CN101273153B - 溅射靶、透明导电膜和触摸板用透明电极 - Google Patents
溅射靶、透明导电膜和触摸板用透明电极 Download PDFInfo
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- CN101273153B CN101273153B CN2006800350780A CN200680035078A CN101273153B CN 101273153 B CN101273153 B CN 101273153B CN 2006800350780 A CN2006800350780 A CN 2006800350780A CN 200680035078 A CN200680035078 A CN 200680035078A CN 101273153 B CN101273153 B CN 101273153B
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Abstract
本发明的目的在于提供一种铟含量少高密度且低电阻的溅射靶、及使用该溅射靶制作的透明导电膜和触摸板用透明电极。本发明的溅射靶，以铟、锡、锌为主要成分，由In/(In+Sn+Zn)表示的原子比为0.10～0.35，由Sn/(In+Sn+Zn)表示的原子比为0.15～0.35，由Zn/(In+Sn+Zn)表示的原子比为0.50～0.70，并且，该溅射靶是含有由In2O3(ZnO)m(m为3～9的整数)表示的六方晶层状化合物及由Zn2SnO4表示的尖晶石结构化合物的氧化物的烧结体。
Description
技术领域
本发明涉及削减了铟的溅射靶、透明导电膜和触摸板用透明电极。
背景技术
近年来，显示装置的发展迅猛，液晶显示装置(LCD)、电致发光(EL)显示装置、或场发射显示装置(FED)等作为个人电脑、文字处理设备等的办公机器、工厂中的控制系统用的显示装置得到使用。这些显示装置均具有由透明导电性氧化物夹着显示元件的夹层结构。
作为这样的透明导电性氧化物，如非专利文献1所公开，通过溅射法、离子镀敷法或蒸镀法成膜的铟锡氧化物(以下简称为ITO)或者铟锌氧化物(以下简称为IZO)占据着主流。
ITO由氧化铟和氧化锡构成，透明性和导电性优异，另外可以用强酸进行蚀刻加工，还有与基板的密着性也优异。另外，IZO在ITO的特征之外，弱酸进行的蚀刻加工优异，可实现电极的高精细化。
然而，近年来由于面板显示器(FPD)的急速普及，发生了在FPD中作为必须的透明电极的主要原料的铟的供给不稳定。另外，铟与锌、锡比具有有害性，从该观点出发也要求限制其使用量。另一方面，在ITO和IZO等的透明导电膜用靶中铟的含量高(80～90原子％)。为此，强烈要求减少ITO和IZO的靶中的铟量。
另一方面，还对如下方法进行了研究：作为由IZO构成的靶，含有由In2O3(ZnO)m(m为2～20的整数。)表示的六方晶层状化合物，并且将该六方晶层状化合物的晶粒直径定为5μm以下值，由此，防止球粒(ノジュ一ル)的发生抑制异常放电(专利文献1，专利文献2)。
专利文献1：WO01/038599手册
专利文献2：特开平06-234565号公报
非专利文献1：“透明导电膜的技术”((株)欧姆社出版，日本学术振兴会，透明氧化物·光电子材料第166委员会编，1999)
发明内容
本发明的目的在于提供一种铟含量少，高密度并且低电阻的靶及利用该靶制作的透明导电膜和触摸板用透明电极。
在IZO中将铟含量削减到35原子％以下，为了提高密度用高温烧结时，所得到的靶的电阻变得极高。即，在IZO的靶中，难以同时提高相对密度和降低体电阻，并且很难减少铟含量。
发明者们锐意研究的结果发现，在铟含量在35原子％以下的IZO中，在为了提高密度而在高温烧结时，电阻极高的ZnO数大的六方晶化合物(m为10以上的In2O3(ZnO)m)产生。此外，发明者们还发现通过得到在1300～1700℃进行了烧结的含有由In2O3(ZnO)m(m为3～9的整数)表示的六方晶层状化合物和由Zn2SnO4表示的尖晶石结构化合物的氧化物的烧结体，能够制造即使铟含量在35％以下，也能够提高靶的相对密度，体电阻低的靶。
根据本发明，提供了以下的溅射靶。
1、含有以铟、锡、锌为主要成分，由In/(In+Sn+Zn)表示的原子比为0.10～0.35，由Sn/(In+Sn+Zn)表示的原子比为0.15～0.35，由Zn/(In+Sn+Zn)表示的原子比为0.50～0.70，由In2O3(ZnO)7表示的六方晶层状化合物及由Zn2SnO4表示的尖晶石结构化合物的氧化物的烧结体的溅射靶。
2、根据1所述的溅射靶，在X射线衍射中，所述六方晶层状化合物的最大峰强度I(In2O3(ZnO)7)、所述尖晶石结构化合物的最大峰强度I(Zn2SnO4)及由SnO2表示的金红石结构化合物的最大峰强度I(SnO2)满足下述关系：
(I(In2O3(ZnO)m))/(I(Zn2SnO4))＜1
(I(In2O3(ZnO)7))/(I(Zn2SnO4))＜1
(I(SnO2))/(I(In2O3(ZnO)7))＜1
(I(SnO2))/(I(Zn2SnO4))＜1。
(I(SnO2))/(I(In2O3(ZnO)7))＜1
(I(SnO2))/(I(Zn2SnO4))＜1。
3、根据1或2所述的溅射靶，在所述X射线衍射中，所述尖晶石结构化合物的峰值在狭窄角转移。
4、根据1～3中任一项所述的溅射靶，体电阻为0.5～300mΩcm。
5、根据1～4中任一项所述的溅射靶，相对密度为90％以上。
6、一种透明导电膜，利用1～5中任一项所述的溅射靶，通过溅射法成膜而成。
7、一种触摸板用透明电极，使用6所述的透明导电膜。
附图说明
图1是表示在实施例1中得到的溅射靶的X射线衍射谱的图。
具体实施方式
本发明的溅射靶为以铟、锡、锌为主要成分，含有由In2O3(ZnO)m (m为3～9的整数)表示的六方晶层状化合物及由Zn2SnO4表示的尖晶石结构化合物的氧化物的烧结体。
该氧化物在六方晶层状化合物和尖晶石结构化合物之外，还可以含有方铁锰矿(ビツクスバイト)结构化合物、纤维锌矿(ウルルツ)化合物、金红石结构化合物。另外，本发明的溅射靶在不损坏本发明的效果的基础上，除了铟、锡、锌之外，还可以含有铝、鎵、镁、硼、锗、铌、钼、钨、钇、銻、鉿、钽、钙、铍、锶、铯、镧类。
在本发明的靶中，由In/(In+Sn+Zn)表示的原子比为0.10～0.35，优选为0.11～0.29，更优选为0.12～0.24，特别优选为0.14～0.24。
比0.10小时有可能靶的相对密度低或体电阻变高，比0.35大时铟消减的效果小。
在本发明的靶中，由Sn/(In+Sn+Zn)表示的原子比为0.15～0.35，优选为0.18～0.34，更优选为0.20～0.33。在该范围之外时，由In2O3(ZnO)m (m为3～9的整数)表示的六方晶层状化合物、由Zn2SnO4表示的尖晶石结构化合物难以共存，靶的体电阻有可能变高。
在本发明的靶中，由Zn/(In+Sn+Zn)表示的原子比为0.50～0.70，优选为0.51～0.69，更优选为0.52～0.65。在该范围之外时，由In2O3(ZnO)m (m为3～9的整数)表示的六方晶层状化合物、由Zn2SnO4表示的尖晶石结构化合物难以共存，靶的体电阻有可能变高。
本发明的溅射靶，在X线衍射中，由In2O3(ZnO)m表示的六方晶层状化合物的最大峰强度(I(In2O3(ZnO)m))、由Zn2SnO4表示的尖晶石结构化合物的最大峰强度(I(Zn2SnO4))及由SnO2表示的金红石结构化合物的最大峰强度(I(SnO2))优选满足下述关系：
(I(In2O3(ZnO)m))/(I(Zn2SnO4))＜1
(I(SnO2))/(I(In2O3(ZnO)m))＜1
(I(SnO2))/(I(Zn2SnO4))＜1
关于(I(In2O3(ZnO)m))/(I(Zn2SnO4))优选为比0.3小，在所述的范围之外时，溅射靶的体电阻有可能升高。
本发明的溅射靶，在X线衍射中，优选为由Zn2SnO4表示的尖晶石结构化合物的峰值(2θ)在狭窄角(负方向)转移。所述的转移量优选为0.01度以上，更优选为0.02度以上，特别优选为0.03度以上。
如果转移的角度小于0.01度则载体不充分靶的电阻有可能变高。这被认为是其它原子向Zn2SnO4中的固溶量(原子数)不充分，载体电子没有充分发生。
本发明的溅射靶的体电阻优选为0.5～300mΩcm，更优选为0.6～200mΩcm，进一步优选为0.7～150mΩcm，特别优选为0.8～100mΩcm。
如果比0.5mΩcm小则成为尘埃由于和附着在靶上的透明导电膜片的电阻差，有可能电荷(charge)发生成为异常放电的原因。另外，如果比300mΩcm大，则有可能变得稳定而难以进行DC溅射。
本发明的溅射法的相对密度优选为90％以上，更优选为95％以上，进一步优选为98％以上，特别优选为99％以上。
如果比90％小则成膜速度变慢，靶的强度有可能降低。
本发明的透明导电膜是通过溅射法成膜所述溅射靶而得到的。
透明导电膜的比电阻优选为1～100mΩcm，更优选为2～10mΩcm。膜厚优选为10～1000nm，更优选为50～600nm，特别优选为100～400nm。
通常导电膜的比电阻越低越为优选，但是触摸板用透明导电膜优选为有一定程度高的比电阻，具有所述的比电阻的本发明的透明导电膜特别适于作为触摸板用透明电极。
另外，通过调整成膜时的氧的分压，或成膜后在氧存在下进行热处理 等控制载体密度，也能够使用于TFT(薄膜晶体管)等的半导体用途。
被成膜的透明导电膜在35℃用草酸系蚀刻液进行蚀刻的速度一般为20～1000nm/分钟，优选为30～300nm/分钟，特别优选为50～200nm/分钟。如果比20nm/分钟慢则不仅制造时的频率慢，而且有可能蚀刻残渣残留。如果比1000nm/分钟快而变得过快，则有可能不能控制线宽等。
接着说明本发明的溅射靶的制造方法。
作为溅射靶的制造方法，通常包括：混合原料的工序、和加压成形制作成形体的工序、和烧制成形体的工序。
能够利用公知的例如特开2002-069544号公报、特开2004-359984号公报、专利03628554号公报等的方法。
特别是调整铟、锡、锌的配合量，能够制造由In2O3(ZnO)m(m为3～9的整数)表示的六方晶层状化合物。
下述表示适合的溅射靶的制造方法的一个例子。
(1)配合工序
用于靶的制造原料的各种金属氧化物，优选利用通常的粉碎机，例如湿式球磨机或颗粒球磨机，或者超音波装置，均匀地进行混合粉碎。
这时，配合成：由In/(In+Sn+Zn)表示的原子比为0.10～0.35，由Sn/(In+Sn+Zn)表示的原子比为0.15～0.35，由Zn/(In+Sn+Zn)表示的原子比为0.50～0.70。
(2)预烧工序
接着，在得到铟化合物和锌化合物和及锡化合物的混合物后，优选在任意工序预烧该化合物。在该预烧工序中，优选在500～1200℃，1～100小时的条件下，进行热处理。
其理由为，在低于500℃或低于1小时的热处理条件下，铟化合物和锌化合物、锡化合物的热分解有时不充分。另一方面，热处理条件为超过1200℃或超过100小时时，有时会发生粒子粗大化。
因此，特别优选为在800～1200的温度范围，2～50小时的条件下，进行热处理(预烧)。
还有，在此得到的预烧物，优选在成形烧结前粉碎。该预烧物的粉碎可以用用球磨机、滚碎机、微粒球磨机、喷射球磨机等，使粒径为0.01～ 1.0μm。
(3)成形工序
接着，优选在成形工序中，使用得到的预烧物，成形为作为靶适当的形状。
作为如此的成形处理可以进行模具成形、铸造成形、射出成形等，为了得到烧结密度高的烧结体，优选通过CIP(冷静水压)等成形后进行下述的烧结处理。
还有在成形处理时，也可以使用聚乙烯醇、甲基纤维素、聚腊、油精酸等成形辅助剂。
(4)烧制工序
接着，在对所得到的微粉末进行造粒后，通过挤压成形成形为希望的形状，进行烧制，进行HIP(热静水压)烧制等。
这时的烧制条件通常为在1100～1700℃，优选为1200～1600℃，更优选为1300～1500℃，其中，通常烧制30分钟～360小时，优选为8～180小时，更优选为12～96小时。通常在氧气气氛或氧气加压下烧制。另一方面，在不含氧气的气氛中烧制粉末混合物，或在1700℃以上的温度中烧制时，Sn和Sn化合物气化有可能损伤烧制炉，或有可能m为10以上的六方晶层状化合物(In2O3(ZnO)m)生成。另外，在比1100℃低时则有可能不生成结晶型，靶的烧结密度不提高，而靶的电阻提高，强度下降。
另外，这时的升温速度为5～600℃/小时(优选为50～500℃/小时、更优选为100～400℃/小时)。如果比600℃/小时快则有时会生成六方晶层状化合物，尖晶石结晶的形成变得不充分，如果比5℃/小时慢则有可能会花费过多时间，生产性下降。
另外，降温速度为5～600℃/小时(优选为50～500℃/小时、更优选为100～400℃/小时)。如果比600℃/小时快则有时会生成六方晶层状化合物，尖晶石结晶的形成变得不充分，如果比5℃/小时慢则有可能会花费过多时间，生产性下降。
(5)还原工序
在得到的烧结体中，为了使体电阻全体均匀化，在任意工序中优选在还原工程中进行还原处理。
作为这样的还原方法可以适用用还原性气体进行的方法和真空烧制或用惰性气体进行的还原等。
另外，用还原性气体时，能够使用氢、甲烷、一氧化碳、或这些气体和氧的混合气体。另外，在通过惰性气体中的烧制进行的还原时，能够使用氮、氩、或这些气体和氧的混合气体等。
还有，还原温度为100～800℃，优选为200～800℃。另外，还原时间为0.01～10小时，优选为0.05～5小时。
(6)加工工序
这样烧结得到的烧结体，优选在加工工序中，切削加工成适于向溅射装置安装的形状，另外安装衬板等等安装工具作为溅射靶。靶的厚度通常为2～20mm，优选为3～12mm，特别优选为4～6mm。另外，也可以将多个靶安装在一个衬板上作为实质上一个靶。另外，优选为对表面用80～4000号的金刚石磨石进行精磨，特别优选为用100～1000号的金刚石磨石进行精磨。使用比80号小的金刚石磨石时，靶有可能易出现裂纹。研磨优选在靶的长方向上进行其强度会提高。
[实施例]
[实施例1]
(1)溅射靶的制造
作为原料，以原子比[In/(In+Sn+Zn)]成为0.16，原子比[Sn/(In+Sn+Zn)]成为0.20，原子比[Zn/(In+Sn+Zn)]成为0.64的方式混合各个与4N相当的平均粒径为1μm以下的氧化铟、氧化锌、氧化锡，将其供给湿式球磨机，进行20小时混合粉碎，得到原料微粉末。
取出得到的混合浆料，进行过滤、干燥及造粒。对该造粒物施与294MPa的压力，以冷静水压挤压成形。将其装入烧制炉，在氧气加压下，在1400℃烧制48小时，得到烧结体(靶)。升温速度为到1000℃为50℃/小时、到1400℃为150℃/小时。降温速度为100℃/小时。
(2)溅射靶的评价
对于所得到的靶，通过阿基米德法测定其相对密度，及通过四探针法测定其体电阻值。其结果为相对密度为99％，体电阻值为80mΩcm。另外，以JIS R 1601的标准，进行抗折力的测定。
另外，对于从该烧结体采取的试料，通过X线衍射法观察透明导电材料中的结晶状态的结果为，在所得到的靶中，确认到有由In2O3(ZnO)7 表示的六方晶层状化合物、由Zn2SnO4表示的尖晶石结构化合物及由In2O3 表示的方铁锰矿结构化合物。
在图1中显示X线衍射法的结果。从该图中发现尖晶石结构化合物的峰值在狭窄角转移0.05度。
还有，X线衍射测定的测定条件如下所述。
装置：(株)リガク制Ultima-III
X射线：Cu-Kα线(波长1.5406A，通过石墨单色光镜单色化)
2θ-θ发射法，连续扫描(1.0°/分)
取样间隔：0.02°
狭缝DS，SS：2/3°，RS：0.6mm
此外，将所得到的烧结体包埋在树脂中，以粒径为0.05μm的氧化铝粒子研磨其表面后，用EPMA测定在烧结体表面的30μm×30μm的四方框内观察的各晶粒直径。在3个框内进行同样的测定，算出各粒径的平均值，确认到该烧结体中由In2O3(ZnO)3表示的六方晶层状化合物和由In2O3表示的方铁锰矿结构化合物的晶粒直径均在20m以下。
另外，切削加工由(1)得到的烧结体，用#400号金刚石磨石研磨，制作直径约10cm，厚度约5mm的溅射靶，用AFM法进行表面粗糙度的测定。研磨面的表面粗糙度Ra为0.3μm。
(3)透明导电性氧化物的成膜
在DC磁电反应溅射装置中安装由(1)得到的溅射靶，在室温下，在玻璃基板上成膜透明导电膜。
喷射条件为喷射压力1×10-1Pa，到达压力5×10-4Pa，基板温度200℃，输入功率120W，成膜时间15分钟。
其结果为在玻璃基板上形成膜厚约100nm的透明导电性氧化物。
(4)透明导电性氧化物的评价
对上述得到的在玻璃上的透明导电膜的导电性，用四探针法测定比电阻为3mΩ/cm。
另外，用和(2)相同方法对该透明导电膜进行X线衍射，其结果为 确认为非晶质。另一方面，对于膜表面的平滑性，因为P-V值(JISB0601基准)为5nm，所以确认为良好。
对于该透明导电性氧化物的透明性，通过分光光度计，波长500nm的光线的光线透过率为88％，透明性也优异。
还有，用具有代表性的草酸系蚀刻液(草酸5wt％)在35℃对该透明导电膜进行蚀刻，蚀刻速度为100nm/分钟。另外，在200％的过渡蚀刻后，用电子显微镜(SEM)观察蚀刻痕，残存少的为良好。
(6)异常放电的发生数
将由(1)得到的溅射靶安装在DC磁电反应溅射装置中由(1)，利用在氩气中添加含3％的氢气的混合气体，除此之外，与所述的(2)在同一条件下，连续地进行240小时溅射，监视有无异常放电，但一次都没有确认到。
[实施例2、比较例1～4]
将原料的组成比调制成表1所示的原子比，除此之外，和实施例1同样进行制作评价。表1和表2显示结果。其中，关于溅射，在比较例1、3、4中利用的是RF磁电溅射。
[表1]
[表2]
利用本发明的溅射靶成膜的透明导电膜，适用于液晶显示器等的显示器和触摸板、用于太阳能电池等的透明电极。
Claims (7)
1.一种溅射靶，其特征在于，以铟、锡、锌为主成分，
由In/(In+Sn+Zn)表示的原子比为0.10～0.35，
由Sn/(In+Sn+Zn)表示的原子比为0.15～0.35，
由Zn/(In+Sn+Zn)表示的原子比为0.50～0.70，
并且，该溅射靶是含有由In2O3(ZnO)m表示的六方晶层状化合物及由Zn2SnO4表示的尖晶石结构化合物的氧化物的烧结体，相对密度为90％以上，其中，m是3～9的整数。
2.根据权利要求1所述的溅射靶，其特征在于，在X射线衍射中，所述六方晶层状化合物的最大峰强度I(In2O3(ZnO)m)、所述尖晶石结构化合物的最大峰强度I(Zn2SnO4)及由SnO2表示的金红石结构化合物的最大峰强度I(SnO2)满足下述关系：
(I(In2O3(ZnO)m))/(I(Zn2SnO4))＜1
(I(SnO2))/(I(In2O3(ZnO)m))＜1
(I(SnO2))/(I(Zn2SnO4))＜1。
3.根据权利要求1或2所述的溅射靶，其特征在于，在所述X射线衍射中，所述尖晶石结构化合物的峰值在狭窄角移动。
4.根据权利要求1或2所述的溅射靶，其特征在于，体电阻为0.5～300mΩcm。
5.根据权利要求3所述的溅射靶，其特征在于，体电阻为0.5～300mΩcm。
6.一种透明导电膜，其特征在于，利用权利要求1～5中任一项所述的溅射靶，通过溅射法成膜而成。
7.一种触摸板用透明电极，其特征在于，使用权利要求6所述的透明导电膜。
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| US20090308635A1 (en) | 2009-12-17 |
| WO2007037191A1 (ja) | 2007-04-05 |
| KR20080049072A (ko) | 2008-06-03 |
| TWI400346B (zh) | 2013-07-01 |
| KR101314946B1 (ko) | 2013-10-04 |
| TW200724702A (en) | 2007-07-01 |
| JPWO2007037191A1 (ja) | 2009-04-09 |
| US8304359B2 (en) | 2012-11-06 |
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