• Korean Journal of Materials Research
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• v.16 no.12
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• pp.771-776
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• 2006

In this study, we report a method to synthesize the aluminum nitride (AlN) powders from aluminum oxyhydroxide (AlOOH). AlOOH powders were prepared from the aluminum hydroxide ($Al(OH)_3$) by heattreatment at the reaction temperature of $350^{\circ}C$. Simple heat treatment of AlOOH in the flow of $NH_3$ gas leads to the formation of hexagonal AlN powders through intermediate conversion of ${\delta}-,\;{\gamma}-$ and ${\alpha}-Al_2O_3$. The FTIR transmission spectra show a broad peak related to Al-N bonds centered around 690 $cm^{-1}$ confirming the presence of AlN. The major peaks in Raman spectra were observed in 250 $cm^{-1}$ and 659 $cm^{-1}$. From the results, synthesized powders from the AlOOH powders were confirmed AlN powders.

• Journal of the Korean Ceramic Society
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• v.22 no.6
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• pp.80-86
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• 1985

Aluminum nitride (AlN) was synthesized from aluminum (Al) powders as a starting material in the tempe-rature range of 450~1, 15$0^{\circ}C$ in the presence of 90% $N_2$-10%$H_2$ gases. The thermogravimentric analysis showed that the nitridation of Al powders started at about 43$0^{\circ}C$ and escalated greatly from 53$0^{\circ}C$. The scanning electron microcopic observation revealed that AlN crystals were different in shape with varying temperature of nitridation. The crystals of AlN which were formed in the lower temperature than the melting point of Al were spherical while those of AlN in the higher temperature were fibrous. The yield of AlN was determined quantitatively by both XRD method and weight gain between before and after the nitridation of Al compacts. It was considered that the former was available for the specimen which was made in the high nitriding temperature. But the latter was unavilable for the same one probably because of the volatile loss of Al in the higher temperature.

• Proceedings of the Korean Powder Metallurgy Institute Conference
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• 2006.09b
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• pp.1294-1295
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• 2006

Various reactions and the in-situ formation of new phases can occur during the mechanical alloying process. In the present study, Al powders were strengthened by AlN, using the in-situ processing technique during mechanical alloying. Differential thermal analysis and X-ray diffraction studies were carried out in order to examine the formation behavior of AlN. It was found that the precursors of AlN were formed in the Al powders and transformed to AlN at temperatures above $600^{\circ}C$. The hot extrusion process was utilized to consolidate the composite powders. The microstructure of the extrusions was examined by SEM and TEM. In order to investigate the mechanical properties of the extrusions, compression tests and hardness measurements were carried out. It was found that the mechanical properties and the thermal stability of the Al/AlN composites were significantly greater than those of conventional Al matrix composites.

• Journal of Powder Materials
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• v.12 no.3
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• pp.214-219
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• 2005

In order to investigate the formation of AlN, mechanical alloying was carried out in $N_2$ and $NH_3$ atmosphere. Differential thermal analysis (DTA), x-ray diffraction (XRD) and chemical analysis were carried out to examine the formation behavior of aluminum nitrides. No diffraction pattern of AlN was observed in XRD analysis of the as-milled powders in $NH_3\;or\;N_2$ atmosphere. However, DTA and chemical analysis indicated that the precursors for AlN were formed in the Al powders milled in $NH_3$ atmosphere. The AlN precursors transformed to AlN after heat treatment at and above $600^{\circ}C$. It was considered that the reaction between Al and $NH_3$ was possible by the formation of fresh Al surface during mechanical alloying of Al powders.

• Journal of the Korean Ceramic Society
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• v.40 no.8
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• pp.720-724
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• 2003

Aluminum nitride (AlN) powders were synthesized by using a mixture of an aluminum nitrate or sulfate salt and carbon (mole ratio of $Al^{3+}$ to carbon=L : 30). The AlN was obtained by calcining the mixture under a flow of nitrogen in the temperature range 1100-1$600^{\circ}C$ and then burning out the residual carbon. The process of conversion of the salt to AlN was monitored by XRD and $^{27}$ Al magic-angle spinning (MAS) NMR spectroscopy. The salt decomposed to ${\gamma}$-alumina and then converted to AlN without phase transition from ${\gamma}$-to-$\alpha$-alumina. $^{27}$ Al MAS NMR spectroscopy shows that the formation of AlN commenced at 110$0^{\circ}C$. AlN powders obtained from the sulfate salt were superior to those from the nitrate salt in terms of homogeneity and crystallinity. A very small amount of AlN whiskers was obtained by calcining a mixture of an aluminum sulfate salt and carbon at 115$0^{\circ}C$ for 40 h, and the growth of the whiskers is well explained by the particle-to-particle self-assembly mechanism.

• Journal of the Korean Ceramic Society
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• v.24 no.1
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• pp.23-32
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• 1987

Synthesis of high purity ultrafine Si3N4 and ${\beta}$-Sialon powders was investigated via the simultaneous reduction and nitriding of amorphous SiO2, SiO2-Al2O3 system prepaerd by hydrolysis of alkoxides, using carbonablack as a reducing agent. In Si(OC2H5)4-C2H5 OH-H2 O-NH4OH system, hydrolysis rate increased with increasing reaction temperature and pH. Pure ${\alpha}$-Si3N4 was formed at 1350$^{\circ}C$ for 5 hrs in N2 atmosphere. In Si(OC2H5)4-Al(OC3H7)3-C6H6-H2 O-NH4OH system, weight loss increased as Si/Al ratio decreased. Single phase ${\beta}$-Sialon consisted of Si/Al=2 was formed at 1350$^{\circ}C$ in N2 and minor phases of ${\alpha}$-Si3N4, AIN, and X-phase were existed besides theSialon phase at other Si/Al ratios. The Si3N4 and Sialon powders synthesized from alkoxides consisted of uniform find particles of 0.05-0.2$\mu\textrm{m}$ in diameter, respectively.

• Journal of the Korean Magnetics Society
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• v.4 no.4
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• pp.347-354
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• 1994

The structural change and magnetic properties of mechanically milled Fe-N and Mn-Al alloy powders have been investigated by XRD, TEM, VSM, $M\"{o}ssbauer$ spectroscopy and inelastic neutron scattering measurements. During milling of ${\gamma}'-Fe_{4}N$ powders, and fcc ${\gamma}'-Fe_{4}N$ phase is transformed to a bct ${\alpha}'-Fe(N)$ phase by stress-induced martensitic transformation, being accompanied by an initial increase in saturation magnetization. During annealing the bct ${\alpha}'-Fe(N)$ nanocrystalline phase which is obtained by mechanical grinding for a long time, an ${\alpha}'-Fe_{16}N_{2}$ phase partially appears as an intermediate phase at 673~773 K, causing an increase in saturation magnetization. During milling of Mn-45, 70 and 85 at.% Al mixed powders, Al atoms are partially solubilized into an ${\alpha}-Mn$ phase. The Al supersaturated ${\alpha}-Mn-type$ phases change from paramagnetic to ferromagnetic : the saturation magnetization is 11 emu/g for the as-milled Mn-70 at.% Al powders. Moreover, by removing almost all Al atoms from the as-milled Mn-85 at.% Al powders using chemical leaching, the saturation magnetization increases up to 36 emu/g. The above bct ${\alpha}'-Fe(N)$ and ferromagnetic ${\alpha}-Mn$ type alloys are the magnetic materials found for the first time, by using the present mechanochemical process.

• 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.

• Particle and aerosol research
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• v.10 no.4
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• pp.177-182
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• 2014

In this study, nickel-coated aluminum (Ni/Al) powders were synthesized for the utilization of energetic applications. Oxide materials present at the surface of Al powders of $45{\mu}m$ in averaged size were removed by using sodium hydroxide(NaOH) solution which is used for controlling pH. Nickel material is coated into the surface of oxide-removed Al powders by electroless-plating process. The microstructure of fabricated Ni/Al powders shows that nickel layers with a few hundreds nm were very homogeneously formed onto the surface of Al powders. The oxidation behavior of Ni/Al exihibit somewhat faster oxidation rate than that of pure Al with surface oxidation. Also, the higher exothermic reaction was observed from the Ni/Al powders. From the result of this, nickel coating is very promising method to obtain highly reactive and safe Al powders for energetic applications.

• Journal of the Korean Crystal Growth and Crystal Technology
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• v.27 no.5
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• pp.223-228
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• 2017

Aluminum nitride (AlN) powder was successfully synthesized at low temperature via carbothermal reduction and nitridation (CRN) assisted by microwave heating. The synthesis processes of AlN powder were investigated with X-ray diffraction, FE-SEM, FT-IR and TGA/DSC. Aluminum nitrate was used as an oxidizer and aluminum source, urea as fuel, and glucose as carbon source. These starting materials were mixed with D.I water and reacted in a flask at $100^{\circ}C$ for 20 minutes. After the reaction was finished, black foamy intermediate product was formed, which was considered to be an amorphous $Al_2O_3$ particles through intermediate product obtained by solution combustion synthesis (SCS) at the results of X-ray diffraction patterns and FT-IR. This intermediate product was nitridated at temperatures of $1300^{\circ}C$ and $1400^{\circ}C$ in $N_2$ atmosphere by a microwave heating furnace and then decarbonated at $600^{\circ}C$ for 2 hours in air. It should be noticed from FE-SEM images that as nitridated particles, identified as AlN from X-ray diffraction patterns, are covered with carbon residues. After decarbonating the nitridated powders, the spherical pure AlN powders were obtained without alumina and their particle sizes were dependent on the nitridating temperature with high temperature of $1400^{\circ}C$ giving large particles of around 70~100 nm.