CN1727514A - 溅射靶及其制备方法 - Google Patents

溅射靶及其制备方法 Download PDF

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CN1727514A
CN1727514A CNA2005100713029A CN200510071302A CN1727514A CN 1727514 A CN1727514 A CN 1727514A CN A2005100713029 A CNA2005100713029 A CN A2005100713029A CN 200510071302 A CN200510071302 A CN 200510071302A CN 1727514 A CN1727514 A CN 1727514A
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J·E·M·范德尔斯特雷藤
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
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    • C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
    • C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
    • C23C14/34—Sputtering
    • C23C14/3407—Cathode assembly for sputtering apparatus, e.g. Target
    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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    • C03C17/00—Surface treatment of glass, not in the form of fibres or filaments, by coating
    • C03C17/22—Surface treatment of glass, not in the form of fibres or filaments, by coating with other inorganic material
    • C03C17/23—Oxides
    • C03C17/245—Oxides by deposition from the vapour phase
    • C03C17/2456—Coating containing TiO2
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    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
    • C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
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    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/04—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the coating material
    • C23C4/10—Oxides, borides, carbides, nitrides or silicides; Mixtures thereof
    • C23C4/11—Oxides
    • C—CHEMISTRY; METALLURGY
    • C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
    • C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
    • C23C4/12—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge characterised by the method of spraying
    • C23C4/134—Plasma spraying
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2217/00—Coatings on glass
    • C03C2217/20—Materials for coating a single layer on glass
    • C03C2217/21—Oxides
    • C03C2217/212—TiO2
    • C—CHEMISTRY; METALLURGY
    • C03—GLASS; MINERAL OR SLAG WOOL
    • C03C—CHEMICAL COMPOSITION OF GLASSES, GLAZES OR VITREOUS ENAMELS; SURFACE TREATMENT OF GLASS; SURFACE TREATMENT OF FIBRES OR FILAMENTS MADE FROM GLASS, MINERALS OR SLAGS; JOINING GLASS TO GLASS OR OTHER MATERIALS
    • C03C2218/00—Methods for coating glass
    • C03C2218/10—Deposition methods
    • C03C2218/15—Deposition methods from the vapour phase
    • C03C2218/154—Deposition methods from the vapour phase by sputtering

Abstract

一种制备溅射靶的方法，该靶含有亚化学计量二氧化钛TiOx，其中x小于2，电导率小于0.5ohm.cm，还可以与二氧化铌混合，该方法包括在缺氧和不含含氧化合物的气氛中，在靶基底上以等离子喷涂二氧化钛TiO2，还可以是喷涂与氧化铌的混合物，在防止亚化学计量的二氧化钛与氧结合的条件下，经冷却固化的TiOx即被涂覆到靶基底上。

Description

溅射靶及其制备方法
本发明是申请日为1997年1月3日、进入国家阶段申请号为97192593.3的题为“溅射靶及其制备方法”的国际申请(PCT/EP97/00020)的分案申请。
技术领域
本发明涉及一种改进的高速溅射靶的制备方法，尤其涉及一种具有高电导率的含有亚化学计量二氧化钛的，用于大功率D.C.溅射的溅射靶的制备方法。
背景技术
通常用各种氧化物(如二氧化硅)和氮化物(如氮化硅)的溅射涂层在多种衬底上形成具有重要特性的光学涂层。已知这种光学涂层的应用场合包括玻璃窗上的低辐射率膜，反射镜上的冷反射镜，镜框玻璃或TV屏幕上照相版和防反射涂层的增强镜。通常这些涂层都是由几种不同反射指数的不同涂层叠加而成，优选地将高低反射指数的涂层相结合，生产滤光片。对于防反射涂层，优选地将可能呈现最高和最低反射指数的两种材料相结合。这种材料是二氧化钛和二氧化硅。这些材料的另一个优点是耐用性强。对玻璃窗上的低辐射率膜来说，优选地将银涂层与一种高反射指数的材料相结合，以减少银层的反射，改进光的透射。
二氧化钛涂层具有很高的反射指数，由此它能用于提供高反射指数的涂层，或者为光学叠加层提供高反射指数的涂层。生产二氧化钛涂层的现有工艺包括使用钛金属作为溅射靶，使用氧气作为等离子气体中的一个组分。由此在溅射过程中将钛转变成二氧化钛。尽管这种工艺能够生产出满意的二氧化钛涂层，但是沉积速率非常低，比用氧化锌和/或氧化锡涂覆的速率低得多。
作为二氧化钛的代用材料，建议使用另一种材料如氧化铌。尽管可以使用铌金属靶，以稍高于采用钛的等同方法的速率在衬底上涂布二氧化铌，但铌非常昂贵。
JP-A-07-233469描述了一种通过在非氧化气氛中以热压二氧化钛粉末，并将压制品烧结成块来制备溅射靶的方法。烧结后的压制品含有TiOx，其中1＜x＜2，电阻率为10ohm.cm，它对大功率的D.C溅射来说太高了。而溅射过程的稳定性和电弧速率两者都极大地取决于靶的电导率，尤其是在大功率下。
JP-A-62-161945描述了一种生产陶瓷溅射靶的方法，其中采用水等离子体喷涂主要含有ZrO2、TiO2、SiO2、Ta2O3、Al2O3、Fe2O3或这些材料混合物的陶瓷材料，以生产一种可用作溅射靶的成形体。该溅射靶用于非导电靶材料的高频率溅射。
因此，需要一种改进的含有亚化学计量TiO2的溅射靶的制备方法，该方法不包括JP-A-07-233469的热压和烧结步骤，能够生产出电导率足够高的可用作大功率下复杂形状的大型靶。
发明内容
目前，我们意外地发现，可在大功率下从含有亚化学计量二氧化钛的靶可以D.C.溅射二氧化钛，在衬底上提供一种亚化学计量或化学计量的涂层。
因此，本发明提供了一种制备溅射靶的方法，该靶含有亚化学计量二氧化钛TiOx，其中x小于2，电导率小于0.5ohm.cm，还可以与二氧化铌混合，该方法包括在缺氧和不含含氧化合物的气氛中，在靶基底上以等离子喷涂二氧化钛TiO2，还可以是喷涂与氧化铌的混合物，在防止亚化学计量的二氧化钛与氧结合的条件下，经冷却固化的TiOx即被涂覆到靶基底上。
亚化学计量的二氧化钛TiOx，其中x小于2，在已有技术领域，已知x通常从1.55到1.95。当根据本发明的方法生产溅射靶时，电导率将会改变，这取决于化学计量，最优选的电导率为0.02ohm.cm。
在实施本发明方法时，将二氧化钛TiO2以等离子溅射在靶基底上，如衬管或衬板，例如导电材料的靶基底，如不锈钢或钛金属、铝或铜。靶可以是任何一种已有技术公知类型的靶，例如转动靶或平面磁控靶。
在等离子喷涂过程中，等离子火焰对二氧化钛作用，使二氧化钛从其晶格失去一些氧原子，优选地从其颗粒表面失去氧原子。二氧化钛被转变成亚化学计量形式，即偏离化学计量的缺氧的二氧化钛。用于等离子喷涂的主要等离子气体最好是氩气，可用氢气作次要等离子气体，以便使颗粒温度达到最高。经等离子喷涂的二氧化钛最好其粒径在1-60微米的范围内，优选地从1微米到20微米。在防止亚化学计量的二氧化钛再获取氧转以再变成TiO2的条件下，对涂覆在靶基底上的亚化学计量的二氧化钛进行固化。优选地在等离子喷涂过程中，对靶基底进行水冷却，以便使呈亚化学计量的二氧化钛骤冷，并改进其电导率。为了生产出高温等离子体和有助于还原，至关重要的是在等离子气体中使用一定量的氢气或氮气。由于氢具有还原能力，所以优选地使用氢。优选地使用高于2000℃的颗粒温度，更优选的是2500℃。
在本发明的一特殊实施例中，可将二氧化钛与氧化铌一起以等离子喷涂。
另一方面，本发明还提供一种制备亚化学计量二氧化钛TiOx的方法，其中x小于2，电导率小于0.1ohm.cm，该方法包括在缺氧和不含含氧化合物的气氛中，对二氧化钛进行等离子处理。在实施该方法时，优选地通过等离子火焰喷涂二氧化钛，例如采用氩气和氢气的混合物作为等离子气体的等离子火焰。优选地等离子火焰在高温下操纵，以将颗粒的温度升高到2000℃以上。
根据本发明方法生产的溅射靶具有很高的电导率，无需昂贵的电弧折流器、或D.C.开关式电源、或其中用中等频率电源将两个靶连续用作阳极和阴极的Twin-mag系统、或任何气体控制系统特殊要求，就可采用传统的D.C.电源，在大功率下运行。采用本发明方法生产的靶，可在高达100Kw的功率下进行D.C.溅射。主要结论是在如长3.5m、直径150mm的可转动的大型靶基底上可涂覆厚达6mm的涂层。
由于二氧化钛的熔点比金属钛高，所以用本发明方法生产的靶不会有明显的电弧问题，所谓的“蒸汽电弧”问题是由于金属的熔点较低而引起的。即使对二氧化钛出现一些电弧，对靶几乎无损害。
具体实施方式
下面参照实施例对本发明进行进一步描述。
实施例1
一个在内部水冷到35℃的可转动的靶，包括一个直径为133mm、长为800mm的不锈钢管，采用氩气作为主等离子气体，氢气作为次等离子气体，如上所述通过等离子喷涂粒径为10-40μm的二氧化钛(金红石)，在靶上涂覆厚度为4-10mm的亚化学计量的二氧化钛TiOx，其中x小于2。使用了72升气体(60％氩，40％氢)。功率是45Kw(455A，96V)。
实施例2
使用市场有售的呈锐钛矿晶体形式的含有二氧化钛的白颜料。这种粉末是化学计量的并且是电绝缘的。将粉末机械成团并压成薄片，经研磨、筛分(70-100μm)并在空气中于1300℃下烧结。然后将烧结体进行研磨，并筛分成粒径为10-40μm的颗粒。颗粒是具有金红石晶体结构的黄的化学计量的不导电的二氧化钛。
用氩气作为主等离子气，氢气作为次等离子气，通过等离子喷涂上述金红石粉末，以制备由铝衬管(长2.50m，直径133mm)构成的可转动的靶。使用了75升气体(40％氩，60％氢)。功率是50Kw(110V，455A)。在氮气气氛下进行等离子喷涂。
靶以100rpm的转速转动，喷管移动速度是2.5m/min，直到涂层为4mm厚。铝管的内侧用水冷却到35℃的温度。涂覆后靶的电阻率为0.07ohm.cm。接着在高达100Kw的功率下，对靶进行试验，在溅射设备中靶运行状况良好，没有明显的电弧产生。其二氧化钛的沉积速率比用反应气体溅涂金属钛靶的沉积速率高6倍。
实施例3
在200mBar的压力下，使用粒径为1-10μm的呈锐钛矿类型的二氧化钛，用低压真空等离子体重复实施例2。采用低压等离子体，可使用较小粒径的粉末。
在实施例2的条件下，在靶基底上进行喷涂，锐钛矿被转化成亚化学计量的金红石类型的二氧化钛。涂覆后的靶的电阻率为0.02ohm.cm。
实施例4
对粒径为0.1-2μm的氧化铌(重量占25份)和二氧化钛(重量占75份)的混合物进行成团和压实，干燥后在空气中于1300℃的温度下进行烧结。然后将烧结体研磨成粒径为10-40μm的颗粒。
然后在实施例2给定的条件下，在铝衬管上，将粉末混合物以等离子喷涂成4mm的涂层。涂覆后的靶的电阻率为0.5ohm.cm，因此可用作D.C.溅射靶。

Claims (16)

1、一种制备溅射靶的方法，该靶含有亚化学计量的二氧化钛TiOx，其中x小于2，该方法包括在缺氧和不含含氧化合物的气氛中，在靶基底上以等离子喷涂二氧化钛TiO2，在防止亚化学计量的二氧化钛与氧结合的条件下，经冷却固化的TiOx即被涂覆到靶基底上。
2、权利要求1的方法，其特征在于，在等离子喷涂过程中，对靶基底进行水冷却。
3、权利要求1或2的方法，其特征在于，使用氩气作为等离子气体，氢气作为次等离子气体进行等离子喷涂。
4、前述权利要求之一的方法，其特征在于，靶基底是钛、不锈钢、铝或铜。
5、权利要求4的方法，其特征在于，靶基底是可转动的靶或平面磁控靶。
6、前述权利要求之一的方法，其特征在于，进行等离子喷涂的二氧化钛的粒径在1-60微米的范围内。
7、前述权利要求之一的方法，其特征在于，经等离子喷涂的是二氧化钛与Nb2O3的混合物。
8、前述权利要求之一的方法，其特征在于，亚化学计量的二氧化钛TiOx的x值在1.55到1.95的范围内。
9、前述权利要求之一的方法，其特征在于，溅射靶的电导率小于0.5ohm.cm。
10、前述权利要求之一的方法，其特征在于，溅射靶的电导率大约为0.02ohm.cm。
11、一种溅射靶，该靶含有亚化学计量二氧化钛TiOx，其中x小于2，该溅射靶可通过下列方法得到，在缺氧和不含含氧化合物的气氛中，在靶基底上等离子喷涂二氧化钛TiO2，在防止亚化学计量的二氧化钛与氧结合的条件下，经冷却固化的TiOx即被涂覆到靶基底上。
12、权利要求11的溅射靶，其特征在于，其电导率小于0.5ohm.cm。
13、权利要求11的溅射靶，其特征在于，其电导率大约为0.02ohm.cm。
14、一种制备亚化学计量二氧化钛TiOx的方法，其中x小于2，电导率小于0.1ohm.cm，该方法包括在缺氧和不含任何含氧化合物的气氛中，对二氧化钛进行等离子处理。
15、权利要求14的方法，其特征在于，通过温度高于2000℃的等离子火焰喷涂二氧化钛。
16、权利要求15的方法，其特征在于，等离子火焰采用氩气和氢气的混合物作为等离子气体。
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