反应共溅射Ni-TiN纳米复合膜的制备与性能

发布时间：2018-04-01 12:33

本文选题：磁控溅射　切入点：Ni-TiN　出处：《沈阳大学》2015年硕士论文

【摘要】：在过去的几十年里,Ti N薄膜以其高硬度、高耐磨性以及金黄的色泽被广泛应用于机械、航天、电子等领域。然而,较低的韧性限制了Ti N薄膜潜在的应用。因此,需要研究综合力学性能优良的材料来满足发展的需求。纳米复合膜具有优异的综合使用性能,因此相关研究成为材料科学研究热点之一。本文利用磁控共溅射技术,通过改变薄膜制备工艺过程中的N2流量、Ni靶溅射功率、基体温度和负偏压四个工艺参数制备了一系列的Ni-Ti N纳米复合膜,利用XRD、扫描电镜、原子力显微镜、纳米压痕仪、电化学工作站和多功能表面性能测试仪对所制备薄膜的相结构、表面形貌、耐腐蚀性能和力学性能等进行了系统表征研究,获得如下结论。研究了N2流量对Ni-Ti N纳米复合膜的影响,结果表明:随着N2流量的增加,Ti N的平均晶粒尺寸逐渐减小,薄膜的平均沉积速率也在减小,膜表面粗糙度则先减小后增大。在N2流量为16 m L/min时,表面粗糙度最小,为2.75 nm,此时,膜基结合力也达到最大,为28 N。通过Ni靶功率对Ni-Ti N纳米复合膜的影响研究,发现:在Ni靶功率较低时,薄膜的平均晶粒尺寸较大,择优取向为Ti N(111)晶面,随着Ni靶功率的增加,择优取向变为Ti N(200)晶面,平均晶粒尺寸逐渐减小,表明Ni的加入明显地起到了细化晶粒的作用。在Ni靶功率为35 W时,薄膜表面最平滑,粗糙度值最小为3.14 nm,此时膜基结合力和耐腐蚀性最好。当Ni靶功率从25 W增至45 W时,硬度、弹性模量分别从15.1 GPa和288 GPa增至21.1 GPa和290.5GPa,此时H3/E2的值也最大。但是当Ni靶功率增加至55 W,薄膜的硬度和弹性模量又分别减小到18.2 GPa和281.4 GPa。基体温度对Ni-Ti N纳米复合膜的影响有:当温度从100°C上升至400°C时,薄膜的择优取向由Ti N(111)转变为(200)晶面,平均晶粒尺寸先减小后增大,薄膜的膜基结合力和耐蚀性先升高后降低。在200°C时平均晶粒尺寸最小,为12.5nm,薄膜表面平整致密,表面粗糙度最小。在300°C时薄膜的膜基结合力和耐蚀性最好。基体负偏压对Ni-Ti N纳米复合膜的影响与基体温度的影响大致相同。随着负偏压的增加,薄膜的择优取向由Ti N(111)晶面变为(200)晶面,薄膜平均晶粒尺寸先减小后增大,而力学性能和耐蚀性则先增加再下降。在负偏压为-80 V时平均晶粒尺寸为最小,为13.6 nm,薄膜的硬度和弹性模量分别达到最大值的19.2 GPa和311 GPa,膜基结合力达到最大值的41 N,耐腐蚀性最好。在负偏压为-120 V时,表面粗糙度最小,为3.14 nm。通过Ni-Ti N纳米复合膜与304不锈钢基体的耐腐蚀性对比试验发现,Ni-Ti N纳米复合膜的耐腐蚀性明显好于304不锈钢基体。
[Abstract]:Tin thin films have been widely used in mechanical, aerospace, electronic and other fields for their high hardness, high wear resistance and golden color in the past few decades. However, the low toughness limits the potential applications of tin thin films. It is necessary to study the materials with excellent comprehensive mechanical properties to meet the needs of development. The nanocomposite films have excellent comprehensive performance, so the related research has become one of the research hotspots in material science. In this paper, the magnetron co-sputtering technology is used. A series of Ni-Ti N nanocomposite films were prepared by changing the N 2 flow rate Ni target sputtering power, substrate temperature and negative bias voltage. The phase structure, surface morphology, corrosion resistance and mechanical properties of the films were systematically studied by electrochemical workstation and multifunctional surface performance tester. The results show that the average grain size of Ni-Ti N decreases with the increase of N 2 flow rate, and the average deposition rate decreases with the increase of N 2 flow rate. The surface roughness of the film decreases first and then increases. When N 2 flow rate is 16 m L/min, the surface roughness is the smallest, which is 2.75 nm. At this time, the adhesion of the film is the highest, which is 28 N. the effect of Ni target power on the Ni-Ti N nanocomposite film is studied. It is found that when the power of Ni target is low, the average grain size of the thin film is larger, and the preferred orientation is Ti (N) 111). With the increase of the power of Ni target, the preferred orientation becomes the Ti (N) ~ (200)) plane, and the average grain size decreases gradually. The results show that the addition of Ni plays an obvious role in grain refinement. When the power of Ni target is 35 W, the surface of the film is smoother, the roughness is minimum 3.14 nm, and the adhesion and corrosion resistance of the film is the best. When the power of Ni target is increased from 25 W to 45 W, the surface of the film is smoother and the roughness is the minimum of 3.14 nm. Hardness, The modulus of elasticity increased from 15.1 GPa and 288 GPa to 21.1 GPa and 290.5 GPA, respectively, and the value of H3/E2 was the highest. However, when the target power of Ni was increased to 55 W, the hardness and modulus of elasticity of the film decreased to 18.2 GPa and 281.4 GPa.The substrate temperature was applied to Ni-Ti N nanocomplex. The effect of the film is as follows: when the temperature rises from 100 掳C to 400 掳C, The preferred orientation of the thin films was changed from Ti _ (N _ (111)) to ~ (200)). The average grain size first decreased and then increased, and the film substrate adhesion and corrosion resistance first increased and then decreased. At 200 掳C, the average grain size was the smallest (12.5 nm), and the film surface was flat and compact. The surface roughness is the smallest. The film has the best adhesion and corrosion resistance at 300 掳C. the effect of negative bias voltage on the Ni-Ti N nanocomposite film is approximately the same as that of the substrate temperature. The preferred orientation of the thin film changes from the Ti (N + 111) crystal plane to the crystal plane (200). The average grain size of the film decreases first and then increases, while the mechanical properties and corrosion resistance increase first and then decrease. The average grain size is the smallest when the negative bias voltage is -80 V. The hardness and elastic modulus of the film reached 19.2 GPa and 311GParespectively of the maximum value, and the maximum adhesion of the film was 41N, and the corrosion resistance was the best. When the negative bias voltage was -120V, the surface roughness was the smallest. The results show that the corrosion resistance of Ni-Ti N nanocomposite film is better than that of 304 stainless steel substrate.
【学位授予单位】：沈阳大学
【学位级别】：硕士
【学位授予年份】：2015
【分类号】：TB383.2

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