• Journal of the Korean Ceramic Society
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• v.41 no.2
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• pp.118-124
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• 2004

The properties of AlN made by carbothermal reaction depend on the starting materials, quantity of liquid, the liquid-vapor phase reaction, the N$_2$ flow rate, and the reaction temperature. AlN whisker was synthesized by the VLS and VS methods. Solid ${\alpha}$-A1$_2$O$_3$(AES-11) was carbothermally reduced with carbon black in a high-purity N$_2$ atmosphere with AlF$_3$ to cause whisker grown and additional aluminum liquid to increase whisker yield. Aluminum nitride was perfectly formed at reaction temperatures of 1600$^{\circ}C$. At reaction temperature higher than 1600$^{\circ}C$ the aluminum nitride was completely formed, while the composition remains unaffected. Needle-shaped whiskers formed best at 1600$^{\circ}C$ while higher temperatures disrupted whisker formation. Adding 0 to 15 wt% aluminum to the synthesis favorably affects the microstructure for formation of needle-shaped AlN whisker. Additions over 15 wt% degraded formation of AlN whisker.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2016.11a
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• pp.105-105
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• 2016

Recently, high power impulse magnetron sputtering (HIPIMS) has attracted considerable attentions due to its high potential for industrial applications. By pulsing the sputtering target with high power density and short duration pulses, a high plasma density and high ionization of the sputtered species can be obtained. HIPIMS has exhibited several merits such as increased coating density, good adhesion, microparticle-free and smooth surface, which make the HIPIMS technique desirable for synthesizing hard coatings. However, hard coatings present intrinsic defects (columnar structures, pinholes, pores, discontinuities) which can affect the corrosion behavior, especially when substrates are active alloys like steel or in a wear-corrosion process. Atomic layer deposition (ALD), a CVD derived method with a broad spectrum of applications, has shown great potential for corrosion protection of high-precision metallic parts or systems. In ALD deposition, the growth proceeds through cyclic repetition of self-limiting surface reactions, which leads to the thin films possess high quality, low defect density, uniformity, low-temperature processing and exquisite thickness control. These merits make ALD an ideal candidate for the fabrication of excellent oxide barrier layer which can block the pinhole and other defects left in the coating structure to improve the corrosion protection of hard coatings. In this work, CrN/Al2O3/CrN multilayered coatings were synthesized by a hybrid process of HIPIMS and ALD techniques, aiming to improve the CrN hard coating properties. The influence of the Al2O3 interlayer addition, the thickness and intercalation position of the Al2O3 layer in the coatings on the microstructure, surface roughness, mechanical properties and corrosion behaviors were investigated. The results indicated that the dense Al2O3 interlayer addition by ALD lead to a significant decrease of the average grain size and surface roughness and greatly improved the mechanical properties and corrosion resistance of the CrN coatings. The thickness increase of the Al2O3 layer and intercalation position change to near the coating surface resulted in improved mechanical properties and corrosion resistance. The mechanism can be explained by that the dense Al2O3 interlayer acted as an excellent barrier for dislocation motion and diffusion of the corrosive substance.

• Applied Microscopy
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• v.44 no.2
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• pp.79-82
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• 2014

Aluminum nitride (AlN) powder was easily synthesized by the direct nitridation of Al melt containing ~20 wt.% Mg catalyst and the nitriding behavior was investigated by thermodynamic calculation and through observations of electron microscopy and X-ray diffraction. The addition of Mg catalyst decreased the nitriding temperature below $1,000^{\circ}C$, which is comparable to the high nitriding temperature of $1,400^{\circ}C$ required in carbothermal method. It was caused by a significant increase of the solubility of nitrogen gas due to the increase of Mg catalyst in Al melt. The dissolved nitrogen gas met Mg catalyst and was transformed into metastable $Mg_3N_2$. Finally the metastable phase reacted with Al to AlN.

• Journal of Sensor Science and Technology
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• v.32 no.6
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• pp.425-431
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• 2023

An asymmetric metal-semiconductor-metal Al_0.24Ga_0.76N ultraviolet (UV) sensor was fabricated, and the effects of local Joule heating were investigated. After dielectric breakdown, the current density under a reverse bias of 2.0 V was 1.1×10^-9 A/cm², significantly lower than 1.2×10^-8 A/cm² before dielectric breakdown; moreover, the Schottky behavior of the Ti/Al/Ni/Au electrode changed to ohmic behavior under forward bias. The UV-to-visible rejection ratio (UVRR) under a reverse bias of 7.0 V before dielectric breakdown was 87; however, this UVRR significantly increased to 578, in addition to providing highly reliable responsivity. Transmission electron microscopy revealed interdiffusion between adjacent layers, with nitrogen vacancies possibly formed owing to local Joule heating at the AlGaN/Ti/Al/Ni/Au interfaces. X-ray photoelectron microscopy results revealed decreases in the peak intensities of the O 1s binding energies associated with the Ga-O bond and OH-, which act as electron-trapping states on the AlGaN surface. The reduction in dark current owing to the proposed local heating method is expected to increase the sensing performance of UV optoelectronic integrated devices, such as active-pixel UV image sensors.

• 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.

• Transactions of Materials Processing
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• v.8 no.3
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• pp.227-227
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• 1999

The effects of intermediate annealing (IA) and the final cold rolling (CR) condition on the microstructure and sagging resistance during brazing were investigated using three layer clad sheets composed of the Al-7.5 wt.%Si alloy (filler, thickness: 10 ㎛)/Al-1.3 wt.%Mn based alloy (core, 80㎛)/Al-7.5 wt.%Si alloy (filler, 10㎛). Also, the effect of 1.2∼2 wt.% Zn addition into the core on the sagging resistance of the clad sheets was determined. It was revealed that all the clad sheets fabricated by the optimum condition (IA at 690 K and CR to 20∼45%) show excellent sagging resistance with a limited erosion due to the formation of a coarsely recrystallized grain structure in the core during brazing. It was also revealed that the recrystallization behavior of the Al-1.3 wt.%Mn based alloy is hardly affected by the addition of 1.2-2 wt.%Zn during the brazing cycle. Therefore, the sagging resistance of the clad sheets is found to be governed not by the Zn content added in the A1-1.3wt.%Mn based core, but by the intermediate annealing and final cold rolling condition.

• Journal of the Korean Society for Heat Treatment
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• v.12 no.3
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• pp.221-230
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• 1999

The surface nitrogen permeation of Al alloyed 0.14%C-13%Cr stainless steels was investigated after heat treating at $1050^{\circ}C{\sim}1150^{\circ}C$ in the nitrogen gas atmosphere. The strong affinity between Al and nitrogen permeates the nitrogen through the interior of the steels. Two precipitates of round type and needle type are observed at the surface layer. These precipitates mainly consist of AlN containing plenty of aluminum. The surface layer of 0.53%Al alloyed specimen shows ferrite phase, while the surface layers of 1.65%Al and 2.27%Al alloyed specimens appear ${\gamma}$ plus ${\alpha}$ phases. The depth of nitrogen permeation depends upon the Al content and microstructure of the matrix. The 1.65%Al alloyed specimen representing ${\alpha}+{\gamma}$ matrix phases at the nitrogen permeation temperature shows the maximum case depth in this experiment. Although the surface hardness increases by raising the Al content of the specimen owing to the increase of nitride precipitation density, the nitride precipitation deteriorates the corrosion resistance in the solution of HCl, $H_2SO_4$, and $FeCl_3$.

• Korean Journal of Materials Research
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• v.5 no.2
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• pp.169-177
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• 1995

The diffusion barrier property of 100-nm-thick titanium nitride (TiN) film between Cu and Si was investigated using sheet resistance measurements, etch-pit observation, x-ray diffractometry, Auger electron spectroscopy, and transmission electron microscopy. The TiN barrier fails due to the formation of crystalline defects (dislocations) and precipitates (presumably Cu-silicides) in the Si substrate which result from the predominant in-diffusion of Cu through the TiN layer. In contrast with the case of Al, it is identified that the TiN barrier fails only the in-diffusion of Cu because there is no indication of Si pits in the Si substrate. In addition, it appears that the stuffing of TiN does not improve the diffusion barrier property in the Cu/TiN/Si structure. This indicates that in the case of Al, the chemical effect that impedes the diffusion of Al by the reaction of Al with $TiO_{2}$ which is present in the grain boundaries of TIN is very improtant. On the while, in the case of Cu, there is no chemical effect because Cu oxides, such as $Cu_{2}O$ or CuO, is thermodynamically unstable in comparison with $TiO_{2}$. For this reason, it is considered that the effect of stuffing of TiN on the diffusion barrier property is not significant in the Cu/ TiN/Si structure.

• Journal of Welding and Joining
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• v.12 no.4
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• pp.85-101
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• 1994

Effect of Cr, Cu and Ni metal powders addition on the alloyed layer of aluminum alloy (AC2B) has been investigated with the plasma transferred arc (PTA) overlaying process. The overlaying conditions were 125-200A in plasma arc current, 150mm/min in process speed and 5-20g/min in powder feeding rate. Main results obtained are summarized as follows: 1) It was made clear that formation of thick surface alloyed layer on aluminum alloy is possible by PTA overlaying process. 2) The range of optimum alloying conditions were much wider in case of Cu and Ni powder additions than the case of Cr powder addition judging from the surface appearance and the bead macrostructure. 3) Alloyed layer with Cu showed almost the homogeneous microstructure through the whole layer by eutectic reaction. alloyed layers with Cr and Ni showed needle-like and agglomerated microstructures, the structure of which has compound layer in upper zone of bead by peritectic and eutectic-peritectic reactions, respectively. 4) Microconstituents of the alloyed layer were analyzed as A1+CrA $l_{7}$ eutectics, C $r_{2}$al sub 11/, CrA $l_{4}$, C $r_{4}$A $l_{9}$ and C $r_{5}$A $l_{*}$ 8/ for Cr addition, Al+CuA $l_{2}$(.theta.) eutectics and .theta. for Cu addition, and Al+NiA $l_{3}$ eutectics. NiA $l_{3}$, N $i_{2}$A $l_{3}$ and NiAl for Ni addition. 5) Concerning defect of the alloyed layer, many blow holes were seen in Cr and Ni additions although there was lesser in Cu addition. Residual gas contents in blow hole for Cu and Ni alloyed layer were confirmed as mainly $H_{2}$ and a littie of $N_{2}$ Cracking was observed in compound zone of the alloyed layer in case of Cr and Ni addition but not in Cu alloyed layer.r.r.

• Journal of the Korean Ceramic Society
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• v.36 no.2
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• pp.193-202
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• 1999

Al powder, AlN powder, SiC whisker and sintering aids were wet-mixed, and then the specimens prepared with mixed powder were reacted by nitridation at 600∼1400$^{\circ}C$ for 5 hrs. It was cleat that the higher nitridation and the more SiC whisker content were, the better bending strength was. The specimen of Al50/AlN50 reacted at 1400$^{\circ}C$ for 5hrs had the nitridation percent of 97%, the shrinkage under 2%, and the relative density of 78%. And the maximum bending strength of reaction-bonded specimen was 250 MPa. The specimens completely nitrided were post-sintered at 1700, 1800 and 1900$^{\circ}C$ for 2hrs. The post-sintered body had the shrinkage under 6% and the relative density of 86%. Because of the formation of solid solution between AlN and SiC whisker over 1800$^{\circ}C$, the promotion of mechanical properties according to SiC whisker addition was not observed. The post-sintered body had the maximum bending strength of 195 MPa.