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【中文】传输方向可调式的多级磁场电弧离子镀方法
【EN】The adjustable multi-stage magnetic field arc ions electroplating method of transmission direction

申请(专利)号:CN201510575622.1国省代码:河南 41
申请(专利权)人:【中文】魏永强【EN】Wei Yongqiang
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摘要:
【中文】传输方向可调式的多级磁场电弧离子镀方法,属于材料表面处理技术领域,本发明为解决低熔点的纯金属或多元合金材料和非金属材料(比如石墨)在电弧离子镀中的大颗粒问题和低熔点靶材使用局限,拓展电弧离子镀靶材使用范围和薄膜制备的领域。本发明方法包括:一、将待镀膜的工件置于真空室内的样品台上,接通相关电源;二、薄膜沉积:待真空室内的真空度小于10‑2Pa时,通入工作气体并调整气压,开启镀膜电源,偏压电源,通过多级磁场直管磁过滤装置消除大颗粒缺陷和保证电弧等离子体的传输效率,再利用传输方向可调式磁场装置保证电弧等离子体可以到达真空室内任意位置的基体表面,设置所需工艺参数,进行薄膜沉积。【EN】Paragraph:The adjustable multi-stage magnetic field arc ions electroplating method of transmission direction, belong to technical field of material surface treatment, the present invention is the bulky grain solved the problems, such as the pure metal or multicomponent alloy material and nonmetallic materials (such as graphite) of low melting point in arc ion plating and low melting point target using limitation, expands the field of arc ion plating target use scope and film preparation.The method of the present invention includes: one, workpiece to be coated is placed on the indoor sample stage of vacuum, connects line related;Two, film deposits: to the indoor vacuum degree of vacuum less than 10‑2When Pa, it is passed through working gas and adjusts air pressure, open plated film power supply, grid bias power supply, bulky grain defect is eliminated by multi-stage magnetic field straight tube magnetic filter and guarantees the efficiency of transmission of arc-plasma, the adjustable magnetic field device of transmission direction is recycled to guarantee that arc-plasma can reach the matrix surface of any position in vacuum chamber, technological parameter needed for being arranged carries out film deposition.

主权项:
【中文】1.传输方向可调式的多级磁场电弧离子镀方法,其特征在于,该方法所使用装置包括偏压电源(1)、弧电源(2)、电弧离子镀靶源(3)、多级磁场装置(4)、多级磁场电源(5)、传输方向可调式磁场装置(6)、传输方向可调式磁场电源(7)、真空室(8)、样品台(9); 该方法包括以下步骤: 步骤一、将待处理的基体工件置于真空室(8)内的样品台(9)上,工件接偏压电源(1)的脉冲输出端,安装在真空室(8)上的电弧离子镀靶源(3)接通弧电源(2),多级磁场装置(4)接通多级磁场电源(5),传输方向可调式磁场装置(6)接通传输方向可调式磁场电源(7); 步骤二、薄膜沉积:将真空室(8)抽真空,待真空室(8)内的真空度小于10Pa时,通入工作气体至0.01Pa~10Pa; 开启偏压电源(1),偏压电源(1)输出脉冲的峰值电压值为0~1.2kV,脉冲频率为0Hz~80kHz,脉冲宽度1~90%;通过调节偏压电源(1)输出的偏压幅值,脉冲频率和脉冲宽度,控制基体工件对金属等离子体的有效吸引和离子能量的调节,进行薄膜的沉积和控制低熔点的纯金属或多元合金材料及非金属材料在薄膜中的比例,实现纯金属薄膜、不同元素比例的化合物陶瓷薄膜、功能薄膜及具有纳米多层或梯度结构的薄膜制备,偏压电源(1)通过脉冲频率、脉冲偏压幅值和脉冲偏压的占空比分别调整,来控制单位时间到达基体工件表面的电弧等离子体能量峰值强度和密度,偏压电源(1)输出脉冲为单脉冲、直流脉冲复合或多脉冲复合,所制备薄膜的微观结构和性能通过偏压电源(1)的脉冲偏压参数进行调整,对电弧等离子体的能量进行调节,利用脉冲偏压的幅值、脉冲宽度和频率实现高能离子对薄膜生长的钉扎效应,改善薄膜生长的晶体组织和应力状态,提高膜基结合强度; 开启弧电源(2),通过电弧的弧斑运动对电弧离子镀靶源(3)的表面进行清洗,调节需要的工艺参数,弧电源(2)输出的电流值为10~300A,弧电源(2)输出的电流为直流、脉冲或者直流脉冲复合; 电弧离子镀靶源(3)采用的靶体材料为低熔点的纯金属或多元合金靶材及非金属材料,突破了传统电弧离子镀靶源(3)采用低熔点的纯金属或多元合金材料及非金属材料的限制,实现薄膜成分和微观结构的灵活调节; 开启多级磁场电源(5)调节多级磁场装置(4),保持电弧等离子体在电弧离子镀靶源(3)稳定产生和对大颗粒缺陷进行过滤消除,使电弧等离子体以较高的传输效率通过多级磁场装置(4),再利用传输方向可调式磁场电源(7)调节传输方向可调式磁场装置(6),保证电弧等离子体到达真空室内任意位置的基体工件表面,进行薄膜的快速沉积,通过多级磁场装置(4)和传输方向可调式磁场装置(6)实现大颗粒缺陷的清除和电弧等离子体的高效传输; 多级磁场装置(4)对电弧在靶表面的烧蚀进行有效控制,消除由于烧蚀不均产生的“馒头靶”现象,实现均匀烧蚀和靶材的高效利用,多级磁场装置(4)消除大颗粒缺陷并保证离化率接近100%的电弧等离子体的高效传输,多级磁场装置(4)结合电弧离子镀靶源的工艺参数,实现利用多套沉积装置调节产生的复合等离子体中各种元素的离子比例,实现不同元素比例的多元多层薄膜的快速沉积; 传输方向可调式磁场装置(6)弥补了直线型磁过滤方法在传输方向上不能灵活调节的缺陷,有利于高离化率等离子体在任意位置工件表面的化学合成反应成膜,传输方向可调式磁场装置(6)调节电弧等离子体在真空室中的传输方向,实现真空室(8)内任意位置基体工件表面薄膜的快速沉积; 反复执行步骤一至步骤二,来制备纯金属薄膜、不同元素比例的化合物陶瓷薄膜、功能薄膜及具有纳米多层或梯度结构的薄膜; 步骤三、单独采用传统电弧离子镀、脉冲阴极弧、多级磁场过滤装置和传输方向可调式磁场装置结合直流偏压、脉冲偏压或直流脉冲复合偏压进行薄膜沉积,来制备纯金属薄膜、不同元素比例的化合物陶瓷薄膜、功能薄膜及具有纳米多层或梯度结构的薄膜。【EN】1. the adjustable multi-stage magnetic field arc ions electroplating method of transmission direction, which is characterized in that this method institute use device includes Grid bias power supply (1), arc power (2), arc ion plating target source (3), multi-stage magnetic field device (4), multi-stage magnetic field power supply (5), transmission Direction-adjustable magnetic field device (6), the adjustable magnetic field power supply of transmission direction (7), vacuum chamber (8), sample stage (9); Method includes the following steps: Step 1: substrate work-piece to be processed is placed on the sample stage (9) in vacuum chamber (8), workpiece connects grid bias power supply (1) Arc power (2) are connected in pulse output end, the arc ion plating target source (3) being mounted on vacuum chamber (8), multi-stage magnetic field device (4) It connects multi-stage magnetic field power supply (5), the adjustable magnetic field device of transmission direction (6) connects the adjustable magnetic field power supply of transmission direction (7); Step 2: film deposits: vacuum chamber (8) being vacuumized, to the vacuum degree in vacuum chamber (8) less than 10When Pa, it is passed through work Make gas to 0.01Pa~10Pa; Open grid bias power supply (1), grid bias power supply (1) export pulse peak voltage be 0~1.2kV, pulse frequency be 0Hz~ 80kHz, pulse width 1 ~ 90%;By adjusting the bias amplitude of grid bias power supply (1) output, pulse frequency and pulse width, control Adjusting of the substrate work-piece to the effective attraction and ion energy of metallic plasma, carries out the deposition of film and controls low melting point The ratio of pure metal or multicomponent alloy material and nonmetallic materials in the film realizes pure metal film, different element ratio Compound ceramic film, function film and the film preparation with nanometer multilayer or gradient-structure, grid bias power supply (1) pass through pulse The duty ratio of frequency, pulsed bias amplitude and pulsed bias adjusts separately, and reaches substrate work-piece surface to control the unit time Arc-plasma energy peak intensity and density, grid bias power supply (1) output pulse is pulse, DC pulse is compound or more arteries and veins Rush compound, the microstructure and properties of prepared film are adjusted by the pulsed bias parameter of grid bias power supply (1), to electric arc The energy of plasma is adjusted, and realizes that energetic ion is raw to film using the amplitude, pulse width and frequency of pulsed bias Long pinning effect improves the texture and stress state of film growth, improves film substrate bond strength; It opens arc power (2), the surface in arc ion plating target source (3) is cleaned by the spots moving of electric arc, adjusting needs The technological parameter wanted, arc power (2) output current value be 10 ~ 300A, arc power (2) output electric current be direct current, pulse or Person's DC pulse is compound; The target body material that arc ion plating target source (3) uses is the pure metal of low melting point or multicomponent alloy target and non-metallic material Material breaches conventional arc ion plating target source (3) using the pure metal or multicomponent alloy material and nonmetallic materials of low melting point The flexible modulation of thin film composition and microstructure is realized in limitation; It opens multi-stage magnetic field power supply (5) and adjusts multi-stage magnetic field device (4), keep arc-plasma in arc ion plating target source (3) stablize and generate and elimination is filtered to bulky grain defect, arc-plasma is made to pass through multistage with higher efficiency of transmission Magnetic field device (4) recycles the adjustable magnetic field power supply of transmission direction (7) to adjust the adjustable magnetic field device of transmission direction (6), guarantees Arc-plasma reaches the substrate work-piece surface of any position in vacuum chamber, carries out the fast deposition of film, passes through multistage magnetic Field device (4) and the adjustable magnetic field device of transmission direction (6) realize the efficient of bulky grain removal of defect and arc-plasma Transmission; Ablation of the multi-stage magnetic field device (4) to electric arc on target surface control effectively, and eliminates " the steamed bun generated due to ablation unevenness Head target " phenomenon, realizes uniform ablation and the efficient utilization of target, multi-stage magnetic field device (4) eliminate bulky grain defect and guarantee from The high efficiency of transmission of arc-plasma of the rate close to 100%, the technique that multi-stage magnetic field device (4) combines arc ion plating target source Parameter is realized the ion ratio for being adjusted various elements in the compound plasma generated using more set precipitation equipments, realized different The fast deposition of the multi-component multi-layer film of element ratio; The adjustable magnetic field device of transmission direction (6) compensates for linear type Magnetic filter method and is unable to flexible modulation in the transmit direction Defect, be conducive to high ionization level plasma at an arbitrary position workpiece surface chemosynthesis reaction film forming, transmission direction is adjustable Formula magnetic field device (6) adjusts the transmission direction of arc-plasma in a vacuum chamber, realizes vacuum chamber (8) interior any position matrix The fast deposition of workpiece surface film; Step 1 is executed repeatedly to step 2, to prepare pure metal film, the compound ceramic film of different element ratios, function Film and film with nanometer multilayer or gradient-structure; Step 3: individually adjustable using conventional arc ion plating, pulsed cathode arc, multi-stage magnetic field filter device and transmission direction Magnetic field device combination Dc bias, pulsed bias or the compound bias of DC pulse carry out film deposition, come prepare pure metal film, Compound ceramic film, function film and the film with nanometer multilayer or gradient-structure of different element ratios.


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说明书

【中文】

传输方向可调式的多级磁场电弧离子镀方法

技术领域

本发明涉及传输方向可调式的多级磁场电弧离子镀方法,属于材料表面处理技术领域。

背景技术

电弧离子镀技术可以获得包括碳离子在内的几乎所有金属离子,同时以高离化率、绕射性好、膜基结合力好、涂层质量好、沉积效率高和设备操作简便等优点而受到重视,是目前在工业中得到广泛应用的物理气相沉积制备技术之一。其不仅可以用于制备金属防护涂层,还可以通过工艺方法的调节,实现氮化物、碳化物等高温陶瓷涂层的制备,同时在功能薄膜领域也有应用。即使对于形状非规则的零部件,电弧离子镀也可以实现薄膜的快速沉积,甚至也作为纳米多层和超晶格薄膜制备方法(Tay B K, Zhao Z W, Chua D H C.Review of metal oxide films deposited by filtered cathodic vacuum arctechnique [J]. Mater Sci Eng R, 2006, 52(1-3): 1-48.)。但是在电弧离子镀制备薄膜的过程中,由于弧斑电流密度高达2.5~5×1010A/m2,引起靶材表面的弧斑位置处出现熔融的液态金属,在局部等离子体压力的作用下以液滴的形式喷溅出来,附着在薄膜表面或镶嵌在薄膜中形成“大颗粒”(Macroparticles)缺陷(Boxman R L, Goldsmith S.Macroparticle contamination in cathodic arc coatings: generation, transportand control [J]. Surf Coat Tech, 1992, 52(1): 39-50.)。就像PM2.5对空气质量的污染一样,相对于厚度级别为微米或亚微米的薄膜,尺寸在0.1-10微米的大颗粒缺陷对薄膜的质量和性能有着严重的危害。随着薄膜材料和薄膜技术应用的日益广泛,大颗粒缺陷问题的解决与否成为电弧离子镀方法进一步发展的瓶颈,严重制约了其在新一代薄膜材料制备中的应用。

目前,为了解决电弧离子镀方法在使用低熔点的纯金属或多元合金材料易产生大颗粒缺陷的问题,目前主要采用磁过滤的办法过滤掉大颗粒,如中国专利用于材料表面改性的等离子体浸没离子注入装置(公开号:CN1150180,公开日期:1997年5月21日)中采用90°磁过滤弯管对脉冲阴极弧的大颗粒进行过滤,美国学者Anders等人(Anders S, AndersA, Dickinson M R, MacGill R A, Brown I G. S-shaped magnetic macroparticlefilter for cathodic arc deposition [J]. IEEE Trans Plasma Sci, 1997, 25(4):670-674.)和河南大学的张玉娟等(张玉娟, 吴志国, 张伟伟等. 磁过滤等离子体制备TiN薄膜中沉积条件对薄膜织构的影响. 中国有色金属学报. 2004, 14(8): 1264-1268.)制作了“S”磁过滤弯管对阴极弧的大颗粒进行过滤,还有美国学者Anders等人(Anders A,MacGill R A. Twist filter for the removal of macroparticles from cathodic arcplasmas [J]. Surf Coat Tech, 2000, 133-134: 96-100.)提出的Twist filter的磁过滤,这些方法虽然在过滤和消除大颗粒方面有一定效果,但是等离子体的传输效率损失严重,使离子流密度大大降低。基于即能过滤大颗粒又能保证效率的基础上,中国专利真空阴极弧直管过滤器(公开号:CN1632905,公开日期:2005年6月29日)中提出直管过滤的方法,但是这又降低了过滤效果。上海交通大学的戴华等人提出了一种可调式弯曲型磁过滤装置(Dai H, Shen Y, Li L, Li X, Cai X, Chu P K. A flexible curvilinearelectromagnetic filter for direct current cathodic arc source [J]. Rev SciInstrum, 2007, 78(9): 095103-095106.和戴华. 真空阴极电弧离子镀层中宏观颗粒去除技术研究 [D]; 上海交通大学博士论文, 2009.),可以通过调节过滤器弯道的曲率,在宏观颗粒去除效果以及镀膜效率之间取得平衡。1992年美国华生科学实验室的Lossy等人采用在等离子体出口处施加弯曲磁场,来改变等离子体的方向(Lossy R, Pappas D L,Roy R A, Cuomo J J, Sura V M. Filtered arc deposition of amorphous diamond[J]. Appl Phys Lett, 1992, 61(2): 171-173.),在直线型过滤装置出口的一端有一个可以将等离子体束沿着初始轴线偏离20°的磁场,实现大颗粒和等离子体的分离,消除了大颗粒对薄膜的不利影响。还有学者提出了磁岛式直线型磁过滤装置(Kleiman A, MarquezA, Boxman R L. Performance of a magnetic island macroparticle filter in atitanium vacuum arc [J]. Plasma Sources Sci Technol, 2008, 17(1): 015008.和Bolt H, Koch F, Rodet J L, Karpov D, Menzel S. Al2O3 coatings deposited byfiltered vacuum arc - characterization of high temperature properties [J].Surf Coat Tech, 1999, 116-119: 956-962.),通过在直线型磁场中间附加一个磁场,来改变等离子体的传输方向,同时阻挡大颗粒从直线型过滤器中输出。总之,相关的研究人员通过对比各种磁过滤方法(Anders A. Approaches to rid cathodic arc plasmas ofmacro- and nanoparticles: a review [J]. Surf Coat Tech, 1999, 120-121319-330.和Takikawa H, Tanoue H. Review of cathodic arc deposition for preparingdroplet-free thin films [J]. IEEE Trans Plasma Sci, 2007, 35(4): 992-999.)发现电弧离子镀等离子体通过磁过滤装置后保持高的传输效率和消除大颗粒非常难以兼顾,严重影响着该技术在优质薄膜沉积中的应用。

发明内容

本发明目的是为了为解决传统电弧离子镀方法易产生大颗粒缺陷、磁过滤技术引起电弧等离子体传输效率低和采用低熔点的纯金属或多元合金材料和非金属材料(比如石墨)作为靶材在传统电弧离子镀方法中存在的大颗粒、通过多级磁场直管磁过滤方法消除电弧等离子体中含有的大颗粒缺陷,同时保证电弧等离子体以较高的传输效率通过直管过滤装置,再利用传输方向可调式磁场装置使镀膜空间内任意位置的基体工件表面在施加负偏压的情况可以连续、致密的制备优质薄膜,实现对薄膜中元素含量添加控制、降低使用合金靶的生产成本、提高薄膜的沉积效率、减少放电不稳定性和大颗粒缺陷对薄膜生长和性能的不利影响,提出了传输方向可调式的多级磁场电弧离子镀方法。

本发明方法所使用装置包括偏压电源1、弧电源2、电弧离子镀靶源3、多级磁场装置4、多级磁场电源5、传输方向可调式磁场装置6、传输方向可调式磁场电源7、真空室8、样品台9;

该方法包括以下步骤:

步骤一、将待处理的基体工件置于真空室8内的样品台9上,工件接偏压电源1的脉冲输出端,安装在真空室8上的电弧离子镀靶源3接通弧电源2,多级磁场装置4接通多级磁场电源5,传输方向可调式磁场装置6接通传输方向可调式磁场电源7;

步骤二、薄膜沉积:将真空室8抽真空,待真空室8内的真空度小于10-2Pa时,通入工作气体至0.01Pa~10Pa;

开启偏压电源1,偏压电源1输出脉冲的峰值电压值为0~1.2kV,脉冲频率为0Hz~80kHz,脉冲宽度1~90%;通过调节偏压电源1输出的偏压幅值,脉冲频率和脉冲宽度,控制基体工件对金属等离子体的有效吸引和离子能量的调节,进行薄膜的沉积和控制低熔点的纯金属或多元合金材料及非金属材料(比如石墨)在薄膜中的比例,实现纯金属薄膜、不同元素比例的化合物陶瓷薄膜、功能薄膜及具有纳米多层或梯度结构的优质薄膜制备;

开启弧电源2,通过电弧的弧斑运动对电弧离子镀靶源3的表面进行清洗,调节需要的工艺参数,弧电源2输出的电流值为10~300A,开启多级磁场电源5调节多级磁场装置4,保持电弧等离子体在电弧离子镀靶源3稳定产生和对大颗粒缺陷进行过滤消除,使电弧等离子体以较高的传输效率通过多级磁场装置4,再利用传输方向可调式磁场电源7调节传输方向可调式磁场装置6,保证电弧等离子体到达真空室内任意位置的基体工件表面,进行薄膜的快速沉积。

本发明的优点:a. 多级磁场磁过滤装置可以消除大颗粒缺陷并保证离化率接近100%的电弧等离子体的高效传输;b. 多级磁场装置结合电弧离子镀靶源的工艺参数,可以实现利用多套沉积装置调节产生的复合等离子体中各种元素的离子比例,实现不同元素比例的多元多层薄膜的快速沉积;c. 传输方向可调式磁场装置可以调节电弧等离子体在真空室中的传输方向,实现真空室内任意位置基体工件表面薄膜的快速沉积;d. 可以利用磁场对电弧在靶表面的烧蚀进行有效控制,消除由于烧蚀不均产生的“馒头靶”现象,实现均匀烧蚀和靶材的高效利用;e. 所制备薄膜的微观结构和性能可以通过脉冲偏压参数进行调整,利用脉冲偏压的幅值、脉冲宽度和频率实现高能离子对薄膜生长的钉扎效应,改善薄膜生长的晶体组织和应力状态,提高膜基结合强度;f. 由于消除了低熔点的纯金属或多元合金材料和非金属材料(比如石墨)在电弧离子镀中的应用限制,可以实现原来多元薄膜制备过程中这些元素的添加和不同元素比例的灵活调整;g. 所制备的薄膜避免了低熔点元素的大颗粒缺陷,晶体组织更加致密,可以进一步提高薄膜的力学性能。

步骤三、可以单独采用传统电弧离子镀、脉冲阴极弧、多级磁场过滤装置和传输方向可调式磁场装置结合直流偏压、脉冲偏压或直流脉冲复合偏压进行薄膜沉积,来制备纯金属薄膜、不同元素比例的化合物陶瓷薄膜、功能薄膜及具有纳米多层或梯度结构的优质薄膜。

附图说明

图1是本发明传输方向可调式的多级磁场电弧离子镀方法简图,图2为偏压电源的脉冲波形图。

具体实施方式

具体实施方式一:下面结合图1和图2说明本实施方式,本实施方式传输方向可调式的多级磁场电弧离子镀方法所使用装置包括偏压电源1、弧电源2、电弧离子镀靶源3、多级磁场装置4、多级磁场电源5、传输方向可调式磁场装置6、传输方向可调式磁场电源7、真空室8、样品台9;

该方法包括以下步骤:

步骤一、将待处理的基体工件置于真空室8内的样品台9上,工件接偏压电源1的脉冲输出端,安装在真空室8上的电弧离子镀靶源3接通弧电源2,多级磁场装置4接通多级磁场电源5,传输方向可调式磁场装置6接通传输方向可调式磁场电源7;

步骤二、薄膜沉积:将真空室8抽真空,待真空室8内的真空度小于10-2Pa时,通入工作气体至0.01Pa~10Pa;

开启偏压电源1,偏压电源1输出脉冲的峰值电压值为0~1.2kV,脉冲频率为0Hz~80kHz,脉冲宽度1~90%;通过调节偏压电源1输出的偏压幅值,脉冲频率和脉冲宽度,控制基体工件对金属等离子体的有效吸引和离子能量的调节,进行薄膜的沉积和控制低熔点的纯金属或多元合金材料及非金属材料(比如石墨)在薄膜中的比例,实现纯金属薄膜、不同元素比例的化合物陶瓷薄膜、功能薄膜及具有纳米多层或梯度结构的优质薄膜制备;

开启弧电源2,通过电弧的弧斑运动对电弧离子镀靶源3的表面进行清洗,调节需要的工艺参数,弧电源2输出的电流值为10~300A,开启多级磁场电源5调节多级磁场装置4,保持电弧等离子体在电弧离子镀靶源3稳定产生和对大颗粒缺陷进行过滤消除,使电弧等离子体以较高的传输效率通过多级磁场装置4,再利用传输方向可调式磁场电源7调节传输方向可调式磁场装置6,保证电弧等离子体到达真空室内任意位置的基体工件表面,进行薄膜的快速沉积。

偏压电源1输出波形为直流、单脉冲、直流脉冲复合或多脉冲复合。

弧电源2输出直流、单脉冲、直流脉冲复合或多脉冲复合。

电弧离子镀靶源3采用高熔点或低熔点的纯金属或多元合金材料,可以使用单个靶、多个靶或复合靶,进行纯金属薄膜、不同元素比例的化合物陶瓷薄膜、功能薄膜、多元多层、超晶格、具有纳米多层或梯度结构的优质薄膜。

工作气体选用氩气,或工作气体选用氮气、乙炔、甲烷、硅烷或氧气中一种或多种的混合气体,来制备纯金属薄膜、不同元素比例的化合物陶瓷薄膜、功能薄膜、多元多层、超晶格、具有纳米多层或梯度结构的薄膜。

传输方向可调式的多级磁场电弧离子镀方法的提出,为电弧离子镀的进一步推广应用创造了有利条件,可以充分利用电弧离子镀技术的产生稳定持续、离化率高的金属等离子体,通过多级磁场装置清除大颗粒缺陷和实现电弧等离子体的高效传输,同时弥补了直线型磁过滤方法在传输方向上不能灵活调节的缺陷,有利于高离化率等离子体在任意位置工件表面的化学合成反应成膜;同时结合偏压电场,对电弧等离子体的能量进行调节,制备不同元素比例的化合物陶瓷薄膜、功能薄膜、多元多层、超晶格和具有梯度结构的薄膜或纯金属薄膜。

具体实施方式二:本实施方式与实施方式一的不同之处在于,该方法还包括:

步骤三、可以单独采用传统电弧离子镀、脉冲阴极弧、多级磁场过滤装置和传输方向可调式磁场装置结合直流偏压、脉冲偏压或直流脉冲复合偏压进行薄膜沉积,来制备纯金属薄膜、不同元素比例的化合物陶瓷薄膜、功能薄膜及具有纳米多层或梯度结构的优质薄膜。

具体实施方式三:本实施方式与实施方式一的不同之处在于,反复执行步骤一至步骤三,制备具有不同应力状态、微观结构和元素比例的多层结构薄膜,其他与实施方式一相同。

具体实施方式四:本实施方式与实施方式一的不同之处在于,反复执行步骤一至步骤三,制备具有不同应力状态、微观结构和元素比例的多层结构薄膜,其他与实施方式一相同。

步骤二中可以使用2套或者以上的电弧离子镀靶源3、多级磁场装置4和调节传输方向可调式磁场装置6配合的电弧离子镀装置进行以各种纯金属元素和多元合金材料为靶材的薄膜沉积,然后进行步骤三,然后反复执行步骤二和步骤三,如此反复,制备具有不同应力状态、微观结构、元素比例和多元多层结构的薄膜。

【EN】

The adjustable multi-stage magnetic field arc ions electroplating method of transmission direction

Technical field

The present invention relates to the adjustable multi-stage magnetic field arc ions electroplating methods of transmission direction, belong to surface treatment technology of material

Field.

Background technique

Arc ion plating (aip) can obtain nearly all metal ion including carbon ion, while with high ionization

Rate, it is diffractive good, film-substrate cohesion is good, coating quality is good, deposition efficiency is high and equipment operation is easy the advantages that and be taken seriously,

It is one of the physical vapour deposition (PVD) technology of preparing being used widely in the industry at present.It is anti-that it can be not only used for preparing metal

Coating is protected, can also be by the adjusting of process, the preparation of the high-temperature ceramic coatings such as realization nitride, carbide, while

Also there is application in function film field.Even for the irregular components of shape, the fast of film is also may be implemented in arc ion plating

Speed deposition, or even also it is used as nanometer multilayer and superlattice film preparation method (Tay B K, Zhao Z W, Chua D H C.

Review of metal oxide films deposited by filtered cathodic vacuum arc

Technique [J] Mater Sci Eng R, 2006,52 (1-3): 1-48.).But it is prepared in arc ion plating thin

During film, since arc spot current density is up to 2.5 ~ 5 × 1010A/m2, cause to melt at the arc spot position of target material surface

The liquid metal melted, splash comes out in droplets under the action of local plasma pressure, be attached to film surface or

Inlay formation " bulky grain " (Macroparticles) defect (Boxman R L, Goldsmith S. in the film

Macroparticle contamination in cathodic arc coatings: generation, transport

And control [J] Surf Coat Tech, 1992,52 (1): 39-50.).Dirt just as PM2.5 to air quality

Dye is the same, is the film of micron or sub-micron relative to thickness rank, and size is in 0.1-10 microns of bulky grain defect to film

Quality and performance have serious harm.As thin-film material and thin film technique are applied increasingly extensive, bulky grain defect is asked

The bottleneck for becoming arc ions electroplating method whether solution and further developing of topic, seriously constrains it in thin-film material system of new generation

Application in standby.

Currently, in order to solve arc ions electroplating method using low melting point pure metal or multicomponent alloy material be also easy to produce greatly

It is the problem of grain defect, main at present that bulky grain is filtered out using the method for Magnetic filter, as Chinese patent changes for material surface

Property plasma immersion and ion implantation device (publication number: CN1150180, publication date: on May 21st, 1997) in use

90 ° of magnetic filters are filtered the bulky grain of pulsed cathode arc, American scholar Anders et al. (Anders S, Anders

A, Dickinson M R, MacGill R A, Brown I G. S-shaped magnetic macroparticle

filter for cathodic arc deposition [J]. IEEE Trans Plasma Sci, 1997, 25(4):

670-674.) and the Zhang Yujuan of He'nan University etc. (the filtered cathode arc plasma such as Zhang Yujuan, Wu Zhiguo, Zhang Weiwei prepares TiN

In film sedimentary condition to film texture influence China YouSe Acta Metallurgica Sinica 2004,14 (8): 1264-1268.) system

Made " S " magnetic filter to be filtered the bulky grain of cathode arc, there are also American scholar Anders et al. (Anders A,

MacGill R A. Twist filter for the removal of macroparticles from cathodic arc

Plasmas [J] Surf Coat Tech, 2000,133-134:96-100.) propose Twist filter magnetic mistake

Filter, although these methods have certain effect in terms of filtering and eliminating bulky grain, the efficiency of transmission loss of plasma is tight

Weight, substantially reduces ion current density.Based on can filter on the basis of bulky grain can guarantee efficiency again, Chinese patent vacuum yin

The method that straight tube filtering is proposed in polar arc straight filter (publication number: CN1632905, publication date: on June 29th, 2005),

But which in turn reduces filter effects.Dai Hua of Shanghai Communications University et al. proposes a kind of adjustable flexure type magnetic filter

(Dai H, Shen Y, Li L, Li X, Cai X, Chu P K. A flexible curvilinear

electromagnetic filter for direct current cathodic arc source [J]. Rev Sci

Instrum, 2007,78 (9): macroscopic particles are gone in 095103-095106. and Dai Hua vacuum cathode arc ion plating layer

Except technical research [D];Shanghai Communications University's doctoral thesis, 2009.), can by adjusting the curvature of filter bend,

Balance is obtained between macroscopic particles removal effect and plating membrane efficiency.The Lossy et al. of the research laboratory Hua Sheng, the U.S. in 1992

Using at plasma exit apply bent magnetic field, come change plasma direction (Lossy R, Pappas D L,

Roy R A, Cuomo J J, Sura V M. Filtered arc deposition of amorphous diamond

[J] Appl Phys Lett, 1992,61 (2): 171-173.), there is one in one end of linear type filter device outlet

It can realize the separation of bulky grain and plasma by plasma beam along 20 ° of initial axis runout of magnetic field, eliminate big

Adverse effect of the particle to film.There are also scholars to propose magnetic island formula linear type magnetic filter (Kleiman A, Marquez

A, Boxman R L. Performance of a magnetic island macroparticle filter in a

Titanium vacuum arc [J] Plasma Sources Sci Technol, 2008,17 (1): 015008. He

Bolt H, Koch F, Rodet J L, Karpov D, Menzel S. Al2O3 coatings deposited by

filtered vacuum arc - characterization of high temperature properties [J].

Surf Coat Tech, 1999,116-119:956-962.), by adding a magnetic field among linear type magnetic field, come

Change the transmission direction of plasma, while bulky grain being stopped to export from straight line type filter.In short, relevant researcher

By comparing various Magnetic filter method (Anders A. Approaches to rid cathodic arc plasmas of

macro- and nanoparticles: a review [J]. Surf Coat Tech, 1999, 120-121319-330.

With Takikawa H, Tanoue H. Review of cathodic arc deposition for preparing

Droplet-free thin films [J] IEEE Trans Plasma Sci, 2007,35 (4): 992-999.) hair

Existing arc ion plating plasma keeps high efficiency of transmission and elimination bulky grain to be very difficult to take into account after passing through magnetic filter,

Drastically influence application of the technology in high-quality thin-film deposition.

Summary of the invention

The invention aims to solve, conventional arc ion electroplating method is also easy to produce bulky grain defect, Magnetic filter technology is drawn

Play arc-plasma transmission efficiency is low and using low melting point pure metal or multicomponent alloy material and nonmetallic materials (such as stone

Ink) it is eliminated as target bulky grain present in conventional arc ion electroplating method, by multi-stage magnetic field straight tube Magnetic filter method

The bulky grain defect contained in arc-plasma, while guaranteeing that arc-plasma passes through straight tube mistake with higher efficiency of transmission

Device is filtered, the adjustable magnetic field device of transmission direction is recycled to keep the substrate work-piece surface of any position in plated film space negative in application

The case where bias, continuous, densification can prepare high-quality thin-film, realize and control constituent content addition in film, reduce to use and close

The production cost of gold target, the deposition efficiency for improving film reduce discharge instability and bulky grain defect to film growth and property

The adverse effect of energy, proposes the adjustable multi-stage magnetic field arc ions electroplating method of transmission direction.

The method of the present invention institute use device includes grid bias power supply 1, arc power 2, arc ion plating target source 3, multi-stage magnetic field dress

Set the adjustable magnetic field device 6 of 4, multi-stage magnetic field power supply 5, transmission direction, the adjustable magnetic field power supply 7 of transmission direction, vacuum chamber 8, sample

Sample platform 9;

Method includes the following steps:

Step 1: substrate work-piece to be processed is placed on the sample stage 9 in vacuum chamber 8, workpiece connects the arteries and veins of grid bias power supply 1

Output end is rushed, arc power 2 is connected in the arc ion plating target source 3 being mounted on vacuum chamber 8, and multi-stage magnetic field device 4 connects multistage magnetic

Field ionization source 5, the adjustable magnetic field device 6 of transmission direction connect the adjustable magnetic field power supply 7 of transmission direction;

Step 2: film deposits: vacuum chamber 8 being vacuumized, to the vacuum degree in vacuum chamber 8 less than 10-2When Pa, it is passed through work

Make gas to 0.01Pa~10Pa;

Open grid bias power supply 1, grid bias power supply 1 export pulse peak voltage be 0~1.2kV, pulse frequency be 0Hz~

80kHz, pulse width 1 ~ 90%;The bias amplitude exported by adjusting grid bias power supply 1, pulse frequency and pulse width, control base

Adjusting of the body workpiece to the effective attraction and ion energy of metallic plasma, carries out the deposition of film and controls the pure of low melting point

The ratio of metal or multicomponent alloy material and nonmetallic materials (such as graphite) in the film realizes pure metal film, different members

It the compound ceramic film of plain ratio, function film and is prepared with the high-quality thin-film of nanometer multilayer or gradient-structure;

Arc power 2 is opened, the surface in arc ion plating target source 3 is cleaned by the spots moving of electric arc, adjusting needs

The technological parameter wanted, the current value that arc power 2 exports are 10 ~ 300A, open multi-stage magnetic field power supply 5 and adjust multi-stage magnetic field device 4,

It keeps arc-plasma to stablize generation in arc ion plating target source 3 and be filtered elimination to bulky grain defect, makes electric arc etc.

Gas ions, by multi-stage magnetic field device 4, recycle the adjustable magnetic field power supply 7 of transmission direction to adjust transmission with higher efficiency of transmission

Direction-adjustable magnetic field device 6 guarantees that arc-plasma reaches the substrate work-piece surface of any position in vacuum chamber, carries out thin

The fast deposition of film.

Advantages of the present invention: a. multi-stage magnetic field magnetic filter can eliminate bulky grain defect and guarantee that ionization level is close

The high efficiency of transmission of 100% arc-plasma;B. the technological parameter in multi-stage magnetic field device combination arc ion plating target source, can be with

It realizes the ion ratio for adjusting various elements in the compound plasma generated using more set precipitation equipments, realizes different element ratios

The fast deposition of the multi-component multi-layer film of example;C. the adjustable arc-plasma of the adjustable magnetic field device of transmission direction is true

Transmission direction in empty room realizes the fast deposition of any position substrate work-piece surface film in vacuum chamber;D. it can use magnetic

Ablation of the field to electric arc on target surface control effectively, and eliminates " steamed bun target " phenomenon generated due to ablation unevenness, realizes equal

The efficient utilization of even ablation and target;E. the microstructure and properties of prepared film can be carried out by pulsed bias parameter

Adjustment is realized the pinning effect that energetic ion grows film using the amplitude, pulse width and frequency of pulsed bias, is improved thin

The texture and stress state of film growth, improve film substrate bond strength;F. due to eliminating the pure metal of low melting point or polynary

The application limitation of alloy material and nonmetallic materials (such as graphite) in arc ion plating, may be implemented original multi-element film system

The addition of these elements and being adjusted flexibly for different element ratios during standby;G. prepared film avoids low melting point member

The bulky grain defect of element, texture is finer and close, can be further improved the mechanical property of film.

Step 3: conventional arc ion plating, pulsed cathode arc, multi-stage magnetic field filter device and transmission side can individually be used

Film deposition is carried out to adjustable magnetic field device combination Dc bias, pulsed bias or the compound bias of DC pulse, it is pure to prepare

Metallic film, the compound ceramic film of different element ratio, function film and high-quality with nanometer multilayer or gradient-structure

Film.

Detailed description of the invention

Fig. 1 is the adjustable multi-stage magnetic field arc ions electroplating method schematic diagram of transmission direction of the present invention, and Fig. 2 is grid bias power supply

Timing chart.

Specific embodiment

Specific embodiment 1: illustrating present embodiment below with reference to Fig. 1 and Fig. 2, present embodiment transmission direction is adjustable

The multi-stage magnetic field arc ions electroplating method institute use device of formula includes grid bias power supply 1, arc power 2, arc ion plating target source 3, more

It is grade magnetic field device 4, multi-stage magnetic field power supply 5, the adjustable magnetic field device 6 of transmission direction, the adjustable magnetic field power supply 7 of transmission direction, true

Empty room 8, sample stage 9;

Method includes the following steps:

Step 1: substrate work-piece to be processed is placed on the sample stage 9 in vacuum chamber 8, workpiece connects the arteries and veins of grid bias power supply 1

Output end is rushed, arc power 2 is connected in the arc ion plating target source 3 being mounted on vacuum chamber 8, and multi-stage magnetic field device 4 connects multistage magnetic

Field ionization source 5, the adjustable magnetic field device 6 of transmission direction connect the adjustable magnetic field power supply 7 of transmission direction;

Step 2: film deposits: vacuum chamber 8 being vacuumized, to the vacuum degree in vacuum chamber 8 less than 10-2When Pa, it is passed through work

Make gas to 0.01Pa~10Pa;

Open grid bias power supply 1, grid bias power supply 1 export pulse peak voltage be 0~1.2kV, pulse frequency be 0Hz~

80kHz, pulse width 1 ~ 90%;The bias amplitude exported by adjusting grid bias power supply 1, pulse frequency and pulse width, control base

Adjusting of the body workpiece to the effective attraction and ion energy of metallic plasma, carries out the deposition of film and controls the pure of low melting point

The ratio of metal or multicomponent alloy material and nonmetallic materials (such as graphite) in the film realizes pure metal film, different members

It the compound ceramic film of plain ratio, function film and is prepared with the high-quality thin-film of nanometer multilayer or gradient-structure;

Arc power 2 is opened, the surface in arc ion plating target source 3 is cleaned by the spots moving of electric arc, adjusting needs

The technological parameter wanted, the current value that arc power 2 exports are 10 ~ 300A, open multi-stage magnetic field power supply 5 and adjust multi-stage magnetic field device 4,

It keeps arc-plasma to stablize generation in arc ion plating target source 3 and be filtered elimination to bulky grain defect, makes electric arc etc.

Gas ions, by multi-stage magnetic field device 4, recycle the adjustable magnetic field power supply 7 of transmission direction to adjust transmission with higher efficiency of transmission

Direction-adjustable magnetic field device 6 guarantees that arc-plasma reaches the substrate work-piece surface of any position in vacuum chamber, carries out thin

The fast deposition of film.

1 output waveform of grid bias power supply is direct current, pulse, DC pulse is compound or multiple-pulse is compound.

The output of arc power 2 direct current, pulse, DC pulse is compound or multiple-pulse is compound.

Arc ion plating target source 3 can be used single using high-melting-point or the pure metal or multicomponent alloy material of low melting point

Target, multiple targets or composition target carry out pure metal film, the compound ceramic film of different element ratio, function film, polynary more

Layer, superlattices, the high-quality thin-film with nanometer multilayer or gradient-structure.

It is one or more in nitrogen, acetylene, methane, silane or oxygen that working gas selects argon gas or working gas to select

Mixed gas, to prepare pure metal film, the compound ceramic film of different element ratio, function film, multi-component multi-layer, super

Lattice, the film with nanometer multilayer or gradient-structure.

The it is proposed of the adjustable multi-stage magnetic field arc ions electroplating method of transmission direction is the further genralrlization of arc ion plating

Using advantage is created, the generation of arc ion plating (aip) can be made full use of to stablize lasting, metal that ionization level is high etc.

Gas ions remove bulky grain defect by multi-stage magnetic field device and realize the high efficiency of transmission of arc-plasma, compensate for simultaneously

Linear type Magnetic filter method is unable to the defect of flexible modulation in the transmit direction, is conducive to high ionization level plasma in any position

Set the chemosynthesis reaction film forming of workpiece surface;In combination with biasing electric field, the energy of arc-plasma is adjusted, is made

The compound ceramic films of standby different element ratios, function film, multi-component multi-layer, superlattices and film with gradient-structure or

Pure metal film.

Specific embodiment 2: present embodiment and embodiment one the difference is that, this method further include:

Step 3: conventional arc ion plating, pulsed cathode arc, multi-stage magnetic field filter device and transmission side can individually be used

Film deposition is carried out to adjustable magnetic field device combination Dc bias, pulsed bias or the compound bias of DC pulse, it is pure to prepare

Metallic film, the compound ceramic film of different element ratio, function film and high-quality with nanometer multilayer or gradient-structure

Film.

Specific embodiment 3: present embodiment and embodiment one the difference is that, execute step 1 extremely repeatedly

Step 3 prepares the multilayer films with different stress, microstructure and element ratio, other and embodiment one

It is identical.

Specific embodiment 4: present embodiment and embodiment one the difference is that, execute step 1 extremely repeatedly

Step 3 prepares the multilayer films with different stress, microstructure and element ratio, other and embodiment one

It is identical.

2 sets or above arc ion plating target source 3, multi-stage magnetic field device 4 and adjusting transmission can be used in step 2

The arc ion plating apparatus that direction-adjustable magnetic field device 6 cooperates is carried out using various pure metal elements and multicomponent alloy material as target

The film of material deposits, and then carries out step 3, then executes step 2 and step 3 repeatedly, and repeatedly, preparation has difference

Stress state, microstructure, element ratio and multi-component multi-layer structure film.

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