CN101180687B - 透明导电膜及透明导电膜的制造方法 - Google Patents
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- H01B1/00—Conductors or conductive bodies characterised by the conductive materials; Selection of materials as conductors
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Abstract
本发明提供具备可实用的耐湿性和作为透明导电膜所必需的特性,且成本低的ZnO类透明导电膜及其制造方法。在氧化锌(ZnO)中掺杂III族元素并使其在基体上生长而得的透明导电膜中,使其具备具有c轴朝向相互不同的多个方向的结晶结构的区域。在氧化锌(ZnO)中掺杂III族元素并使其在基体上生长而得的透明导电膜中,使ZnO(002)摇摆曲线半宽度在13.5°以上。以III族元素氧化物的掺杂量满足透明导电膜中的III族元素氧化物的比例在7~40重量%的范围内的条件,在ZnO中掺杂III族元素氧化物。介以SiNλ薄膜在基体上形成透明导电膜。对基体施加偏压的同时,以薄膜形成方法在基体上形成透明导电膜。
Description
技术领域
本发明涉及透明导电膜及其制造方法,具体涉及以氧化锌(ZnO)为主要成分的透明导电膜及其制造方法。
背景技术
近年来,透明电极被广泛用于平板显示器和太阳能电池等。并且,作为透明电极的材料,广泛使用ITO(掺锡氧化铟)。
然而,铟(In)是价格高且可能资源枯竭的物质,所以对使用其它材料的透明电极的需求不断增长。并且,作为不使用ln的透明电极,进行着使用价格低、可稳定供应的锌(Zn)的氧化物(ZnO)的ZnO类透明电极的开发。
另外,ZnO在化学计量学组成上是绝缘体,但可以通过氧缺失产生的剩余电子和对Zn位的元素置换(掺杂)赋予导电性。并且,作为以这样的ZnO为主要成分的透明电极,在目前也已经可以制成电阻率ρ在10-4Ωcm级的电极。
然而,ZnO类透明导电膜在实用性方面存在耐湿性不足的问题。即,以往的ZnO类透明导电膜中存在大量的氧缺失,如果放置于湿度高的环境下,则存在载流子由于对氧缺失的水分吸附(再氧化)而减少,导致高电阻化的问题。作为使用ITO的透明电极的耐湿性的标准之一,在85℃、85%RH的气氛中经过720小时后的电阻变化率被定为±10%,但无法获得满足该条件的ZnO类透明导电膜。
另外,被预测今后作为用途的扩展的在柔性基板上形成ZnO类透明导电膜的情况下,由于柔性基板透过水分,因此存在不仅从透明导电膜的表面,透明导电膜的劣化因透过柔性基板的水分的影响而进一步加剧的问题。
为了解决这样的问题,研究了各种用于使ZnO类透明导电膜的耐湿性提高的方法,其方法大致分为以下的两种方法:
(1)设置SiN阻挡膜来抑制自基板侧的水分透过的方法;
(2)通过加热成膜等改善ZnO的膜质(结晶性)的方法。
然而,目前的实际情况是还无法获得具备可实用的耐湿性的ZnO类透明导电膜。
另外,作为涉及在ZnO中掺杂元素来赋予导电性的技术,例如提出有以下的技术方案。
(a)使用ZnO的分子射线或Zn和O的分子射线制作ZnO膜时,通过使用I A族(H)、IIIA族(B、Al、Ga、In)或VII族(F、Cl、I、Br)中的任意原子的分子射线在ZnO膜中掺杂杂质,以良好的控制性使电阻降低的方法(参照专利文献1)。
(b)由掺杂了周期表VB族或VIB族的元素的氧化锌形成的透明导电体,它是在基材上层叠相对于元素原子和锌原子的总原子数含有0.1~10原子%上述元素的透明导电膜而得的透明导电体(参照专利文献2)。
(c)在基板上具备阳电极、阴电极和夹于这些电极间的有机层,作为阳电极使用了由含有1种或2种以上的Ir、Mo、Mn、Nb、Os、Re、Ru、Rh、Cr、Fe、Pt、Ti、W和V的氧化物的材料形成的电极的透明导电膜的有机EL元件(参照专利文献3)。
(d)使用掺杂或不掺杂II族元素、VII族元素、I族元素或V族元素中的任意元素的导电性ZnO等透明导电性材料的晶体管(参照专利文献4)。
(e)氧化锌薄膜的c轴∶a轴的取向性的比在100∶1以上,且掺杂了铝、镓、硼等III族和VII族的化合物中的至少1种的透明导电膜(参照专利文献5)。
(f)以通式(ZnO)m·In2O3(m=2~20)表示的六方晶层状化合物的In或Zn元素被选自Sn、Y、Ho、Pb、Bi、Li、Al、Ga、Sb、Si、Cd、Mg、Co、Ni、Zr、Hf、Sc、Yb、Lu、Fe、Nb、Ta、W、Te、Au、Pt和Ge的至少一种元素置换而得的六方晶层状化合物,它是平均厚度为0.001μm~0.3μm,平均纵横比(平均长径/平均厚度)为3~1000的氧化铟锌类六方晶层状化合物(参照专利文献6)。
并且,这些ZnO类透明导电膜的耐湿性也存在如上所述的问题。
专利文献1:日本专利特开平7-106615号公报
专利文献2:日本专利特开平8-050815号公报
专利文献3:日本专利特开平11-067459号公报
专利文献4:日本专利特开2000-150900号公报
专利文献5:日本专利特开2000-276943号公报
专利文献6:国际公开第2001/056927号文本
发明的揭示
本发明的目的在于解决上述课题,提供具备可实用的耐湿性和作为透明导电膜所必需的特性,且成本低的ZnO类透明导电膜及其制造方法。
为了解决上述课题,本申请的发明(权利要求1)的透明导电膜是在氧化锌(ZnO)中掺杂III族元素并使其在基体上生长而得的透明导电膜,其特征在于,具备具有c轴朝向相互不同的多个方向的结晶结构的区域。
此外,权利要求2的透明导电膜是在氧化锌(ZnO)中掺杂III族元素并使其在基体上生长而得的透明导电膜,其特征在于,ZnO(002)摇摆曲线半宽度在13.5°以上。
此外,权利要求3的透明导电膜如权利要求1或2的发明的构成,其特征在于,前述透明导电膜通过对前述基体施加偏压的同时进行薄膜形成而获得。
此外,权利要求4的透明导电膜如权利要求3的发明的构成,其特征在于,前述薄膜形成采用选自溅射法、蒸镀法、离子电镀法、激光烧蚀法和电弧等离子体蒸镀法的1种方法来实施。
此外,权利要求5的透明导电膜如权利要求1~4中的任一项的发明的构成,其特征在于,以氧化锌(ZnO)为主要成分,以7~40重量%的比例含有III族元素氧化物。
此外,权利要求6的透明导电膜如权利要求1~5中的任一项的发明的构成,其特征在于,前述透明导电膜介以SiNx薄膜形成于基体上。
此外,权利要求7的透明导电膜如权利要求1~6中的任一项的发明的构成,其特征在于,前述基体以选自玻璃、水晶、蓝宝石、Si、SiC、聚对苯二甲酸乙二醇酯(PET)、聚萘二甲酸乙二醇酯(PEN)、聚醚砜(PES)、聚酰亚胺、环烯烃类聚合物和聚碳酸酯的至少1种为主要成分。
此外,权利要求8的透明导电膜如权利要求1~7中的任一项的发明的构成,其特征在于,前述III族元素为选自Ga、Al和In的至少1种。
此外,权利要求9的透明导电膜的制造方法是用于制造包含氧化锌(ZnO)和III族元素的透明导电膜的透明导电膜的制造方法,其特征在于,具备使用包含氧化锌(ZnO)和III族元素氧化物的原料,以III族元素氧化物的掺杂量在7~40重量%的范围内的条件通过薄膜形成方法在基体上成膜,在基体上形成具备具有c轴朝向相互不同的多个方向的结晶结构的区域的透明导电膜的工序。
此外,权利要求10的透明导电膜的制造方法是用于制造包含氧化锌(ZnO)和III族元素的透明导电膜的透明导电膜的制造方法,其特征在于,具备使用包含氧化锌(ZnO)和III族元素氧化物的原料,以III族元素氧化物的掺杂量在7~40重量%的范围内的条件通过薄膜形成方法在基体上成膜,在基体上形成ZnO(002)摇摆曲线半宽度在13.5°以上的透明导电膜的工序。
此外,权利要求11的透明导电膜的制造方法是用于制造包含氧化锌(ZnO)和III族元素的透明导电膜的透明导电膜的制造方法,其特征在于,具备使用由包含氧化锌(ZnO)和III族元素氧化物的组合物形成的烧结体靶材,以III族元素氧化物的掺杂量在7~40重量%的范围内的条件通过选自溅射法、蒸镀法、离子电镀法、激光烧蚀法和电弧等离子体蒸镀法的1种方法在基体上成膜,在基体上形成具备具有c轴朝向相互不同的多个方向的结晶结构的区域的透明导电膜的工序。
此外,权利要求12的透明导电膜的制造方法是用于制造包含氧化锌(ZnO)和III族元素的透明导电膜的透明导电膜的制造方法,其特征在于,具备使用由包含氧化锌(ZnO)和III族元素氧化物的组合物形成的烧结体靶材,以III族元素氧化物的掺杂量在7~40重量%的范围内的条件通过选自溅射法、蒸镀法、离子电镀法、激光烧蚀法和电弧等离子体蒸镀法的1种方法在基体上成膜,在基体上形成ZnO(002)摇摆曲线半宽度在13.5°以上的透明导电膜的工序。
此外,权利要求13的透明导电膜的制造方法如权利要求9~12中的任一项的发明的构成,其特征在于,使通过以前述薄膜形成方法成膜而形成前述透明导电膜的基体的温度和前述III族元素氧化物的掺杂量的关系呈图4的以点a、b、c确定的范围内的关系。
此外,权利要求14的透明导电膜的制造方法如权利要求11~13中的任一项的发明的构成,其特征在于,通过前述选自溅射法、蒸镀法、离子电镀法、激光烧蚀法和电弧等离子体蒸镀法的1种方法成膜时,在对前述基体施加偏压的同时进行成膜。
此外,权利要求15的透明导电膜的制造方法如权利要求9~14中的任一项的发明的构成,其特征在于,基于前述薄膜形成方法的成膜在使背压达到1×10-4Pa以下的真空室内进行。
此外,权利要求16的透明导电膜的制造方法的特征在于,在前述基体上形成SiNx薄膜后,通过权利要求9~15中的任一项所述的方法介以前述SiNx薄膜于前述基体上形成前述透明导电膜。
此外,权利要求17的透明导电膜的制造方法如权利要求9~16中的任一项的发明的构成,其特征在于,前述基体以选自玻璃、水晶、蓝宝石、Si、SiC、聚对苯二甲酸乙二醇酯(PET)、聚萘二甲酸乙二醇酯(PEN)、聚醚砜(PES)、聚酰亚胺、环烯烃类聚合物和聚碳酸酯的至少1种为主要成分。
此外,权利要求18的透明导电膜的制造方法如权利要求9~17中的任一项的发明的构成,其特征在于,前述III族元素为选自Ga、Al和In的至少1种。
本申请的发明(权利要求1)的透明导电膜是在氧化锌(ZnO)中掺杂III族元素并使其在基体上生长而得的透明导电膜,具备具有c轴朝向相互不同的多个方向的结晶结构的区域,所以可以提供具备实用水平的耐湿性且成本也低的ZnO类透明导电膜。
作为本申请的权利要求1的发明的透明导电膜中,可获得良好的耐水性的原因被认为在于,如以往那样结晶柱状生长而具有c轴朝向同一方向的单一取向结构的透明导电膜的情况下,水分透过晶界而侵入内部,使耐湿性劣化,而本申请的发明的具备具有c轴朝向相互不同的多个方向的结晶结构的区域的透明导电膜中,膜结构的变化抑制水分产生的氧缺陷的再氧化。
另外,本发明的透明导电膜中,除具有c轴朝向相互不同的多个方向的结晶结构的区域以外的区域中,可以存在非晶质区域或具有介于非晶质和晶质之间的所谓准结晶结构的区域等。
此外,权利要求2的透明导电膜是在氧化锌(ZnO)中掺杂III族元素并使其在基体上生长而得的透明导电膜,ZnO(002)摇摆曲线半宽度在13.5°以上,c轴朝向同一方向的程度低,因此可以抑制氧缺陷的再氧化,能够提供具备实用水平的耐湿性且成本也低的ZnO类的透明导电膜。
另外,本发明中,将ZnO(002)摇摆曲线半宽度在13.5°以上作为要件的原因在于,ZnO(002)摇摆曲线半宽度在13.5°以上的ZnO膜中,c轴朝向同一方向的程度充分低至可以抑制、防止氧缺陷的再氧化的程度。
此外,如权利要求3的透明导电膜那样,权利要求1或2的发明的构成中,透明导电膜通过对基体施加偏压的同时进行薄膜形成而获得的情况下,可以使III族元素氧化物的掺杂量降低且使耐湿性提高,能够制造低电阻且耐湿性良好的透明导电膜。
此外,如权利要求4的透明导电膜那样,权利要求3的发明的构成中,前述薄膜形成采用选自溅射法、蒸镀法、离子电镀法、激光烧蚀法和电弧等离子体蒸镀法的1种方法来实施的情况下,可以更高效地制造低电阻且耐湿性良好的透明导电膜。
此外,如权利要求5的透明导电膜那样,在权利要求1~4中的任一项的发明的构成中,以氧化锌(ZnO)为主要成分,以7~40重量%的比例含有III族元素氧化物的情况下,可以高效地形成具备具有c轴朝向相互不同的多个方向的结晶结构的区域的透明导电膜或者ZnO(002)摇摆曲线半宽度在13.5°以上的透明导电膜,能够使本发明更具实效。
另外,使III族元素氧化物的掺入量在7~40重量%的范围内的原因在于,如果掺入量不到7重量%,则难以高效地形成具备具有c轴朝向相互不同的多个方向的结晶结构的区域的透明导电膜或者ZnO(002)摇摆曲线半宽度在13.5°以上的透明导电膜,而如果掺入量超过40重量%,则难以获得可实用的低电阻率的透明电极。
此外,如权利要求6的透明导电膜那样,在权利要求1~5中的任一项的发明的构成中,介以SiNx薄膜在基体上形成透明导电膜的情况下,例如基体为如由树脂材料形成的柔性基板等可透过水分的材料时,也可以高效地抑制、防止透过柔性基板(基体)的水分到达透明导电膜,确保足够的耐湿性,能够使本发明更具实效。
此外,本申请的发明中,如权利要求7那样,基体可以使用以选自玻璃、水晶、蓝宝石、Si、SiC、聚对苯二甲酸乙二醇酯(PET)、聚萘二甲酸乙二醇酯(PEN)、聚醚砜(PES)、聚酰亚胺、环烯烃类聚合物和聚碳酸酯的至少1种为主要成分的材料,如果采用本申请的发明,则可以在由这些材料形成的基体上获得具备实用水平的耐湿性且成本也低的ZnO类透明导电膜。
此外,如权利要求8的透明导电膜那样,在权利要求1~7中的任一项的发明的构成中,通过III族元素使用选自Ga、Al和In的至少1种,可以提供具备实用水平的耐湿性且成本也低的ZnO类透明导电膜。
另外,作为III族元素(掺杂元素)的种类,从实现充分的低电阻化的角度来看,最好是使用Ga,但使用作为其它III族元素的Al或In的情况下,也可以获得接近于使用Ga时的效果。
此外,权利要求9的透明导电膜的制造方法使用包含氧化锌(ZnO)和III族元素氧化物的原料,以III族元素氧化物的掺杂量在7~40重量%的范围内的条件通过薄膜形成方法在基体上成膜,所以可以在不需要特别复杂的工序的情况下,容易且可靠地在基体上形成具备具有c轴朝向相互不同的多个方向的结晶结构的区域的透明导电膜。
另外,该权利要求9的发明中,作为上述薄膜形成方法,可以使用以溅射法、蒸镀法、离子电镀法、激光烧蚀法、电弧等离子体蒸镀法、CVD法、溶胶-凝胶法等为代表的各种公知的方法。
此外,权利要求10的透明导电膜的制造方法具备通过使用包含氧化锌(ZnO)和III族元素氧化物的原料,以III族元素氧化物的掺杂量在7~40重量%的范围内的条件采用薄膜形成方法在基体上成膜,从而形成ZnO(002)摇摆曲线半宽度在13.5°以上的透明导电膜的工序,所以可以在不需要特别复杂的工序的情况下,容易且可靠地在基体上形成具备具有c轴朝向相互不同的多个方向的结晶结构的区域的透明导电膜。
此外,该权利要求9的发明中,作为上述薄膜形成方法,也可以使用以溅射法、蒸镀法、离子电镀法、激光烧蚀法、电弧等离子体蒸镀法、CVD法、溶胶-凝胶法等为代表的各种公知的方法。
权利要求11的透明导电膜的制造方法在制造包含氧化锌(ZnO)和III族元素的透明导电膜时,具备通过使用由包含氧化锌(ZnO)和III族元素氧化物的组合物形成的烧结体靶材,以III族元素氧化物的掺杂量在7~40重量%的范围内的条件采用选自溅射法、蒸镀法、离子电镀法、激光烧蚀法和电弧等离子体蒸镀法的1种方法在基体上成膜,从而在基体上形成具备具有c轴朝向相互不同的多个方向的结晶结构的区域的透明导电膜的工序,所以使用与用于实施上述薄膜形成方法的通常的装置基本相同的结构的装置,可以高效且低成本地制造具备实用水平的耐湿性的ZnO类的透明导电膜。
另外,通过事先求出预先形成的ZnO膜中的III族元素的掺杂量与靶材中的III族元素氧化物的比例的关系,使用由以规定比例包含氧化锌(ZnO)和III族元素氧化物的组合物形成的烧结体靶材,以上述薄膜形成方法进行成膜,从而可以可靠地获得所需掺杂量的ZnO膜。
此外,权利要求12的透明导电膜的制造方法在制造包含氧化锌(ZnO)和III族元素的透明导电膜时,具备通过使用由包含氧化锌(ZnO)和III族元素氧化物的组合物形成的烧结体靶材,以III族元素氧化物的掺杂量在7~40重量%的范围内的条件采用选自溅射法、蒸镀法、离子电镀法、激光烧蚀法和电弧等离子体蒸镀法的1种方法在基体上成膜,从而在基体上形成ZnO(002)摇摆曲线半宽度在13.5°以上的透明导电膜的工序,所以使用与用于实施上述薄膜形成方法的通常的装置基本相同的结构的装置,可以高效且低成本地制造具备实用水平的耐湿性的ZnO类的透明导电膜。
此外,如权利要求13的透明导电膜的制造方法那样,在权利要求9~12中的任一项的发明的构成中,使通过以薄膜形成方法成膜而形成透明导电膜的基体的温度和III族元素氧化物的掺杂量的关系呈图4的以点a、b、c确定的范围内的关系,从而可以高效地形成具备具有c轴朝向相互不同的多个方向的结晶结构的区域的透明导电膜或者ZnO(002)摇摆曲线半宽度在13.5°以上的透明导电膜,能够使本发明更具实效。
即,通过根据III族元素氧化物的掺杂量,将进行采用上述薄膜形成方法的成膜来形成透明导电膜时的基体的温度控制在图4的以点a、b、c确定的范围内,从而控制ZnO膜(透明导电膜)的结晶状态,可以高效地形成具备具有c轴朝向相互不同的多个方向的结晶结构的区域的透明导电膜或者ZnO(002)摇摆曲线半宽度在13.5°以上的透明导电膜,能够使本发明更具实效。
另外,图4的点a和b的连线的斜率可以根据成膜条件进行调整(变化),而且通过适当调整点a和b的连线的斜率,可以更高效地控制ZnO膜的结晶状态,获得特性良好的透明导电膜。
此外,如权利要求14的透明导电膜的制造方法那样,在权利要求11~13中的任一项的发明的构成中,通过前述选自溅射法、蒸镀法、离子电镀法、激光烧蚀法和电弧等离子体蒸镀法的1种方法成膜时,在对前述基体施加偏压的同时进行成膜的情况下,可以使III族元素氧化物的掺杂量降低且使耐湿性提高,能够可靠地制造低电阻且耐湿性良好的透明导电膜。
此外,如权利要求1 5的透明导电膜的制造方法那样,在权利要求9~14中的任一项的发明的构成中,通过在使背压达到1×10-4Pa以下的真空室内进行基于薄膜形成方法的成膜,从而可以更可靠地制造兼具实用水平的电阻率和耐湿性的ZnO类的透明导电膜。
此外,如权利要求16的透明导电膜的制造方法那样,通过在基体上形成SiNx薄膜后,以权利要求9~15中的任一项所述的方法介以前述SiNx薄膜于前述基体上形成前述透明导电膜,从而在例如基体为由树脂材料形成的柔性基板等可透过水分的材料时,也可以高效地抑制、防止透过柔性基板(基体)的水分到达透明导电膜,确保足够的耐湿性,能够使本发明更具实效。
此外,本发明的透明导电膜的制造方法中,如权利要求17那样,基体可以使用以选自玻璃、水晶、蓝宝石、Si、SiC、聚对苯二甲酸乙二醇酯(PET)、聚萘二甲酸乙二醇酯(PEN)、聚醚砜(PES)、聚酰亚胺、环烯烃类聚合物和聚碳酸酯的至少1种为主要成分的材料,如果采用本申请的发明的透明导电膜的制造方法,则可以在由这些材料形成的基体上形成具备实用水平的耐湿性且成本也低的ZnO类透明导电膜。
此外,如权利要求18的透明导电膜的制造方法,在权利要求9~17中的任一项的发明的构成中,通过III族元素使用选自Ga、Al和In的至少1种,可以高效地形成具备实用水平的耐湿性且成本也低的ZnO类透明导电膜。
另外,作为III族元素(掺杂元素)的种类,从实现充分的低电阻化的角度来看,最好是使用Ga。但是,使用作为其它III族元素的Al或In的情况下,也可以获得接近于使用Ga时的效果。
另外,如上所示,In为高价的物质,但因为被用作添加物(掺杂剂),所以与像以往那样用作主要成分的情况相比,可以大幅降低成本。
附图的简单说明
图1为表示ZnO膜(透明导电膜)中的Ga2O3的掺杂浓度与电阻率等的关系的图。
图2为表示对以往的ZnO膜(透明导电膜)进行耐湿性试验(85℃、85%RH)时的经过时间与电阻变化率的关系的图。
图3为表示对本申请的发明的ZnO膜(透明导电膜)进行耐湿性试验(85℃、85%RH)时的经过时间与电阻变化率的关系的图。
图4为表示制造本申请的发明的透明导电膜时的III族元素氧化物掺杂浓度与加热温度的关系的图。
图5为表示向ZnO膜(透明导电膜)中的Ga2O3掺杂浓度与c轴取向性的关系的线图。
图6为表示本申请的发明的范围外的Ga2O3掺杂浓度为4.1重量%的样品的透射电子显微镜图像的图。
图7为表示本申请的发明的范围内的Ga2O3掺杂浓度为22.8重量%的样品的透射电子显微镜图像的图。
图8为表示本申请的发明的范围外的Ga2O3掺杂浓度为4.1重量%的样品的结晶结构的模式图。
图9为表示本申请的发明的范围内的Ga2O3掺杂浓度为22.8重量%的样品的结晶结构的模式图。
图10为显示本申请的发明的范围外的Ga2O3掺杂浓度为4.1重量%的样品的表面状态的原子力显微镜照片。
图11为显示本申请的发明的范围内的Ga2O3掺杂浓度为22.8重量%的样品的表面状态的原子力显微镜照片。
图12为对于本申请的发明的范围外的Ga2O3掺杂浓度为4.1重量%的样品的X射线衍射的ZnO(002)入射极点图。
图13为对于本申请的发明的范围内的Ga2O3掺杂浓度为12.6重量%的样品的X射线衍射的ZnO(002)入射极点图。
图14为对于本申请的发明的范围内的Ga2O3掺杂浓度为22.8重量%的样品的X射线衍射的ZnO(002)入射极点图。
图15为表示向ZnO膜(透明导电膜)中的Ga2O3掺杂浓度与ZnO(002)摇摆曲线半宽度的关系的图。
图16为表示本申请的发明的实施例2中对于形成于柔性基板(PEN基板)上的ZnO膜(透明导电膜)进行耐湿性试验(85℃、85%RH)时的经过时间与电阻变化率的关系的图。
图17为表示本申请的发明的实施例4中对于形成于柔性基板(PEN基板)上的ZnO膜(透明导电膜)进行耐湿性试验(85℃、85%RH)时的经过时间与电阻变化率的关系的图。
图18为表示向基板施加的偏压与ZnO膜(透明导电膜)的c轴取向性的关系的线图。
图19(a)~(d)为对于分别向基板施加-80V~+40V的偏压的同时制成的ZnO膜的X射线衍射的ZnO(002)入射极点图。
图20为表示通过本申请的发明的实施例4的方法制成的透明导电膜的透射电子显微镜图像的图。
图21为表示向基板施加的偏压与电阻率和Ga2O3的掺杂浓度的关系的图。
符号的说明
B:晶界,G:晶粒,R:区域。
实施发明的最佳方式
以下,示例本发明的实施例,对本发明的特征点更具体地进行说明。
在氧化锌(ZnO)中掺杂III族元素氧化物并使其在基体上生长而得的本发明的透明导电膜中,作为向ZnO的掺杂剂(III族元素),具代表性的是Ga、Al、In。
如果将这些III族元素(III族元素氧化物)掺杂到ZnO中,则2价的Zn位被3价的阳离子置换,因此剩余电子成为载流子,呈现出n型的导电性。如果再使用溅射法、蒸镀法、离子电镀法、激光烧蚀法、电弧等离子体蒸镀法、CVD法、溶胶-凝胶法等成膜方法以氧供给低于化学计量学比的条件使其生长,则形成的膜中产生氧缺陷,剩余电子成为载流子,最终呈现出n型的导电性。
因此,掺入了III族元素的ZnO是将基于位点置换的给体型的杂质添加和基于氧缺陷的电子产生这两者作为载流子的供给源的n型半导体。
此外,在氧化锌(ZnO)中掺杂了III族元素的导电体中,例如文献“南内嗣等,J.Vac.Soc.(真空),Vol.47,No.10,(2004)734.”中报道了将Ga作为掺杂剂的情况下的掺杂量与物性的关系,如图1所示,以Ga2O3换算,掺杂量为2~4重量%时达到最低的电阻率。因此,如果考虑到作为透明导电膜的应用,则使掺杂量在可以获得低电阻率的ZnO膜的所述2~4重量%的范围内是有利的。
另外,若增加掺杂量则电阻率相对增大,因此即使扩大掺杂量的范围,可使用的范围通常也最多达到2~6重量%左右。这是因为,如果考虑到作为透明导电膜的应用,则使电阻率尽量低是有利的,不需要特意增加掺杂量来提高电阻率。
然而,减少了掺杂量的ZnO膜被确认在耐湿试验中伴随显著的劣化。例如,从前述文献可知,对于Ga2O3换算浓度为2~4重量%的ZnO膜进行了耐湿性试验(85℃、85%RH)后确认,经过200小时后,形成于玻璃基板上的ZnO膜和形成于使用了作为塑料中的1种的PEN(聚萘二甲酸乙二醇酯)的柔性基板上的ZnO膜分别产生了约30%和约60%的电阻变化(电阻率的增大)(图2)。这样的电阻率的劣化水平是无法实用化的劣化水平。
此外,发明者考虑到基于ZnO膜的耐湿试验的电阻率劣化(电阻率的增大)的原因很可能是在于氧缺陷的化学不稳定性,尝试采取了(1)故意向真空室内导入水而将氧缺陷封端的方法、(2)加热基板而促进结晶的方法等对策。然而,这些方法都无法获得足够的效果。
于是,发明者进一步进行实验、研究,将III族元素的掺杂量相对以往的掺杂量大幅增加,结果发现基于ZnO膜的耐湿试验的电阻率劣化(电阻率的增大)显著得到抑制,进一步反复进行实验、研究,从而完成了本发明。
如前所述,ZnO的载流子供给来自于位点置换和氧缺陷这两方面,技术上难以定量地分析各自的贡献程度。然而,定性地来看,认为通过尽可能减少氧缺陷的贡献而使位点置换的贡献比例占主导,可能会缓解化学不稳定性,因而进行了将III族元素的掺杂量相对以往的掺杂量大幅增加的高浓度掺杂,考察所得ZnO膜的特性。
即,准备无掺杂的ZnO溅射靶材和配置于其上的Ga2O3颗粒,通过配置于无掺杂的ZnO溅射靶材上的Ga2O3颗粒的数量调整掺杂浓度而进行溅射,从而在玻璃基板上形成掺杂了Ga2O3的ZnO膜,通过ICP组成分析定量评价Ga2O3颗粒数与Ga2O3掺杂浓度的关系。
其结果为,确认Ga2O3颗粒数与Ga2O3掺杂浓度的关系呈如下的关系。
(1)Ga2O3颗粒数1个 :Ga2O3掺杂浓度4.1重量%,
(2)Ga2O3颗粒数1.5个 :Ga2O3掺杂浓度6.5重量%,
(3)Ga2O3颗粒数2个 :Ga2O3掺杂浓度8.1重量%,
(4)Ga2O3颗粒数2.5个 :Ga2O3掺杂浓度10.8重量%,
(5)Ga2O3颗粒数3个 :Ga2O3掺杂浓度12.6重量%,
(6)Ga2O3颗粒数5个 :Ga2O3掺杂浓度22.8重量%。
对于这样制成的Ga的掺杂浓度在4.1~22.8重量%的范围内的样品,进行了耐湿性试验(85℃、85%RH),结果如图3所示,Ga2O3的掺杂浓度在8.1重量%以上的样品的情况下,200小时后也未确认到电阻率的大幅劣化(电阻变化率的大幅增大)。相反地,掺杂浓度为低于作为本申请的发明的下限侧的范围的7.0重量%的4.1重量%和6.5重量%的情况下,确认24小时后的电阻变化率为约13%,200小时后的电阻变化率达到20%以上,即电阻率的劣化增大,无法获得实用水平的ZnO膜。
此外,同样地在使用了PEN(聚萘二甲酸乙二醇酯)的柔性基板上形成ZnO膜的情况下,如果Ga2O3的掺杂浓度达到7.0重量%以上,则200小时后也未确认到电阻的大幅劣化,但如果Ga2O3的掺杂浓度低于7.0重量%,则电阻变化率增大,产生不理想的结果。
以下,示例具体的实施例,对本发明的特征点更具体地进行说明。
实施例1
作为基体,准备由无碱玻璃(康宁7059)形成的玻璃基板。接着,通过用异丙醇和UV照射清洁该玻璃基板,获得洁净表面。
此外,作为溅射靶材,准备烧结密度在80%以上的直径6英寸的ZnO烧结体靶材。
另外,作为掺杂用,准备由Ga氧化物(Ga2O3)形成的直径10mm的颗粒(Ga2O3颗粒)。
接着,本实施例1中,将Ga2O3颗粒配置于上述ZnO烧结体靶材上的侵蚀区域,进行溅射,从而在基体上形成掺杂了Ga2O3的ZnO膜。
另外,Ga2O3的掺杂量通过调整上述Ga2O3颗粒的数量来进行调整。
进行溅射时,将玻璃基板设置于溅射装置的真空室中,抽真空至5×10-5Pa后,在不加热玻璃基板(基体)的情况下进行溅射。
此外,本实施例1中,溅射气体使用高纯度氩气,导入溅射气体至真空室内的压力达到1Pa。
另外,本发明的透明导电膜的制造方法中,可以通过加热基体来控制所形成的ZnO膜的结晶结构,但该情况下,理想的是使基体的温度和III族元素氧化物的掺杂量的关系呈图4的以点a、b、c确定的三角形形状的区域R的范围内的关系。该情况下,通过根据成膜条件调整点a和b的连线的斜率,可以高效地控制ZnO膜的结晶状态,获得特性更好的透明导电膜。
接着,以RF电力500W的条件开始溅射,进行成膜,形成具有规定膜厚的以规定的比例掺杂了Ga的ZnO膜(透明导电膜)。另外,成膜得到的ZnO膜的设定膜厚为400nm。
接着,对于成膜得到的ZnO膜进行采用湿法蚀刻的图案形成后,使用探针式轮廓仪确认膜厚相对于设定膜厚达到±15%。
对于上述的样品,通过4探针测定求得的电阻率如下:
(1)Ga2O3颗粒的数量为1个时,5.9×10-4Ωcm;
(2)Ga2O3颗粒的数量为3个时,9.1×10-4Ωcm;
(3)Ga2O3颗粒的数量为5个时,4.8×10-3Ωcm。
此外,薄层电阻如下:
(1)Ga2O3颗粒的数量为1个时,13Ω/□;
(2)Ga2O3颗粒的数量为3个时,22Ω/□;
(3)Ga2O3颗粒的数量为5个时,116Ω/□。
此外,可见区域的透光率在Ga2O3颗粒的数量为1个、3个和5个的情况下都达到80%以上。
此外,成膜得到的ZnO膜的表面粗糙度(Rms)如下:
(1)Ga2O3颗粒的数量为1个时,6.969nm(第1次),7.437nm(第2次);
(2)Ga2O3颗粒的数量为3个时,4.062nm(第1次),4.834nm(第2次);
(3)Ga2O3颗粒的数量为5个时,4.091nm(第1次),4.235nm(第2次)。
由该结果可知,随着掺杂浓度的上升,粒生长受到抑制,ZnO膜的表面变得平坦。
另外,Ga2O3颗粒数与Ga2O3掺杂浓度的关系如实施发明的最佳方式的栏中所述,呈如下的关系:
(1)Ga2O3颗粒数1个 :Ga2O3掺杂浓度4.1重量%,
(2)Ga2O3颗粒数1.5个 :Ga2O3掺杂浓度6.5重量%,
(3)Ga2O3颗粒数2个 :Ga2O3掺杂浓度8.1重量%,
(4)Ga2O3颗粒数2.5个 :Ga2O3掺杂浓度10.8重量%,
(5)Ga2O3颗粒数3个 :Ga2O3掺杂浓度12.6重量%,
(6)Ga2O3颗粒数5个 :Ga2O3掺杂浓度22.8重量%。
此外,对于这些样品,如实施发明的最佳方式的栏中所述,在玻璃基板上Ga2O3颗粒数在2个(即Ga2O3掺杂浓度8.1重量%)以上的条件的情况下,200小时后也未确认到电阻的大幅劣化(电阻变化率的大幅增大)(参照图3)。
但是,Ga2O3颗粒数为1个(Ga2O3掺杂浓度4.1重量%)和1.5个(Ga2O3掺杂浓度6.5重量%)的情况下,确认电阻变化率随时间增大,24小时后的电阻变化率为约13%,200小时后的电阻变化率达到20%以上。
此外,图5为上述(1)的Ga2O3掺杂浓度4.1重量%的样品、上述(5)的Ga2O3掺杂浓度12.6重量%的样品和上述(6)的Ga2O3掺杂浓度22.8重量%的样品的基于X射线衍射法的θ-2θ扫描的图。
如图5所示,Ga2O3掺杂浓度4.1重量%的样品出现较大的c轴峰,但Ga2O3掺杂浓度12.6重量%的样品的c轴峰显著变小,而Ga2O3掺杂浓度22.8重量%的样品完全未确认到c轴峰,可知随Ga2O3掺杂浓度的升高,c轴取向的程度变弱。
也由此认为,本申请的发明的ZnO膜的耐湿性提高的原因在于,Ga2O3掺杂浓度升高,c轴取向变弱,从而氧缺陷的再氧化受到抑制。
此外,图6为表示本申请的发明的范围外的Ga2O3掺杂浓度为4.1重量%的样品的透射电子显微镜图像的图,图7为表示本申请的发明的范围内的Ga2O3掺杂浓度22.8重量%的样品的透射电子显微镜图像的图。
此外,图8为表示本申请的发明的范围外的Ga2O3掺杂浓度为4.1重量%的样品的结晶结构的模式图,图9为表示本申请的发明的范围内的Ga2O3掺杂浓度22.8重量%的样品的结晶结构的模式图。
另外,图8和图9中,晶粒G内的多条平行的线模式化表示晶格距离。
如图6和图8所示,可知Ga2O3掺杂浓度低至4.1重量%的本申请的发明的范围外的ZnO膜的向基板法线方向的c轴取向占主导,c轴的朝向一致,而且晶粒G为柱状,形成典型的柱状生长。
相反地,Ga2O3掺杂浓度高至22.8重量%的本申请的发明的范围内的ZnO膜如图7和图9所示,可知c轴朝向相互不同的多个方向(图7),晶粒G不为柱状(图9)。另外,推测在晶界B可能存在非晶质或具有介于非晶质和晶质之间的所谓准结晶结构的区域等。
另外,可以说表示本申请的发明的范围内的ZnO膜的结晶结构的图7和图9证实了本发明的技术思想,即,c轴朝向相互不同的多个方向的情况下,氧缺失不易被再氧化,耐湿性提高。
此外,图10为显示本申请的发明的范围外的Ga2O3掺杂浓度为4.1重量%的样品的表面状态的原子力显微镜照片,图11为显示本申请的发明的范围内的Ga2O3掺杂浓度为22.8重量%的样品的表面状态的原子力显微镜照片。
本申请的发明的范围外的Ga2O3掺杂浓度为4.1重量%的样品的情况如图10所示,表面确认到c轴的方向一致的结晶产生的凹凸,但本申请的发明的范围内的Ga2O3掺杂浓度为22.8重量%的样品的c轴朝向相互不同的多个方向,因此在表面未确认到明显的结晶产生的凹凸或晶界,形成平坦的状态。
可以说该图10和图11也证实了本发明的技术思想,即,c轴朝向相互不同的多个方向的情况下,氧缺失不易被再氧化,耐湿性提高。
此外,图12为对于本申请的发明的范围外的Ga2O3掺杂浓度为4.1重量%的样品的X射线衍射的ZnO(002)入射极点图,图13和图14为对于本申请的发明的范围内的Ga2O3掺杂浓度为12.6重量%和22.8重量%的各样品的X射线衍射的ZnO(002)入射极点图。
由图12可知,Ga2O3掺杂浓度低至4.1重量%的本申请的发明的范围外的ZnO膜的c轴一致朝向基板法线方向。
相反地,本申请的发明的范围内的Ga2O3掺杂浓度为12.6重量%的样品如图13所示,与图12的本申请的发明的范围外的样品相比,c轴方向的一致程度极低。
另外,图14的本申请的发明的范围内的Ga2O3掺杂浓度为22.8重量%的样品与本申请的发明的范围外的图12的样品相比,c轴方向的一致程度极低。
因此,可以说该图12、图13和图14也证实了本发明的技术思想,即,c轴朝向相互不同的多个方向的情况下,氧缺失不易被再氧化,耐湿性提高。
此外,图15为表示Ga2O3掺杂浓度与ZnO(002)摇摆曲线半宽度的关系的图。
如图15所示,若Ga2O3掺杂浓度达到7重量%以上,则ZnO(002)摇摆曲线半宽度在13.5°以上。由此,如果摇摆曲线半宽度达到13.5°以上,则ZnO膜的c轴取向程度弱,耐湿性提高。
由本实施例1可知,在广泛使用的玻璃基板上可以形成具备可实用的耐湿性的透明导电膜。
此外,作为III族元素(掺杂元素)的种类,从实现充分的低电阻化的角度来看,最好是使用Ga,但使用作为其它III族元素的Al或In的情况下,也可以获得接近于使用Ga时的效果。
此外,在掺入作为III族元素的Ga以及Al和In中的至少一方的至少2种III族元素的情况下,也可以获得同样的效果。
另外,除了作为III族元素的Ga以外,同时添加除III族元素以外的其它掺杂剂的情况下,也可以获得本发明的基本效果。
实施例2
上述的实施例1中,对形成透明导电膜的基体为玻璃基板的情况进行了说明,但本实施例2中,作为形成透明导电膜的基体,使用由PEN(聚萘二甲酸乙二醇酯)形成的基板(柔性基板),通过与上述实施例1的情况同样的方法进行基板的预处理。
然后,与上述实施例1的情况同样地,作为溅射靶材,准备烧结密度在80%以上的直径6英寸的ZnO烧结体靶材。
另外,与上述实施例1的情况同样地,准备由Ga氧化物(Ga2O3)形成的直径10mm的掺杂用颗粒(Ga2O3颗粒)。
此外,本实施例2中,Ga2O3的掺杂量也通过调整上述Ga2O3颗粒的数量来进行调整。
接着,使用与上述实施例1的情况同样的溅射装置,以同样的方法、同样的条件进行溅射,在PEN基板(柔性基板)上形成掺杂了Ga的ZnO膜(透明导电膜)。
接着,对于成膜得到的ZnO膜进行采用湿法蚀刻的图案形成后,使用探针式轮廓仪确认达到设定膜厚。
对于上述的样品,通过4探针测定求得的电阻率如下:
(1)Ga2O3颗粒的数量为1个时,6.7×10-4Ωcm;
(2)Ga2O3颗粒的数量为3个时,8.1×10-4Ωcm;
(3)Ga2O3颗粒的数量为5个时,3.4×10-3Ωcm。
此外,薄层电阻如下:
(1)Ga2O3颗粒的数量为1个时,15Ω/□;
(2)Ga2O3颗粒的数量为3个时,20Ω/□;
(3)Ga2O3颗粒的数量为5个时,77Ω/□。
此外,可见光区域的透光率在Ga2O3颗粒的数量为1个、3个和5个的情况下都达到80%以上。
另外,通过ICP组成分析进行了定量评价,结果确认实施例2的情况下确认Ga2O3颗粒数与Ga2O3掺杂浓度的关系呈如下的关系:
(1)Ga2O3颗粒数1个:Ga2O3掺杂浓度5.5重量%,
(2)Ga2O3颗粒数3个:Ga2O3掺杂浓度14.8重量%,
(3)Ga2O3颗粒数5个:Ga2O3掺杂浓度28.5重量%。
然后,对本实施例2中制成的样品进行了高温高湿的耐湿性试验,结果如图16所示,Ga2O3颗粒数为1个、Ga2O3掺杂浓度为5.5重量%的情况下,电阻随时间显著增大,但Ga2O3颗粒数为3个,Ga2O3掺杂浓度为14.8重量%的情况下,200小时后的电阻的变化率(增大率)为8.8%,Ga2O3颗粒数为5个、Ga2O3掺杂浓度28.5重量%的情况下,200小时后的电阻的变化率(增大率)为7.8%,确认与Ga2O3颗粒数1个(Ga2O3掺杂浓度5.5重量%)的情况相比,耐湿性显著提高。
由本实施例2可知,通过本发明的方法制造的ZnO类的透明导电膜也可以应用于使用了由PEN形成的柔性基板的所谓柔性器件。
实施例3
使用由PET(聚对苯二甲酸乙二醇酯)形成的基板(柔性基板)代替上述实施例2中使用的由PEN(聚萘二甲酸乙二醇酯)形成的基板(柔性基板),以与上述实施例2的情况同样的方法和条件进行溅射,形成掺入了Ga的ZnO膜(透明导电膜)。
接着,对于得到的ZnO膜(透明导电膜),以同样的条件测定了特性,结果确认可获得具有与上述实施例2同样的特性的ZnO膜(透明导电膜)。
由此可知,在广泛使用的由PEN(聚对苯二甲酸乙二醇酯)形成的基板(柔性基板)上也可以形成可实用的透明导电膜。
实施例4
作为基体,准备由无碱玻璃(康宁1737)形成的玻璃基板。接着,通过用异丙醇和UV照射清洁该玻璃基板(基体),获得洁净表面。
此外,作为溅射靶材,准备烧结密度在80%以上的直径4英寸的ZnO烧结体靶材。
另外,作为掺杂用,准备由Ga氧化物(Ga2O3)形成的直径10mm的颗粒(Ga2O3颗粒)。
本实施例4中,将Ga2O3颗粒配置于上述ZnO烧结体靶材上的侵蚀区域,进行溅射,从而在基体上形成掺杂了Ga2O3的ZnO膜。
另外,Ga2O3的掺杂量通过调整上述Ga2O3颗粒的数量来进行调整。
进行溅射时,将玻璃基板设置于溅射装置的真空室中,抽真空至5×10-5Pa后,在不加热玻璃基板的情况下,对基体施加-80V偏压,进行溅射。
此外,本实施例4中,溅射气体使用高纯度氩气,导入溅射气体至真空室内的压力达到1Pa。
接着,以RF电力250W的条件开始溅射,进行成膜,形成具有规定膜厚的以规定的比例掺杂了Ga的ZnO膜(透明导电膜)。另外,成膜得到的ZnO膜的设定膜厚为400nm。
接着,对于成膜得到的ZnO膜进行采用湿法蚀刻的图案形成后,使用探针式轮廓仪确认膜厚相对于设定膜厚达到±15%。
成膜得到的ZnO膜的Ga的掺杂浓度为4.5重量%,电阻率为8.3×10-4Ωcm。
此外,对于该ZnO膜实施了85℃、85%RH的耐湿试验,结果如图17所示,经过1000小时后的电阻变化率为+10%,获得了良好的结果。另外,图17表示将向玻璃基板(基体)施加的偏压设为-80V时的电阻变化率的数据的同时,还一并表示对于将向玻璃基板施加的偏压设为-40V、0V、+40V制成的样品(透明导电膜)进行测定而得的电阻变化率的数据。
如上所述,确认通过对玻璃基板(基体)施加-80V偏压来进行溅射而成膜得到的ZnO膜耐湿性显著提高,经过1000小时后的电阻变化率良好,为+10%。为了探究其原因,改变向玻璃基板(基体)施加的偏压,制成透明导电膜,进行了结构分析。
图18为对于将向基板施加的偏压分别设为-80V、0V、+40V而制成的样品的基于X射线衍射的θ-2θ扫描的图。
如图18所示,与施加了正偏压的情况和未施加偏压的情况相比,施加了负偏压的情况下,确认c轴峰变弱的倾向,如果施加-80V的偏压,则确认c轴峰基本消失。
此外,图19(a)、(b)、(c)、(d)为对于将向基板施加的偏压分别设为-80V、0V、+40V而制成的透明导电膜的X射线衍射的ZnO(002)入射极点图。如图19(a)所示,将向玻璃基板施加的偏压设为-80V而制成的透明导电膜明显地确认到发生c轴的散乱。
此外,图20为表示将向玻璃基板施加的偏压设为-80V而制成的透明导电膜的透射电子显微镜图像的图。由图20可知,施加了-80V的偏压的ZnO膜的情况下,c轴倾斜生长,以与高浓度掺杂膜同样的结晶结构进行生长。
如上述实施例1~3所示,推测以高浓度掺杂III族元素(Ga)的情况下耐水性的提高是基于III族元素(Ga)的高浓度掺杂产生的c轴柱状结构的散乱而使H2O扩散的活化能增大的机理,但认为向玻璃基板施加偏压的同时进行溅射的情况下ZnO膜的耐水性的提高是基于c轴柱状生长因Ar+离子产生的轰击效果和Ar+离子向膜中的侵入而受到抑制。
另外,表1表示通过WDX(波长分散型X射线元素分析)分析ZnO膜中的Ar含量而得的结果。
[表1]
偏压(V) | 含量(重量%) | |||||||
O | Si | Ar | Ca | Zn | Ga | Sb | Ba | |
-80 | 25.8 | 2.9 | 0.6 | 0.6 | 64.3 | 3.4 | 0.4 | 2.0 |
-80 | 24.6 | 2.5 | 0.8 | 0.5 | 66.4 | 3.1 | 0.3 | 1.8 |
-40 | 24.3 | 1.9 | 0.2 | 0.4 | 68.3 | 2.9 | 0.5 | 1.6 |
0 | 23.4 | 1.7 | 0.2 | 0.4 | 69.0 | 3.7 | 0.3 | 1.3 |
+40 | 23.9 | 1.9 | 0.2 | 0.5 | 68.4 | 3.3 | 0.3 | 1.5 |
如表1所示,随着负偏压的绝对值的增大,Ar的侵入量增加。
此外,图21为表示向玻璃基板施加的偏压与电阻率和Ga2O3的掺杂浓度的关系的图。
由图21可知,向玻璃基板的偏压的施加几乎不影响电阻率。因此,通过向玻璃基板施加偏压的同时进行成膜,可以同时实现低电阻化和高耐湿化。
另外,本实施例4的向玻璃基板施加偏压的同时形成透明导电膜的方法的情况下,作为掺杂元素的种类,从实现低电阻化的角度来看,最好是Ga,但使用作为III族元素的Al或In的情况下,也预期具有同样的效果。此外,在Ga中再加入Al或In的情况下,也预期具有同样的效果。
此外,实施例4中,通过向基体施加负偏压的同时进行薄膜形成,可以获得耐湿性良好的透明导电膜,但向基体施加的偏压的正负和偏压的值(绝对值)等较好是根据III族元素的重量和掺杂浓度等条件设定最适的条件,根据情况,也可以存在较好是施加与上述实施例4的情况不同的值(绝对值)的正偏压的同时进行薄膜形成的情况。
实施例5
使用由PET(聚对苯二甲酸乙二醇酯)形成的基板(柔性基板)代替上述实施例4中使用的由无碱玻璃形成的基板(基体),以与上述实施例4的情况同样的方法和条件进行溅射,向该柔性基板施加偏压的同时进行溅射,形成掺入了Ga的ZnO膜(透明导电膜)。
接着,对于得到的ZnO膜(透明导电膜),以同样的条件测定了特性,结果确认可获得具有与上述实施例4同样的特性的ZnO膜(透明导电膜)。
由此可知,在广泛使用的由PET(聚对苯二甲酸乙二醇酯)形成的基板(柔性基板)上也可以形成可实用的透明导电膜。
另外,上述实施例1~5中,在玻璃基板、PEN基板和PET基板上形成了ZnO膜(透明导电膜),但也可以形成于玻璃、水晶、蓝宝石、Si等的单晶基板上,该情况下也可以获得与上述的形成于玻璃基板上的情况同样的效果。
此外,上述实施例1~5中,对直接在基体上形成ZnO膜(透明导电膜)的情况进行了说明,但在如柔性基板那样透过水分的基板上形成ZnO膜(透明导电膜)的情况下,通过介以SiNx薄膜在基体上形成ZnO膜(透明导电膜),可以使透明导电膜的耐湿性进一步提高,也可以使耐湿试验中的经过1000小时后的电阻变化率为0。
本发明在其它方面也并不局限于上述的各实施例,关于形成透明导电膜的基体的形状和构成材料的种类、III族元素的种类和掺杂量、透明导电膜的具体成膜条件等,在本发明的范围内可以进行各种应用、变形。
产业上利用的可能性
如上所述,采用本申请的发明,可以高效且可靠地制造具备可实用的耐湿性和作为透明导电膜所必需的特性且成本低的ZnO类的透明导电膜。
因此,本发明可以广泛地用于平板显示器和太阳能电池的透明电极等各种用途。
Claims (33)
1.透明导电膜,它是在氧化锌(ZnO)中掺杂III族元素并使其在基体上生长而得的透明导电膜,其特征在于,具备具有c轴朝向相互不同的多个方向的结晶结构的区域,以氧化锌(ZnO)为主要成分,以22.8~40重量%的比例含有III族元素氧化物。
2.如权利要求1所述的透明导电膜,其特征在于,前述透明导电膜通过对前述基体施加偏压的同时进行薄膜形成而获得。
3.如权利要求2所述的透明导电膜,其特征在于,前述薄膜形成采用选自溅射法、蒸镀法、离子电镀法、激光烧蚀法和电弧等离子体蒸镀法的1种方法。
4.如权利要求1或2所述的透明导电膜,其特征在于,前述透明导电膜介以SiNx薄膜形成于基体上。
5.如权利要求1或2所述的透明导电膜,其特征在于,前述基体以选自玻璃、水晶、蓝宝石、Si、SiC、聚对苯二甲酸乙二醇酯(PET)、聚萘二甲酸乙二醇酯(PEN)、聚醚砜(PES)、聚酰亚胺、环烯烃类聚合物和聚碳酸酯的至少1种为主要成分。
6.如权利要求1或2所述的透明导电膜,其特征在于,前述III族元素为选自Ga、Al和In的至少1种。
7.透明导电膜,它是在氧化锌(ZnO)中掺杂III族元素并使其在基体上生长而得的透明导电膜,其特征在于,ZnO(002)摇摆曲线半宽度在13.5°以上,以氧化锌(ZnO)为主要成分,以22.8~40重量%的比例含有III族元素氧化物。
8.如权利要求7所述的透明导电膜,其特征在于,前述透明导电膜通过对前述基体施加偏压的同时进行薄膜形成而获得。
9.如权利要求8所述的透明导电膜,其特征在于,前述薄膜形成采用选自溅射法、蒸镀法、离子电镀法、激光烧蚀法和电弧等离子体蒸镀法的1种方法。
10.如权利要求7或8所述的透明导电膜,其特征在于,前述透明导电膜介以SiNx薄膜形成于基体上。
11.如权利要求7或8所述的透明导电膜,其特征在于,前述基体以选自玻璃、水晶、蓝宝石、Si、SiC、聚对苯二甲酸乙二醇酯(PET)、聚萘二甲酸乙二醇酯(PEN)、聚醚砜(PES)、聚酰亚胺、环烯烃类聚合物和聚碳酸酯的至少1种为主要成分。
12.如权利要求7或8所述的透明导电膜,其特征在于,前述III族元素为选自Ga、Al和In的至少1种。
13.透明导电膜的制造方法,它是用于制造包含氧化锌(ZnO)和III族元素的透明导电膜的方法,其特征在于,具备使用包含氧化锌(ZnO)和III族元素氧化物的原料,以III族元素氧化物的掺杂量在22.8~40重量%的范围内的条件通过薄膜形成方法在基体上成膜,在基体上形成具备具有c轴朝向相互不同的多个方向的结晶结构的区域的透明导电膜的工序。
14.如权利要求13所述的透明导电膜的制造方法,其特征在于,基于前述薄膜形成方法的成膜在使背压达到1×10-4Pa以下的真空室内进行。
15.如权利要求13所述的透明导电膜的制造方法,其特征在于,前述基体以选自玻璃、水晶、蓝宝石、Si、SiC、聚对苯二甲酸乙二醇酯(PET)、聚萘二甲酸乙二醇酯(PEN)、聚醚砜(PES)、聚酰亚胺、环烯烃类聚合物和聚碳酸酯的至少1种为主要成分。
16.如权利要求13所述的透明导电膜的制造方法,其特征在于,前述III族元素为选自Ga、Al和In的至少1种。
17.透明导电膜的制造方法,它是用于制造包含氧化锌(ZnO)和III族元素的透明导电膜的方法,其特征在于,具备使用包含氧化锌(ZnO)和III族元素氧化物的原料,以III族元素氧化物的掺杂量在22.8~40重量%的范围内的条件通过薄膜形成方法在基体上成膜,在基体上形成ZnO(002)摇摆曲线半宽度在13.5°以上的透明导电膜的工序。
18.如权利要求17所述的透明导电膜的制造方法,其特征在于,基于前述薄膜形成方法的成膜在使背压达到1×10-4Pa以下的真空室内进行。
19.如权利要求17所述的透明导电膜的制造方法,其特征在于,前述基体以选自玻璃、水晶、蓝宝石、Si、SiC、聚对苯二甲酸乙二醇酯(PET)、聚萘二甲酸乙二醇酯(PEN)、聚醚砜(PES)、聚酰亚胺、环烯烃类聚合物和聚碳酸酯的至少1种为主要成分。
20.如权利要求17所述的透明导电膜的制造方法,其特征在于,前述III族元素为选自Ga、Al和In的至少1种。
21.透明导电膜的制造方法,它是用于制造包含氧化锌(ZnO)和III族元素的透明导电膜的方法,其特征在于,具备使用由包含氧化锌(ZnO)和III族元素氧化物的组合物形成的烧结体靶材,以III族元素氧化物的掺杂量在22.8~40重量%的范围内的条件通过选自溅射法、蒸镀法、离子电镀法、激光烧蚀法和电弧等离子体蒸镀法的1种方法在基体上成膜,在基体上形成具备具有c轴朝向相互不同的多个方向的结晶结构的区域的透明导电膜的工序。
22.如权利要求21所述的透明导电膜的制造方法,其特征在于,通过前述选自溅射法、蒸镀法、离子电镀法、激光烧蚀法和电弧等离子体蒸镀法的1种方法成膜时,在对前述基体施加偏压的同时进行成膜。
23.如权利要求21所述的透明导电膜的制造方法,其特征在于,基于前述薄膜形成方法的成膜在使背压达到1×10-4Pa以下的真空室内进行。
24.如权利要求21所述的透明导电膜的制造方法,其特征在于,前述基体以选自玻璃、水晶、蓝宝石、Si、SiC、聚对苯二甲酸乙二醇酯(PET)、聚萘二甲酸乙二醇酯(PEN)、聚醚砜(PES)、聚酰亚胺、环烯烃类聚合物和聚碳酸酯的至少1种为主要成分。
25.如权利要求21所述的透明导电膜的制造方法,其特征在于,前述III族元素为选自Ga、Al和In的至少1种。
26.透明导电膜的制造方法,它是用于制造包含氧化锌(ZnO)和III族元素的透明导电膜的方法,其特征在于,具备使用由包含氧化锌(ZnO)和III族元素氧化物的组合物形成的烧结体靶材,以III族元素氧化物的掺杂量在22.8~40重量%的范围内的条件通过选自溅射法、蒸镀法、离子电镀法、激光烧蚀法和电弧等离子体蒸镀法的1种方法在基体上成膜,在基体上形成ZnO(002)摇摆曲线半宽度在13.5°以上的透明导电膜的工序。
27.如权利要求26所述的透明导电膜的制造方法,其特征在于,通过前述选自溅射法、蒸镀法、离子电镀法、激光烧蚀法和电弧等离子体蒸镀法的1种方法成膜时,在对前述基体施加偏压的同时进行成膜。
28.如权利要求26所述的透明导电膜的制造方法,其特征在于,基于前述薄膜形成方法的成膜在使背压达到1×10-4Pa以下的真空室内进行。
29.如权利要求26所述的透明导电膜的制造方法,其特征在于,前述基体以选自玻璃、水晶、蓝宝石、Si、SiC、聚对苯二甲酸乙二醇酯(PET)、聚萘二甲酸乙二醇酯(PEN)、聚醚砜(PES)、聚酰亚胺、环烯烃类聚合物和聚碳酸酯的至少1种为主要成分。
30.如权利要求26所述的透明导电膜的制造方法,其特征在于,前述III族元素为选自Ga、Al和In的至少1种。
31.透明导电膜的制造方法,其特征在于,在前述基体上形成SiNx薄膜后,通过权利要求13、14、17、18、21、22、23、26、27、28所述的方法介以前述SiNx薄膜于前述基体上形成前述透明导电膜。
32.如权利要求31所述的透明导电膜的制造方法,其特征在于,前述基体以选自玻璃、水晶、蓝宝石、Si、SiC、聚对苯二甲酸乙二醇酯(PET)、聚萘二甲酸乙二醇酯(PEN)、聚醚砜(PES)、聚酰亚胺、环烯烃类聚合物和聚碳酸酯的至少1种为主要成分。
33.如权利要求31或32所述的透明导电膜的制造方法,其特征在于,前述III族元素为选自Ga、Al和In的至少1种。
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JP2011171304A (ja) | 2011-09-01 |
KR100949261B1 (ko) | 2010-03-25 |
WO2007080738A1 (ja) | 2007-07-19 |
CN101180687A (zh) | 2008-05-14 |
EP1981036A1 (en) | 2008-10-15 |
US7867636B2 (en) | 2011-01-11 |
JPWO2007080738A1 (ja) | 2009-06-11 |
JP5181677B2 (ja) | 2013-04-10 |
EP1981036A4 (en) | 2014-03-12 |
KR20080011674A (ko) | 2008-02-05 |
US20080050595A1 (en) | 2008-02-28 |
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