CN101568665A - SnO2系溅射靶 - Google Patents

SnO2系溅射靶 Download PDF

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CN101568665A
CN101568665A CNA2008800012016A CN200880001201A CN101568665A CN 101568665 A CN101568665 A CN 101568665A CN A2008800012016 A CNA2008800012016 A CN A2008800012016A CN 200880001201 A CN200880001201 A CN 200880001201A CN 101568665 A CN101568665 A CN 101568665A
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sputtering target
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森中泰三
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Mitsui Mining and Smelting Co Ltd
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Abstract

本发明提供一种使溅射膜的膜应力的绝对值减小、并且从溅射阴极的周边结构物上的膜剥离少的SnO2系烧结体靶。该烧结体靶由烧结体制成，所述烧结体含有高于10ppm且低于1质量％的Sb2O3、总质量为20质量％以下的Ta2O5和/或Nb2O5，余量为SnO2和不可避免的杂质。

Description

SnO2系溅射靶
技术领域
本发明涉及SnO2系溅射靶，具体而言，涉及在平板显示器、触摸面板、太阳能电池等各种用途中为了确保透明电极、防静电、电磁波屏蔽、气体阻挡、热线反射等各种膜功能而使用的SnO2系溅射靶。
背景技术
近年来，SnO2系薄膜用于平板显示器、触摸面板、太阳能电池等广泛的用途中。该SnO2系薄膜在工业上以喷射法和CVD法进行制造为主流。但是，这些方法不适用于在大面积的情况下使膜厚均匀化，成膜工艺的控制也很困难，并且在成膜时导致高温或者能够产生作为污染物质的氯类气体，因此，要求没有这些缺点的新的制造方法。
另一方面，还尝试了采用溅射法来制造SnO2系薄膜，作为用于该方法的溅射靶，为了降低靶的比电阻而添加了Sb2O3的SnO2-Sb2O3靶已经专门在工业上被实用化。但是，以往的SnO2系烧结体靶在随着累计功率的增加而使膜附着量增加时，容易产生大量从溅射阴极的周边结构物上发生膜剥离而形成的颗粒。已知该颗粒如果附着在薄膜上，则导致薄膜的性能恶化，从而成为薄膜缺陷的原因。因此，要求在溅射时从周边结构物上发生膜剥离少的SnO2系溅射靶。
作为SnO2-Sb2O3系材料，例如提出了以下的材料。已知一种在1450℃以上进行烧结而得到的烧结体，该烧结体包含换算成氧化物总量为20质量％以下的Nb或者Nb和Ta、10ppm以下作为不可避免的杂质的Sb2O3，余量为SnO2(例如，参照日本专利第3957917号公报)。另外，已知一种在820℃以下进行烧结而得到的SnO2-Sb2O3烧结体，该烧结体含有10.2质量％的Sb2O3(例如，参照日本专利第3662168号公报)。此外，已知一种在800℃下烧结而得到的氧化锡-氧化亚锑烧结体靶，该烧结体靶含有3～10质量％的Sb2O3，余量为SnO2和不可避免的杂质(例如，参照日本专利第3710021号公报)。此外，已知一种在1500℃下烧结而得到的锡-锑氧化物烧结体靶，该烧结体靶含有6质量％的氧化锑、5～20质量％的氧化锌，余量为SnO2(例如，参照日本特开2003-73819号公报)。但是，在这些所有的文献中，对于由含有高于10ppm且低于1质量％的Sb2O3的烧结体制成，且溅射膜的膜应力的绝对值小、在溅射时从溅射阴极的周边结构物上的膜剥离也少的SnO2系溅射靶没有任何公开。
发明内容
本发明人等发现：在SnO2系溅射靶中，通过将Sb2Ox添加量规定为高于10ppm且低于1质量％，在使用所获得的SnO2系烧结体制成溅射靶时，可得到膜应力的绝对值小的溅射膜，并且在溅射时从溅射阴极的周边结构物上的膜剥离也少。
因此，本发明的目的在于提供一种SnO2系烧结体靶，所述溅射靶由含有高于10ppm且低于1质量％的Sb2O3而形成的烧结体制成，并且该溅射靶中溅射膜的膜应力的绝对值小、在溅射时从溅射阴极的周边结构物上的膜剥离也少。
即，本发明的SnO2系溅射靶由烧结体制成，所述烧结体含有高于10ppm且低于1质量％的Sb2O3、总质量为20质量％以下的Ta2O5和/或Nb2O5，余量为SnO2和不可避免的杂质。
附图说明
图1是用于评价膜剥离的溅射装置的概略模式图。
具体实施方式
SnO2系溅射靶
本发明的SnO2系溅射靶由烧结体制成，所述烧结体含有高于10ppm且低于1质量％的Sb2O3和总质量为20质量％以下、优选为1～20质量％的Ta2O5和/或Nb2O5，余量为SnO2和不可避免的杂质。如果将这样的SnO2系烧结体制成溅射靶使用，则可以得到膜应力的绝对值小的溅射膜，并且在溅射时可以减少从溅射阴极的周边结构物上的膜剥离。
按照本发明的优选方案，优选Sb2O3的含量为11～9000ppm，更优选为100～6000ppm，进一步优选为300～2000ppm。在使用由上述组成范围内的烧结体制成的溅射靶进行溅射时，可以进一步减小得到的溅射膜的膜应力的绝对值，并可以进一步减少溅射时从溅射阴极的周边结构物上的膜剥离。
按照本发明的优选方案，Ta2O5的含量优选为0～15质量％，并且Nb2O5的含量优选为0～15质量％。通过使用上述组成范围内的原料混合粉末，可以利用能够制造比较大型的烧结体的冷压法或浇铸法来制造烧结体，并且可以在1300℃以上的高温条件下进行烧结。
按照本发明的优选方案，本发明的溅射靶优选由在1300℃以上进行烧结而得到的烧结体制成，更优选为1350～1650℃，进一步优选为1500～1650℃。在上述温度范围进行烧结而得到的烧结体可充分地进行液相烧结，得到烧结密度高的烧结体。
按照本发明的优选方案，本发明的溅射靶优选由相对密度为60％以上的烧结体制成，更优选为75％以上，进一步优选为95％以上。在上述相对密度范围内，可以加速溅射时的成膜速度、并延长靶的使用时间，还可以减少溅射中产生弧光。另外，如果提高烧结密度，则可以减少烧结体内部的气泡等。
按照本发明的优选方案，优选在将本发明的溅射靶用于溅射时获得膜应力的绝对值为1050MPa以下的溅射膜，更优选为1000MPa以下。在上述膜应力值的范围内时，从溅射阴极的周边结构物上的膜剥离少，从而可以抑制因膜剥离而产生颗粒。
SnO2系溅射靶的制造方法
本发明的SnO2系溅射靶的制造方法没有特别限定，可以按照下面所示的优选方式进行。即，按照本发明的优选方案，首先，准备以SnO2为主成分、且含有高于10ppm且低于1质量％的Sb2O3并含有总质量为20质量％以下的Ta2O5和/或Nb2O5的未烧结的成型体。在本发明中，未烧结的成型体只要是将含有上述组成的原料粉成型而得到的成型体即可，可以按照任意的方法进行成型，例如，可以将SnO2粉末、Sb2O3粉末、Ta2O5粉末以及Nb2O5粉末以满足上述组成的配合量进行混合，制备原料粉，再通过将该原料粉成型来制作成型体。
按照本发明的优选方案，使用原料粉而得到的未烧结的成型体优选向原料粉中添加粘合剂而容易赋予规定形状的成型体。作为这样的粘合剂，只要是通过加热而消失或飞散的公知的粘合剂即可，没有特别限定，可以使用聚乙烯醇水溶液等。干燥和加热的方法也没有限定，但优选首先在50～130℃下进行5～30小时的干燥，然后在500～800℃下加热6～24小时以进行脱脂。
按照本发明的优选方案，优选在1300℃以上对如上所述准备的未烧结的成型体进行烧结，更优选为1350～1650℃，进一步优选为1500～1650℃。通过在上述温度范围进行烧结，可以充分地进行液相烧结，从而提高烧结密度，此外，还可以防止SnO2熔融，从而容易制造所期望形状的烧结体。
按照本发明的优选方案，烧结优选进行2～20小时，更优选为3～12小时，进一步优选为4～8小时。如果在上述范围内，则可以抑制电力消耗量，并确保高的生产率，同时可以充分地进行烧结。
按照本发明的优选方案，烧结优选在含氧气氛中进行，以确保高的烧结密度，例如，可以在氧加压气氛下、氧气氛下或大气气氛下进行。
实施例
例1～37
(1)溅射靶的制作
首先，准备下面的4种原料粉末。
SnO2粉末：纯度99.9％(4N)、平均粒径0.7～1.1μm、比表面积2.0～2.7m2/g
Ta2O5粉末：纯度99.9％(3N)、平均粒径0.6～0.8μm、比表面积2.0～3.1m2/g
Nb2O5粉末：纯度99.9％(3N)、平均粒径0.6～1.0μm、比表面积2.1～2.7m2/g
Sb2O3粉末：纯度99.9％(3N)、平均粒径0.6～1.0μm
在各例中，分别称量上述4种原料粉末，用干式球磨机混合21小时。向该混合粉中添加聚乙烯醇水溶液，充分混合后，填充到尺寸为400×800mm的金属模中，以800kgf/cm2的压力进行冲压成型。将该成型体在80℃下干燥12小时。将该干燥体在氧气氛下于表1所示的烧结温度进行8小时烧结，得到烧结体。此时，升温速度控制在400℃/小时、降温速度控制在100℃/小时。将得到的烧结体机械加工成直径152.4mm、厚度5mm的大小，得到SnO2系溅射靶。另外，对于烧结体的加工端财，用乳钵粉碎，再将该粉碎后的粉末、硝酸和盐酸的混酸以及超纯水加入到特氟隆(注册商标)制容器中，进行水解后，制成标准溶液。使用ICP质谱分析装置(Agilent公司制造4500)以ICP质谱分析法进行得到的标准溶液中的Ta、Nb和Sb等各元素的测定。换算成氧化物后的值如表1所示。
(2)评价
对于得到的溅射靶，进行下面所示的各种评价试验。
评价1：相对密度的测定
通过阿基米德法测定各溅射靶的相对密度。此时，各原料的密度为SnO2：6.95g/cm3、Ta2O5：8.74g/cm3、Nb2O5：4.47g/cm3，计算出加重平均密度(理论密度)，将该加重平均密度作为100％，计算出相对密度。其结果如表1所示。
评价2：溅射膜的膜应力的评价
将例1～37得到的溅射靶金属键合在无氧铜制成的背板上。然后，在下面所示的条件下对金属键合后的各溅射靶进行使用直流电源的溅射，在硅片上溅射成膜。
阴极：强磁场磁电路
靶/基板间距离：50mm
溅射室最大压力：＜1×10-4Pa
基板温度：室温(未加热)
导入气体：氩气+氧气(氧浓度为1体积％)
导入气体分压：0.67Pa
直流施加功率：360W
膜厚：500nm
基板：φ4英寸×525μm硅片
使用FLX-2320-5(东朋技术株式会社制造)对这样得到的溅射膜测定曲率半径，使用下面的计算式计算出应力。膜应力的负号表示为压缩应力。
σ＝Eb2/{6(1-v)*rd}
σ：应力
E：基板的杨氏模量
B：基板的厚度
v：基板的泊松比
d：膜厚
r：成膜后的基板的曲率半径(通过牛顿法测定)
结果如表1所示，可知使用满足本发明的组成的溅射靶成膜而得到的溅射膜都具有低的膜应力。
评价3：膜剥离的评价
使用图1所示的溅射装置如下所述对例1～37得到的溅射靶进行膜剥离的评价。图1所示的溅射装置在腔室1内具有：用于放置靶2的背板3、与背板3相对设置的基板架4。并且，在腔室1内还设置有保护靶2和背板3的侧面的屏蔽接地5、以及防止在腔室1上形成包覆膜的防粘板6。
首先，将各溅射靶金属键合在腔室1内的背板3上。然后，在下面所示的溅射条件下对金属键合后的靶2进行连续放电。连续放电后，观察附着在基板架4、屏蔽接地5以及防粘板6上的膜，将明显发生膜剥离的情况作为×、将未发生明显的膜剥离的情况作为○。
阴极：强磁场磁电路
靶/基板间距离：50mm
溅射室最大压力：＜1×10-4Pa
导入气体：氩气+氧气(氧浓度为1体积％)
导入气体分压：0.67Pa
直流施加功率：360W
膜厚：500nm
溅射时间：连续30小时放电
屏蔽接地：刚铝石#60喷砂处理的制品
基板架：刚铝石#60喷砂处理的制品
防粘板：刚铝石#60喷砂处理的制品
结果如表1所示，可知使用满足本发明的组成的溅射靶连续放电后，附着在图1所示的基板架4、屏蔽接地5以及防粘板6上的膜均未产生膜剥离。
[表1]
Figure A20088000120100091

Claims (5)

1.SnO2系溅射靶，其由烧结体制成，所述烧结体含有高于10ppm且低于1质量％的Sb2O3、总质量为20质量％以下的Ta2O5和/或Nb2O5，余量为SnO2和不可避免的杂质。
2.权利要求1所述的溅射靶，其中，Sb2O3的含量为11～9000ppm。
3.权利要求1所述的溅射靶，其中，Sb2O3的含量为100～6000ppm。
4.权利要求1所述的溅射靶，其中，Sb2O3的含量为300～2000ppm。
5.权利要求1～4中任一项所述的溅射靶，其中，Ta2O5的含量为0～15质量％，且Nb2O5的含量为0～15质量％。
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