CN1208495C - 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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CN1208495C
CN1208495C CNB971925933A CN97192593A CN1208495C CN 1208495 C CN1208495 C CN 1208495C CN B971925933 A CNB971925933 A CN B971925933A CN 97192593 A CN97192593 A CN 97192593A CN 1208495 C CN1208495 C CN 1208495C
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J·E·M·范德尔斯特雷藤
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    • C23C4/00—Coating by spraying the coating material in the molten state, e.g. by flame, plasma or electric discharge
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    • C03C2217/212—TiO2
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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。
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。
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，电阻率小于0.5ohm.cm，还可以与氧化铌混合，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，最优选的电阻率为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，电阻率小于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。
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 (10)

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，其电阻率小于0.5ohm.cm，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，其中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，并且进行等离子喷涂的二氧化钛的粒径在1-60微米的范围内。
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的方法，其特征在于，靶基底是钛、不锈钢、铝或铜。
4、权利要求3的方法，其特征在于，靶基底是可转动的靶或平面磁控靶。
5.权利要求1的方法，其特征在于，与氧化铌一起等离子喷涂二氧化钛以便形成含有亚化学计量的二氧化钛和氧化铌的溅射靶。
6、权利要求1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。
7、权利要求1的方法，其特征在于，溅射靶的电阻率为0.02ohm.cm。
8、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，其电阻率小于0.5ohm.cm，该溅射靶是通过下列方法得到的，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，其中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，并且进行等离子喷涂的二氧化钛的粒径在1-60微米的范围内。
9、权利要求8的溅射靶，其特征在于，其电阻率为0.02ohm.cm。
10.权利要求8的溅射靶，其特征在于，与氧化铌一起等离子喷涂二氧化钛以便形成含有亚化学计量的二氧化钛和氧化铌的溅射靶。
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