Ta_xMe_(1-x)N硬质薄膜及其DLC复合润滑薄膜的制备与性能研究
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摘要
目前军事上用于制备零部件的主要材料仍然是Cr12MoV等模具钢,但现代武器服役环境的不断复杂化以及制造业的快速发展对零部件提出了越来越高的要求,单一零部件已经不能适应复杂的环境,需要对其进行不同的表面处理。近年来,随着加工更加快速连续、加工材料更加复杂以及加工尺度更加微小的精细加工业的快速发展,硬质薄膜、涂层(低于10gm)等表面处理的研究及应用变得越来越普遍。经过表面处理后,零件强度、韧性以及耐磨损性能都得到了有效的提升。当前,对薄膜综合性能(高耐蚀、耐磨、自润滑)需求的提高导致传统的单一硬质薄膜越来越难以有效保护零件。因此,开发新型复合多层薄膜成为目前薄膜、涂层技术提高零部件综合防护的重要途径。
类金刚石(DLC)薄膜具有低摩擦系数、高硬度、高耐磨性的特点,可作为Cr12MoV表面改性的首选材料,但较低的热稳定性,以及与衬底的低结合强度制约了其应用。TaN薄膜作为硬质过渡金属氮化物在相关研究中展示了耐蚀性好、硬度及热稳定性高,摩擦系数低的特点,具有作为硬质耐磨薄膜及复合DLC承载层的研究前景。本论文旨在设计并获得与Cr12MoV衬底相匹配的TaxMe1-xN多层复合DLC润滑薄膜,提高薄膜的综合性能,达到钢基材料表面改性用硬质薄膜材料的要求。本文依照TaxMe1-xN单层→TaxMe1-xN多层→TaxMe1-xN多层复合DLC的顺序,采用全方位离子注入(Pill)、微波电子回旋共振等离子体(微波ECR)增强磁控溅射及化学气相沉积复合制备了DLC/TaxMe1-xN多层润滑薄膜。这种薄膜在磨损过程中产生白润化,提高了使用寿命。当外加载荷升高导致表层DLC失效后,薄膜体系承载层仍然能够保持较低的摩擦系数,以及较好耐磨性,防止了润滑层失效导致的摩擦副磨损加剧,达到了对Cr12MoV衬底耐磨润滑的改性要求。论文主要包括如下研究内容：
(1)首先在掌握反应室内等离子密度变化规律的基础上,采用微波ECR增强磁控溅射技术在Cr12MoV衬底上制备了几组TaN薄膜,重点研究了温度、气压、偏压对TaN薄膜结构与性能的影响,并且分析了相关影响因素对薄膜力学性能的影响机理。制备的TaN薄膜呈现六方结构,摩擦系数低于0.2。薄膜硬度随制备温度升高逐渐增加,573K时硬度达到最高值39.36GPa,但在低真空度热处理时出现氧化现象；TaN薄膜硬度与弹性模量随制备气压增加而降低,随脉冲偏压上升而增加,-100V时达到最高值,并随着偏压继续增加而降低。通过对不同影响因素分析发现,制备温度、气压、偏压影响了薄膜形核生长过程中离子结合能量以及膜基界面质量,导致薄膜性能的改变。在制备温度较低、气压0.1Pa、Ar/N2流量比4.5/1、脉冲偏压-100V时制备的TaN薄膜具有最佳的力学性能、耐磨性能。
(2)在TaN薄膜最佳制备工艺基础上添加过渡金属Me(Me=Ti、Cr)进行TaxMe1-xN复合制备,重点研究了掺杂量对TaxMe1-xN薄膜结构与性能的影响,分析讨论了复合第二相粒子对薄膜力学性能的影响机制。复合制备的TaxMe1-xN薄膜由TaN六方结构转变为三元固溶氮化物立方结构；当Ti/Ti+Ta、Cr/Cr+Ta分别达到0.43、0.61时,薄膜力学性能分别达到最佳值,其中Ta0.57Ti0.43N薄膜硬度为33±2GPa,结合强度为27N；Ta0.39Cr0.61N薄膜硬度为30±1.5GPa,结合强度为29N；薄膜摩擦系数随Ti、Cr掺杂量增加上升,最高值接近0.4。通过分析发现,适当比例的掺杂Ti、Cr有利于TaxMe1-xN薄膜形核以及晶粒尺寸降低,进而产生固溶、细晶强化作用。
(3)在TaN及TaxMe1-xN薄膜最佳制备工艺的基础上进行了TaN/Ta、TaxMe1-xN/Me、 TaxMe1-xN/MeN/Me多层薄膜的制备,并对软硬多层薄膜提高结合强度机理进行了分析。制备的TaN/Ta薄膜在调制厚度为250nm时达到最佳力学性能,硬度为26-27GPa,结合强度为36N,耐磨性显著上升；TaxMe1-xN/Me、TaxMe1-xN/MeN/Me多层薄膜与单层TaxMe1-xN薄膜相比,耐磨性能及膜基结合强度显著得到提升,结合强度高于50N。通过分析发现,适当的调制周期下,软硬多层结构有效的缓解了薄膜应力,同时界面增加阻止了脆性层裂纹扩展,从而改善了薄膜耐磨性、结合强度。
(4)分析了衬底轰击、注入对TaN薄膜性能的影响,并首次采用全方位离子注入与微波ECR增强磁控溅射相结合的方式了制备了多层界面注入TaN/Ta薄膜。高能Ar+离子轰击衬底形成均匀的山峰状结构,沉积TaN薄膜后表面均匀性、致密性明显改善,膜基结合强度达到30N以上；采用-16kV偏压在衬底上注入Ta、TaN过渡层后,TaN薄膜的结合强度提高到36N以上；多层界面注入Ta的TaN/Ta多层薄膜,膜基结合强度达到55N以上。通过分析发现高能Ar+离子轰击衬底增加了衬底表面积,增大了界面剪切抗力；注入形成非晶扩散区,有效的改善界面质量,降低了界面能；多层界面注入形成多个非晶扩散区,并保持了软硬多层薄膜结构中韧性层降低应力,提供剪切带的特性,有效的改善了膜基结合强度。
(5)采用微波ECR化学气相沉积与磁控溅射相结合的方式分别制备了DLC薄膜,DLC润滑膜,并对润滑机理进行了分析。采用掺杂MoS2、Ti制备的DLC润滑薄膜非晶网络中弥散了大量的MoS2润滑相,有效的降低了DLC薄膜的摩擦系数,当C靶电流1.5A,MoS2靶电流0.3A时,薄膜摩擦系数达到最小值0.074,硬度为14GPa。通过分析发现弥散在DLC非晶网络中的MOS2司滑相对薄膜力学性能及摩擦系数有较大影响,通过改变溅射能量及制备偏压调控薄膜沉积过程中C-C、C-H、S-H结合可以有效控制薄膜中S/Mo值及sp3键含量,进而平衡薄膜力学性能与润滑性。
(6)采用全方位离子注入、微波ECR增强磁控溅射及化学气相沉积结合的方式制备了TaxMe1-xN多层复合DLC润滑薄膜。与单层DLC掺杂薄膜相比,结合强度提高了4倍、耐磨性提高了5-10倍。在1N,转速100r/min的磨损条件下起到润滑作用；在3N,转速400r/min磨损条件下,DLC层失效,氮化物承载层起到了耐磨作用,TaN/Ta多层薄膜由于摩擦系数低于0.15,形成了润滑梯度,保持了体系稳定性。
Currently, a large number of parts used in military are still prepared by die steels such as Crl2MoV. However, the requirements of the parts'performance are upgrading with the increasing complexity of the service environment for military weapons and the rapid development of modern manufacturing. The Cr12MoV components have not been able to meet the complex environment, so surface treatments become necessary way. In recently years, with the development of machining industries towards rapid and continuous processing of complex and small-scale materials, surface treatments as hard film, coating (less than10um) have been common methods for improving the service performance of the parts. Through the processing, parts'strength, toughness and wear resistance have been improved, and the service life of components is also improved. At present, the traditional hard films can no longer meet the requirement for the surface treatment of steel substrates due to the demand of better comprehensive performance (anti-corrosion, anti-wear, especially self-lubricating), so preparation of new composite films becomes important problems to be solved in this field.
Diamond-like carbon (DLC) film shows low friction coefficient, high hardness, wear resistance, and could be the first choice for surface modification of Cr12MoV steels. However, the application of DLC film has been restricted by the low thermal stability and low adhesion strength with steel-base materials. Moreover, the TaN film in relevant research shows high corrosion resistance, hardness, thermal stability, and low friction coefficient, demonstrating the prospect as hard wear-resistant and bearing layer of composite DLC film. This paper aimed to design and prepare DLC films composited with TaxMe1-xN multilayer films to match Cr12MoV steels, in order to improve comprehensive performance of the film. In this paper, DLC/TaxMe1-xN were prepared by PSII, MW-ECR MS and CVD, following the order of TaxMe1-xN→TaxMe1-xN multilayer→DLC/TaxMe1-xN multilayer. The functional graded DLC films improved the employ life of substrates by the lubrication. And the system also could keep the wear resistance of the system with a lower friction coefficient when the DLC layer failed under the increasing loads, for preventing the failure of parts due to a sudden increase of the friction coefficient. The film met the performance modification requirement of Crl2MoV. The contents of this thesis are divided into sections as follows:
(1) First, on the basis of plasma density variation in the deposition system, several groups of TaN films were prepared on Cr12MoV substrate using MW-ECR enhanced magnetron sputtering by controlling the process parameters. It focused on the influence of temperature, pressure, and bias on the structure and properties of TaN films, and the influence mechanism of different factors on film mechanical properties was discussed. TaN film exhibited hexagonal structure, and the coefficient of friction was less than0.2. The film hardness, modulus increased with increasing preparing temperature, the film hardness deposited under573K was39.36GPa, but the oxidation was found while the film was heat treatment in lower vacuum; The film hardness and modulus decreased with the increasing pressure; the values increased with the increase of bias, reached the maximum value at-100V, then decreased. Integrated consideration of different factors, it was found preparing temperature, pressure, and bias affect the ion energy and the quality of the interface between coating and substrate in the thin film nucleation and growth, resulting in the change of film properties. The mechanical properties and wear resistance of film attained the best value under lower preparing temperature, with pressure of0.1Pa, Ar/N2ratio of4.5/1, pulse bias voltage of-100V.
(2) Transition metals of Ti and Cr were added into TaN films, the influence of doping amount on the TaxMe1-xN film structure and performance were investigated. The influence mechanism of doped second particle on film mechanical properties was also discussed. The structure of composite TaxMe1-xN film transited from hexagonal to cubic; When the Ti/Ti+Ta ratio reached0.43, the hardness of Ta0.57Ti0.43N film reached the maximum value of33±2GPa, adhesion strength reached27GPa; When Cr/Cr+Ta ratio was0.61, the Ta0.39Cr0.61N film showed the maximum hardness of30±1.5GPa, adhesion strength of29N; the friction coefficient increased from0.2to0.4with the increase of Ti, Cr contents. It was found that doped proper Ti, Cr into TaN film is in favor of film nucleation, reduction of grain size, and solid solution strengthen, resulting in the improvement of film properties。
(3) The multilayer structure of TaN/Ta、TaxMe1-xN/Me、TaxMe1-xN/MeN/Me films were prepared on the basis of the TaN and TaxMe1-xN deposition. The strength mechanism of soft/hard multilayer structure on bonding strength was analyzed. TaN/Ta multilayer films with modulation thickness around250nm showed the best mechanical properties, hardness was26～27GPa, adhesion strength was around36N, wear resistance significantly increased; Compared to the monolayer TaxMe1-xN film, the wear resistance and bonding strength of TaxMe1-xN/Me、TaxMe1-xN/MeN/Me multilayer films were improved by the multilayer structure, the adhesion strength increased up to50N, the wear resistance was significantly improved. It was found that soft/hard structure with appropriate modulation period effectively relieve the film stress, and prevent crack propagation in the brittle layer, resulting in the improvement of the wear-resistance and adhesion strength.
(4) The influence of bombardment and injection on the properties of TaN film was discussed, and the TaN/Ta film was prepared by multilayer injection for the first time. The surface roughness of substrate increased with the increase of uniform mountain-like structure by high-energy Ar ion bombardment processing. After the deposition of TaN film, the uniformity and compactness of surface were significantly improved, the adhesion strength increased up to30N; The TaN film on the substrate injected with Ta and TaN at16kV bias showed better adhesion strength, which was up to36N; multilayer injected TaN/Ta films with Ta showed better adhesion strength up to55N. It was found the substrate surface area increased with increasing energy of Ar ion bombardment, which improved the shear resistance at the interface, resulting in the improvement of adhesion; Amorphous diffusion zone formed by implantation of Ta reduced the interfacial energy, leading to the improvement of interface quality; The adhesion strength of multilayer injected TaN/Ta were improved due to the formation of more diffusion zones between the TaN/Ta interfaces, meanwhile, the soft layer resulted in the reduction of stress due to the characteristics of shear bands.
(5) MW-ECR magnetron sputtering and chemical vapor deposition were used to prepare DLC films and DLC lubrication films, and the lubrication mechanism was also analyzed. It was found the friction coefficient of DLC film was reduced by doping MoS2in the amorphous DLC network. When C current was1.5A, MoS2current0.3A, the friction coefficient attained the lowest value of0.074, and the hardness was around14GPa. It was found that the MoS2dispersed in the amorphous DLC influenced on the mechanical properties and friction coefficient of DLC film. The Mo/S ratio and sp3contents could be changed by the sputtering energy and bias, for changing the C-C, C-H, and S-H bond, resulting in the balance of the mechanical properties and lubricity of films.
(6) MW-ECR enhanced sputtering, chemical deposition, and implantation were used to prepare multilayer DLC/TaxMe1-xN functional gradient multilayer lubricant films. Compared to the DLC film without support layer, the wear resistance was significantly improved up to4times, adhesion was increased up to5-10times. The DLC film showed lower friction coefficient under1N; when the DLC lubricant layer failed under higher load (3N,400r/min), the nitride bearing layer played wear-resisted role, friction coefficient of DLC/TaN/Ta system was still lower than0.15after the failure of DLC layer, maintaining the stability of system.
类金刚石(DLC)薄膜具有低摩擦系数、高硬度、高耐磨性的特点,可作为Cr12MoV表面改性的首选材料,但较低的热稳定性,以及与衬底的低结合强度制约了其应用。TaN薄膜作为硬质过渡金属氮化物在相关研究中展示了耐蚀性好、硬度及热稳定性高,摩擦系数低的特点,具有作为硬质耐磨薄膜及复合DLC承载层的研究前景。本论文旨在设计并获得与Cr12MoV衬底相匹配的TaxMe1-xN多层复合DLC润滑薄膜,提高薄膜的综合性能,达到钢基材料表面改性用硬质薄膜材料的要求。本文依照TaxMe1-xN单层→TaxMe1-xN多层→TaxMe1-xN多层复合DLC的顺序,采用全方位离子注入(Pill)、微波电子回旋共振等离子体(微波ECR)增强磁控溅射及化学气相沉积复合制备了DLC/TaxMe1-xN多层润滑薄膜。这种薄膜在磨损过程中产生白润化,提高了使用寿命。当外加载荷升高导致表层DLC失效后,薄膜体系承载层仍然能够保持较低的摩擦系数,以及较好耐磨性,防止了润滑层失效导致的摩擦副磨损加剧,达到了对Cr12MoV衬底耐磨润滑的改性要求。论文主要包括如下研究内容：
(1)首先在掌握反应室内等离子密度变化规律的基础上,采用微波ECR增强磁控溅射技术在Cr12MoV衬底上制备了几组TaN薄膜,重点研究了温度、气压、偏压对TaN薄膜结构与性能的影响,并且分析了相关影响因素对薄膜力学性能的影响机理。制备的TaN薄膜呈现六方结构,摩擦系数低于0.2。薄膜硬度随制备温度升高逐渐增加,573K时硬度达到最高值39.36GPa,但在低真空度热处理时出现氧化现象；TaN薄膜硬度与弹性模量随制备气压增加而降低,随脉冲偏压上升而增加,-100V时达到最高值,并随着偏压继续增加而降低。通过对不同影响因素分析发现,制备温度、气压、偏压影响了薄膜形核生长过程中离子结合能量以及膜基界面质量,导致薄膜性能的改变。在制备温度较低、气压0.1Pa、Ar/N2流量比4.5/1、脉冲偏压-100V时制备的TaN薄膜具有最佳的力学性能、耐磨性能。
(2)在TaN薄膜最佳制备工艺基础上添加过渡金属Me(Me=Ti、Cr)进行TaxMe1-xN复合制备,重点研究了掺杂量对TaxMe1-xN薄膜结构与性能的影响,分析讨论了复合第二相粒子对薄膜力学性能的影响机制。复合制备的TaxMe1-xN薄膜由TaN六方结构转变为三元固溶氮化物立方结构；当Ti/Ti+Ta、Cr/Cr+Ta分别达到0.43、0.61时,薄膜力学性能分别达到最佳值,其中Ta0.57Ti0.43N薄膜硬度为33±2GPa,结合强度为27N；Ta0.39Cr0.61N薄膜硬度为30±1.5GPa,结合强度为29N；薄膜摩擦系数随Ti、Cr掺杂量增加上升,最高值接近0.4。通过分析发现,适当比例的掺杂Ti、Cr有利于TaxMe1-xN薄膜形核以及晶粒尺寸降低,进而产生固溶、细晶强化作用。
(3)在TaN及TaxMe1-xN薄膜最佳制备工艺的基础上进行了TaN/Ta、TaxMe1-xN/Me、 TaxMe1-xN/MeN/Me多层薄膜的制备,并对软硬多层薄膜提高结合强度机理进行了分析。制备的TaN/Ta薄膜在调制厚度为250nm时达到最佳力学性能,硬度为26-27GPa,结合强度为36N,耐磨性显著上升；TaxMe1-xN/Me、TaxMe1-xN/MeN/Me多层薄膜与单层TaxMe1-xN薄膜相比,耐磨性能及膜基结合强度显著得到提升,结合强度高于50N。通过分析发现,适当的调制周期下,软硬多层结构有效的缓解了薄膜应力,同时界面增加阻止了脆性层裂纹扩展,从而改善了薄膜耐磨性、结合强度。
(4)分析了衬底轰击、注入对TaN薄膜性能的影响,并首次采用全方位离子注入与微波ECR增强磁控溅射相结合的方式了制备了多层界面注入TaN/Ta薄膜。高能Ar+离子轰击衬底形成均匀的山峰状结构,沉积TaN薄膜后表面均匀性、致密性明显改善,膜基结合强度达到30N以上；采用-16kV偏压在衬底上注入Ta、TaN过渡层后,TaN薄膜的结合强度提高到36N以上；多层界面注入Ta的TaN/Ta多层薄膜,膜基结合强度达到55N以上。通过分析发现高能Ar+离子轰击衬底增加了衬底表面积,增大了界面剪切抗力；注入形成非晶扩散区,有效的改善界面质量,降低了界面能；多层界面注入形成多个非晶扩散区,并保持了软硬多层薄膜结构中韧性层降低应力,提供剪切带的特性,有效的改善了膜基结合强度。
(5)采用微波ECR化学气相沉积与磁控溅射相结合的方式分别制备了DLC薄膜,DLC润滑膜,并对润滑机理进行了分析。采用掺杂MoS2、Ti制备的DLC润滑薄膜非晶网络中弥散了大量的MoS2润滑相,有效的降低了DLC薄膜的摩擦系数,当C靶电流1.5A,MoS2靶电流0.3A时,薄膜摩擦系数达到最小值0.074,硬度为14GPa。通过分析发现弥散在DLC非晶网络中的MOS2司滑相对薄膜力学性能及摩擦系数有较大影响,通过改变溅射能量及制备偏压调控薄膜沉积过程中C-C、C-H、S-H结合可以有效控制薄膜中S/Mo值及sp3键含量,进而平衡薄膜力学性能与润滑性。
(6)采用全方位离子注入、微波ECR增强磁控溅射及化学气相沉积结合的方式制备了TaxMe1-xN多层复合DLC润滑薄膜。与单层DLC掺杂薄膜相比,结合强度提高了4倍、耐磨性提高了5-10倍。在1N,转速100r/min的磨损条件下起到润滑作用；在3N,转速400r/min磨损条件下,DLC层失效,氮化物承载层起到了耐磨作用,TaN/Ta多层薄膜由于摩擦系数低于0.15,形成了润滑梯度,保持了体系稳定性。
Currently, a large number of parts used in military are still prepared by die steels such as Crl2MoV. However, the requirements of the parts'performance are upgrading with the increasing complexity of the service environment for military weapons and the rapid development of modern manufacturing. The Cr12MoV components have not been able to meet the complex environment, so surface treatments become necessary way. In recently years, with the development of machining industries towards rapid and continuous processing of complex and small-scale materials, surface treatments as hard film, coating (less than10um) have been common methods for improving the service performance of the parts. Through the processing, parts'strength, toughness and wear resistance have been improved, and the service life of components is also improved. At present, the traditional hard films can no longer meet the requirement for the surface treatment of steel substrates due to the demand of better comprehensive performance (anti-corrosion, anti-wear, especially self-lubricating), so preparation of new composite films becomes important problems to be solved in this field.
Diamond-like carbon (DLC) film shows low friction coefficient, high hardness, wear resistance, and could be the first choice for surface modification of Cr12MoV steels. However, the application of DLC film has been restricted by the low thermal stability and low adhesion strength with steel-base materials. Moreover, the TaN film in relevant research shows high corrosion resistance, hardness, thermal stability, and low friction coefficient, demonstrating the prospect as hard wear-resistant and bearing layer of composite DLC film. This paper aimed to design and prepare DLC films composited with TaxMe1-xN multilayer films to match Cr12MoV steels, in order to improve comprehensive performance of the film. In this paper, DLC/TaxMe1-xN were prepared by PSII, MW-ECR MS and CVD, following the order of TaxMe1-xN→TaxMe1-xN multilayer→DLC/TaxMe1-xN multilayer. The functional graded DLC films improved the employ life of substrates by the lubrication. And the system also could keep the wear resistance of the system with a lower friction coefficient when the DLC layer failed under the increasing loads, for preventing the failure of parts due to a sudden increase of the friction coefficient. The film met the performance modification requirement of Crl2MoV. The contents of this thesis are divided into sections as follows:
(1) First, on the basis of plasma density variation in the deposition system, several groups of TaN films were prepared on Cr12MoV substrate using MW-ECR enhanced magnetron sputtering by controlling the process parameters. It focused on the influence of temperature, pressure, and bias on the structure and properties of TaN films, and the influence mechanism of different factors on film mechanical properties was discussed. TaN film exhibited hexagonal structure, and the coefficient of friction was less than0.2. The film hardness, modulus increased with increasing preparing temperature, the film hardness deposited under573K was39.36GPa, but the oxidation was found while the film was heat treatment in lower vacuum; The film hardness and modulus decreased with the increasing pressure; the values increased with the increase of bias, reached the maximum value at-100V, then decreased. Integrated consideration of different factors, it was found preparing temperature, pressure, and bias affect the ion energy and the quality of the interface between coating and substrate in the thin film nucleation and growth, resulting in the change of film properties. The mechanical properties and wear resistance of film attained the best value under lower preparing temperature, with pressure of0.1Pa, Ar/N2ratio of4.5/1, pulse bias voltage of-100V.
(2) Transition metals of Ti and Cr were added into TaN films, the influence of doping amount on the TaxMe1-xN film structure and performance were investigated. The influence mechanism of doped second particle on film mechanical properties was also discussed. The structure of composite TaxMe1-xN film transited from hexagonal to cubic; When the Ti/Ti+Ta ratio reached0.43, the hardness of Ta0.57Ti0.43N film reached the maximum value of33±2GPa, adhesion strength reached27GPa; When Cr/Cr+Ta ratio was0.61, the Ta0.39Cr0.61N film showed the maximum hardness of30±1.5GPa, adhesion strength of29N; the friction coefficient increased from0.2to0.4with the increase of Ti, Cr contents. It was found that doped proper Ti, Cr into TaN film is in favor of film nucleation, reduction of grain size, and solid solution strengthen, resulting in the improvement of film properties。
(3) The multilayer structure of TaN/Ta、TaxMe1-xN/Me、TaxMe1-xN/MeN/Me films were prepared on the basis of the TaN and TaxMe1-xN deposition. The strength mechanism of soft/hard multilayer structure on bonding strength was analyzed. TaN/Ta multilayer films with modulation thickness around250nm showed the best mechanical properties, hardness was26～27GPa, adhesion strength was around36N, wear resistance significantly increased; Compared to the monolayer TaxMe1-xN film, the wear resistance and bonding strength of TaxMe1-xN/Me、TaxMe1-xN/MeN/Me multilayer films were improved by the multilayer structure, the adhesion strength increased up to50N, the wear resistance was significantly improved. It was found that soft/hard structure with appropriate modulation period effectively relieve the film stress, and prevent crack propagation in the brittle layer, resulting in the improvement of the wear-resistance and adhesion strength.
(4) The influence of bombardment and injection on the properties of TaN film was discussed, and the TaN/Ta film was prepared by multilayer injection for the first time. The surface roughness of substrate increased with the increase of uniform mountain-like structure by high-energy Ar ion bombardment processing. After the deposition of TaN film, the uniformity and compactness of surface were significantly improved, the adhesion strength increased up to30N; The TaN film on the substrate injected with Ta and TaN at16kV bias showed better adhesion strength, which was up to36N; multilayer injected TaN/Ta films with Ta showed better adhesion strength up to55N. It was found the substrate surface area increased with increasing energy of Ar ion bombardment, which improved the shear resistance at the interface, resulting in the improvement of adhesion; Amorphous diffusion zone formed by implantation of Ta reduced the interfacial energy, leading to the improvement of interface quality; The adhesion strength of multilayer injected TaN/Ta were improved due to the formation of more diffusion zones between the TaN/Ta interfaces, meanwhile, the soft layer resulted in the reduction of stress due to the characteristics of shear bands.
(5) MW-ECR magnetron sputtering and chemical vapor deposition were used to prepare DLC films and DLC lubrication films, and the lubrication mechanism was also analyzed. It was found the friction coefficient of DLC film was reduced by doping MoS2in the amorphous DLC network. When C current was1.5A, MoS2current0.3A, the friction coefficient attained the lowest value of0.074, and the hardness was around14GPa. It was found that the MoS2dispersed in the amorphous DLC influenced on the mechanical properties and friction coefficient of DLC film. The Mo/S ratio and sp3contents could be changed by the sputtering energy and bias, for changing the C-C, C-H, and S-H bond, resulting in the balance of the mechanical properties and lubricity of films.
(6) MW-ECR enhanced sputtering, chemical deposition, and implantation were used to prepare multilayer DLC/TaxMe1-xN functional gradient multilayer lubricant films. Compared to the DLC film without support layer, the wear resistance was significantly improved up to4times, adhesion was increased up to5-10times. The DLC film showed lower friction coefficient under1N; when the DLC lubricant layer failed under higher load (3N,400r/min), the nitride bearing layer played wear-resisted role, friction coefficient of DLC/TaN/Ta system was still lower than0.15after the failure of DLC layer, maintaining the stability of system.
引文
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