利用化学和机械协同作用的CVD金刚石抛光机理与技术
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摘要
金刚石是集多种优越的物理、化学、光学和热学性能于一身的材料极品。它不但是自然界已知材料中硬度最大、摩擦系数最小、导热性能最好的材料,而且具有优良的电绝缘性、较宽的透光波段、优秀的半导体特性和化学惰性,被视为21世纪最有发展前途的工程材料,具有广泛的应用前景和巨大的市场潜力。化学气相沉积(CVD)金刚石的出现打破了天然金刚石数量稀少、尺寸过小及价格昂贵等限制,使金刚石的应用不再局限于传统的刀具和模具领域,逐渐向光学、热学、电子半导体及声学等高科技领域发展。然而由于其生长机制的限制,CVD金刚石晶粒粗大,表面粗糙度和精度较差,无法满足上述领域对金刚石超光滑、高精度和低损伤的表面质量要求。平坦化技术已经成为CVD金刚石应用于高新技术领域的关键技术之一。
金刚石的高硬度和良好化学稳定性给目前常用的加工技术带来了挑战。机械抛光加工效率极低,容易引入裂纹和划痕等损伤；化学作用较强的激光抛光、电火花加工和化学刻蚀等方法会遇到加工表面质量较差、残留有变质层等问题。借助化学和机械的协同作用去除金刚石材料将为CVD金刚石的高效、超精密和低损伤抛光提供新思路。为此,探索化学和机械协同作用下金刚石的微观去除机理,研究化学机械协同作用抛光的相关技术是实现CVD金刚石平坦化的关键。
本文从化学热力学和化学动力学理论入手,研究化学和机械协同作用去除金刚石材料的相关理论,分别采用摩擦化学抛光技术和化学机械抛光技术为粗、精加工技术实现CVD金刚石高效、超精密、低损伤的抛光。主要的研究工作如下：
(1)通过化学反应热力学和化学动力学分析,论证过渡金属催化金刚石向石墨转化的可行性,揭示金刚石向石墨转化的金属催化机制,提出摩擦化学抛光盘材料应具备未配对电子、垂直对准原则、高温硬度和高温抗氧化性等基本条件；研究化学和机械协同作用下金刚石氧化的化学动力学理论,建立化学机械抛光金刚石的化学动力学模型。揭示金刚石的表面结构、机械摩擦引入的晶格畸变和氧化剂的氧化性是金刚石氧化的驱动力。
(2)根据摩擦化学抛光盘的材料要求,采用机械合金化结合真空热压烧结技术制备FeNiCr合金基抛光盘。表征FeNiCr合金基抛光盘材料的硬度、抗氧化性能及抛光性能。结果表明：FeNiCr合金基抛光盘材料的硬度和高温抗氧化性能均优于304不锈钢和高速钢。抛光时材料去除率达到3.7μm/min,远高于TiAl合金基、304不锈钢和高速钢三种抛光盘的抛光效率。根据理论分析和试验研究,摩擦化学抛光机理是,金刚石在摩擦热和金属催化作用下先转化为石墨,然后以机械、扩散或氧化的形式去除。
(3)研制高效稳定的抛光液是化学机械抛光CVD金刚石的前提。根据理论分析和试验研究,在K2FeO4、KMnO4、Na2MoO4、K2Cr2O7、CrO3、KIO4、H2O2、(NH4)2S2O8等八种氧化剂中,K2FeO4抛光效果最好。另外,最佳磨料为粒径2μm的碳化硼磨料,最佳抛光盘为玻璃盘。在此基础上,分析高铁酸钾抛光液的氧化性、物理和化学稳定性,通过实验确定较佳的氧化剂浓度、磷酸浓度和催化剂分别为15g/100ml水、4-7.5ml/100ml水和粒径30nm的催化剂T粉末。采用X射线衍射、拉曼光谱及XPS光电子能谱分析研究抛光后CVD金刚石的表面成分,揭示化学机械抛光CVD金刚石的材料去除机理。结果表明,抛光后金刚石表面存在C-C、C-OH、C-O-C、C=O和O=C-OH等多种形式官能团。化学机械抛光CVD金刚石的材料去除机理是：高铁酸钾在酸性条件下将水氧化为自由基氧,自由基氧吸附在CVD金刚石和固体催化剂表面,逐步氧化金刚石表面碳原子。磨粒的机械划擦作用使金刚石产生一层厚度约为2nm畸变层,保证化学反应的持续进行。
(4)搭建局部加热式化学机械抛光试验台和小尺寸晶片摩擦力在线测量装置,研究化学机械抛光温度、压力、抛光盘转速、氧化剂浓度对材料去除率及摩擦力的影响规律。根据理论分析和试验研究,合理的摩擦化学抛光工艺为：抛光压力为6.5Mpa,抛光盘转速为11000r/min:合理的化学机械抛光工艺为：抛光压力为266.7kPa,抛光盘转速为70r/min,抛光头转速为23r/min,抛光温度为50℃。化学机械抛光CVD金刚石的摩擦系数在0.060～0.065范围内变化,为混合摩擦状态。采用优化的抛光工艺抛光后,CVD金刚石表面粗糙度可达到Ra0.187nm,表面没有划痕和损伤。
Diamond possesses excellent physical, thermal, optical and chemical properties, such as highest hardness, good chemical inertness, high thermal conductivity, high elasticity modulus, large electrical resistance, wide electronic gap, wide-range transparency and low friction coefficient. As a21st century engineering material, it has many promising applications and potential markets. The debut of CVD (Chemical vapor deposition) diamond will break through the limitations of rare, expensive and small size natural diamond, and greatly expands the application field of diamond from the traditional tool, mold to the fields of optical, thermal, electronic semiconductors, acoustics, and so on. However, the columnar growth of CVD diamond results in a polycrystalline nature and the grain sizes increase with film thickness. Therefore, if CVD diamonds are to be used in these fields, it is extremely important for their surfaces to be precisely machined and highly polished.
The extreme hardness and good chemical inertness of a CVD diamond bring a great challenge to its polishing methods:The traditional mechanical polishing method yields extremely low polishing rate and may cause micro scratches on the polished surface. Other methods including laser polishing, electrical discharge machining and chemical etching may introduce markable damage layer to diamond surface. Nevertheless, Chemical and mechanical polishing is expected to provide new ideas in planarizing CVD diamonds with untrapresicion and damage-free surface. It is necessary to investigate the mechanical removal mechanism and develop a chemically assisted mechanical polishing and planarization technique for CVD diamonds.
Base on the theory of chemical thermodynamics and kinetics, this study focues on polishing CVD diamonds with tribochemical polishing (TCP) method and chemical and mechanical polishing (CMP) method by investigating material removal mechanism involved in the two methods. Main contents and results are as follows:
(1) According to the analysis of chemical thermodynamics and kinetics, diamond could convert into graphite with the catalysis of transition metals. Based on this analysis, the study investigates the catalytic mechanisms of TCP and dentifies four requirements for the polishing plate, i.e. unpaired d electrons, vertical alignment rule, high hardness and oxidation resistance at elevated temperature. Based on the thermokinetic analysis of diamond oxidation, the study proposes a chemical thermokinetic model and predicts that mechanical scratching, surface energy and strong oxidizing reaction are responsible for material removal in the CMP process of diamond polishing.
(2) Based on the requirements for TCP process, an FeNiCr alloy polishing plate is designed and prepared by using the mechanical alloying and hot-press sintering techniques. The FeNiCr alloy polishing plate has higher hardness and oxidation resistance than stainless steel304and high-speed steel. It provides a material removal rate of3.7μm/min in CVD diamond polishing, which is higher than that of stainless steel304plate, high-speed steel plate and TiAl alloy plate. The study futher interprets the material removal mechanism in the TCP process as diamond first converts into graphite and other non-diamond carbons under the heating and the catalytic actions of the transition metal, then the graphite and non-diamond carbons are then removed by mechanical friction, oxidation and diffusion into the polishing plate.
(3)Slurry preparation is necessary for the CMP process. According to the standard electrode potentials of common oxidants, eight oxidants including K2FeO4、KMnO4、 Na2MoO4、K2Cr2O7、CrO3、KIO4、H2O2、(NH4)2S2O8are chosen to prepare CMP slurries. Theoretical analysis and experimental results show that K2Fe04is the best oxidant, and2μm boron carbide abrasive and glass plate are the best abrasive and polishing plate, respectively. The physical and chemical stability and oxidability of the slurries are also investigated. The study identifies that K2FeO4and phosphoric acid have their ideal concentrations of15g/100ml and7.5ml/100ml, respectively. Catalyst T shows the best catalytic effect in the CMP process. X-ray diffraction spectroscopy, Raman spectroscopy, and X-ray photoelectron spectroscopy are used to analyze the surface chemical composition of CVD diamonds and investigate the mechanisms of material removal. The results shows that the "C-O","C-OH","C-O-C","C=O" and "O=C-OH" groups form on diamond surface. The study illustrates the step by step carbon oxidation process as:radical oxygen is formed as a result of potassium ferrate decomposition in the acid solution, and then oxidizes carbon by adsorbing onto the surface of diamond and solid catalyst. The mechanical scratching action of an abrasive produces a damage layer with a thickness of about2nm to promote the oxidation process of the diamond carbon.
(4) In order to study the influences of temperature, polishing pressure, the rotational speed of polishing head and the concentration of oxidant on material removal rate and friction, a local heating device and a friction measurement device are designed and fabricated for the CMP processes. The study finds that an ideal polishing pressure of6.5MPa and rotational speeds of polishing plate of11000r/min in TCP process, and an ideal polishing pressure of266.7kPa, polishing temperature of50℃, rotational speeds of polishing plate and head of 70r/min and23r/min in CMP process, respectively, with the coefficient of friction in the range of0.060～0.065. With the utilization of the polishing process, CVD diamonds are polished with surface roughness of0.187nm with no surface scratches nor damages.
金刚石的高硬度和良好化学稳定性给目前常用的加工技术带来了挑战。机械抛光加工效率极低,容易引入裂纹和划痕等损伤；化学作用较强的激光抛光、电火花加工和化学刻蚀等方法会遇到加工表面质量较差、残留有变质层等问题。借助化学和机械的协同作用去除金刚石材料将为CVD金刚石的高效、超精密和低损伤抛光提供新思路。为此,探索化学和机械协同作用下金刚石的微观去除机理,研究化学机械协同作用抛光的相关技术是实现CVD金刚石平坦化的关键。
本文从化学热力学和化学动力学理论入手,研究化学和机械协同作用去除金刚石材料的相关理论,分别采用摩擦化学抛光技术和化学机械抛光技术为粗、精加工技术实现CVD金刚石高效、超精密、低损伤的抛光。主要的研究工作如下：
(1)通过化学反应热力学和化学动力学分析,论证过渡金属催化金刚石向石墨转化的可行性,揭示金刚石向石墨转化的金属催化机制,提出摩擦化学抛光盘材料应具备未配对电子、垂直对准原则、高温硬度和高温抗氧化性等基本条件；研究化学和机械协同作用下金刚石氧化的化学动力学理论,建立化学机械抛光金刚石的化学动力学模型。揭示金刚石的表面结构、机械摩擦引入的晶格畸变和氧化剂的氧化性是金刚石氧化的驱动力。
(2)根据摩擦化学抛光盘的材料要求,采用机械合金化结合真空热压烧结技术制备FeNiCr合金基抛光盘。表征FeNiCr合金基抛光盘材料的硬度、抗氧化性能及抛光性能。结果表明：FeNiCr合金基抛光盘材料的硬度和高温抗氧化性能均优于304不锈钢和高速钢。抛光时材料去除率达到3.7μm/min,远高于TiAl合金基、304不锈钢和高速钢三种抛光盘的抛光效率。根据理论分析和试验研究,摩擦化学抛光机理是,金刚石在摩擦热和金属催化作用下先转化为石墨,然后以机械、扩散或氧化的形式去除。
(3)研制高效稳定的抛光液是化学机械抛光CVD金刚石的前提。根据理论分析和试验研究,在K2FeO4、KMnO4、Na2MoO4、K2Cr2O7、CrO3、KIO4、H2O2、(NH4)2S2O8等八种氧化剂中,K2FeO4抛光效果最好。另外,最佳磨料为粒径2μm的碳化硼磨料,最佳抛光盘为玻璃盘。在此基础上,分析高铁酸钾抛光液的氧化性、物理和化学稳定性,通过实验确定较佳的氧化剂浓度、磷酸浓度和催化剂分别为15g/100ml水、4-7.5ml/100ml水和粒径30nm的催化剂T粉末。采用X射线衍射、拉曼光谱及XPS光电子能谱分析研究抛光后CVD金刚石的表面成分,揭示化学机械抛光CVD金刚石的材料去除机理。结果表明,抛光后金刚石表面存在C-C、C-OH、C-O-C、C=O和O=C-OH等多种形式官能团。化学机械抛光CVD金刚石的材料去除机理是：高铁酸钾在酸性条件下将水氧化为自由基氧,自由基氧吸附在CVD金刚石和固体催化剂表面,逐步氧化金刚石表面碳原子。磨粒的机械划擦作用使金刚石产生一层厚度约为2nm畸变层,保证化学反应的持续进行。
(4)搭建局部加热式化学机械抛光试验台和小尺寸晶片摩擦力在线测量装置,研究化学机械抛光温度、压力、抛光盘转速、氧化剂浓度对材料去除率及摩擦力的影响规律。根据理论分析和试验研究,合理的摩擦化学抛光工艺为：抛光压力为6.5Mpa,抛光盘转速为11000r/min:合理的化学机械抛光工艺为：抛光压力为266.7kPa,抛光盘转速为70r/min,抛光头转速为23r/min,抛光温度为50℃。化学机械抛光CVD金刚石的摩擦系数在0.060～0.065范围内变化,为混合摩擦状态。采用优化的抛光工艺抛光后,CVD金刚石表面粗糙度可达到Ra0.187nm,表面没有划痕和损伤。
Diamond possesses excellent physical, thermal, optical and chemical properties, such as highest hardness, good chemical inertness, high thermal conductivity, high elasticity modulus, large electrical resistance, wide electronic gap, wide-range transparency and low friction coefficient. As a21st century engineering material, it has many promising applications and potential markets. The debut of CVD (Chemical vapor deposition) diamond will break through the limitations of rare, expensive and small size natural diamond, and greatly expands the application field of diamond from the traditional tool, mold to the fields of optical, thermal, electronic semiconductors, acoustics, and so on. However, the columnar growth of CVD diamond results in a polycrystalline nature and the grain sizes increase with film thickness. Therefore, if CVD diamonds are to be used in these fields, it is extremely important for their surfaces to be precisely machined and highly polished.
The extreme hardness and good chemical inertness of a CVD diamond bring a great challenge to its polishing methods:The traditional mechanical polishing method yields extremely low polishing rate and may cause micro scratches on the polished surface. Other methods including laser polishing, electrical discharge machining and chemical etching may introduce markable damage layer to diamond surface. Nevertheless, Chemical and mechanical polishing is expected to provide new ideas in planarizing CVD diamonds with untrapresicion and damage-free surface. It is necessary to investigate the mechanical removal mechanism and develop a chemically assisted mechanical polishing and planarization technique for CVD diamonds.
Base on the theory of chemical thermodynamics and kinetics, this study focues on polishing CVD diamonds with tribochemical polishing (TCP) method and chemical and mechanical polishing (CMP) method by investigating material removal mechanism involved in the two methods. Main contents and results are as follows:
(1) According to the analysis of chemical thermodynamics and kinetics, diamond could convert into graphite with the catalysis of transition metals. Based on this analysis, the study investigates the catalytic mechanisms of TCP and dentifies four requirements for the polishing plate, i.e. unpaired d electrons, vertical alignment rule, high hardness and oxidation resistance at elevated temperature. Based on the thermokinetic analysis of diamond oxidation, the study proposes a chemical thermokinetic model and predicts that mechanical scratching, surface energy and strong oxidizing reaction are responsible for material removal in the CMP process of diamond polishing.
(2) Based on the requirements for TCP process, an FeNiCr alloy polishing plate is designed and prepared by using the mechanical alloying and hot-press sintering techniques. The FeNiCr alloy polishing plate has higher hardness and oxidation resistance than stainless steel304and high-speed steel. It provides a material removal rate of3.7μm/min in CVD diamond polishing, which is higher than that of stainless steel304plate, high-speed steel plate and TiAl alloy plate. The study futher interprets the material removal mechanism in the TCP process as diamond first converts into graphite and other non-diamond carbons under the heating and the catalytic actions of the transition metal, then the graphite and non-diamond carbons are then removed by mechanical friction, oxidation and diffusion into the polishing plate.
(3)Slurry preparation is necessary for the CMP process. According to the standard electrode potentials of common oxidants, eight oxidants including K2FeO4、KMnO4、 Na2MoO4、K2Cr2O7、CrO3、KIO4、H2O2、(NH4)2S2O8are chosen to prepare CMP slurries. Theoretical analysis and experimental results show that K2Fe04is the best oxidant, and2μm boron carbide abrasive and glass plate are the best abrasive and polishing plate, respectively. The physical and chemical stability and oxidability of the slurries are also investigated. The study identifies that K2FeO4and phosphoric acid have their ideal concentrations of15g/100ml and7.5ml/100ml, respectively. Catalyst T shows the best catalytic effect in the CMP process. X-ray diffraction spectroscopy, Raman spectroscopy, and X-ray photoelectron spectroscopy are used to analyze the surface chemical composition of CVD diamonds and investigate the mechanisms of material removal. The results shows that the "C-O","C-OH","C-O-C","C=O" and "O=C-OH" groups form on diamond surface. The study illustrates the step by step carbon oxidation process as:radical oxygen is formed as a result of potassium ferrate decomposition in the acid solution, and then oxidizes carbon by adsorbing onto the surface of diamond and solid catalyst. The mechanical scratching action of an abrasive produces a damage layer with a thickness of about2nm to promote the oxidation process of the diamond carbon.
(4) In order to study the influences of temperature, polishing pressure, the rotational speed of polishing head and the concentration of oxidant on material removal rate and friction, a local heating device and a friction measurement device are designed and fabricated for the CMP processes. The study finds that an ideal polishing pressure of6.5MPa and rotational speeds of polishing plate of11000r/min in TCP process, and an ideal polishing pressure of266.7kPa, polishing temperature of50℃, rotational speeds of polishing plate and head of 70r/min and23r/min in CMP process, respectively, with the coefficient of friction in the range of0.060～0.065. With the utilization of the polishing process, CVD diamonds are polished with surface roughness of0.187nm with no surface scratches nor damages.
引文
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