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离子束辅助沉积Ti-Cu-N纳米复合膜

Ti-Cu-N Hard Nanocomposite Films Prepared by Ion Beam Assisted Deposition

【作者】 冯丹

【导师】 李凤岐;

【作者基本信息】 沈阳理工大学 , 物理电子学, 2015, 硕士

【摘要】 本文采用离子束辅助沉积技术在不锈钢和高速钢基体上制备Ti-Cu-N纳米复合薄膜。用X射线光电子谱(XPS)、X射线衍射仪(XRD)、扫描电镜(SEM)、透射电镜(TEM)和纳米压痕仪等方法对制备的试样进行分析,研究基体基体脉冲偏压和离子束离子源放电电流对薄膜的化学成分、结构、形貌、硬度以及弹性模量的影响。分析了不同工艺参数对薄膜结构及性能的影响。研究了离子束的轰击作用对薄膜的成分、形貌以及硬度的影响。结果表明,在304不锈钢基体上,不改变离子束能量的条件下,随着基体脉冲偏压的增加Cu含量先减少然后增加,在1.47at.%-2.75at.%之间变化,当基体偏压为-600V时最小值为1.47at.%,同时择优取向也由Ti N(111)转变为Ti N(220),所有偏压下的Ti N都是面心立方结构(B1-Na Cl)。薄膜的Cu2p峰均对应纯金属Cu,晶粒的平均尺寸在11nm-16nm之间变化。硬度随着基体偏压的增加而减小,当偏压为-100V时,薄膜硬度达到最大值:27.2GPa。在M2高速钢基体上沉积Ti-Cu-N纳米复合薄膜,在离子束的轰击作用下,随着基体偏压在-100V到-900V之间的改变,薄膜中Cu含量在1.05at.%-2.50at.%之间变化。同时,薄膜的结构也受到影响,在-100V出现Ti N(111)择优取向,当基体偏压增加到-300V时,择优取向改变为Ti N(220)。薄膜的Cu2p峰均对应纯金属Cu,晶粒的平均尺寸在11nm-17nm之间变化。硬度和弹性模量随着基体偏压的增加而增大,当偏压为-900V时,薄膜硬度和弹性模量达到最大值,分别为:29.92GPa、476GPa。在304不锈钢基体上,基体偏压为-600V时,改变离子源放电电流时薄膜中Cu含量在1.19at.%-1.80at.%之间发生变化。同时,离子源放电电流在10A、20A、30A、40A时,只存在Ti N(220)择优取向。薄膜的Cu2p峰均对应纯金属Cu。随着离子源放电电流的增加,硬度和弹性模量也发生改变,离子源放电电流为10A时,Cu含量为1.50at.%,薄膜硬度和弹性模量达到最大值:39.73GPa,535.85GPa。在基体M2高速钢上基体上,基体脉冲偏压为-600V时,随着离子源放电电流的变化,Ti-Cu-N纳米复合薄膜中Cu含量在1.138-1.55at.%之间变化。离子源放电电流从10A增加到40A时,只存在Ti N(220)择优取向。随着离子源放电电流增加,薄膜的表面形貌也发生改变,大颗粒数量明显减少。薄膜的硬度和弹性模量随着离子源放电电流的增加先增加后减少,并在离子源放电电流为30A时达到最大值39.24GPa和544.59GPa,此时Cu含量1.157 at.%。

【Abstract】 The structures and corresponding mechanical properties of Ti-Cu-N nanocomposite films synthesized by ion beam assisted deposition on the matrix of SS and HSS were studied in this paper. The influences of ion bean discharge current and substrate bias voltages on chemical compositions, structures, morphology, hardness and elastic modulus of the films were examined with X-ray photoelectron spectroscopy(XPS), X-ray diffraction(XRD), scanning electron microscope(SEM), Transmission electron microscopy(TEM) and Nano indentation apparatus. The influences of process parameters on the structures and properties of the films were analyzed.The results showed that the content of Cu in Ti-Cu-N nanocomposite films on SS substrate increased firstly and then decreased between 1.47 at.% and 2.75 at.% when the bias voltages increased and the ion beam energy was constant. The minimum value of Cu content was 1.47 at.% was obtained at the bias voltage of-600 V. Meanwhile, the preferred orientation changed from Ti N(111) to Ti N(220). Ti N at all bias voltages had face-centered cubic structures(B1-Na Cl). Cu2 p peaks of the film corresponded to pure metal Cu. The average grain size changes between 11 nm and 16 nm. The hardness decreased when the bias voltages increased. The maximum values of the hardness was 27.2 GPa while the bias voltage was-100 V.The content of Cu in Ti-Cu-N nanocomposite films on HSS substrate appeared to be in the range of 1.05-2.50 at.% when the bias voltages changed from-100 V to-900 V. Meanwhile, the films exhibited a preferred orientation Ti N(111) texture when the substrate bias voltages were-100 V. The preferred orientation changed to be Ti N(220) when the substrate bias voltages increase to-300 V to-900 V. Cu2 p peaks of the films corresponded to pure metal Cu, and the average grain size changed between 11 nm and 17 nm. The value of the hardness and elasticity modulus increased when the bias voltages increased,and the maximum values were 29.92 GPa and 476 GPa were obtained while the bias voltage was-900 V.The content of Cu in Ti-Cu-N nanocomposite films on SS substrate appeared to be in the range of 1.19-1.80 at.% at the bias voltage-600 V when the discharge current changed from 10 A to 40 A. The films on SS substrate exhibited only a preferred orientation Ti N(220) texture when the discharge currents were 10A-40 A. Cu2 p peaks of the films correspond to pure metal Cu. The value of the hardness and elasticity modulus changed when the discharge current increased. The maximum values of the hardness and elasticity modulus were 39.73 GPa and 535.85 GPa respectively at discharge current of 10 A. Meanwhile, the corresponding content of Cu was 1.50 at.%.The content of Cu in Ti-Cu-N nanocomposite films on HSS substrate changed from 1.14 at.% to 1.55 at.% at the bias voltage-600 V when the discharge current changed. The films exhibited a preferred orientation Ti N(220) texture when the discharge current were in the range of 10A-40 A. The SEM morphologies showed that the amount of macroparticles(MPs) on the surface of the films decreased when the discharge current increased. With the discharge current increased, the hardness of the films increased firstly and then decreased. The hardness and elasticity modulus of the films reached the maximum 39.24 GPa and 544.59 GPa at the discharge current of 30 A, while the content of Cu was 1.16 at.%.

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