CN1206201A - 透明导电组合物、由其形成的透明导电层及其制造方法 - Google Patents
透明导电组合物、由其形成的透明导电层及其制造方法 Download PDFInfo
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Abstract
本发明提供一种透明导电组合物,由其形成的透明导电层及其制造方法。组合物包含透明导电颗粒;金属醇盐[M1(OR)4];金属(M2)颗粒或它的盐(M2X);以及催化剂。其中M1、M2、R、X定义如说明书所述。因此,通过低温烧结工艺,可得到改善了导电率、透光度和硬度的透明导电层。
Description
本发明涉及透明导电组合物、由其形成的透明导电层及其制造方法，特别涉及用做家用电器的抗静电层和电磁波屏蔽层，和平板显示器的外加电源透明的电解质的组合物，由组合物形成的透明导电层及其制造方法。
透明导电层为形成在绝缘材料层的表面上的具有高的透光度的薄膜。透明导电层包括铂(Pt)或金(Au)的金属薄膜，和氧化铟锡(ITO)、氧化锡、氧化钛或氧化锑的金属氧化物薄膜。
一般来说，使用溅射法、淀积法或离子束法制成透明导电层。当计划用以上一个方法形成透明导电层时，要求使用如真空装置的昂贵设备，因此增加了制造成本。此外，由于使用以上方法的制造工艺在真空条件下进行，因此制造出的薄膜的尺寸极为有限。
要解决以上问题，已提出一种制造透明导电层的方法，包括步骤：将含透明导电颗粒的分散体涂敷在基板上形成透明导电层，然后在所得结构上形成由金属醇盐的水解产物制成的保护层。由以上方法形成的透明导电层的结构显示在图1中。
参考图1，形成在基板11上的导电层12的透明导电颗粒14没有直接地相互接触，在透明导电颗粒14之间的空间存在着空隙。这里，参考数字13代表金属醇盐的水解产物制成的保护层。
然而，制造透明导电层中使用的溶剂留在空隙中。透明导电颗粒之间的空隙增加了透明导电层的接触电阻，因而降低了该层的导电率。
为了得到具有优良导电率的透明导电层，有必要在还原气氛中进行高温(400℃或更高)烧结工艺。然而，很难对如塑料的具有很差耐热性的产品进行高温烧结工艺，该方法会毁坏涂敷设备，很难实用。
本发明的目的是提供一种用于具有优良导电率的透明导电层的组合物。
本发明的另一目的是提供一种具有优良导电率、透光度和硬度的透明导电层。
本发明的再一目的是提供一种制造透明导电层的方法。
要达到第一个目的，提供的透明导电组合物包括透明导电颗粒；金属醇盐[M1(OR)4]；金属(M2)颗粒或它的盐(M2X)；以及催化剂，
其中金属醇盐[M1(OR)4]选自由Si(OR)4、Ti(OR)4、Sn(OR)4和Zr(OR)4组成的族中的一个，其中R为C1～C4烷基，金属(M2)为选自由银(Ag)、金(Au)、铂(Pt)、铜(Cu)、镍(Ni)、铅(Pb)、钴(Co)、铑(Rh)、钌(Ru)、和锡(Sn)组成的族中的一个，X为选自由氯根、硝酸根和磺酸根组成的族中的一个。
要达到第二个目的，提供的透明导电层包括透明导电颗粒、金属醇盐[M1(OR)4]的水解产物和金属(M2)颗粒，
其中金属醇盐[M1(OR)4]选自Si(OR)4、Ti(OR)4、Sn(OR)4和Zr(OR)4，其中R为C1～C4烷基，金属(M2)至少为选自由银(Ag)、金(Au)、铂(Pt)、铜(Cu)、镍(Ni)、铅(Pb)、钴(Co)、铑(Rh)、钌(Ru)、和锡(Sn)组成的族中的一个。
要达到第三个目的，提供的制造透明导电层的方法包括：
(a)将含透明导电颗粒的第一组合物涂敷在基板上；以及
(b)在所得结构上涂敷含金属醇盐[M1(OR)4]；金属(M2)颗粒或它的盐(M2X)；以及催化剂的第二组合物，并干燥和加热所得结构，
其中金属醇盐[M1(OR)4]选自Si(OR)4、Ti(OR)4、Sn(OR)4和Zr(OR)4，其中R为C1～C4烷基，金属(M2)为选自由银(Ag)、金(Au)、铂(Pt)、铜(Cu)、镍(Ni)、铅(Pb)、钴(Co)、铑(Rh)、钌(Ru)、和锡(Sn)组成的族中的一个，X为选自由氯根、硝酸根和磺酸根组成的族中的一个。
下面结合附图详细地介绍优选实施例，本发明的这些目的和优点将变得更明显，其中：
图1为常规方法形成的透明导电层的结构图；以及
图2为本发明的透明导电层的结构图。
根据本发明，为了使金属盐(M2X)的水解反应(反应式(1))不可逆，使用如硅醇盐的金属醇盐[M1(OR)4]的溶胶-硅胶反应。其结果，金属离子(M2)含在硅酸盐的网络结构中，如下面的反应式(2)所示。
其中M2代表金属离子，X为氯根、硝酸根或磺酸根。
此外，本发明的透明导电组合物还包括能在反应方程(2)中还原金属盐(M2X)的还原剂。当将还原剂加到组合物时，反应方程(2)所代表的反应的反应速度增加。
对于还原剂，可使用NaBH4、SnCl2、二元醇或酮类。最好，1摩尔的金属醇盐中的还原剂的含量为1×10-4～8×10-2mol％。当还原剂在以上的范围内时，反应方程(2)所代表的反应的反应速度最高。
本发明的金属(M2)颗粒至少选自由银(Ag)、金(Au)、铂(Pt)、铜(Cu)、镍(Ni)、铅(Pb)、钴(Co)、铑(Rh)、钌(Ru)、和锡(Sn)组成的族中。特别是，优选抗氧化的Ag、Au和Pt。这里，优选金属(M2)颗粒的直径为5-90nm。如果金属颗粒的直径小于5nm，那么透明导电层的电阻率不够。如果金属颗粒的直径超过90nm，那么它的透光度减小。
对于本发明的金属盐(M2X)，可以使用溶于水醇或酮类的材料。特别是，优选使用包括金属(M2)的氯化物、硝酸盐或磺酸盐。
最好，金属盐(M2X)的金属(M2)与金属醇盐[M1(OR)4]的金属(M1)的摩尔比为0．01∶1～0．2∶1。如果金属M2与金属M1的摩尔比小于0．01／1，那么对透明导电层的导电率的改善效果减小。另一方面，如果摩尔比超过0．2／1，那么它的透光度急剧减小，很难实用。
本发明的催化剂促进金属醇盐的水解反应，并包括如盐酸或硝酸等酸。这里，1摩尔金属醇盐中催化剂的含量为0．01～0．04mol％。
本发明对溶剂没有严格限制。然而，一般来说，可以使用如甲醇、乙醇和丁醇等醇类溶剂、纯水或它们的混合物。
对于本发明的透明导电颗粒，可使用如氧化铟锡(ITO)、氧化锡、氧化铟、氧化钛或氧化锑钛(ATO)等金属氧化物。
下面详细地介绍使用本发明的透明导电组合物制造透明导电层的方法。
首先，直径为5～120nm的透明导电颗粒分散在溶剂中制备第一组合物。然后，将组合物涂在基板上，并干燥所得结构。这里，干燥步骤可以省略。
金属醇盐[M1(OR)4]、金属盐(M2X)、纯水和醇类溶剂混合，然后硝酸或盐酸加到混合物中制备第二组合物。这里，金属醇盐[M1(OR)4]选自Si(OR)4、Ti(OR)4、Sn(OR)4和Zr(OR)4，其中R为C1～C4烷基。
将以上制备的第二组合物涂在基板上并干燥。然后，在160～300℃，优选180～200℃加热所得结构30～60分钟，得到图2所示的透明导电层。这里，参考数字21代表基极，参考数字22代表透明导电层，参考数字23代表金属醇盐的水解产物，参考数字24代表金属(M2)颗粒，参考数字25代表透明导电颗粒。如图2所示，金属(M2)颗粒25存在于透明导电颗粒22间的空隙里。因此，得到的透明导电薄层具有优良的导电率。
下面详细介绍本发明的实施例，然而，本发明并不局限于下面介绍的实施例。
实施例1
直径约为80nm的2．5g的掺锡氧化铟颗粒分散在包括20g的甲醇、67．5g乙醇和10g丁醇的混合溶剂中，制备第一组合物。
4．5g的原硅酸四乙酯加到包括30g的甲醇、50g乙醇、12g丁醇和4g的纯水的混合溶剂中，然后将0．6g的硝酸(HNO3)和0．3g的硝酸银(AgNO3)加到混合物中。在室温下搅拌约24小时制备第二组合物。
在约90rpm旋转干净的玻璃基板的同时，将50cc的第一组合物倒在玻璃基板上，然后将玻璃基板的旋转速度增加到约150rpm。之后，和第一组合物相同的方式将60cc的第二组合物涂在所得结构上。随后对其上涂有第一和第二组合物的基板进行干燥，然后在200℃下进行1小时的烧结，完成透明导电层的制作。
实施例2
除了再将0．001g作为还原剂的NaBH4加到第二组合物中外，用与实施例1相同的方式制造透明导电层。
实施例3
除了用下面的方式制备第一组合物外，用与例1相同的方式制造透明导电层。
4．5g的原硅酸四乙酯加到包括30g的甲醇、50g乙醇、12g丁醇和4g的纯水的混合溶剂中，然后将0．6g的硝酸(HNO3)和0．2g的HAuCl4·4H2O加到混合物中。在室温下搅拌得到的混合物约30小时制备第一组合物。
实施例4
除了用下面的方式制备第二组合物外，用与例1相同的方式制造透明导电层。
4．5g的原硅酸四乙酯加到包括30g的甲醇、50g乙醇、12g丁醇和4g的纯水的混合溶剂中，然后将0．6g的硝酸(HNO3)和0．2g的HAuCl4·4H2O和0．3g的氯化锡(SnCl2·2H2O)加到混合溶剂中。在室温下搅拌得到的混合物约30小时制备第二组合物。
对比例1
除了将0．036g的硝酸银(AgNO3)加到第二组合物外，用与例1相同的方式制造透明导电层。
对比例2
除了将0．73g的硝酸银(AgNO3)加到第二组合物外，用与例1相同的方式制造透明导电层。
对比例3
除了不将硝酸银(AgNO3)加到第二组合物外，用与例1相同的方式制造透明导电层。
对比例4
除了仅将第二组合物涂在玻璃基板上外，用与例1相同的方式制造透明导电层。
测量实施例1～4和对比例1～4的透明导电层的表面电阻、透光度和铅笔硬度(pencil hardness)，结果显示在表1中。
表1
| 透明导电层 | 表面电阻(Ω/□) | 透光度(％) | 铅笔硬度(H) |
| 实施例1 | 7.5×103 | 98 | 8 |
| 实施例2 | 5.0×103 | 98 | 8 |
| 实施例3 | 4.3×103 | 98 | 8 |
| 实施例4 | 1.1×103 | 98 | 8 |
| 对比例1 | 1.2×105 | 98 | 8 |
| 对比例2 | 6.0×103 | 87 | 5 |
| 对比例3 | 1.3×105 | 98 | 8 |
| 对比例4 | 1.2×1012 | 99 | 9 |
从表1中可看出，实施例1-4制造的透明导电层的表面电阻大大地低于对比例1-4的表面电阻，并且与对比例1-4相比，例1-4制造的透明导电层的透光度和铅笔硬度也很优良。
另一方面，在对比例1的透明导电层中，层的透光度和铅笔硬度很优良，而在改善导电率时效果轻微。此外，对比例2的透明导电层的导电率很优良，而它的透光度和铅笔硬度很差。此外，在没有加入硝酸银的对比例3和4中，透明导电层的透光度和铅笔硬度很优良，而它的表面电阻很差。
本发明提供以下效果。首先，与现有技术的透明导电层相比，透明导电层的导电率、透光度和硬度得到改善。第二，根据本发明的制造透明导电层的方法不要求高温烧结工艺和附加的真空设备，所以降低了制造成本。第三，可通过低温烧结工艺制造透明导电层，所以本发明的制造方法可以适用于不具有良好的耐热性的基板。
Claims (24)
1．一种透明导电组合物，包括透明导电颗粒；金属醇盐[M1(OR)4]；金属(M2)颗粒或它的盐(M2X)；以及催化剂，
其中金属醇盐[M1(OR)4]选自Si(OR)4、Ti(OR)4、Sn(OR)4和Zr(OR)4，其中R为C1～C4烷基，金属(M2)为选自由银(Ag)、金(Au)、铂(Pt)、铜(Cu)、镍(Ni)、铅(Pb)、钴(Co)、铑(Rh)、钌(Ru)、和锡(Sn)组成的族中的一个，X为选自由氯根、硝酸根和磺酸根组成的族中的一个。
2．根据权利要求1的组合物，还包括还原剂。
3．根据权利要求2的组合物，其中还原剂选自由NaBH4、SnCl2、二元醇和酮类组成的族中的一个。
4．根据权利要求2的组合物，其中1摩尔的金属醇盐中的还原剂的含量为1×10-4～8×10-2mol％。
5．根据权利要求1的组合物，其中透明导电颗粒的直径为5-120nm。
6．根据权利要求1的组合物，其中金属(M2)与金属(M1)的摩尔比为0．01∶1～0．2∶1。
7．根据权利要求1的组合物，其中金属(M2)颗粒的直径为5-90nm。
8．根据权利要求1的组合物，其中催化剂选自由盐酸和硝酸组成的族中的酸。
9．根据权利要求1的组合物，其中1摩尔金属醇盐中催化剂的含量为0．01～0．04mol％。
10．一种透明导电层，包括透明导电颗粒、金属醇盐[M1(OR)4]的水解产物和金属(M2)颗粒，
其中金属醇盐[M1(OR)4]选自Si(OR)4、Ti(OR)4、Sn(OR)4和Zr(OR)4，其中R为C1～C4烷基，金属(M2)至少为选自由银(Ag)、金(Au)、铂(Pt)、铜(Cu)、镍(Ni)、铅(Pb)、钴(Co)、铑(Rh)、钌(Ru)、和锡(Sn)组成的族中的一个。
11．根据权利要求10的透明导电层，其中透明导电颗粒的直径为5-120nm。
12．根据权利要求10的透明导电层，其中金属(M2)与金属(M1)的摩尔比为0．01∶1～0．2∶1。
13．根据权利要求10的透明导电层，其中金属(M2)颗粒的直径为5-90nm。
14．一种制造透明导电层的方法，包括：
(a)将含透明导电颗粒的第一组合物涂敷在基板上；以及
(b)在所得结构上涂敷含金属醇盐、金属(M2)颗粒或它的盐(M2X)、以及催化剂的第二组合物，并干燥和加热所得结构，
其中金属醇盐[M1(OR)4]选自Si(OR)4、Ti(OR)4、Sn(OR)4和Zr(OR)4，其中R为C1～C4烷基，金属(M2)至少为选自由银(Ag)、金(Au)、铂(Pt)、铜(Cu)、镍(Ni)、铅(Pb)、钴(Co)、铑(Rh)、钌(Ru)、和锡(Sn)组成的族中的一个，X为选自由氯根、硝酸根和磺酸根组成的族中的一个。
15．根据权利要求14的方法，其中第二组合物还包括还原剂。
16．根据权利要求15的方法，其中还原剂选自由NaBH4、SnCl2、二元醇和酮类组成的族中的一个。
17．根据权利要求15的方法，其中1摩尔的金属醇盐中还原剂的含量为1×10-4～8×10-2mol％。
18．根据权利要求10或11的方法，其中步骤(b)的加热在160-300℃下进行。
19．根据权利要求14的方法，其中透明导电颗粒的直径为5-120nm。
20．根据权利要求14的方法，其中金属(M2)与金属(M1)的摩尔比为0．01∶1～0．2∶1。
21．根据权利要求14的方法，其中金属(M2)颗粒的直径为5-90nm。
22．根据权利要求14的方法，其中干燥工艺在步骤(b)之前进行。
23．根据权利要求14的方法，其中催化剂选自由盐酸和硝酸组成的族中的酸。
24．根据权利要求14的方法，其中1摩尔金属醇盐中催化剂的含量为0．01～0．04mol％。
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| DE102007013181B4 (de) | 2007-03-20 | 2017-11-09 | Evonik Degussa Gmbh | Transparente, elektrisch leitfähige Schicht |
| JP4477052B2 (ja) * | 2007-10-03 | 2010-06-09 | 株式会社東芝 | 金属ナノ粒子無機複合体の製造方法および金属ナノ粒子無機複合体 |
| EP3457813A1 (en) * | 2008-04-22 | 2019-03-20 | Datec Coating Corporation | Thick film high temperature thermoplastic insulated heating element |
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| JP4477083B2 (ja) * | 2008-09-24 | 2010-06-09 | 株式会社東芝 | 金属ナノ粒子無機複合体の製造方法、金属ナノ粒子無機複合体およびプラズモン導波路 |
| US8834957B2 (en) | 2008-11-05 | 2014-09-16 | Lg Chem, Ltd. | Preparation method for an electroconductive patterned copper layer |
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| EP2206801A1 (en) * | 2008-12-24 | 2010-07-14 | Seb Sa | Composite cookware comprising a vitreous protective coating |
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| WO1989003114A1 (en) * | 1987-09-30 | 1989-04-06 | Catalysts & Chemicals Industries Co., Ltd. | Transparent conductive ceramic-coated base, process for its production, and its use |
| US4945282A (en) | 1987-12-10 | 1990-07-31 | Hitachi, Ltd. | Image display panel having antistatic film with transparent and electroconductive properties and process for processing same |
| EP0423337B1 (en) * | 1988-08-24 | 1995-06-07 | CATALYSTS & CHEMICALS INDUSTRIES CO., LTD. | Coating fluid for forming transparent conductive ceramic coating, base material coated with transparent conductive ceramic and production thereof, and application of base material coated with transparent conductive ceramic |
| US4954282A (en) * | 1989-04-19 | 1990-09-04 | Lever Brothers Company | Acyl isethionate skin cleansing compositions |
| DE69130921T2 (de) * | 1990-11-21 | 1999-06-24 | Catalysts & Chem Ind Co | Überzugslösung zur bildung eines durchsichtigen, leitfähigen films, verfahren zu deren herstellung, leitfähiges substrat, verfahren zur dessen herstellung, und anzeigevorrichtung mit einem durchsichtigen, leitfähigen substrat |
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| JP3517890B2 (ja) * | 1993-02-18 | 2004-04-12 | 日産化学工業株式会社 | 液晶表示素子用絶縁膜形成用塗布液 |
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-
1996
- 1996-12-10 KR KR1019960064007A patent/KR100234170B1/ko not_active IP Right Cessation
-
1997
- 1997-12-09 DE DE19754664A patent/DE19754664C2/de not_active Expired - Fee Related
- 1997-12-09 BR BR9706620A patent/BR9706620A/pt not_active Application Discontinuation
- 1997-12-09 US US08/987,323 patent/US5993973A/en not_active Expired - Fee Related
- 1997-12-10 JP JP09340211A patent/JP3100569B2/ja not_active Expired - Fee Related
- 1997-12-10 CN CN97108398A patent/CN1096684C/zh not_active Expired - Fee Related
-
1999
- 1999-07-29 US US09/362,739 patent/US6335056B1/en not_active Expired - Fee Related
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103310875A (zh) * | 2012-03-15 | 2013-09-18 | 南美特科技股份有限公司 | 透明电极及其制作方法 |
| CN105358640A (zh) * | 2013-07-29 | 2016-02-24 | 富士胶片株式会社 | 导电膜形成用组合物和导电膜的制造方法 |
Also Published As
| Publication number | Publication date |
|---|---|
| BR9706620A (pt) | 1999-05-04 |
| US5993973A (en) | 1999-11-30 |
| US6335056B1 (en) | 2002-01-01 |
| KR19980045796A (ko) | 1998-09-15 |
| DE19754664C2 (de) | 2001-10-04 |
| MX9709935A (es) | 1998-07-31 |
| CN1096684C (zh) | 2002-12-18 |
| JP3100569B2 (ja) | 2000-10-16 |
| JPH10261326A (ja) | 1998-09-29 |
| KR100234170B1 (ko) | 2000-01-15 |
| DE19754664A1 (de) | 1998-09-03 |
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