DLC基固体润滑复合薄膜制备及性能表征
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摘要
类金刚石(DLC)薄膜因其诸多独特的性能,包括高硬度、低摩擦系数、高电阻率、高热导率、良好的化学稳定性和突出的抗腐蚀能力等优点,已经在机械、信息技术、航空航天、光学和医学等方面得到了广泛应用。近来,DLC薄膜的复合化与多功能化逐渐成为研究热点。本文结合航空航天需要,旨在探索类金刚石基固体润滑复合薄膜的制备与性能表征。
采用等离子体增强磁控溅射法成功制备了引入W_xC及WS_2颗粒的类金刚石基固体润滑复合薄膜。通过拉曼光谱仪、X射线衍射仪、X射线光电子能谱仪、原子力显微镜、扫描电镜(能谱仪)、透射电镜、纳米压痕力学测试、膜基结合力测试和摩擦系数测试考察了沉积总气压(Pt)、直流沉积偏压(U_d)、WS_2靶溅射功率(P_(WS2))等工艺参数对薄膜性能的影响。
结果表明:采用磁控溅射法制备的复合薄膜也具有典型的类金刚石结构肩峰特征,但WE_2和W_xC的引入使薄膜复合化之后引起sp~3键含量一定程度的下降;改变沉积偏压(U_d),可改变沉积速率和沉积粒子的能量,进而控制薄膜中sp~3键,在U_d=-200V时,复合薄膜有最高含量sp~3键。复合薄膜主要以层状方式长大,WS_2和W_xC颗粒尺寸约300nm。元素W主要以WC、单质W和WO_3的形式存在。
复合薄膜的力学性能随沉积参数变化较大,硬度和弹性模量随沉积总气压以及沉积偏压的绝对值的增大都先增大后减小,随WS_2靶溅射功率先减小后增大再降低,在Pt=0.38Pa,U_d=-200V,P_(WS2)=160W工艺参数下复合薄膜有最高的纳米硬度(约7.5GPa)和弹性模量(约125GPa);Pt=0.38Pa,U_d=-200V下复合薄膜还有最优的膜基结合性能,此时薄膜脱落的临界载荷接近80N。
WS_2和W_xC的引入使薄膜复合化之后导致薄膜大气下摩擦行为变为不稳摩擦,磨合期显著延长到500秒左右,稳定摩擦系数升高幅度超过70%;稳定摩擦系数随沉积偏压的绝对值的增大先稍微降低,再逐渐增大,随WS_2靶溅射功率的增大变化不大。在U_d=-200V,P_(WS2)=160W下有最低约0.04的大气下稳定阶段摩擦系数且稳定对磨时间超过35min。复合薄膜真空中摩擦系数高于大气下数值且即时值跳跃幅度较大,U_d=-100V,-200V沉积偏压下最低约0.14。真空中稳定摩擦系数随沉积总气压的增大先减小再增大,Pt=0.38Pa及0.21Pa与U_d=-200V工艺参数配合下可获得相对最低,约0.14的稳定摩擦系数。WS_2和W_xC的引入使DLC薄膜复合化后减缓了薄膜的石墨化,表明该复合化手段可初步改善原单一DLC薄膜的热稳定性。
Diamond-like carbon(DLC) films has been applied in many fields,such as mechanics,information technology,aerospace and aviation,optics and iatrology,due to their special properties,including high hardness,low coefficient of friction,high resistance,high thermal conductivity,well chemistry-stability and outstanding performance of erosion resistance.Recently,multifunctional composite films built in DLC matrix have been extensively studied.This work aims at exploring the preparation and characteristic of the DLC-based composite films to meet the potential need of aerospace and aviation.
The DLC-based composite films were prepared successfully by plasma enhanced magnetron sputtering deposition technology.The characteristics were performed to check the influence of deposition ambience,direct current bias and the power of WS_2 target on the as-deposited films by Raman spectrum,XRD, XPS,AFM,SEM(EDS),TEM,nano-indentation tests,adhesion tests,friction coefficient tests,respectively.
The results indicated that the composite films also had the typical structure of DLC films while these particles could result in a fall of relative content of sp~3; with the increase of the DC bias voltage,the relative content of sp~3 increased first and then decreased,having the most sp~3 content while-200V bias was applied;the as-deposited composite films had laminated structure,and W_xC and WS_2 particles were inlaid as islands;the composite films were composed of DLC matrix and particles,while the particles were mostly W_xC(X≈2) and W with an average dimension of about 300nm.
The mechanical property of the composite films changed evidently with the deposition parameters.The nano-hardness and elastic modulus increased at the beginning and then reduced with the accretion of total pressure and the absolute value of DC bias voltage as well as the power of WS_2 target while it was in the range of 80～210W;The supreme hardness and elastic modulus were obtained with the parameters of Pt=0.38Pa,U_d=-200V and P_(WS2)=160W;the best cohesive property between the films and substrate were also achieved when the parameters were Pt=0.38Pa and U_d=-200V,with a critical load up to 80N.
The friction behavior in air(T=26℃,RH=34%) became unstable after the introduction of W_xC and WS_2 particles,requiring a longer accommodation stage up to almost 500s,and the coefficient of friction of stable stage climbed remarkably by 70%;the coefficient of friction of stable stage fell a little and then increased with the enhancement of the absolute value of DC bias voltage while change a little with increasing power of WS_2 target;the lowest coefficient of friction of stable stage was about 0.04 and its duration could be as long as 35min when the deposition parameters were fixed at U_d=-200v and P_(WS2)=160W;the friction behavior in vacuum was worse than that in air including higher coefficient of friction of stable stage and more unstable performance;the best result was 0.14 in vacuum,which was obtained when the parameters were Pt=0.21Pa or0.38Pa and U_d=-200V;the transformation to graphite was delayed after the introduction of W_xC and WS_2 particles,that is,the composite films have better thermal stability.
采用等离子体增强磁控溅射法成功制备了引入W_xC及WS_2颗粒的类金刚石基固体润滑复合薄膜。通过拉曼光谱仪、X射线衍射仪、X射线光电子能谱仪、原子力显微镜、扫描电镜(能谱仪)、透射电镜、纳米压痕力学测试、膜基结合力测试和摩擦系数测试考察了沉积总气压(Pt)、直流沉积偏压(U_d)、WS_2靶溅射功率(P_(WS2))等工艺参数对薄膜性能的影响。
结果表明:采用磁控溅射法制备的复合薄膜也具有典型的类金刚石结构肩峰特征,但WE_2和W_xC的引入使薄膜复合化之后引起sp~3键含量一定程度的下降;改变沉积偏压(U_d),可改变沉积速率和沉积粒子的能量,进而控制薄膜中sp~3键,在U_d=-200V时,复合薄膜有最高含量sp~3键。复合薄膜主要以层状方式长大,WS_2和W_xC颗粒尺寸约300nm。元素W主要以WC、单质W和WO_3的形式存在。
复合薄膜的力学性能随沉积参数变化较大,硬度和弹性模量随沉积总气压以及沉积偏压的绝对值的增大都先增大后减小,随WS_2靶溅射功率先减小后增大再降低,在Pt=0.38Pa,U_d=-200V,P_(WS2)=160W工艺参数下复合薄膜有最高的纳米硬度(约7.5GPa)和弹性模量(约125GPa);Pt=0.38Pa,U_d=-200V下复合薄膜还有最优的膜基结合性能,此时薄膜脱落的临界载荷接近80N。
WS_2和W_xC的引入使薄膜复合化之后导致薄膜大气下摩擦行为变为不稳摩擦,磨合期显著延长到500秒左右,稳定摩擦系数升高幅度超过70%;稳定摩擦系数随沉积偏压的绝对值的增大先稍微降低,再逐渐增大,随WS_2靶溅射功率的增大变化不大。在U_d=-200V,P_(WS2)=160W下有最低约0.04的大气下稳定阶段摩擦系数且稳定对磨时间超过35min。复合薄膜真空中摩擦系数高于大气下数值且即时值跳跃幅度较大,U_d=-100V,-200V沉积偏压下最低约0.14。真空中稳定摩擦系数随沉积总气压的增大先减小再增大,Pt=0.38Pa及0.21Pa与U_d=-200V工艺参数配合下可获得相对最低,约0.14的稳定摩擦系数。WS_2和W_xC的引入使DLC薄膜复合化后减缓了薄膜的石墨化,表明该复合化手段可初步改善原单一DLC薄膜的热稳定性。
Diamond-like carbon(DLC) films has been applied in many fields,such as mechanics,information technology,aerospace and aviation,optics and iatrology,due to their special properties,including high hardness,low coefficient of friction,high resistance,high thermal conductivity,well chemistry-stability and outstanding performance of erosion resistance.Recently,multifunctional composite films built in DLC matrix have been extensively studied.This work aims at exploring the preparation and characteristic of the DLC-based composite films to meet the potential need of aerospace and aviation.
The DLC-based composite films were prepared successfully by plasma enhanced magnetron sputtering deposition technology.The characteristics were performed to check the influence of deposition ambience,direct current bias and the power of WS_2 target on the as-deposited films by Raman spectrum,XRD, XPS,AFM,SEM(EDS),TEM,nano-indentation tests,adhesion tests,friction coefficient tests,respectively.
The results indicated that the composite films also had the typical structure of DLC films while these particles could result in a fall of relative content of sp~3; with the increase of the DC bias voltage,the relative content of sp~3 increased first and then decreased,having the most sp~3 content while-200V bias was applied;the as-deposited composite films had laminated structure,and W_xC and WS_2 particles were inlaid as islands;the composite films were composed of DLC matrix and particles,while the particles were mostly W_xC(X≈2) and W with an average dimension of about 300nm.
The mechanical property of the composite films changed evidently with the deposition parameters.The nano-hardness and elastic modulus increased at the beginning and then reduced with the accretion of total pressure and the absolute value of DC bias voltage as well as the power of WS_2 target while it was in the range of 80～210W;The supreme hardness and elastic modulus were obtained with the parameters of Pt=0.38Pa,U_d=-200V and P_(WS2)=160W;the best cohesive property between the films and substrate were also achieved when the parameters were Pt=0.38Pa and U_d=-200V,with a critical load up to 80N.
The friction behavior in air(T=26℃,RH=34%) became unstable after the introduction of W_xC and WS_2 particles,requiring a longer accommodation stage up to almost 500s,and the coefficient of friction of stable stage climbed remarkably by 70%;the coefficient of friction of stable stage fell a little and then increased with the enhancement of the absolute value of DC bias voltage while change a little with increasing power of WS_2 target;the lowest coefficient of friction of stable stage was about 0.04 and its duration could be as long as 35min when the deposition parameters were fixed at U_d=-200v and P_(WS2)=160W;the friction behavior in vacuum was worse than that in air including higher coefficient of friction of stable stage and more unstable performance;the best result was 0.14 in vacuum,which was obtained when the parameters were Pt=0.21Pa or0.38Pa and U_d=-200V;the transformation to graphite was delayed after the introduction of W_xC and WS_2 particles,that is,the composite films have better thermal stability.
引文
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