• Journal of the Korean Ceramic Society
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• v.43 no.7 s.290
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• pp.445-450
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• 2006

The preparation of AlN powder by SHS in the system of $Al-AlN-NH_4Cl$ was investigated in this study. In the preparation of AlN powder, the effect of gas pressure and the composition such as Al, AlF, and additive in mixture on the reactivity were investigated. At 60 atm of the initial inert gas pressure in reactor, the optimum composition for the preparation of pure AlN was 35 wt%Al+5 wt% $NH_4Cl+60wt%$AlN. The AlN powder synthesized in this condition was a single phase AlN with a whisker morphology.

• Journal of the Korean Society for Heat Treatment
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• v.18 no.5
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• pp.281-287
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• 2005

Titanium aluminium nitride((TiAl)N) film is anticipated as an advanced coating film with wear resistance used for drills, bites etc. and with corrosion resistance at a high temperature. In this study, (TiAl)N thin films were deposited both at room temperature and at elevated substrate temperatures of 573 to 773 K by using a two-facing-targets type DC sputtering system in a mixture Ar and $N_2$ gases. Atomic compositions of the binary Ti-Al alloy target is Al-rich (25Ti-75Al (atm%)). Process parameters such as precursor volume %, substrate temperature and Ar/$N_2$ gas ratio were optimized. The crystallization processes and phase transformations of (TiAl)N thin films were investigated by X-ray diffraction, field-emission scanning electron microscopy. The microhardness of (TiAl)N thin films were measured by a dynamic hardness tester. The films obtained with Ar/$N_2$ gas ratio of 1:3 and at 673 K substrate temperature showed the highest microhardness of $H_v$ 810. The crystallized and phase transformations of (TiAl)N thin films were $Ti_2AlN+AlN{\rightarrow}TiN+AlN$ for Ar/$N_2$ gas ratio of 1:3, $Ti_2AlN+AlN{\rightarrow}TiN+AlN{\rightarrow}Ti_2AlN+TiN+AlN$ for Ar/$N_2$ gas ratio of 1:1 and $TiN+AlN{\rightarrow}Ti_2AlN+TiN+AlN{\rightarrow}Ti_2AlN+AlN{\rightarrow}Ti_2AlN+TiN+AlN$ for Ar/$N_2$ gas ratio of 3:1. The above results are discussed in terms of crystallized phases and microhardness.

• Journal of Powder Materials
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• v.11 no.4
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• pp.294-300
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• 2004

This study for preparation of aluminum nitride (AlN) with high purity was carried out by self-propagating high-temperature synthesis method in two different systems, $Al-N_{2}$ and $Al-N_{2}$-AlN, with the change of nitrogen gas pressure and dilution factor. On the occasion of $Al-N_{2}$ system, unreacted aluminum was detected in the product in spite of high nitrogen pressure, 10 MPa, This may be caused by obstructing nitrogen gas flow to inner part of molten and agglomerate of aluminum, formed in pre-heating zone. In $Al-N_{2}$-AlN system, AlN with a purity of 95% or ever can be prepared in the condition of $f_{Dil}\geq0.5$, $P_{N_{2}}\geq$ 1 MPa, and the purity can be elevated to 98% over in the condition of $f_{Dil}$ = 0.7 and $P_{N_{2}}$ = 10 MPa.

• Journal of the Korean Ceramic Society
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• v.33 no.10
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• pp.1089-1094
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• 1996

In this study the formation mechanism of AlN synthesized by SHS(Self-propagating high-temperature Syn-thesis) was studied in order to obtain uniform AlN powder size and morphology. Based on the morphology of AlN synthesized and the calculation of the temperature of Al powder as a function AlN layer thickness the formation mechanism of AlN was proposed.

• Journal of the Korean Ceramic Society
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• v.28 no.4
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• pp.269-278
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• 1991

Fine AlN powder was synthesized by carbothermal reduction and nitridation of alumimun hydroxide prepared from Al-isopropoxide. AlN ceramics with Y2O3 and CaO were prepared by hot-pressing under the pressure of 30 MPa at 180$0^{\circ}C$ for 1 h in N2 atmosphere. Grain boundary behavior and purification mechanism of AlN lattice were examined by heat treatment of AlN ceramics at 185$0^{\circ}C$ for 1-6 h in N2 atmosphere. AlN ceramics without sintering additives showed poor sinterability. However, Y2O3-doped and CaO-doped AlN ceramics were fully densified nearly to theoretical density. As the heat treatment time increased, c-axis lattice parameter increased. This is attributed to the removal of Al2O3 in AlN lattice. This purification effect of AlN attice depended upon the quantity of secondary oxide phase in the inintial stage of heat treatment and the heat treatment time.

• 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.

• Korean Journal of Materials Research
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• v.9 no.10
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• pp.962-969
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• 1999

Elastic and elasto-plastic stress analyses of AlN/Cu and AlN/W pints produced by active-metal brazing method using Ag-Cu-Ti insert-metal were performed with use of Finite-Element-Method(FEM). The results of stress analyses were compared with those from the pint strength tests and the observations of fracture behaviors. It was shown that a remarkably larger maximum principal stress is built in the AlN/Cu pint compared to the A1N/ W joint. Especially, the stress concentration with tensile component was confirmed at the free surface close to the bonded interface of AlN/Cu. The elasto-plastic analysis under consideration of stress relaxation effect of Ag-Cu-Ti insert possessing a so-called 'soft-metal effect' showed that the insert leads to a lowering of maximum principal stress in AlNiCu pint, even though an increase of the insert thickness above 100$\mu\textrm{m}$ could not bring its further decrease. The maximum pint strengths measured by shear test were 52 and 108 MPa for AlNiCu and AlN/W pints. respectively. Typical fractures of AlN/Cu pints occurred in a form of 'dome' which initiated from the free surface of AlN close to the bonded interface and proceeded towards the AlN inside forming a large angle. AlN/W pints were usually fractured at AlN side along the interface of AlN/insert-metal.

• 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.26 no.1
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• pp.31-36
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• 1989

In order to synthesize AlN-polytypes from AlN-SiO2-Al2O3 system, composition A (AlN/SiO2/Al2O3=1/0.3/0.05, mole ratio) and composition B(AlN-SiO2-Al2O3=1/0.2/0.05, mole ratio) were used. AlN-polytypes were produced by nitriding the mixture at 175$0^{\circ}C$~190$0^{\circ}C$ under N2 atmosphere. For lower reaction temperature, 15R phase was produced and in the case of higher reaction temperature, AlN phase was only produced. As each composition was heated at 185$0^{\circ}C$ in N2 atmosphere, produced main phases were 15R phase for composition A and 21R phase for composition B respectively. The fracture surfaces of produced reactants showed porous skeleton structure.

• Korean Journal of Materials Research
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• v.22 no.10
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• pp.539-544
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• 2012

We have grown AlN nanorods and AlN films using plasma-assisted molecular beam epitaxy by changing the Al source flux. Plasma-assisted molecular beam epitaxy of AlN was performed on c-plane $Al_2O_3$ substrates with different levels of aluminum (Al) flux but with the same nitrogen flux. Growth behavior of AlN was strongly affected by Al flux, as determined by in-situ reflection high energy electron diffraction. Prior to the growth, nitridation of the $Al_2O_3$ substrate was performed and a two-dimensionally grown AlN layer was formed by the nitridation process, in which the epitaxial relationship was determined to be [11-20]AlN//[10-10]$Al_2O_3$, and [10-10]AlN//[11-20]$Al_2O_3$. In the growth of AlN films after nitridation, vertically aligned nanorod-structured AlN was grown with a growth rate of $1.6{\mu}m/h$, in which the growth direction was <0001>, for low Al flux. However, with high Al flux, Al droplets with diameters of about $8{\mu}m$ were found, which implies an Al-rich growth environment. With moderate Al flux conditions, epitaxial AlN films were grown. Growth was maintained in two-dimensional or three-dimensional growth mode depending on the Al flux during the growth; however, final growth occurred in three-dimensional growth mode. A lowest root mean square roughness of 0.6 nm (for $2{\mu}m{\times}2{\mu}m$ area) was obtained, which indicates a very flat surface.