• 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 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.

• The Transactions of The Korean Institute of Electrical Engineers
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• v.61 no.1
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• pp.89-93
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• 2012

c-BN films were deposited on SKH-51 steels by electron assisted hot filament CVD method and microstructure development was studied processing parameters such as bias voltage, temperature, etching and phase transformation at boundary layer between BN compound and steel to develop a high performance wear resistance tools. A negative bias voltage higher than 200V at substrate temperature of $800^{\circ}C$ and gas pressure of 20 torr in B2H6-NH3-H2 gas system was one of optimum conditions to produce c-BN films on the SKH-51 steels. Thin layer of hexagonal boron nitride phase was observed at the interface between c-BN layer and substrate.

• 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.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.

• Proceedings of the Korean Vacuum Society Conference
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• 1998.02a
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• pp.120-120
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• 1998

Boron nitride (BN) films have attracted a growing interest for a variety of t technological applications due to their excellent characteristics, namely hardness, c chemical inertness, and dielectrical behavior, etc. There are two crystalline phases 1551; of BN that are analogous to phases of carbon. Hexagonal boron nitride (h-BN) has a a layered s$\sigma$ucture which is spz-bonded structure similar to that of graphite, and is t the stable ordered phase at ambient conditions. Cubic boron nitride (c-BN) has a z zinc blende structure with sp3-bonding like as diamond, 따ld is the metastable phase a at ambient conditions. Among of their prototypes, especially 삼Ie c-BN is an i interesting material because it has almost the same hardness and thermal c conductivity as di없nond. C Conventionally, significant progress has been made in the experimental t techniques for synthesizing BN films using various of the physical vapor deposition 밍ld chemical vapor deposition. But, the major disadvantage of c-BN films is that t they are much more difficult to synthesize than h-BN films due to its narrow s stability phase region, high compression stress, and problem of nitrogen source c control. Recent studies of the metalorganic chemical vapor deposition (MOCVD) of I III - V compound have established that a molecular level understanding of the d deposition process is mandatory in controlling the selectivity parameters. This led t to the concept of using a single source organometallic precursor, having the c constituent elements in stoichiometric ratio, for MOCVD growth of 삼Ie required b binary compound. I In this study, therefore, we have been carried out the growth of h-BN thin f films on silicon substrates using a single source precursors. Polycrystalline h-BN t thin films were deposited on silicon in the temperature range of $\alpha$)() - 900 $^{\circ}$C from t the organometallic precursors of Boron-Triethylamine complex, (CZHs)3N:BRJ, and T Tris(dimethylamino)Borane, [CH3}zNhB, by supersonic molecular jet and remote p plasma assisted MOCVD. Hydrogen was used as carrier gas, and additional nitrogen w was supplied by either aDlIDonia through a nozzle, or nitrogen via a remote plasma. T The as-grown films were characterized by Fourier transform infrared spectroscopy, x x-ray pthotoelectron spectroscopy, Auger electron spectroscopy, x-ray diffraction, t transmission electron diffraction, optical transmission, and atomic force microscopy.roscopy.

• 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.

• Journal of the Korean Institute of Electrical and Electronic Material Engineers
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• v.33 no.5
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• pp.373-379
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• 2020

In this study, TiN-coated cBN (cubic-structure boron nitride) powders were successfully synthesized by a sol-gel method using titanium (IV) isopropoxide (TTIP) and by controlling the heat treatment conditions. After the sol-gel process, amorphous nano-sized TiO_x was uniformly coated on the surface of cBN powder particles. The obtained TiO_x-coated cBN powders were heated at 1,000~1,300℃ for 1 or 6 h in a flow of 95%N₂-5%H₂ mixed gas. With increasing temperature, the chemical composition of the TiO_x coating layer changed in the order of TiO₂→Ti₆O₁₁→Ti₄O₇→TiN due to reduction of the Ti ions. The TiN coating layer was observable in the samples heated at 1,200℃ and appeared as the main phase in the sample heated at 1,300℃. The resulting thickness of the TiN coating layer of the sample heated at 1,300℃ was approximately 45~50 nm.

• Proceedings of the Korea Crystallographic Association Conference
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• 2003.05a
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• pp.6-6
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• 2003

Highly crystalline 5H-polytypic form of sp3-bonded boron nitride (BN) was grown by pulsed-laser-vaporization of BN, where synchronous reactive-plasma packets assisted the crystal growth in the vapor phase. The structure of the product crystallites (˙5 micrometers) was confirmed by using transmission electron diffraction and electron energy loss spectroscopy. This material proved to have a sharp and dominant band at 225 nm by cathode luminescence at room temperatures and corresponding monochromatic images revealed that they uniformly emitted the ultraviolet light. Considering that cubic BN has already been doped as p- and n- type semiconductors, this material may be applied to the light-emitting devices working at almost the deepest limit of the UV region that is functional without vacuum.