CN1867693B - 溅射靶材 - Google Patents

溅射靶材 Download PDF

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CN1867693B
CN1867693B CN2004800298903A CN200480029890A CN1867693B CN 1867693 B CN1867693 B CN 1867693B CN 2004800298903 A CN2004800298903 A CN 2004800298903A CN 200480029890 A CN200480029890 A CN 200480029890A CN 1867693 B CN1867693 B CN 1867693B
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长谷川浩一
石井信雄
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Ishifuku Metal Industry Co Ltd
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    • C23C14/3414—Metallurgical or chemical aspects of target preparation, e.g. casting, powder metallurgy
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Abstract

本发明提供由向Ag中添加特定少量的P使之合金化而成的Ag基合金构成的具有高反射率且耐热性优异的溅射靶材。

Description

溅射靶材
技术领域
本发明涉及维持高反射率同时提高了耐热性的薄膜形成用溅射靶材、及使用该溅射靶材形成的薄膜。
背景技术
在CD(Compact Disc)、DVD(Digital Versatile Disc)等光学记录介质上使用的反射膜、在反射型STN(Super Twist Nematic)液晶显示装置、有机EL(Electro luminescence)显示装置等中使用的光反射性导电膜，一般使用Al或Al合金。
上述光学记录介质和液晶显示装置、有机EL显示装置等用途中使用的光反射性薄膜，一般通过制作具有所要求性质的溅射靶材，使用该溅射靶材利用RF(高频)溅射法或DC(直流)溅射法等成膜而进行制造。
采用上述方法制造的由Al或Al合金构成的薄膜，具有某种程度的反射率且电阻低，而且在表层形成钝态被膜，因此在空气中也具有稳定的耐蚀性，但由Al或Al合金构成的薄膜的反射率，例如在波长为700nm的光的情况下为80％左右，对于要求高反射率的用途并不能充分满足。
为此，提出了下述方案：在要求具有高反射率的薄膜的、例如CD或DVD所代表的光盘介质上，代替Al或Al合金使用Au或Ag作为溅射靶材而形成薄膜；另外，还提出了对于反射型STN液晶显示装置，作为薄膜材料使用反射率高的Ag的方案。
CD或DVD所代表的光盘介质、反射型STN液晶显示装置等，有时在使用条件下置身于高温中，但Ag的情况下，当达到高温状态，例如200℃以上时，引起膜的凝聚等，存在反射率降低的问题。
发明内容
本发明的主要目的是，提供维持高反射率同时耐热性得到改善的Ag基合金构成的薄膜形成用的溅射靶材。
本发明人为达到上述目的而反复刻苦研讨，结果此次发现：向Ag中添加特定少量的P而使之合金化，能够得到维持Ag具有的高反射率同时耐热性格外提高的Ag基合金；向Ag中加入特定少量的P，而且还少量添加In、Sn、Zn、Au、Pt、Pd之类的金属元素而使之合金化，能够得到耐蚀性和耐热性一起提高了的Ag基合金；另外，向Ag中加入特定少量的P，而且还少量添加Cu、Ni、Fe、Bi之类的金属元素而使之合金化，Ag基合金的耐热性更进一步提高；等等，从而完成了本发明。
这样，本发明提供一种具有高反射率的薄膜形成用溅射靶材，其特征在于，由含有0.005-1.0mass％P的Ag基合金构成。
本发明还提供一种具有高反射率的薄膜形成用溅射靶材，其特征在于，由含有0.005-1.0mass％P、和0.01-2.0mass％的选自In、Sn和Zn的至少1种金属元素的Ag基合金构成。
本发明还提供一种具有高反射率的薄膜形成用溅射靶材，其特征在于，由含有0.005-1.0mass％P、和0.01-0.9mass％Au和/或0.01-5.0mass％Pd和/或0.01-0.9mass％Pt的Ag基合金构成。
本发明还提供一种具有高反射率的薄膜形成用溅射靶材，其特征在于，由含有0.005-1.0mass％P、和0.01-5.0mass％的选自Cu、Ni、Fe及Bi的至少1种金属元素的Ag基合金构成.
本发明还提供一种具有高反射率的薄膜形成用溅射靶材，其特征在于，由含有0.005-1.0mass％P、0.01-2.0mass％的选自In、Sn和Zn的至少1种金属元素、和0.01-0.9mass％Au和/或0.01-5.0mass％Pd和/或0.01-0.9mass％Pt的Ag基合金构成。
本发明还提供一种具有高反射率的薄膜形成用溅射靶材，其特征在于，由含有0.005-1.0mass％P、和0.01-2.0mass％的选自In、Sn和Zn的至少1种金属元素、及0.01-5.0mass％的选自Cu、Ni、Fe及Bi的至少1种金属元素的Ag基合金构成。
本发明还提供一种具有高反射率的薄膜形成用溅射靶材，其特征在于，由含有0.005-1.0mass％P、和0.01-0.9mass％Au和/或0.01-5.0mass％Pd和/或0.01-0.9mass％Pt、及0.01-5.0mass％的选自Cu、Ni、Fe及Bi的至少1种金属元素的Ag基合金构成。
本发明还提供一种具有高反射率的薄膜形成用溅射靶材，其特征在于，由含有0.005-1.0mass％P、和0.01-2.0mass％的选自In、Sn和Zn的至少1种金属元素、和0.01-0.9mass％Au和/或0.01-5.0mass％Pd和/或0.01-0.9mass％Pt、及0.01-5.0mass％的选自Cu、Ni、Fe及Bi的至少1种金属元素的Ag基合金构成。
下面，对本发明的薄膜形成用溅射靶材进一步详细说明。
本发明的溅射靶材，基本上由以Ag为基础、在其中添加P使之合金化而成的Ag基合金构成。P的添加量可在0.005-1.0mass％、优选为0.01-0.75mass％、进一步优选为0.05-0.5mass％的范围内。
本发明的溅射靶材，也能由三元系的Ag基合金构成，该三元系的Ag基合金，是在上述Ag-P二元系合金成分中进一步添加选自In、Sn和Zn的至少1种金属元素(以下叫做“(a)组金属元素”)使之合金化而成的。(a)组金属元素的添加量可分别在0.01-2.0mass％、优选为0.05-1.75mass％、进一步优选为0.1-1.5mass％的范围内。
本发明的溅射靶材，还能由三元系的Ag基合金构成，该三元系的Ag基合金，是在上述Ag-P二元系合金成分中进一步添加选自Au、Pd和Pt的至少1种金属元素(以下叫做“(b)组金属元素”)使之合金化而成的。(b)组金属元素的添加量，可在下述范围内：Au为0.01-0.9mass％、优选为0.05-0.85mass％、进一步优选为0.1-0.8mass％；Pd为0.01-5.0mass％、优选为0.05-3.5mass％、进一步优选为0.1-2.0mass％；而且，Pt为0.01-0.9mass％、优选为0.05-0.85mass％、进一步优选为0.1-0.8mass％。
本发明的溅射靶材，还能由三元系的Ag基合金构成，该三元系的Ag基合金，是在上述Ag-P二元系合金成分中进一步添加选自Cu、Ni、Fe和Bi的至少1种金属元素(以下叫做“(c)组金属元素”)使之合金化而成的。(c)组金属元素的添加量，可分别在0.01-5.0mass％、优选为0.05-3.5mass％、进一步优选为0.1-2.0mass％的范围内。
本发明的溅射靶材，进而也能由四元系的Ag基合金构成，该四元系的Ag基合金，是在上述Ag-P二元系合金成分中添加(a)组金属元素和(b)组金属元素这两者，使之合金化而成的。在该四元系Ag基合金中，(a)组金属元素的添加量可分别在0.01-2.0mass％、优选为0.05-1.75mass％、进一步优选为0.1-1.5mass％的范围内，(b)组金属元素的添加量，可在下述范围内：Au为0.01-0.9mass％、优选为0.05-0.85mass％、进一步优选为0.1-0.8mass％；Pd为0.01-5.0mass％、优选为0.05-3.5mass％、进一步优选为0.1-2.0mass％；而且，Pt为0.01-0.gmass％、优选为0.05-0.85mass％、进一步优选为0.1-0.8mass％。
本发明的溅射靶材，进而也能由四元系的Ag基合金构成，该四元系的Ag基合金，是在上述Ag-P二元系合金成分中添加(a)组金属元素和(c)组金属元素这两者，使之合金化而成的。在该四元系Ag基合金中，(a)组金属元素的添加量可分别在0.01-2.0mass％、优选为0.05-1.75mass％、进一步优选为0.1-1.5mass％的范围内，另外，(c)组金属元素的添加量，可分别在0.01-5.0mass％、优选为0.05-3.5mass％、进一步优选为0.1-2.0mass％的范围内。
本发明的溅射靶材，进而也能由四元系的Ag基合金构成，该四元系的Ag基合金，是在上述Ag-P二元系合金成分中添加(b)组金属元素和(c)组金属元素这两者，使之合金化而成的。在该四元系Ag基合金中，(b)组金属元素的添加量可在下述范围内：Au为0.01-0.9mass％、优选为0.05-0.85mass％、进一步优选为0.1-0.8mass％；Pd为0.01-5.0mass％、优选为0.05-3.5mass％、进一步优选为0.1-2.0mass％；而且，Pt为0.01-0.9mass％、优选为0.05-0.85mass％、进一步优选为0.1-0.8mass％，另外，(c)组金属元素的添加量，可分别在0.01-5.0mass％、优选为0.05-3.5mass％、进一步优选为0.1-2.0mass％的范围内。
本发明的溅射靶材，进而也能由五元系的Ag基合金构成，该五元系的Ag基合金，是在上述Ag-P二元系合金成分中添加(a)组金属元素和(b)组金属元素及(c)组金属元素这3组成分，使之合金化而成的。在该五元系Ag基合金中，(a)组金属元素的添加量可分别在0.01-2.0mass％、优选为0.05-1.75mass％、进一步优选为0.1-1.5mass％的范围内，(b)组金属元素的添加量可在下述范围内：Au为0.01-0.9mass％、优选为0.05-0.85mass％、进一步优选为0.1-0.8mass％；Pd为0.01-5.0mass％、优选为0.05-3.5mass％、进一步优选为0.1-2.0mass％；而且，Pt为0.01-0.9mass％、优选为0.05-0.85mass％、进一步优选为0.1-0.8mass％，另外，(c)组金属元素的添加量，可分别在0.01-5.0mass％、优选为0.05-3.5mass％、进一步优选为0.1-2.0mass％的范围内。
本发明的Ag基合金，能够按照其自身已知的方法制造，例如，通过在Ag中按上述量添加P，或者在Ag和P中分别按上述量添加(a)组金属元素，或者在Ag和P中分别按上述量添加(b)组金属元素，或者在Ag和P中分别按上述量添加(c)组金属元素，或者在Ag和P中分别按上述量添加(a)组金属元素和(b)组金属元素，或者在Ag和P中分别按上述量添加(a)组金属元素和(c)组金属元素，或者在Ag和P中分别按上述量添加(b)组金属元素和(c)组金属元素，或者在Ag和P中分别按上述量添加(a)组金属元素和(b)组金属元素及(c)组金属元素，然后在燃气炉、高频熔化炉等适当的金属熔化炉内在约1000-约1200℃的温度熔融，从而制造。作为熔化时的环境，可使用空气，或者根据需要使用惰性气体环境或真空。
所使用的主原料Ag，能够使用以粒状、板状、块状等形态市售的Ag。通常纯度为99.95％以上，优选为99.99％以上。另外，添加元素P、In、Sn、Zn、Au、Pd、Pt、Cu、Ni、Fe、Bi能够使用以粉末状、粒状、板状、块状等形态市售的物质。通常纯度为99.9％以上，优选为99.95％以上。
这样，能够得到在Ag中按上述比例含有P，或者在Ag中按上述比例含有P和(a)组金属元素，或者在Ag中按上述比例含有P和(b)组金属元素，或者在Ag中按上述比例含有P和(c)组金属元素，或者在Ag中按上述比例含有P和(a)组金属元素及(b)组金属元素，或者在Ag中按上述比例含有P和(a)组金属元素及(c)组金属元素，或者在Ag中按上述比例含有P和(b)组金属元素和(c)组金属元素，或者在Ag中按上述比例含有P和(a)组金属元素和(b)组金属元素及(c)组金属元素的二元至五元系的Ag基合金。由这些Ag基合金构成的溅射靶材，维持着Ag本来具有的高反射率，而且与以往的Ag比，耐热性提高了很多。
因此，本发明的Ag基合金构成的溅射靶材，能够有利地用作要求高反射率的CD和DVD所代表的光盘介质的反射膜用途，另外，能够有利地用作反射型STN液晶显示装置和有机EL显示装置等的光反射性薄膜用途。
另外，在CD和DVD所代表的光盘介质及反射型STN液晶显示装置或有机EL显示装置中，在使用条件下要求耐蚀性。
关于耐硫化性和针对卤元素的耐蚀性，Ag-P二元系合金为与Ag同等的程度，当在Ag-P二元系合金中添加(a)组金属元素和/或(b)组金属元素时，与Ag比，耐蚀性提高，这通过实验得到证实。
用本发明的Ag基合金构成的溅射靶材形成反射膜时，能够利用其自身已知的溅射方法，例如高频(RF)溅射法、直流(DC)溅射法、磁控管溅射法等来进行。
以下通过实施例更具体地说明本发明。
实施例1-1至1-14和比较例1-1至1-3
在Ag和P中根据情况加入In、Sn、Zn、Au、Pd、Pt、Cu、Ni、Fe和Bi之中的至少1种，在燃气炉内加热至约1200℃的温度，熔化之后，铸造加工，制作表1所示组成的溅射靶材。另外，对于表1所示组成的比较例，也同样地制作溅射靶材。
表1
为了调查耐热性，使用表1所示组成的溅射靶材，采用高频(RF)溅射法在玻璃衬底上成膜，使膜厚达到150nm，调查该膜的耐热性。
作为调查方法，测定薄膜的反射率之后，在大气中于200℃热处理1小时，再度测定反射率，利用下述计算式算出热处理前后的反射率的变化率。
变化率(％)＝100-(试验后的反射率/试验前的反射率×100)
表2示出其结果。
表2
Figure S04829890320060419D000071
由表2可知，在测定波长为700nm时，各试样都在反射率的变化率上几乎看不到差别，但测定波长为400nm的场合，比较例1-1至1-3反射率降低，与之相对，实施例1-1至1-14反射率几乎没有降低，耐热性优异。
而且，为了调查耐热性，将与上述同样制作的薄膜在大气中于250℃热处理1小时，然后与上述同样求出热处理前后的反射率的变化率。表3示出其结果。
表3
Figure S04829890320060419D000081
由表3可知，在测定波长为700nm时，各试样都在反射率的变化率上几乎看不到差别，但测定波长为400nm的场合，实施例1-1至1-14的薄膜，与比较例1-1至1-3的薄膜相比，抑制了反射率降低，耐热性非常优异。
实施例2-1至2-5和比较例2-1至2-2
在实际使用环境下，有时要求提高耐蚀性，特别是耐硫化性。于是，与上述实施例同样进行，制作下述表4所示组成的溅射靶材，调查其耐硫化性。
作为其调查方法，使用上述溅射靶材，采用高频(RF)溅射法在玻璃衬底上成膜，使膜厚达到150nm，测定薄膜的反射率之后，将该薄膜在0.01％硫化钠(Na2S)水溶液中浸渍1小时，再度测定反射率，利用下述计算式算出浸渍前后薄膜的反射率的变化率。
变化率(％)＝100-(试验后的反射率/试验前的反射率×100)
表5示出其结果。
表4
表5
Figure S04829890320060419D000092
由表5可知，添加了In、Sn、Zn等的实施例2-1至2-5的薄膜，与比较例2-1至2-2的薄膜相比，抑制了反射率降低，耐硫化性优异。
实施例3-1至3-2和比较例3-1
另外，在实际使用环境下，还有时要求提高耐氯性，因此，也进行了关于耐氯性的调查。
作为调查方法，制作表6所示组成的溅射靶材，使用该溅射靶材，采用高频(RF)溅射法在玻璃衬底上成膜，使膜厚达到150nm，测定该薄膜的反射率之后，将其在3％氯化钠(NaCl)水溶液中浸渍10分钟，再度测定反射率，利用下述计算式算出浸渍前后薄膜的反射率的变化率。
变化率(％)＝100-(试验后的反射率/试验前的反射率×100)
表7示出其结果。
表6
Figure S04829890320060419D000101
表7
Figure S04829890320060419D000102
由表7可知，添加了Au、Pd等的实施例3-1至3-2的薄膜，与比较例3-1的薄膜相比，抑制了反射率降低，耐氯性优异。

Claims (8)

1.一种具有高反射率的薄膜形成用溅射靶材，其特征在于，由含有0.005-1.0mass％P、和0.01-2.0mass％的选自In、Sn和Zn的至少1种金属元素的Ag基合金构成。
2.权利要求1所述的具有高反射率的薄膜形成用溅射靶材，其特征在于，由进一步含有0.01-0.9mass％Au和/或0.01-5.0mass％Pd和/或0.01-0.9mass％Pt的Ag基合金构成。
3.权利要求1所述的具有高反射率的薄膜形成用溅射靶材，其特征在于，由进一步含有0.01-5.0mass％的选自Cu、Ni、Fe及Bi的至少1种金属元素的Ag基合金构成。
4.权利要求1所述的具有高反射率的薄膜形成用溅射靶材，其特征在于，由进一步含有0.01-0.9mass％Au和/或0.01-5.0mass％Pd和/或0.01-0.9mass％Pt、及0.01-5.0mass％的选自Cu、Ni、Fe及Bi的至少1种金属元素的Ag基合金构成。
5.一种具有高反射率的薄膜形成用溅射靶材，其特征在于，由含有0.005-1.0mass％P、和0.01-0.9mass％Au和/或0.01-5.0mass％Pd和/或0.01-0.9mass％Pt的Ag基合金构成。
6.权利要求5所述的具有高反射率的薄膜形成用溅射靶材，其特征在于，由进一步含有0.01-5.0mass％的选自Cu、Ni、Fe及Bi的至少1种金属元素的Ag基合金构成。
7.一种具有高反射率的薄膜形成用溅射靶材，其特征在于，由含有0.005-1.0mass％P、和0.01-5.0mass％的选自Cu、Ni、Fe及Bi的至少1种金属元素的Ag基合金构成。
8.一种薄膜，由权利要求1-7中的任一项所述的Ag基合金形成。
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