• 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 Korean Vacuum Society Conference
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• 2011.02a
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• pp.43-43
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• 2011

BN(Boron Nitride)은 온도와 압력 조건에 따라 안정한 상이 sp3 결합인 cubic 구조의 BN(cBN)과 sp2 결합인 hexagonal 구조의 BN(hBN or tBN)으로 나뉘는데, 이 중 cBN은 우수한 기계적, 물리적, 화학적 특성으로 인해 박막 분야에서 매우 높은 응용가능성을 지니고 있다. 하지만 cBN 박막의 합성과정에서의 필수적인 요소인 높은 압축잔류응력은 cBN을 응용분야에 적용하는데 있어 한계점으로 계속 남아 있었다. 그동안 이러한 잔류응력을 감소시키기 위해 열처리, 이온 주입, 제 3의 물질 첨가 등 다양한 관점에서 접근한 연구들이 진행되어 왔다. 본 연구에서는 cBN 합성과정에서 잔류응력을 감소시키기 위한 방법으로 수소를 첨가하였고, 그에 따른 잔류응력의 변화를 분석하고, 그 과정에서 잔류응력의 형성에 수소가 어떤 역할을 하는지 규명하고자 하였다. cBN 박막은 hBN을 target으로한 unbalanced magnetron sputtering를 사용하여, 실리콘 wafer 위에 합성하였다. 증착압력은 1.3mTorr로, 수소의 첨가량을 증가시키며 잔류응력과 cBN fraction을 관찰하였다. cBN fraction은 FTIR로 분석하였고, 잔류응력은 실리콘 strip의 in-situ 곡률측정법으로 계산하였다. cBN 박막의 조성과 구조 분석, 수소의 역할 규명을 위해 RBS 및 HRTEM을 이용하였다.

• 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.

• Proceedings of the KWS Conference
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• 2007.11a
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• pp.215-217
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• 2007

철계 피삭재 가공 시 적용되는 cBN(cubic Boron-Nitride)의 경우 열적/구조적 안정성으로 인해 융착 시 계면에서 화학적 결합이 어려워, 지립이 단일층으로 형성되어야 하는 융착 공구의 경우 적용되질 못하고 있다. 이러한 문제를 해결하기 위해 세라믹과의 젖음성이 우수한 Ti 성분이 포함된 67Ag+28Cu+5Ti(wt.%) 조성의 합금분말을 이용하여 cBN을 접합을 하였으며, 이때 융착조건은 진공 분위기($6{\times}10^{-6}$Torr), $900^{\circ}C$ 온도에서 5분간 유지하여 융착을 실시하였다. 본 연구의 주목적은 Ti 합금화 된 Ag계 합금분말 및 cBN의 융착 계면에서의 융착 계면거동해석을 통한 건전한 접합공정을 찾는데 있다. 이에 온도 $900^{\circ}C$, 유지시간 5분에서 건전한 융착층을 형성함을 알 수 있었다. 또한 결합력 측정기를 이용하여 결합력을 측정한 결과 diamond와 융착하였을 때가 123N, cBN을 융착하였을 때 107N으로써, cBN 융착이 diamond 융착의 87%정도의 결합력을 보임을 알 수 있었다. 한편 cBN과 Ag-Cu-Ti계 브레이징 필러의 계면에서의 미세조직 및 화학반응의 메커니즘은 SEM, EDS를 이용하여 분석하였다.

• Journal of the Korean institute of surface engineering
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• v.32 no.3
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• pp.351-355
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• 1999

BN films with a high content of cubic phase has been deposited by a variety of techniques. It is well known that c-BN films grow with a unique microstructure consisting of $sp^2$ and $sp^{3-}$ bonded layers. Because of existence of the initially grown $sp^{2-}$ /bonded layer, BN films are not adhesive to the substrates. In this study, post-N$^{+ }$ / implantation was applied to improve the adhesion of the films. A Monte Carlo program TAMIX was used to simulate this modification process. The simulation showed nitrogen concentration profile at $1200\AA$ in depth in case of 50keV -implantation energy. FTIR spectra of the $N^{+}$ implanted specimens demonstrated a strong change of absorption band at 1380 cm$^{ -1 }$The films were also investigated by HRTEM. From these results, it is concluded that the post ion implantation could be an effective technique which improves the adhesion between BN film and substrate.

• Journal of the Korean institute of surface engineering
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• v.41 no.2
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• pp.43-47
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• 2008

Cubic boron nitride(c-BN) films were deposited on tungsten carbide insert tool by microwave plasma enhanced chemical vapor deposition(MPECVD) from a gas mixture of triethyl borate$(B(C_2H_5O)_3)$, ammonia $(NH_3)$, hydrogen$(H_2)$ and argon(Ar). The qualities of deposited thin film were investigated by x-ray diffrac-tion(XRD), field emission scanning electron microscopy(FE-SEM) and micro Raman spectroscope. The surface morphologies of the synthesised BN as well as crystallinity appear to be highly dependent on the flow rate of $B(C_2H_5O)_3$ and $(NH_3)$ gases. The deposited film had more crystallized phases with 5 scem of $B(C_2H_5O)_3$ and $(NH_3)$ gases than with 2 sccm, and the phase was identified as c-BN by micro Raman spectroscope and XRD. The adhesion strength were also increased with increasing flow rates of $B(C_2H_5O)_3$ and $(NH_3)$ gases.

• Korean Journal of Materials Research
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• v.20 no.4
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• pp.194-198
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• 2010

Cubic boron nitride (c-BN) is a promising material for use in many potential applications because of its outstanding physical properties such as high thermal stability, high abrasive wear resistance, and super hardness. Even though 316L austenitic stainless steel (STS) has poor wear resistance causing it to be toxic in the body due to wear and material chips, 316L STS has been used for implant biomaterials in orthopedics due to its good corrosion resistance and mechanical properties. Therefore, in the present study, c-BN films with a $B_4C$ layer were applied to a 316L STS specimen in order to improve its wear resistance. The deposition of the c-BN films was performed using an r.f. (13.56 MHz) magnetron sputtering system with a $B_4C$ target. The coating layers were characterized using XPS and SEM, and the mechanical properties were investigated using a nanoindenter. The friction coefficient of the c-BN coated 316L STS steel was obtained using a pin-on-disk according to the ASTM G163-99. The thickness of the obtained c-BN and $B_4C$ were about 220 nm and 630 nm, respectively. The high resolution XPS spectra analysis of B1s and N1s revealed that the c-BN film was mainly composed of $sp^3$ BN bonds. The hardness and elastic modulus of the c-BN measured by the nanoindenter were 46.8 GPa and 345.7 GPa, respectively. The friction coefficient of the c-BN coated 316L STS was decreased from 3.5 to 1.6. The wear property of the c-BN coated 316L STS was enhanced by a factor of two.

• Proceedings of the Korean Vacuum Society Conference
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• 2000.02a
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• pp.124-124
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• 2000

다이아몬드에 버금가는 높은 경도뿐만 아니라 높은 화학적 안정성 및 열전도성 등 우수한 물리화학적 특성을 가진 입방정 질화붕소(cubic boron nitride)는 마찰.마모, 전자, 광학 등의 여러 분야에서의 산업적 응용이 크게 기대되는 재료이다. 특히 탄화물형성원소에 대해 안정하여 철계금속의 가공을 위한 공구재료로의 응용 또한 크게 기대된다. 이 때문에 각종의 PVD, CVD 공정을 이용하여 c-BN 박막의 합성에 대한 연구가 광범위하게 진행되어 많은 성공사례들이 보고되고 있다. 그러나 c-BN 박막의 유용성에도 불구하고 아직 실제적인 응용이 이루어지지 못한 것은 c-BN 박막의 증착직후 급격한 박리현상 때문이다. 본 연구에서는 평행자기장을 부가한 ME-ARE(Magnetically Enhanced Activated Reactive Evaporation)법을 이용한 c-BN 박막의 합성에서 적용한 증착공정 인자들의 변화에 따른 박리특성 고찰과 함께 다층박막화 및 제 3원소 혼입 방법을 적용하여 박리특성 향상 정도를 조사하였다. BN 박막합성은 전자총에 의해 증발된 보론과 (질소+아르곤) 플라즈마의 활성화반응증착(Activated Reactive Evaporation)에 의해 이루어졌다. 기존의 ARE 장치와 달리 열음극(got cathode)과 양극(anode) 사이에 평행자기장을 부가하여 플라즈마의 증대시켜 반응효율을 높였다. 합성실험용 모재로는 p-type으로 도핑된 (100) Si웨이퍼를 30$\times$40mmzmrl로 절단 후, 10%로 희석된 완충불산용액에 10분간 침적하여 표면의 산화층을 제거한 후 사용하였다. 박막실험실에서의 주요공정변수는 기판바이어스 전압, discharge 전류, Ar/N2가스유량비이었다. 합성된 박막의 결정성 분석을 FTIR을 이용하였으며, BN 박막의상 및 미세구조관찰을 위해 투과전자현미경(TEM;Philips EM400T) 분석을 병행하였고, 박막의 기계적 물성 평가를 위해 미소경도를 측정하였다. 박리특성의 고찰은 대기중에서의 자발적 박리가 일어나 90%이상의 박리가 진행된 시점까지의 시간을 측정하였고, 증착직후 박막의 잔류응력 변화와 연관하여 고찰해 보았다.