硼掺杂金刚石薄膜涂层工具的制备和试验研究
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摘要
金刚石薄膜优良的力学性能使其在工模具和耐磨器件等领域具有广阔的应用前景。然而,由于硬质合金工具中粘接相钴的催石墨化作用,使得金刚石薄膜与硬质合金基体之间的附着力较低,从而阻碍了金刚石薄膜涂层工具的产业化应用。p型金刚石的研究表明在金刚石薄膜的生长过程中进行硼掺杂具有细化金刚石薄膜晶粒、降低薄膜内应力、提高薄膜质量等特点,这对于硼掺杂金刚石薄膜涂层技术在工具方面的应用和发展具有重要的意义。
本文采用偏压增强热丝化学气相沉积法,以丙酮和氢气为原料,以硼酸三甲酯为掺杂源,在高电阻单晶硅片、硬质合金刀具以及硬质合金铜管拉拔模具上分别制备了硼掺杂金刚石薄膜涂层,研究了硼掺杂金刚石薄膜的制备原理、工艺方法及影响因素等。通过采用扫描电子显微镜(SEM)、拉曼光谱(Raman)、X射线衍射(XRD)等不同的表征方法对硼掺杂金刚石薄膜的形貌、结构及质量等进行了详细的研究和分析,通过对难加工材料的切削和钻削加工试验以及对铜管的拉拔生产应用评价了硼掺杂金刚石薄膜涂层刀具及模具的实际使用效果。
研究结果表明:①硼掺杂金刚石膜的制备原理及其相应的晶体生长规律与常规金刚石膜的规律基本相同,可用非平衡热力学耦合模型进行解释。②圆形高阻单晶硅片上制备的硼掺杂金刚石薄膜内存在一定的拉应力,且随硼掺杂浓度的不同而发生变化,晶粒尺寸和薄膜电阻随着硼掺杂浓度的增加而减小。③在带有断屑槽的硬质合金刀片SCMT120408-HM上通过两步法预处理后制备的硼掺杂金刚石薄膜涂层表明两步法预处理可以较好的粗化基体表面,适量的硼掺杂可以提高金刚石的形核密度,并在刀具基体表面生成稳定的硼-钴化合物层,有效抑制钴的催石墨化作用;硼掺杂金刚石的晶粒取向主要为{111}晶面,随着硼掺杂浓度的增加晶粒尺寸减小,且拉曼光谱的中心声子线向低能方向漂移;硼掺杂浓度在3000ppm时金刚石涂层刀具的膜-基附着强度最大,刀具的切削性能最好。④在整体式WC-Co(YG8)硬质合金钻头上在沉积的金刚石薄膜涂层比较均匀,由于硼元素对涂层晶粒的细化和对膜-基附着力的改善,使得硼掺杂金刚石涂层比常规金刚石涂层的质量更均匀,硼掺杂金刚石薄膜涂层钻头具有更好的加工性能。⑤在大孔径铜管拉拔模具内孔上不同位置处沉积的硼掺杂金刚石薄膜涂层表面平整、颗粒细小、厚度均匀一致,薄膜颗粒尺寸在2~5μm之间,硼掺杂金刚石薄膜涂层拉拔模具的实际生产应用效果较好,可以延长模具寿命、节约原材料、提高拉制铜管的质量和生产效率。
The application of diamond coated film to tools, dies and wear-resistant apparatus material have been attracting great interest for the outstanding mechanical characteristics of diamond. However, the adhesive strength of diamond coating and substrate is very poor, which is primarily due to the large mismatch of thermal expansion coefficient and the cobalt-catalyzed formation of non-diamond carbon at the diamond-carbide interface, has restrained the successful development and commercialization of diamond-coated tools. The research of p-type diamond has indicated the incorporation of boron into the diamond coating in the process of diamond deposition is a dynamic boron doping technique, which can decrease the grains sizes, reduce internal stress and improve quality of diamond thin film. It is of great significance for the application and development of boron-doped diamond coating.
In the present paper, boron-doped diamond coatings were deposited on silicon wafers, cemented carbide tools and cemented carbide drawing dies by bias-enhanced hot filament chemical vapor deposition. The trimethyl borate (B(OCH3)3) dissolved in acetone solution was used as the boron resource, the gas mixture of hydrogen and acetone were used as reaction gases. The deposited mechanism, process and influencing factors of boron-doped diamond coatings were studied. The surface morphology and quality of boron doped diamond coatings were studied and analyzed carefully by Scanning electron microscopy (SEM), Raman spectra (Raman) and X-ray diffraction (XRD), etc.. Furthermore, the cutting performance of the boron-doped diamond coated inserts and drills were studied by cutting tests of composite materials, the machining effect of boron-doped diamond coated drawing dies were tested by practical drawing brass tubes.
The research results indicated:①The deposited mechanism and growth law of boron-doped diamond coatings are similar with conventional diamond coatings, which can be interpreted by the non-equilibrium thermodynamics model.②The diamond thin film deposited on round silicon wafers existed internal stress, the grains size and resistance of diamond films decreased as the boron concentration increased.③Diamond films doped with different boron concentrations grown on WC-Co cemented carbide inserts (SCMT120408-HM) showed the two-step pretreatment method could improve mechanical interlocking effect and adhesion between diamond coating and WC-Co substrate effectively. Diamond nucleation density increased as the boron doping concentration was moderate. Meanwhile, the stable cobalt boride compounds were produced on the substrate surface in the process of nucleation, which suppressed outward diffusion of cobalt, reduced the catalytic effect of cobalt. Surface morphology analysis showed a great decrease of grain size as a function of boron concentration increase. Raman spectra of diamond coatings showed that the diamond peaks decreased and downshifted to lower energy as the boron concentration increased. Turning tests displayed that the cutting performance of boron-doped diamond coated inserts have been greatly improved when the boron doping concentration was 3000ppm.④Diamond coatings deposited on conventional cemented carbides YG8(Co 8%) drills showed the grains were faceted with uniform texture. The boron doping decreased the grains size and improved the quality of diamond film, so the machining performance of boron-doped diamond coated drill was better than that of conventional diamond coated drill.⑤The diamond coatings deposited on the inner holes shape of the drawing dies had small surface roughness, uniform thickness and excellent adhesive strength. The films surface was even and the average grain size was 2-5μm. The practical drawing brass tubes test demonstrated the boron-doped diamond coated drawing dies had excellent machining performance, which can prolonged the dies lifetime, saved resource materials, improved the quality of drawing brass tubes and increased production efficiency.
本文采用偏压增强热丝化学气相沉积法,以丙酮和氢气为原料,以硼酸三甲酯为掺杂源,在高电阻单晶硅片、硬质合金刀具以及硬质合金铜管拉拔模具上分别制备了硼掺杂金刚石薄膜涂层,研究了硼掺杂金刚石薄膜的制备原理、工艺方法及影响因素等。通过采用扫描电子显微镜(SEM)、拉曼光谱(Raman)、X射线衍射(XRD)等不同的表征方法对硼掺杂金刚石薄膜的形貌、结构及质量等进行了详细的研究和分析,通过对难加工材料的切削和钻削加工试验以及对铜管的拉拔生产应用评价了硼掺杂金刚石薄膜涂层刀具及模具的实际使用效果。
研究结果表明:①硼掺杂金刚石膜的制备原理及其相应的晶体生长规律与常规金刚石膜的规律基本相同,可用非平衡热力学耦合模型进行解释。②圆形高阻单晶硅片上制备的硼掺杂金刚石薄膜内存在一定的拉应力,且随硼掺杂浓度的不同而发生变化,晶粒尺寸和薄膜电阻随着硼掺杂浓度的增加而减小。③在带有断屑槽的硬质合金刀片SCMT120408-HM上通过两步法预处理后制备的硼掺杂金刚石薄膜涂层表明两步法预处理可以较好的粗化基体表面,适量的硼掺杂可以提高金刚石的形核密度,并在刀具基体表面生成稳定的硼-钴化合物层,有效抑制钴的催石墨化作用;硼掺杂金刚石的晶粒取向主要为{111}晶面,随着硼掺杂浓度的增加晶粒尺寸减小,且拉曼光谱的中心声子线向低能方向漂移;硼掺杂浓度在3000ppm时金刚石涂层刀具的膜-基附着强度最大,刀具的切削性能最好。④在整体式WC-Co(YG8)硬质合金钻头上在沉积的金刚石薄膜涂层比较均匀,由于硼元素对涂层晶粒的细化和对膜-基附着力的改善,使得硼掺杂金刚石涂层比常规金刚石涂层的质量更均匀,硼掺杂金刚石薄膜涂层钻头具有更好的加工性能。⑤在大孔径铜管拉拔模具内孔上不同位置处沉积的硼掺杂金刚石薄膜涂层表面平整、颗粒细小、厚度均匀一致,薄膜颗粒尺寸在2~5μm之间,硼掺杂金刚石薄膜涂层拉拔模具的实际生产应用效果较好,可以延长模具寿命、节约原材料、提高拉制铜管的质量和生产效率。
The application of diamond coated film to tools, dies and wear-resistant apparatus material have been attracting great interest for the outstanding mechanical characteristics of diamond. However, the adhesive strength of diamond coating and substrate is very poor, which is primarily due to the large mismatch of thermal expansion coefficient and the cobalt-catalyzed formation of non-diamond carbon at the diamond-carbide interface, has restrained the successful development and commercialization of diamond-coated tools. The research of p-type diamond has indicated the incorporation of boron into the diamond coating in the process of diamond deposition is a dynamic boron doping technique, which can decrease the grains sizes, reduce internal stress and improve quality of diamond thin film. It is of great significance for the application and development of boron-doped diamond coating.
In the present paper, boron-doped diamond coatings were deposited on silicon wafers, cemented carbide tools and cemented carbide drawing dies by bias-enhanced hot filament chemical vapor deposition. The trimethyl borate (B(OCH3)3) dissolved in acetone solution was used as the boron resource, the gas mixture of hydrogen and acetone were used as reaction gases. The deposited mechanism, process and influencing factors of boron-doped diamond coatings were studied. The surface morphology and quality of boron doped diamond coatings were studied and analyzed carefully by Scanning electron microscopy (SEM), Raman spectra (Raman) and X-ray diffraction (XRD), etc.. Furthermore, the cutting performance of the boron-doped diamond coated inserts and drills were studied by cutting tests of composite materials, the machining effect of boron-doped diamond coated drawing dies were tested by practical drawing brass tubes.
The research results indicated:①The deposited mechanism and growth law of boron-doped diamond coatings are similar with conventional diamond coatings, which can be interpreted by the non-equilibrium thermodynamics model.②The diamond thin film deposited on round silicon wafers existed internal stress, the grains size and resistance of diamond films decreased as the boron concentration increased.③Diamond films doped with different boron concentrations grown on WC-Co cemented carbide inserts (SCMT120408-HM) showed the two-step pretreatment method could improve mechanical interlocking effect and adhesion between diamond coating and WC-Co substrate effectively. Diamond nucleation density increased as the boron doping concentration was moderate. Meanwhile, the stable cobalt boride compounds were produced on the substrate surface in the process of nucleation, which suppressed outward diffusion of cobalt, reduced the catalytic effect of cobalt. Surface morphology analysis showed a great decrease of grain size as a function of boron concentration increase. Raman spectra of diamond coatings showed that the diamond peaks decreased and downshifted to lower energy as the boron concentration increased. Turning tests displayed that the cutting performance of boron-doped diamond coated inserts have been greatly improved when the boron doping concentration was 3000ppm.④Diamond coatings deposited on conventional cemented carbides YG8(Co 8%) drills showed the grains were faceted with uniform texture. The boron doping decreased the grains size and improved the quality of diamond film, so the machining performance of boron-doped diamond coated drill was better than that of conventional diamond coated drill.⑤The diamond coatings deposited on the inner holes shape of the drawing dies had small surface roughness, uniform thickness and excellent adhesive strength. The films surface was even and the average grain size was 2-5μm. The practical drawing brass tubes test demonstrated the boron-doped diamond coated drawing dies had excellent machining performance, which can prolonged the dies lifetime, saved resource materials, improved the quality of drawing brass tubes and increased production efficiency.
引文
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