• Journal of the Korean Ceramic Society
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• v.28 no.8
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• pp.647-653
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• 1991

In order to synthesize fine AlN powder by the direct nitridation of Aluminum metal power added LiF and BaF2 as additives was heated at 150$0^{\circ}C$ for 3 hrs. in nitrogen gas with flow rate of 20 mι/sec. Additives are promoted the nitridation by prevented the aggromerate of powders when 3% LiF and 2% BaF2 were added to Al metal powder. Rate of nitridation was about 100% and average size of AlN powders were very fine such as 0.3 ${\mu}{\textrm}{m}$. Specific surface area of synthesized AlN powder was 3.95$m^2$/g and also O2 and N2 contents were 2.595% and 33.25%, respectively.

• Journal of the Korean Ceramic Society
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• v.43 no.10 s.293
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• pp.595-600
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• 2006

The preparation of $\beta$-SiAlON powder by SHS in the system of $Si-Al-SiO_2-NH_4F(\beta-Si_3N_4)$ was investigated in this study. In the preparation of SiAlON powder, the effect of gas pressure, compositions such as Si, $NH_4F$, \beta-Si_3N_4$ and additive in mixture on the reactivity were investigated. At 50 atm of the initial inert gas pressure in reactor, the optimum composition for the preparation of pure $\beta$-SiAlON was $3Si+Al+2SiO_2+NH_4F$. The $\beta$-SiAlON powder synthesized in this condition was a single phase $\beta$-SiAlON with a rod like morphology.

• Journal of the Korean Ceramic Society
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• v.33 no.4
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• pp.455-463
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• 1996

Aluminium nitride (AlN) powder was prepared by using aluminium (III) complexes with dibasic carboxylate ligands(adipato)(hydroxo) aluminium(III) and (hydroxo)(succinato)aluminium (III) as a precursor. The AlN pow-der was obtained by calcining the complexes without mixing any carbon source under a flow of ammonia at 120$0^{\circ}C$ Contary to the conventional carbothermal reduction and nitridiation the process of decarboniza-tion of the residual carbon was not required because of the reaction of ammonia with carbon at temperature >100$0^{\circ}C$. Fine AlN powder was also prepared by calcining a mixture of an (adipato)(hydroxo)aluminium(III) complex and carbon under a flow of nitrogen at 140$0^{\circ}C$ The AlN powders prepared were ultrafine and their morphology was almost the same as that of powders of two precursors.

• Journal of the Korean Ceramic Society
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• v.48 no.5
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• pp.418-425
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• 2011

In this study, a high energy ball milling process was introduced in order to improve the densification of direct nitrided AlN powder. The sintering behavior and thermal conductivity of the AlN milled powder was investigated. The mixture of AlN powder and 5 wt% $Y_2O_3$ as a sintering additive was pulverized and dispersed by a bead mill with very small $ZrO_2$ bead media. The milled powders were sintered at $1700^{\circ}C-1800^{\circ}C$ for 4 h under $N_2$ atmosphere. The results showed that the sintered density was enhanced with increasing milling time due to the particle refinement as well as the increase in oxygen contents. Appropriate milling time was effective for the improvement of thermal conductivity, but the extensive millied powder formed more fractions of secondary phase during sintering, resulted in the decrease in thermal conductivity. The AlN powder milled for 10min after sintering at $1800^{\circ}C$ revealed the highest thermal conductivity, of 164W/$m{\cdot}K$ in tne densified AlN sintered at $1800^{\circ}C$.

• Resources Recycling
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• v.26 no.3
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• pp.39-46
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• 2017

AlN powder was prepared by carbon reduction and subsequent nitridation method through lab- scale experiments. AlN powder was synthesized using the mixture of high purity $Al_2O_3$ powder and carbon black at $1,600{\sim}1,700^{\circ}C$ for 0.5~6 hours under nitrogen atmosphere (flow rate of nitrogen gas: $4.7{\times}10^{-6}{\sim}20{\times}10^{-6}m^3/sec$) with variation of charged height of the mixture powder. Experimental results showed that size of the synthesized particles grows with increasing of temperature. The reaction activation energy was calculated as 382 kJ/mol at the temperature range, and it was considered that chemical reaction is the rate determining step. Content of oxygen and nitrogen of the prpared samples were 0.71~0.96 wt% and 30.7~35.1 wt%. The results was similar with those of the commercial AlN product.

• Journal of the Korean Ceramic Society
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• v.29 no.6
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• pp.471-479
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• 1992

AlN powder was synthesized by carbothermal reduction and nitridation using Al2(SO4)3.18H2O as the starting material. The synthesized AlN powder was fine but contained oxygen. Therefore carbonaceous material (carbon black or phenol novolac) was added teogether with the sintering aids (CaO, CaF2, CaCl2, Y2O3 and YF3). It was found that pressureless sintering at 1700~180$0^{\circ}C$ after deoxidation at 150$0^{\circ}C$ suppressed the formation of second phase (27R) and reduced the contents of lattice oxygen within AlN ceramics.

• Journal of the Korean Ceramic Society
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• v.27 no.6
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• pp.799-807
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• 1990

In this study, effects of oxide additives on mechanical properties and microstructure of A1N and A1N polytype ceramics were investigated. Fine A1N powder was synthesized by nitriding alumiuim hydroxide prepared from Al-isopropoxide, at 1350$^{\circ}C$ for 10h in N2 atmosphere. By adding 3w/o Y2O3, 0.56w/o CaO, and 10w/o SiO2 to AlN powder, AlN and AlN polytype ceramics were prepared by hot-pressing under the pressure of 30 MPa at 1800$^{\circ}C$ for 1h. AlN ceramics with no additives formed considerable amount of AlON phase, while AlN ceramics doped with Y2O3 or CaO decreased AlON phase and formed Y-Al or Ca-Al oxide compound. AlN＋10w/o SiO2(＋3w/o Y2O3) composition produced AlON and AlN polytype compound having 21R as a major phase. Room temperature flexural strength of AlN ceramics with no additive was 246MPa, and room temperature flexural strength and critical temperature difference by thermal shock(ΔTc) of AlN ceramics dooped with Y2O3 or CaO were 532MPa/340$^{\circ}C$ and 423MPa/300$^{\circ}C$, respectively. Y2O3 and CaO used as sintering agent played roles of densification and oxygen removal of AlN ceramics, and affected grain growth/grain morphologies of AlN ceramics.

• Resources Recycling
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• v.25 no.5
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• pp.75-83
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• 2016

AlN powder was prepared by carbon reduction and subsequent nitridation method through the scale-up experiments of 0.7 ~ 1.5 kg per batch. AlN powder was synthesized using the mixture of $Al_2O_3$ powder and carbon black at $1,550{\sim}1,750^{\circ}C$ for 0.5 ~ 4 hours under nitrogen atmosphere (flow rate of nitrogen gas: $10{\sim}40{\ell}/min$) at $2.0{\times}10^{-1}Torr$. Experimental results showed that $1,700{\sim}1,750^{\circ}C$ for the reaction temperature, 3 hr for reaction time, and $40{\ell}/min$ for the flow rate of nitrogen gas were the optimal conditions. Also, in order to remove carbon in the synthesized AlN, the remained carbon was removed at $650{\sim}750^{\circ}C$ for 1 ~ 2 hr using horizontal tube furnace. The results showed that 1 : 3.2 mol ratio of $Al_2O_3$ to carbon black, reaction temperature of $750^{\circ}C$, reaction time of 2 hours, rotating speed of 1.5 rpm under atmosphere condition were the optimal conditions. Under these conditions, high-purity AlN powder over 99% could be prepared: carbon and oxygen contents of the AlN powder were 835 ppm and 0.77%, respectively.

• Korean Journal of Materials Research
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• v.11 no.10
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• pp.863-868
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• 2001

The present study was carried out to investigate the effect of MA processing variables on the microstructural properties of composite powders and the coefficient of thermal expansion of pulse electric current sintered AlN-Cu powder compacts. The AlN-Cu powders had a size of less than 15 $\mu\textrm{m}$ with 25 nm size of copper crystallite after MA 32 hours. The finely distributed AlN-Cu powder compacts were completely achieved after PECS. The residual oxygen was considerably removed after hydrogen reduction treatment. The residual carbon was completely removed to 97%. The CTE of AlN-Cu powder compacts showed a good consistency with Kingery-Tuner model when the volume fraction of copper was less than 60%. When it was more than 60%, the CTE had a good agreement with Series model.

• Proceedings of the Korean Powder Metallurgy Institute Conference
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• 1999.10a
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• pp.25-25
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• 1999