The deposition of high-quality diamond films and their adhesion on cemented carbides are strongly influenced by the catalytic effect of cobalt under typical deposition conditions. Decreasing Co content on the surface...The deposition of high-quality diamond films and their adhesion on cemented carbides are strongly influenced by the catalytic effect of cobalt under typical deposition conditions. Decreasing Co content on the surface of the cemented carbide is often used for the diamond film deposition. But the leaching of Co from the WC-Co substrate leading to a mechanical weak surface often causes a poor adhesion. In this paper we adopted an implant copper layer prepared by vaporization to improve the mechanical properties of the Co-leached substrate. The diamond films were grown by microwave plasma chemical vapor deposition from CH4:H2 gas mixture. The cross section and the morphology of the diamond film were characterized by scanning electron microscopy (SEM). The non-diamond content in the film was analyzed by Raman spectroscopy. The effects of pretreatment on the concentrations of Co and Cu near the interfacial region were examined by energy dispersive spectrum (EDS) equipped with SEM. The adhesion of the diamond on the substrate was evaluated with a Rockwell-type hardness tester. The results indicate that the diamond films prepared with implant copper layer have a good adhesion to the cemented carbide substrate due to the recovery of the mechanical properties of the Co-depleted substrate after the copper implantation and the formation of less amorphous carbon between the substrate and the diamond film.展开更多
Plasma boronitriding has been successfully employed to overcome the difficulty in diamond growth on ferrous-based substrates. Commercial cobalt-sintered, tungsten-cemented carbides (WC(Co)) were pretreated by a plasma...Plasma boronitriding has been successfully employed to overcome the difficulty in diamond growth on ferrous-based substrates. Commercial cobalt-sintered, tungsten-cemented carbides (WC(Co)) were pretreated by a plasma boronitriding method, diamond was then deposited by microwave-enhanced chemical vapor deposition (MPCVD). The deposited films were characterized by scanning electron microscopy and Raman spectroscopy. Continuous diamond films with a sharp characteristic Raman peak of 1334 cm-1 were grown and adhered well on the boronitrided region of the cemented carbide substrates. On the other hand, a mixture of diamond crystallites, amorphous carbon and graphitic carbon was loosely deposited on the unboronitrided region. A cobalt inert thin layer formed after plasma boronitriding pretreatment enabled the subsequent nucleation and growth of a high-quality CVD diamond.展开更多
Chemically vapor deposited diamond films were etched at different parameters using oxygen plasma produced by a DC (direct current) glow discharge and then polished by a modified mechanical polishing device. Scanning...Chemically vapor deposited diamond films were etched at different parameters using oxygen plasma produced by a DC (direct current) glow discharge and then polished by a modified mechanical polishing device. Scanning electron microscope, atomic force microscope and Raman spectrometer were used to evaluate the surface states of diamond films before and after polishing. It was found that a moderate plasma etching would produce a lot of etch pits and amorphous carbon on the top surface of diamond film. As a result, the quality and the efficiency of mechanical polishing have been enhanced remarkably.展开更多
Diamond films were deposited on the WC-Co cemented carbide and Si3N4 ceramic cutting tool substrates by hot-filament-assisted chemical vapour deposition. The adherence property of diamond films was estimated using the...Diamond films were deposited on the WC-Co cemented carbide and Si3N4 ceramic cutting tool substrates by hot-filament-assisted chemical vapour deposition. The adherence property of diamond films was estimated using the critical load (Pcr) in the indentation test. The adhesive strength of diamond films is related to the intermediate layer between the film and the substrate. Poor adhesion of diamond films to polished cemented carbide substrate is owing to the formation of graphite phase in the interface. The adhesion of diamond films deposited on acid etched cemented carbide substrate is improved, and the peeling-off of the films often happens in the loosen layer of WC particles where the cobalt element is nearly removed. The diamond films' adhesion to cemented carbide substrate whose surface layer is decarbonizated is strengthened dramatically because WC phase forms by reaction between the deposited carbon and tungsten in the surface layer of substrates during the deposition of diamond, which results in chemical combination in the film-substrate interface. The adhesion of diamond films to silicon nitride substrate is the firmest due to the formation of chemical combination of the SiC intermediate layer in the interfaces. In the piston-turning application, the diamond-coated Si3N4 ceramic and the cemented carbide cutting tools usually fail in the form of collapsing of edge and cracking or flaking respectively. They have no built-up edge(BUE) as long as coating is intact.As it wears through, BUE develops and the cutting force on it increases 1 - 3 times than that prior to failure. This can predict the failure of diamond-coated cutting tools.展开更多
Hard, wear-resistant and well-adhesive titanium nitride coatings on cemented carbide cutting tools were prepared by the pulsed high energy density plasma technique at ambient temperature. The results of Auger spectra ...Hard, wear-resistant and well-adhesive titanium nitride coatings on cemented carbide cutting tools were prepared by the pulsed high energy density plasma technique at ambient temperature. The results of Auger spectra analysis indicated that the interface between the coating and substrate was more than 250 nm. Under optimized deposition conditions, the highest critical load measured by nanoscratch tester was more than 90 mN, which meant that the TiN film was well adhesive to the substrate; the highest nanohardness and Young抯 modulus according to nanoindentation tests were near to 27 and 450 GPa. The results of cutting tests evaluated by turning hardened CrWMn steel in industrial conditions indicated that the wear resistance and edge life of the cemented carbide tools were enhanced dramatically because of the deposition of titanium nitride coatings. These improvements were attributed to the three combined effects: the deposition and ion implantation of the pulsed plasma and the becoming finer of the grain sizes.展开更多
Morphologies and structures of diamond films synthesized on cobalt cemented tungsten carbide substrates using DC plasma jet CVD (direct current plasma jet chemical vapor deposition) method were investigated by means o...Morphologies and structures of diamond films synthesized on cobalt cemented tungsten carbide substrates using DC plasma jet CVD (direct current plasma jet chemical vapor deposition) method were investigated by means of SEM, XRD, TEM and Raman spectroscopy. The results show that the high thermal gradient and the high concentration gradient of chemical species within plasma jet have a larger influence on morphologies and quality of diamond films deposited. There are residual compressive stresses with GPa order of magnitude in diamond films, and micro-stresses are quite small. mosaic block sizes, being nanometer order of magnitude, decrease with the increasing of methane concentrations. Average values of dislocation density within diamond films, estimated from the magnitude of mosaic block sizes, are at least 10(10) cm(-2) order of magnitude. This result is also confirmed by calculated value from TEM observation of diamond films. It is shown that both the lattice distortion tested by XRD and FWHM value of diamond Raman peak measured from Raman spectrum have a similar trend of change with methane concentration comparing the results of XRD and Raman spectra.展开更多
采用偏压辅助增强热丝化学气相沉积法(Chemical vapor deposition,CVD),以WC-Co硬质合金为衬底,采用控制沉积参数和添加惰性气体Ar等CVD新工艺,制备性能优良的纳米金刚石薄膜。进一步采用扫描电镜(Scanning electron microscopy,SEM)、...采用偏压辅助增强热丝化学气相沉积法(Chemical vapor deposition,CVD),以WC-Co硬质合金为衬底,采用控制沉积参数和添加惰性气体Ar等CVD新工艺,制备性能优良的纳米金刚石薄膜。进一步采用扫描电镜(Scanning electron microscopy,SEM)、原子力显微镜(Atomic force microscopy,AFM)、拉曼光谱(Raman spectros- copy)、X射线衍射(X-ray diffraction,XRD)和高分辨率透射电镜(High-resolution transmission electron microscopy, HR-TEM)分析了薄膜的纳米效应。研究结果表明:纳米涂层仍然是以金刚石结构为主的多晶体,它晶体颗粒较小(20~80 nm),含有较多的晶界和sp^2结构,涂层表面粗糙度R_a≤50 nm,表面平整光滑,有利于研磨抛光。在此基础上,提出纳米金刚石复合涂层制备新技术,开发研制出各种涂层拉拔模具,在实际生产线上进行了应用,取得了显著的效果。展开更多
文摘The deposition of high-quality diamond films and their adhesion on cemented carbides are strongly influenced by the catalytic effect of cobalt under typical deposition conditions. Decreasing Co content on the surface of the cemented carbide is often used for the diamond film deposition. But the leaching of Co from the WC-Co substrate leading to a mechanical weak surface often causes a poor adhesion. In this paper we adopted an implant copper layer prepared by vaporization to improve the mechanical properties of the Co-leached substrate. The diamond films were grown by microwave plasma chemical vapor deposition from CH4:H2 gas mixture. The cross section and the morphology of the diamond film were characterized by scanning electron microscopy (SEM). The non-diamond content in the film was analyzed by Raman spectroscopy. The effects of pretreatment on the concentrations of Co and Cu near the interfacial region were examined by energy dispersive spectrum (EDS) equipped with SEM. The adhesion of the diamond on the substrate was evaluated with a Rockwell-type hardness tester. The results indicate that the diamond films prepared with implant copper layer have a good adhesion to the cemented carbide substrate due to the recovery of the mechanical properties of the Co-depleted substrate after the copper implantation and the formation of less amorphous carbon between the substrate and the diamond film.
文摘Plasma boronitriding has been successfully employed to overcome the difficulty in diamond growth on ferrous-based substrates. Commercial cobalt-sintered, tungsten-cemented carbides (WC(Co)) were pretreated by a plasma boronitriding method, diamond was then deposited by microwave-enhanced chemical vapor deposition (MPCVD). The deposited films were characterized by scanning electron microscopy and Raman spectroscopy. Continuous diamond films with a sharp characteristic Raman peak of 1334 cm-1 were grown and adhered well on the boronitrided region of the cemented carbide substrates. On the other hand, a mixture of diamond crystallites, amorphous carbon and graphitic carbon was loosely deposited on the unboronitrided region. A cobalt inert thin layer formed after plasma boronitriding pretreatment enabled the subsequent nucleation and growth of a high-quality CVD diamond.
基金National Natural Science Foundation of China(No.50572075)
文摘Chemically vapor deposited diamond films were etched at different parameters using oxygen plasma produced by a DC (direct current) glow discharge and then polished by a modified mechanical polishing device. Scanning electron microscope, atomic force microscope and Raman spectrometer were used to evaluate the surface states of diamond films before and after polishing. It was found that a moderate plasma etching would produce a lot of etch pits and amorphous carbon on the top surface of diamond film. As a result, the quality and the efficiency of mechanical polishing have been enhanced remarkably.
文摘Diamond films were deposited on the WC-Co cemented carbide and Si3N4 ceramic cutting tool substrates by hot-filament-assisted chemical vapour deposition. The adherence property of diamond films was estimated using the critical load (Pcr) in the indentation test. The adhesive strength of diamond films is related to the intermediate layer between the film and the substrate. Poor adhesion of diamond films to polished cemented carbide substrate is owing to the formation of graphite phase in the interface. The adhesion of diamond films deposited on acid etched cemented carbide substrate is improved, and the peeling-off of the films often happens in the loosen layer of WC particles where the cobalt element is nearly removed. The diamond films' adhesion to cemented carbide substrate whose surface layer is decarbonizated is strengthened dramatically because WC phase forms by reaction between the deposited carbon and tungsten in the surface layer of substrates during the deposition of diamond, which results in chemical combination in the film-substrate interface. The adhesion of diamond films to silicon nitride substrate is the firmest due to the formation of chemical combination of the SiC intermediate layer in the interfaces. In the piston-turning application, the diamond-coated Si3N4 ceramic and the cemented carbide cutting tools usually fail in the form of collapsing of edge and cracking or flaking respectively. They have no built-up edge(BUE) as long as coating is intact.As it wears through, BUE develops and the cutting force on it increases 1 - 3 times than that prior to failure. This can predict the failure of diamond-coated cutting tools.
文摘Hard, wear-resistant and well-adhesive titanium nitride coatings on cemented carbide cutting tools were prepared by the pulsed high energy density plasma technique at ambient temperature. The results of Auger spectra analysis indicated that the interface between the coating and substrate was more than 250 nm. Under optimized deposition conditions, the highest critical load measured by nanoscratch tester was more than 90 mN, which meant that the TiN film was well adhesive to the substrate; the highest nanohardness and Young抯 modulus according to nanoindentation tests were near to 27 and 450 GPa. The results of cutting tests evaluated by turning hardened CrWMn steel in industrial conditions indicated that the wear resistance and edge life of the cemented carbide tools were enhanced dramatically because of the deposition of titanium nitride coatings. These improvements were attributed to the three combined effects: the deposition and ion implantation of the pulsed plasma and the becoming finer of the grain sizes.
文摘Morphologies and structures of diamond films synthesized on cobalt cemented tungsten carbide substrates using DC plasma jet CVD (direct current plasma jet chemical vapor deposition) method were investigated by means of SEM, XRD, TEM and Raman spectroscopy. The results show that the high thermal gradient and the high concentration gradient of chemical species within plasma jet have a larger influence on morphologies and quality of diamond films deposited. There are residual compressive stresses with GPa order of magnitude in diamond films, and micro-stresses are quite small. mosaic block sizes, being nanometer order of magnitude, decrease with the increasing of methane concentrations. Average values of dislocation density within diamond films, estimated from the magnitude of mosaic block sizes, are at least 10(10) cm(-2) order of magnitude. This result is also confirmed by calculated value from TEM observation of diamond films. It is shown that both the lattice distortion tested by XRD and FWHM value of diamond Raman peak measured from Raman spectrum have a similar trend of change with methane concentration comparing the results of XRD and Raman spectra.