CN103745829B - 石墨烯复合电极材料的制备方法 - Google Patents

石墨烯复合电极材料的制备方法 Download PDF

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CN103745829B
CN103745829B CN201310746256.2A CN201310746256A CN103745829B CN 103745829 B CN103745829 B CN 103745829B CN 201310746256 A CN201310746256 A CN 201310746256A CN 103745829 B CN103745829 B CN 103745829B
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王烨文
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TCL China Star Optoelectronics Technology Co Ltd
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Shenzhen China Star Optoelectronics Technology Co Ltd
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Abstract

本发明提供一种石墨烯复合电极材料的制备方法，包括以下步骤：步骤1、提供玻璃基板，该玻璃基板的熔点大于1100℃；步骤2、清洗玻璃基板后，在玻璃基板上形成金属薄膜；步骤3、图案化该金属薄膜，以形成电路图形；步骤4、在电路图形上形成石墨烯薄膜，以制得石墨烯复合电极材料。本发明的石墨烯复合电极材料的制备方法，通过耐高温玻璃基板与金属催化剂，在电路图形表面直接生长石墨烯薄膜，不需转移，不会受转移中溶剂影响，成膜质量较高且无需蚀刻，直接形成石墨烯复合电极材料，制程简单，且，由于石墨烯化学性质很稳定，可以起到保护金属电路图形的作用，进而有效延长石墨烯复合电极材料的使用寿命。

Description

石墨烯复合电极材料的制备方法
技术领域
本发明涉及一种复合电极材料的制备方法，尤其涉及一种石墨烯复合电极材料的制备方法。
背景技术
石墨烯（graphene）是一种单层碳原子紧密堆积成二维蜂窝状结构的碳质新材料，石墨烯目前是世上最薄却也是最坚硬的纳米材料，它几乎是完全透明的，只吸收2.3%的光，而电阻率只约10-6Ω·cm，比铜或银更低，为目前世上电阻率最小的材料，其可以通过化学气相沉积（Chemical Vapor Deposition，CVD）法、微机械分离法、取向附生法等方法制备。
石墨烯具有很大的比表面积、高导电性及很高的机械强度，基于石墨烯的这些性质，石墨烯被广泛的运用于合成纳米复合材料，制造电学元件，以及其他一些化学生物传感器等。尽管石墨烯具有十分卓越的性能以及诱人的应用前景，但是目前制约石墨烯发展的很多因素也依然存在，如，高纯度的单层石墨烯很难大规模生产，化学氧化法得到的氧化石墨烯再还原制取的还原氧化石墨烯因难以控制其被还原的程度以及不能避免氧化石墨在化学还原的过程中再次被石墨化等因素均将石墨烯本来所具有的优越性能大打折扣，同样化学气相沉积法中得到的石墨烯依然存在石墨烯被石墨化的过程。因此，怎样得到高比表面，还原程度较高的石墨烯是石墨烯发挥其高性能的关键。基于上述问题，石墨烯作为电极材料应用于显示领域，会产生石墨烯的优越性能受限等问题。
发明内容
本发明的目的在于提供一种石墨烯复合电极材料的制备方法，其制程简单，制得的复合电极材料的使用寿命长。
为实现上述目的，本发明提供一种石墨烯复合电极材料的制备方法，包括以下步骤：
步骤1、提供玻璃基板，该玻璃基板的熔点大于1100℃；
步骤2、清洗玻璃基板后，在玻璃基板上形成金属薄膜；
步骤3、图案化该金属薄膜，以形成电路图形；
步骤4、在电路图形上形成石墨烯薄膜，以制得石墨烯复合电极材料。
所述玻璃基板为氧化钇基、氧化铝基或二氧化硅基玻璃基板。
所述玻璃基板中碱金属总量小于0.3ppm，锆含量小于或等于0.3ppm，钛含量小于或等于1.4ppm，钙含量小于或等于0.6ppm，镁含量小于0.1ppm，硼含量小于0.1ppm，铜含量小于0.01ppm，磷含量小于0.2ppm。
所述玻璃基板中锂含量小于或等于0.001ppm，钾含量小于0.2ppm，钠含量小于或等于0.1ppm。
所述金属薄膜以金属镍、铜或钌为靶材，通过物理气相沉积工艺溅镀形成于玻璃基板上。
所述靶材纯度大于99.9%。
所述金属薄膜厚度10nm-500nm。
所述步骤3包括：在金属薄膜上涂布正光阻，经曝光与显影后，采用铜酸蚀刻出预定的图形，进而形成电路图形。
所述步骤4包括：提供一掩模板，将该掩模板贴附于玻璃基板的形成有电路图形侧，并露出电路图形，然后在电路图形上形成石墨烯薄膜。
所述掩模板由二氧化硅制成；所述石墨烯薄膜通过化学气相沉积工艺形成于电路图形上。
本发明的有益效果：本发明的石墨烯复合电极材料的制备方法，通过耐高温玻璃基板与金属催化剂，在电路图形表面直接生长石墨烯薄膜，不需转移，不会受转移中溶剂影响，成膜质量较高且无需蚀刻，直接形成石墨烯复合电极材料，制程简单，且，由于石墨烯化学性质很稳定，可以起到保护金属电路图形的作用，进而有效延长石墨烯复合电极材料的使用寿命。
为了能更进一步了解本发明的特征以及技术内容，请参阅以下有关本发明的详细说明与附图，然而附图仅提供参考与说明用，并非用来对本发明加以限制。
附图说明
下面结合附图，通过对本发明的具体实施方式详细描述，将使本发明的技术方案及其它有益效果显而易见。
附图中，
图1为本发明石墨烯复合电极材料的制备方法的流程图。
具体实施方式
为更进一步阐述本发明所采取的技术手段及其效果，以下结合本发明的优选实施例及其附图进行详细描述。
请参阅图1，本发明提供一种石墨烯复合电极材料的制备方法，包括以下步骤：
步骤1、提供玻璃基板，该玻璃基板的熔点大于1100℃。
所述玻璃基板选用耐高温玻璃基板，优选熔点大于1100℃的玻璃基板，且该玻璃基板中碱金属（锂、钾、钠）总量小于0.3ppm，锆含量小于或等于0.3ppm，钛含量小于或等于1.4ppm，钙含量小于或等于0.6ppm，镁含量小于0.1ppm，硼含量小于0.1ppm，铜含量小于0.01ppm，磷含量小于0.2ppm，优选的，所述玻璃基板中锂含量小于或等于0.001ppm，钾含量小于0.2ppm，钠含量小于或等于0.1ppm。
在本实施例中，所述玻璃基板为氧化钇基、氧化铝基或二氧化硅基玻璃基板。
步骤2、清洗玻璃基板后，在玻璃基板上形成金属薄膜。
所述金属薄膜以金属镍（Ni）、铜（Cu）或钌（Ru）为靶材，通过物理气相沉积（Physical Vapor Deposition，PVD）工艺溅镀形成于玻璃基板上。所述靶材纯度大于99.9%。所述金属薄膜厚度10nm-500nm。
步骤3、图案化该金属薄膜，以形成电路图形。
具体地，在金属薄膜上涂布正光阻，经曝光与显影后，采用铜酸蚀刻出预定的图形，进而形成电路图形。
步骤4、在电路图形上形成石墨烯薄膜，以制得石墨烯复合电极材料。
具体地，提供一掩模板，将该掩模板贴附于玻璃基板的形成有电路图形侧，并露出电路图形，然后在电路图形上形成石墨烯薄膜。
在本实施例中，所述掩模板由二氧化硅制成，其形变点为1075℃，退火点为1180℃，硬化点为1730℃，最高延续使用温度1100℃，短时间内可在1450℃下运用。因该掩模板耐高温，热膨胀率小，在1000℃左右形变量小，可以有效保证石墨烯薄膜形成的精度。
所述石墨烯薄膜通过化学气相沉积（Chemical Vapor Deposition，CVD）工艺形成于电路图形上。具体地，化学气相沉积工艺中采用CH4与H2/Ar或CH4与H2混合气体，在600-1050℃、40Pa-5kPa的环境下，并可根据沉积时间不同可以得到厚度为0.35nm-50nm，面电阻在0.1-500Ω/□的石墨烯薄膜。
综上所述，本发明的石墨烯复合电极材料的制备方法，通过耐高温玻璃基板与金属催化剂，在电路图形表面直接生长石墨烯薄膜，不需转移，不会受转移中溶剂影响，成膜质量较高且无需蚀刻，直接形成石墨烯复合电极材料，制程简单，且，由于石墨烯化学性质很稳定，可以起到保护金属电路图形的作用，进而有效延长石墨烯复合电极材料的使用寿命。
以上所述，对于本领域的普通技术人员来说，可以根据本发明的技术方案和技术构思作出其他各种相应的改变和变形，而所有这些改变和变形都应属于本发明权利要求的保护范围。

Claims (8)

1.一种石墨烯复合电极材料的制备方法，其特征在于，包括以下步骤：
步骤1、提供玻璃基板，该玻璃基板的熔点大于1100℃；
步骤2、清洗玻璃基板后，在玻璃基板上形成金属薄膜；
步骤3、图案化该金属薄膜，以形成电路图形；
步骤4、在电路图形上形成石墨烯薄膜，以制得石墨烯复合电极材料；
所述步骤4包括：提供一掩模板，将该掩模板贴附于玻璃基板的形成有电路图形侧，并露出电路图形，然后在电路图形上形成石墨烯薄膜；
所述掩模板由二氧化硅制成；所述石墨烯薄膜通过化学气相沉积工艺形成于电路图形上。
2.如权利要求1所述的石墨烯复合电极材料的制备方法，其特征在于，所述玻璃基板为氧化钇基、氧化铝基或二氧化硅基玻璃基板。
3.如权利要求2所述的石墨烯复合电极材料的制备方法，其特征在于，所述玻璃基板中碱金属总量小于0.3ppm，锆含量小于或等于0.3ppm，钛含量小于或等于1.4ppm，钙含量小于或等于0.6ppm，镁含量小于0.1ppm，硼含量小于0.1ppm，铜含量小于0.01ppm，磷含量小于0.2ppm。
4.如权利要求3所述的石墨烯复合电极材料的制备方法，其特征在于，所述玻璃基板中锂含量小于或等于0.001ppm，钾含量小于0.2ppm，钠含量小于或等于0.1ppm。
5.如权利要求1所述的石墨烯复合电极材料的制备方法，其特征在于，所述金属薄膜以金属镍、铜或钌为靶材，通过物理气相沉积工艺溅镀形成于玻璃基板上。
6.如权利要求5所述的石墨烯复合电极材料的制备方法，其特征在于，所述靶材纯度大于99.9％。
7.如权利要求1所述的石墨烯复合电极材料的制备方法，其特征在于，所述金属薄膜厚度10nm-500nm。
8.如权利要求1所述的石墨烯复合电极材料的制备方法，其特征在于，所述步骤3包括：在金属薄膜上涂布正光阻，经曝光与显影后，采用铜酸蚀刻出预定的图形，进而形成电路图形。
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