• Title/Summary/Keyword: nitridation

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Preparation of Aluminum Nitride from an Alkoxide and its Properties (알콕사이드로부터 AlN분말의 합성 및 분말 특성)

  • 이홍림;박세민;조덕호
    • Journal of the Korean Ceramic Society
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    • v.26 no.1
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    • pp.100-108
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    • 1989
  • Aluminum hydroxides were prepared by the alkoxide hydrolysis method using Al-isopropoxide as a starting material and NH4OH as a catalytic agent. When Al-isopropoxide was hydrolyzed in a H2O-NH3 system, only Al(OH)3 was obtained over all pH values. However, AlOOH was formed besides Al(OH)3 when Al-isopropoxide was hydrolyzed in a H2O-NH3-isopropyl alcohol system. The AlOOH/Al(OH)3 ratio was increased as the isopropyl alcohol content was increased. The hydroxides, Al(OH)3 and AlOOH, obtained in this study and the commerical products, $\alpha$-Al2O3 and AlOOH were subjected to the carbothermal reduction and nitridation reaction to product AlN powder, using carbon black as a reducing agent under N2 atmosphere at various temperatures. AlN was synthesized from the obtained Al(OH)3 and the commercial AlOOH at 145$0^{\circ}C$, however, synthesized from the obtained AlOOH and the commercial alpha-alumina at 135$0^{\circ}C$. The temperature difference is assumed to be attributed to the reactivity of those powders. AlN powder prepared from the Al-isopropoxide was observed to have the narrower particle size distribution than that prepared from the commercial $\alpha$-Al2O3 or AlOOH.

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Synthesis of $\alpha$-Sialon Ceramics from an Alkoxide and Their Mechanical Properties(I) (알콕사이드로부터 $\alpha$-Sialon 세라믹스의 제조 및 기계적 성질(I))

  • 이홍림;윤창현;조덕호
    • Journal of the Korean Ceramic Society
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    • v.28 no.2
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    • pp.130-140
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    • 1991
  • The powders of the system Si3N4-Y2O3-AlN were prepared using Si(OC2H5)4 and YCl3.6H2O together with commercial AlN powder. $\alpha$-Si3N4 was prepared by the carbothermal reduction and nitridation of the hydrolyzed gel at 135$0^{\circ}C$ for 10h in N2 atmosphere. YCl3.6H2O was observed to be changed to Y2O3 during the reaction. $\alpha$-Sialon(X=0.2, 0.4, 0.6) ceramics were obtained by hot-pressing the Si3N4-Y2O3-AlN mixture at 178$0^{\circ}C$ for 1h under 30 MPa. The content of $\alpha$-Sialon increased with increasing metal solubility(x value) and $\alpha$-Sialon single phase was obtained at the metal solubility of 0.6. With increasing metal solubility, flexural strength, fracture toughness and thermal shock resistence were decreased, while the microhardness was increased. Large elongated $\beta$-Si3N4 grains were mainly observed at lower metal solubility. Mechanical prorerties of the sintered ceramics with X=0.2 were measured as follows : flexural strength ; 650 MPa, fracture toughness ; 3.63 MN/m3/2, hardness ; 14.7 GPa, thermal shock resistence temperature ; 58$0^{\circ}C$.

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Synthesis of $\beta$다-Sialon with Various Compositions from Kaolin (카올린으로부터 조성이 다른$\beta$다-Sialon의 합성)

  • 최상욱;서규식;이종진
    • Journal of the Korean Ceramic Society
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    • v.23 no.5
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    • pp.17-24
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    • 1986
  • β'-Sialon with different compositions was synthesized by the carbothermal reduction-nitridation of compacts containing kaolin graphite and silicon or aluminum at temperature of 1300-1450℃ under flowing gas of 90% N2-10% H2 or 20hrs. Quantitative analysis of minerals which were formed in the specimens was carried out by using the calibration curve which has been prepared from X-ray diffraction patterns. The obtained results were as follows : 1. In the formation of β'-Sialon by carbothermal reduction-nutridation of Si-Al-O-C system mixtures at 1400℃ for 20hrs. (2) β'-Sialon as a major mineral and α-Al2O3 as a minor mineral were identified in the specimen which was prepared of kaolin and graphite. (3)α-Al2O3 and 15R as a minor minerals were measured in the specimen which was prepared of kaolin aluminum and graphite. (4) AlN instead of α-Al2O3 and 15R was formed in the compacts that excess graphite(=35 wt%) was added to the mixture of kaolin and aluminium. 2. As the reaction time and temperature were increased the formation of β'-Sialon was increased whereas the phases of mllite SiC and Si2ON2 were decreased gradually.

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The behavior of Si During Sintering of Reaction Bonded Silicon Nitride (반응결합 질화수소의 소결시 규소의 거동에 관한 연구)

  • 김재룡;김종희
    • Journal of the Korean Ceramic Society
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    • v.23 no.5
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    • pp.67-74
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    • 1986
  • To investigate the effects of unreacted silicon on the $\alpha$/$\beta$transfornation variation of morphology and mechanical strength of Sintered Reaction Bonded Silicon Nitride the mixtures of $\alpha$-$Si_3N_4$ and Si powder and Reaction Bonded Silicon Nitride were heat treated. The heat-treatments were performed in Ar atmosphere in order to inhibit the nitridation of silicon. In the mixtures heat-trated at 1$700^{\circ}C$ the amount of $\beta$-TEX>$Si_3N_4$transformed from $\alpha$-TEX>$Si_3N_4$was sigmoidally increased and the equiaxed $\alpha$-TEX>$Si_3N_4$grains elongated with the amount of silicon and heat treating time. And large $\beta$-TEX>$Si_3N_4$grains grown into silicon were observed. On the other hand there was no change in the heat-treatment of pure $\alpha$-TEX>$Si_3N_4$In case of the heat-treatment of RBSN the same phenomena due to the silicon appearing from the decomposition of $\alpha$-Smatte and needle were observed. From the three point bending test the strength of the sintered specimens with the and without 5wt% silicon addition had 53Kg/$mm^2$ and 73Kg/$mm^2$ respectively.

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Study on P-type in-situ doped Polysilicon Films (P형 in-situ 도핑 폴리실리콘 막질에 관한 연구)

  • Oh, Jung-Sup;Lee, Sang-Eun;Noh, Jin-Tae;Lee, Sang-Woo;Bae, Kyoung-Sung;Roh, Yong-Han
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.21 no.3
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    • pp.208-212
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    • 2008
  • This paper reports physical properties of in situ boron doped silicon films made from boron source gas and silane ($SiH_4$) gas in a conventional low-pressure chemical vapor deposition vertical furnace. If the p-type polysilicon is formed by boron implantation into undoped polysilicon, the plasma nitridation (PN) process is added on the oxide in order to suppress boron penetration that can be caused during the thermal treatments used in fabrication. In-situ boron doped polysilicon deposition can complete p-type polysilicon film with only one deposition process and need not the PN process, because there is not interdiffusion of dopant at the intermediate temperatures of the subsequent steps. Since in-situ boron doped polysilicon films have higher work function than that of n-type polysilicon and they are compatible with the underlying oxide, they may be promising materials for improving memory cell characteristics if we make its profit of these physical properties.

Influence of Nitrogen Plasma Treatment on Low Temperature Deposited Silicon Nitride Thin Film for Flexible Display (플렉서블 디스플레이 적용을 위한 저온 실리콘 질화막의 N2 플라즈마 처리 영향)

  • Kim, Seongjong;Kim, Moonkeun;Kwon, Kwang-Ho;Kim, Jong-Kwan
    • Journal of the Korean Institute of Electrical and Electronic Material Engineers
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    • v.27 no.1
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    • pp.39-44
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    • 2014
  • Silicon nitride thin film deposited with Plasma Enhanced Chemical Vapor Deposition was treated by a nitrogen plasma generated by Inductively Coupled Plasma at room temperature. The treatment was investigated by Fourier Transform Infrared Spectroscopy and Atomic Force Microscopy on the surface at various RF source powers at two RF bias powers. The amount of hydrogen was reduced and the surface roughness of the films was decreased remarkably after the plasma treatment. In order to understand the causes, we analyzed the plasma diagnostics by Optical Emission Spectroscopy and Double Langmuir Probe. Based on these analysis results, we show that the nitrogen plasma treatment was effective in the improving of the properties silicon nitride thin film for flexible display.

Effect of Mechanical Alloying Atmosphere on Formation of AlN (AlN의 형성에 미치는 기계적 합금화 분위기의 영향)

  • Yu Seung-Hoon;Lee Young Sung;Shin Kwang-Seon
    • 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.

Synthesis and Characterization of Gallium Nitride Powders and Nanowires Using Ga(S2CNR2)3(R = CH3, C2H5) Complexes as New Precursors

  • Jung, Woo-Sik;Ra, Choon-Sup;Min, Bong-Ki
    • Bulletin of the Korean Chemical Society
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    • v.26 no.1
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    • pp.131-135
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    • 2005
  • Gallium nitride (GaN) powders and nanowires were prepared by using tris(N,N-dimethyldithiocarbamato)gallium(III) (Ga(DmDTC)$_3$) and tris(N,N-diethyldithiocarbamato)gallium(III) (Ga(DeDTC)$_3$) as new precursors. The GaN powders were obtained by reaction of the complexes with ammonia in the temperature ranging from 500 to 1100 ${^{\circ}C}$. The process of conversion of the complexes to GaN was monitored by their weight loss, XRD, and $^{71}$Ga magic-angle spinning (MAS) NMR spectroscopy. Most likely the complexes decompose to $\gamma$ -Ga$_2$S$_3$ and then turn into GaN via amorphous gallium thionitrides (GaS$_x$N$_y$). The reactivity of Ga(DmDTC)$_3$ with ammonia was a little higher than that of Ga(DeDTC)$_3$. Room-temperature photoluminescence spectra of asprepared GaN powders exhibited the band-edge emission of GaN at 363 nm. GaN nanowires were obtained by nitridation of as-ground $\gamma$ -Ga$_2$S$_3$ powders to GaN powders, followed by sublimation without using templates or catalysts.

Synthesis of (Ti,Al)N Powder by the Direct Nitridation(II) (직접질화법에 의한 (Ti,Al)N계 복합질화물의 합성(II))

  • Cho, Young-Soo;Lee, Young-Ki;Sohn, Yong-Un;Park, Kyong-Ho;Kim, Seok-Yoon
    • Journal of the Korean Society for Heat Treatment
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    • v.9 no.3
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    • pp.219-227
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    • 1996
  • The purpose of this research is to develop the technology for the synthesis of (Ti,Al)N powder, which shows simultaneously the excellent properties of TiN and AlN, from the Ti-Al intermetallic compounds by the direct nitriding method. The effects of variables such as temperature, Ti-Al intermetallic compounds ($TiAl_3$, TiAl and $Ti_3Al$) were investigated by TG, XRD and SEM. The (Ti,Al)N powder can be easily synthesized from the intermetallic compounds by the direct nitriding method. Among the intermetallic compounds, the nitriding behavior increased with TiAl> $Ti_3Al$ > $TiAl_3$, as the difference of diffusion coefficient for nitrogen in each materials. The ternary nitride such as $Ti_2AlN$ and $Ti_3Al_2N_2$ can be synthesized by the direct nitriding method, although the ternary nitride coexist with TiN and AlN. The ternary nitrides are stable below $1400^{\circ}C$, but these are gradually decomposed into TiN and AlN above $1400^{\circ}C$.

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Synthesis of solar light responsive ZnO/TaON photocatalysts and their photocatalytic activity (태양광 응답형 ZnO/TaON 나노 복합체의 제조 및 광촉매 특성 평가)

  • Kim, Tae-Ho;Jo, Yong-Hyeon;Lee, Su-Wan
    • Proceedings of the Korean Institute of Surface Engineering Conference
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    • 2014.11a
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    • pp.256-257
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    • 2014
  • The effects of the preparation conditions of ZnO-modified TaON on the photocatalytic activity for degradation of rhodamine B dye (Rh. B) under simulated solar light were investigated. The ZnO/TaON nanocomposite were prepared by loading particulate $Ta_2O_5$ with ZnO using different ZnO contents, followed by thermal nitridation at 1123 K for 5 h under $NH_3$ flow (20 ml min.1). The asprepared samples were characterized by XRD, UV-Vis-DRS, and SEM-EDX. The results revealed that the band gap energy absorption edge of as prepared nanocomposite samples was shifted to a longer wavelength as compared to ZnO and $Ta_2O_5$, and the 60 wt% ZnO/TaON nanocomposite exhibited the highest percentage (99.2 %) of degradation of Rh. B and the highest reaction rate constant ($0.0137min^{-1}$) in 4 h which could be attributed to the enhanced absorption of the ZnO/TaON nanocomposite photocatalyst. Hence, these results suggest that the ZnO/TaON nanocomposite exhibits enhanced photocatalytic activity for the degradation of rhodamine B under simulated solar light irradiation in comparison to the commercial ZnO, $Ta_2O_5$, and TaON.

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