• 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.

• Journal of the Korean Vacuum Society
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• v.8 no.2
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• pp.158-158
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• 1999

The post ion implantation has been applied to modify early-grown BN layer and improve the adhesion of the BN films. The effect of ion implantation doses on microstructure and interlayer was investigated by FTIR and HRTEM. And the hardness and delamination life time of N+-implanted BN films were measured. With increasing the ion dose up to 5.0×1015atoms/㎠, the change of IR spectrum is observed. At 5.0×1016atoms/㎠, a drastic transition of cubic phase into hexagonal phase is detected. The change of microstructure of early-grown layers by ion implantation is confirmed using HRTEM. Both microhardness and delamination life time of BN films increase with ion dose. The modification model of early-grown BN layers is briefly discussed based on the displacement per atom and excess boron in the BN film induced by ion irradiation.

• 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.

• 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.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.

• Journal of the Korean Vacuum Society
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• v.8 no.1
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• pp.43-50
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• 1999

We have studied the alignment and the lattice quality of hexagonal rings of h-BN films synthesized by ion beam assisted deposition (IBAD) method. Boron was e-beam evaporated at 1.5 $\AA$/sec and nitrogen gas was ionized using end-hall type ion gun at 60, 80, and 100 eV, respectively. Substrate was either not heated or heated at 200, 400, 500, and $800^{\circ}C$, respectively. As nitrogen ion energy increases, c-axes of hexagonal rings tend to align parallel to the substrate, which is explained by larger compressive stress at higher ion energies. Alignment of c-axis increases with temperature and shows maximum around $400^{\circ}C$. The lattice quality of hexagonal rings improves with temperature. Such behaviors can be understood from two counter trends of increasing the atomic mobility and decreasing compressive stress with temperature. Hardness of h-BN films shows the same trend with the alignment of c-axis. Ion beam assisted deposition method seems to be effective for aligning hexagonal rings and optimizing h-BN properties.

• Proceedings of the Materials Research Society of Korea Conference
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• 1999.11a
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• pp.68-68
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• 1999

• 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 Vacuum Society Conference
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• 2007.02a
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• pp.146-146
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• 2007