densification of 99.6% relative density under the sintering pressure of 50 MPa.

• Korean Journal of Materials Research
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• v.12 no.8
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• pp.600-607
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• 2002

The Ni-Zn synthetic ferrite were acquired from thermally decomposing the metal nitrates Fe(NO$_3$)$_3$.$9H_2$O, Zn($NO_3$)$_2$.$6H_2$O, Ni($NO_3$)$_2$. $6H_2$O, and Cu($NO_3$)$_2$. $3H_2$O at $150^{\circ}C$ for 24 hours and was calcined at $500^{\circ}C$. Each of those was pulverized for 3, 6, 9, and 12 hours in a steel ball mill and was sintered between $700^{\circ}C$ and $1,000^{\circ}C$ for 1 hour, and then their microstructures and electromagnetic properties were examined. We could make the initial specimens chemically bonded in liquid at the temperature as low as $150^{\circ}C$, by using the melting points less than $200^{\circ}C$ of the metal nitrates instead of the mechanical ball milling, then narrowed a distance between the particles into a molecular level, and thus lowed sintering temperature by at least $200^{\circ}C$ to$ 300^{\circ}C$. Their initial permeability was 50 to 400 and their saturation magnetic induction density and coercive force 2,400 G and 0.3 Oe to 0.5 Oe each, which were similar to those of Ni- Zn ferrite synthesized in the conventional process. In the graph of initial permeability vs frequencies, we could observe a $180^{\circ}C$rotation of the magnetic domain, which appears in a broad band of microwave near the resonance frequency.

• Journal of Powder Materials
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• v.20 no.2
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• pp.100-106
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• 2013

Ultra-fine zirconium carbide (ZrC) powder with nano-sized primary particles was synthesized by the carbothermal reduction method by using nano-sized $ZrO_2$ and nano-sized graphite powders mixture. The synthesized ZrC powder was well dispersed after simple milling process. After heat-treatment at $1500^{\circ}C$ for 2 h under vacuum, ultra-fine ZrC powder agglomerates (average size, $4.2{\mu}m$) were facilely obtained with rounded particle shape and particle size of ~200 nm. Ultra-fine ZrC powder with an average particle size of 316 nm was obtained after ball milling process in a planetary mill for 30 minutes from the agglomerated ZrC powder.

• Journal of the Korean Ceramic Society
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• v.31 no.8
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• pp.893-901
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• 1994

In this study, AlN powder of fine particle size and of high purity was synthesized by the carbothermal reduction-nitridation of monodisperse, spherical Al(OH)3 which had been prepared by sol-gel method using Al(O-sec-C4H9)3 as the starting material. Depending on the mixing order and kinds of reducing agents, the optimum condition for the preparation of AlN was determined as follows. AlN single-phase was produced by the carbothermal reduction-nitridation of (1) Benzene-washed Al(OH)3 and the reducing agent, carbon, which was mixed in a ball mill: for 5 hours at 140$0^{\circ}C$ under NH3 atmosphere; (2) The mixture prepared by hydrolysis of alkoxide solution into which carbon had been dispersed beforehand: for 5 hours at 135$0^{\circ}C$ ; (3) Al(OH)3 Poly(furfuryl alcohol) composite powder: for 2.5 hours at 135$0^{\circ}C$; (4) The mixture of Al(OH)3 and polyacrylonitrile: for 5 hours at 140$0^{\circ}C$. Addition of CaF2 increased the nitridation rate when carbon or polyacrylonitrile was used as the reducing agent; but it had no effect on the nitridation rate when furfuryl alcohol was used as the reducing agent.

• Korean Journal of Materials Research
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• v.11 no.9
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• pp.745-750
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• 2001

Ni-33.3at%Si elemental powder mixtures were mechanically alloyed by a high-energy ball mill, followed by CIP (cold isostatic pressing) and HIP (hot isostatic pressing) for different processing conditions. Only elemental phases (Ni and Si) were observed for the 15 min mechanically alloyed (MA 15 min) powder. but $Ni_2$Si and elemental phases were observed to coexist for the 30 min mechanically alloyed (MA 30 min) powder. Elemental Ni and $Ni_2$Si phases were observed for the HIPed compact of MA 15 min powder at 100 and 150 MPa for 2 hr at $800^{\circ}C$. Only the $Ni_2$Si phase was, however, observed for the HIPed compacts of MA 30 min powder. For the HIPed compacts, the highest sintered density was obtained to be 99.5% of theoretical density by a HIP step at $1100^{\circ}C$ at 150MPa for 2hr. The hardness values of the HIPed $Ni_2$Si compacts at $1100^{\circ}C$ at 100/150 MPa for 2 hr were higher than HRC 66. The densification and mechanical property of HIPed $Ni_2$Si compacts were found to depend on more HIP temperature than HIP pressure.

• Korean Journal of Crystallography
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• v.13 no.1
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• pp.31-35
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• 2002

The possibility of producing the pigments from potash feldspar was studied by adopting the mechanical alloying technique under various gas environments. The experiments were carried out by varying grinding time with the addition of copper metal and titanium oxide in N₂, O₂, He, CO₂, H₂and air atmospheres. The mixture of the potash feldspar concentrate and copper and titanium dioxide are finely ground by a planetary ball mill, and then the composite powders were calcined at 1200℃ for 20 minutes. As a result, the calcined feldspar with 1 wt% of Cu has shown various colors like green in air, black in O₂, dark green in CO₂, brown in H₂, purple in He, and pale green in N₂ atmospheres, respectively.