• Journal of the Korean Ceramic Society
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• v.34 no.3
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• pp.249-256
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• 1997

The effect of process parameter of plasma assisted chemical vapor deposition (PACVD) on the variation of the ratio between cubic boron nitride (c-BN) and hexagonal boron nitride (h-BN) in the film was in-vestigated. The plasma was generated by electric power with the frequency between 100 and 500 KHz. BCl3 and NH3 were used as a boron and nitrogen source respectively and Ar and hydrogen were added as a car-rier gas. Films were composed of h-BN and c-BN and its ratio varied with the magnitude of process parameters, voltage of the electric power, substrate bias voltage, reaction pressure, gas composition, sub-strate temperature. TEM observation showed that h-BN phase was amorphous while crystalline c-BN par-ticle was imbedded in h-BN matrix in the case of c-BN and h-BN mixed film.

• The Korean Journal of Ceramics
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• v.3 no.3
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• pp.187-190
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• 1997

The aluminum-magnesium (Al-Mg) aklloys have been proved to be an effective solvent for synthesis of cubic-phase boron nitride (cBN) from hexagonal-phase boron nitride (hBN) at the conditions of high pressures and high temperatures (HP/HT). Various kinds of hBN powders having different crystallinity have been tested for cBN synthesis with Al-Mg solvents. The conversion ratio from hBN to cBN and the shape of synthesized cBN crystals appeared to be affected strongly by chemical composition and added amount of Al-Mg solvents as well as crystallinity of BN powders. As the magnesium content increased in the Al-Mg solvents, the conversion ratio increased and the size of cBN crystals became larger. The crystal facets developed well in the specimens with solvents having high Mg content. It was observed that a hBNlongrightarrowcBN transformation occurred more easily in the specimens having well crystallized hBN powders. Amorphous BN having much $B_2O_3$ impurity exhibited a low threshold temperature for transformation to cBN, which was attributed to crystallization of amorphous BN to well crystallized hBN prior to transformation into cBN with help of $B_2O_3$.

• Journal of Ceramic Processing Research
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• v.17 no.7
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• pp.763-767
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• 2016

The structural characterization of cubic boron nitride (c-BN) thin films was performed using a B4C target in a radio-frequency magnetron sputtering system. The deposition processing conditions, including the substrate bias voltage, substrate temperature, and base pressure were varied. Fourier-transform infrared spectroscopy and X-ray photoelectron spectroscopy were used to analyze the crystal structures and chemical binding energy of the films. For the BN film deposited at room temperature, c-BN was formed in the substrate bias voltage range of -400 V to -600 V. Less c-BN fraction was observed as the deposition temperature increased, and more c-BN fraction was observed as the base pressure increased.

• Journal of the Korean institute of surface engineering
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• v.40 no.2
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• pp.91-97
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• 2007

In this study we investigated the oxygen effect on the nucleation and its residual stress during unbalanced magnetron sputtering. Up to 0.5% in oxygen flow rate, cubic phase (c-BN) was dominated with extremely small fraction of Hexagonal phase (h-BN) of increasing trend with oxygen concentration, whereas hexagonal phase is dominated beyond 0.75% flow rate. Interestingly, the residual stress in cubic-phase-dominated films was substantially reduced with small amount of oxygen (${\sim}0.5%$) down to a low value comparable to the h-BN case. This may be because oxygen atoms break B-N $sp^3$ bonds and make B-O bonds more favorably, increasing $sp^2$ bonds preference, as revealed by FTIR and NEXAFS. It was confirmed by experimental facts that the threshold bias voltage for nucleation and growth of cubic phase were increased from -55 V to -70 V and from -50 V to -60 V respectively. The reduction of residual stress in O-added c-BN films is seemingly resulting from the microstructure of the films. The oxygen tends to increase slightly the amount of h-BN phase in the grain boundary of c-BN and the soft h-BN phase of 3D network including surrounding nano grains of cubic phase may relax the residual stress of cubic phase.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 1999.05a
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• pp.47-48
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• 1999

• The Korean Journal of Ceramics
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• v.6 no.2
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• pp.129-133
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• 2000

Boron nitride films were synthesized with $N_2$ion flux of low energy, up to 100 eV, at different substrate temperatures of no heating, 200, 400, 500, and $800^{\circ}C$, respectively. Boron was supplied by e-beam evaporation at the rate of $1.5\AA$/sec. For all the conditions, hexagonal BN (h-BN) phase was mainly synthesized and high resolution transmission electron microscopy (HRTEM) showed that (002) planes of h-BN phase were aligned vertical to the Si substrate. The maximum alignment occurred around $400^{\circ}C$. In addition to major h-BN phase, transmission electron diffraction (TED) rings identified the formation of cubic BN (c-BN) phase. But HRTEM showed no distinct and continuous c-BN layer. These results suggest that c-BN phase may form in a scattered form even when h-BN phase is mainly synthesized under small momentum transfer by bombarding ions, which are not reconciled with the macro compressive stress model for the c-BN formation.

• Journal of the Korean institute of surface engineering
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• v.46 no.4
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• pp.139-144
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• 2013

c-BN(cubic boron nitride) is known to have extremely high hardness next to diamond, as well as very high thermal and chemical stability. The c-BN in the form of film is useful for wear resistant coatings where the application of diamond film is restricted. However, there is less practical application because of difficult control of processing variables for synthesis of c-BN film as well as unclear mechanism on formation of c-BN. Therefore, in the present study, the structural characterization of c-BN thin film were investigated using $B_4C$ target in r.f. magnetron sputtering system as a function of processing variables. c-BN films were coated on Si(100) substrate using $B_4C$ (99.5% purity). The mixture of nitrogen and argon was used for carrier gas. The deposition processing conditions were changed with substrate bias voltage, substrate temperature and base pressure. Fourier transform infrared microscopy (FT-IR) and X-ray photoelectron spectroscopy (XPS) were used to analyze crystal structures and chemical binding energy of the films. In the case of the BN film deposited at room temperature, c-BN was formed in the substrate bias voltage range of -400 V~ -600 V. Less c-BN fraction was observed as deposition temperature increased and more c-BN fraction was observed as base pressure increased.

• Journal of the Korean institute of surface engineering
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• v.32 no.3
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• pp.467-471
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• 1999

BN films were grown on silicon (l00) substrate by magnetically enhanced activated reactive evaporation (ME-ARE) with pulsed DC power instead of r.f. for substrate biasing. The deposited films were analyzed using Fourier transform infrared spectroscopy (FTIR) and transmission electron microscopy (TEM). FTIR results show that the intensity of absorption band of $sp^2$ bond of BN decreased and that of $sp^3$ bond of c-BN increased with increasing pulsed DC bias voltage applied to substrate. The initially grown layer at the interface was observed by TEM and considered to be of$ sp^2$-bonded BN. The cross-sectional and planar TEM micrographs show that the upper layer on the initial layer was the single phase c-BN. It is concluded that cubic boron nitride films could be synthesized by ME-ARE process with pulsed DC biasing.

• Journal of the Korean Ceramic Society
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• v.49 no.6
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• pp.620-624
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• 2012

The role of moisture remaining inside the deposition chamber during the formation of the cubic boron nitride (c-BN) phase in BN film was investigated. BN films were deposited by an unbalanced magnetron sputtering (UBM) method. Single-crystal (001) Si wafers were used as substrates. A hexagonal boron nitride (h-BN) target was used as a sputter target which was connected to a 13.56 MHz radiofrequency electric power source at 400 W. The substrate was biased at -60 V using a 200 kHz high-frequency power supply. The deposition pressure was 0.27 Pa with a flow of Ar 18 sccm - $N_2$ 2 sccm mixed gas. The inside of the deposition chamber was maintained at a moisture level of 65% during the initial stage. The effects of the evacuation time, duration time of heating the substrate holder at $250^{\circ}C$ as well as the plasma treatment on the inside chamber wall on the formation of c-BN were studied. The effects of heating as well as the plasma treatment very effectively eliminated the moisture adsorbed on the chamber wall. A pre-deposition condition for the stable and repeatable deposition of c-BN is suggested.

• Proceedings of the Korean Institute of Surface Engineering Conference
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• 2013.05a
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• pp.46-47
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• 2013

다이아몬드와 같은 $sp^3$ 결합을 가지며, 다이아몬드 다음으로 경도가 강한 입방정 질화붕소(cBN)는 철계금속가공에의 적합성 및 낮은 증착온도로 인하여 표면 코팅소재로의 응용이 크게 기대되어 왔다. 그러나 증착시 cBN 상의 핵생성 이전에 필연적으로 증착되는 비정질 질화붕소(aBN) 및 육방정 질화붕소(hBN) 층의 대기 하에서의 불안정성 그리고 cBN 상의 증착에 수반되는 높은 압축 잔류응력으로 인해 모재와의 밀착력이 낮아지는 문제점 등으로 인해 응용이 크게 제한되어져 왔다. 본 발표에서는 아르곤(Ar)과 질소($N_2$)를 반응가스로 이용하여 스퍼터링법으로 증착한 질화붕소에서 발생하는 높은 잔류응력의 원인과 이를 낮추기 위해 반응가스에 첨가한 수소의 효과에 대해서 상세히 고찰해 보고자 한다.