CN103778995A - 基于二氧化硅衬底的石墨烯透明导电薄膜的制备方法 - Google Patents

基于二氧化硅衬底的石墨烯透明导电薄膜的制备方法 Download PDF

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CN103778995A
CN103778995A CN201410053173.XA CN201410053173A CN103778995A CN 103778995 A CN103778995 A CN 103778995A CN 201410053173 A CN201410053173 A CN 201410053173A CN 103778995 A CN103778995 A CN 103778995A
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石岳
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Abstract

本发明提供了一种基于二氧化硅衬底的石墨烯透明导电薄膜的制备方法，包括：在石墨烯透明导电薄膜上制备二氧化硅衬底，从而得到基于二氧化硅衬底的石墨烯透明导电薄膜。本发明实施例所述的基于二氧化硅衬底的石墨烯透明导电薄膜的制备方法，在石墨烯透明导电薄膜上制备二氧化硅衬底，避开了现有技术中的难以实现的石墨烯转移步骤，可以方便的制备基于二氧化硅衬底的石墨烯透明导电薄膜，同时可降低成本。

Description

基于二氧化硅衬底的石墨烯透明导电薄膜的制备方法
技术领域
本发明涉及石墨烯透明导电薄膜制备领域，尤其涉及一种基于二氧化硅衬底的石墨烯透明导电薄膜的制备方法。
背景技术
现有的基于二氧化硅衬底的石墨烯透明导电薄膜的制备方法是先通过CVD（Chemical Vapor Deposition,化学气相沉积）在金属衬底上制备出单层石墨烯薄膜，然后再将金属衬底上的石墨烯薄膜转移至SiO2（二氧化硅）衬底上。
现有的基于二氧化硅衬底的石墨烯透明导电薄膜的制备方法的工艺流程如下：
1、通过CVD在铜箔衬底上制备单层石墨烯薄膜；
2、转移介质涂布：通常采用旋涂法，将转移介质旋涂至所述单层石墨烯薄膜表面；
3、Cu（铜）刻蚀：将设置有单层石墨烯薄膜和转移介质的所述铜箔衬底放置在铜刻蚀液中，以将该铜箔衬底刻蚀掉：
4、石墨烯转移：将涂布有转移介质的所述单层石墨烯薄膜转移到二氧化硅衬底上（例如，将二氧化硅衬底先放置在刻蚀槽中，用“捞”的方法将将涂布有转移介质的所述单层石墨烯薄膜与二氧化硅衬底结合在一起，但这种方法不适用于大面积转移；）
5、转移介质去除：通常以丙酮将转移介质清洗去除，再烘干。
但在以上工艺流程中，石墨烯转移步骤是很难实现的，尤其是大尺寸无损石墨烯转移实现困难，并且转移费用非常高。
发明内容
本发明提供了一种基于二氧化硅衬底的石墨烯透明导电薄膜的制备方法，克服了现有的制备石墨烯透明导电薄膜的方法中石墨烯大尺寸无损转移实现困难的问题。
为了达到上述目的，本发明提供了一种基于二氧化硅衬底的石墨烯透明导电薄膜的制备方法，包括：在石墨烯透明导电薄膜上制备二氧化硅衬底，从而得到基于二氧化硅衬底的石墨烯透明导电薄膜。
实施时，本发明所述的基于二氧化硅衬底的石墨烯透明导电薄膜的制备方法具体包括：
石墨烯透明导电薄膜制备步骤：在金属衬底上制备石墨烯透明导电薄膜，以形成第一衬底；
二氧化硅衬底制备步骤：在所述石墨烯透明导电薄膜上制备二氧化硅衬底；
刻蚀步骤：刻蚀掉所述金属衬底，从而得到基于二氧化硅衬底的石墨烯透明导电薄膜。
实施时，所述二氧化硅衬底制备步骤具体包括：
二氧化硅溶胶层形成步骤：在所述石墨烯透明导电薄膜表面形成二氧化硅溶胶层；
干燥步骤：对表面形成有二氧化硅溶胶层的第一衬底进行干燥处理，以在该石墨烯透明导电薄膜上制备二氧化硅衬底。
实施时，二氧化硅溶胶层形成步骤进一步包括：将所述二氧化硅溶胶以旋涂的方式制备在石墨烯透明导电薄膜表面，以形成二氧化硅溶胶层，旋涂的旋转转速为100转/分至900转/分。
实施时，二氧化硅溶胶层形成步骤进一步包括：将所述二氧化硅溶胶以刮涂的方式制备在石墨烯透明导电薄膜表面，以形成二氧化硅溶胶层，刮涂速度为0.1厘米/秒～1厘米/秒。
实施时，二氧化硅溶胶层形成步骤进一步包括：将所述二氧化硅溶胶以浸润的方式制备在石墨烯透明导电薄膜表面，以形成二氧化硅溶胶层，浸润时间为10分钟～60分钟。
实施时，形成于石墨烯透明导电薄膜表面的二氧化硅溶胶层的厚度为1微米至30微米。
与现有技术相比，本发明实施例所述的基于二氧化硅衬底的石墨烯透明导电薄膜的制备方法，在石墨烯透明导电薄膜上制备二氧化硅衬底，避开了现有技术中的难以实现的石墨烯转移步骤，可以方便的制备基于二氧化硅衬底的石墨烯透明导电薄膜，同时可降低成本。
附图说明
图1是本发明实施例所述的基于二氧化硅衬底的石墨烯透明导电薄膜的制备方法的流程图；
图2A、图2B、图2C、图2D、图2E是本发明一具体实施例所述的二氧化硅衬底上制备石墨烯透明导电薄膜的方法的工艺流程图。
具体实施方式
以下结合具体实施例对本发明所述的基于二氧化硅衬底的石墨烯透明导电薄膜的制备方法进行介绍。
本发明实施例所述的基于二氧化硅衬底的石墨烯透明导电薄膜的制备方法，包括：在石墨烯透明导电薄膜上制备二氧化硅衬底，从而得到基于二氧化硅衬底的石墨烯透明导电薄膜。
本发明实施例所述的基于二氧化硅衬底的石墨烯透明导电薄膜的制备方法，通过在石墨烯透明导电薄膜上制备二氧化硅衬底，而并非如现有技术般需将石墨烯转移到二氧化硅衬底上，从而避开了难以实现的石墨烯转移步骤，可以方便的得到基于二氧化硅衬底的石墨烯透明导电薄膜，实现方法简单，成本低。
在具体实施时，由于石墨烯透明导电薄膜很薄，直接在石墨烯透明导电薄膜上制备二氧化硅衬底的难度比较大，因此需先将石墨烯透明导电薄膜制备于金属衬底上，再将二氧化硅衬底制备于石墨烯透明导电薄膜上，这里金属衬底起到支撑作用，之后再将金属衬底刻蚀掉，最终得到基于二氧化硅衬底的石墨烯透明导电薄膜。具体的，如图1所示，本发明实施例所述的基于二氧化硅衬底的石墨烯透明导电薄膜的制备方法可以进一步包括：
石墨烯透明导电薄膜制备步骤11：在金属衬底上制备石墨烯透明导电薄膜，以形成第一衬底；
二氧化硅衬底制备步骤12：在所述石墨烯透明导电薄膜上制备二氧化硅衬底；
刻蚀步骤13：刻蚀掉所述金属衬底，从而得到基于二氧化硅衬底的石墨烯透明导电薄膜。
根据一种具体实施方式，所述石墨烯透明导电薄膜制备步骤包括：
以碳氢化合物为碳源，以化学气象沉积法为成碳方法，在金属衬底上制备石墨烯透明导电薄膜。
根据一种具体实施方式，在金属衬底上制备石墨烯透明导电薄膜时，化学气象沉积所需温度为800℃至1200℃之间。
根据一种具体实施方式，所述二氧化硅衬底制备步骤可以包括：
二氧化硅溶胶层形成步骤：在所述石墨烯透明导电薄膜表面形成二氧化硅溶胶层；
干燥步骤：对表面形成有二氧化硅溶胶层的第一衬底进行干燥处理，以在该石墨烯透明导电薄膜上制备二氧化硅衬底。
根据一种具体实施方式，所述二氧化硅溶胶层形成步骤具体包括：
形成二氧化硅溶胶，该二氧化硅溶胶的旋转粘度大于等于8MPa.s而小于等于15MPa.s，所述二氧化硅溶胶的浓度大于等于35%而小于等于55%；
将所述二氧化硅溶胶以旋涂、浸润或刮涂的方式制备在所述石墨烯透明导电薄膜表面，从而形成二氧化硅溶胶层。
当在石墨烯透明导电薄膜上制备二氧化硅溶胶时，由于石墨烯透明导电薄膜很薄，在受到外力时容易破损，进而导致石墨烯透明导电薄膜的导电性和完整性受到影响，因此为了保证石墨烯透明导电薄膜受到最少的伤害，在实际操作时，采用如下的工艺在石墨烯透明导电薄膜上制备二氧化硅溶胶，以形成二氧化硅溶胶层：
将所述二氧化硅溶胶以旋涂的方式制备在石墨烯透明导电薄膜表面，以形成二氧化硅溶胶层：旋涂的旋转转速为100r/min（转/分）至900r/min，形成于石墨烯透明导电薄膜表面的二氧化硅溶胶层的厚度为1um（微米）至30um;
将所述二氧化硅溶胶以刮涂的方式制备在石墨烯透明导电薄膜表面，以形成二氧化硅溶胶层：刮涂速度为0.1cm/s（厘米/秒）～1cm/s，形成于石墨烯透明导电薄膜表面的二氧化硅溶胶层的厚度为1um（微米）至30um;
将所述二氧化硅溶胶以浸润的方式制备在石墨烯透明导电薄膜表面，以形成二氧化硅溶胶层，浸润时间为10min（分钟）～60min，形成于石墨烯透明导电薄膜表面的二氧化硅溶胶层的厚度为1um（微米）至30um。
根据一种具体实施方式，所述形成二氧化硅溶胶步骤包括：在20℃至40℃的温度下，将正硅酸乙酯、水、乙醇和氨水按比例混合并搅拌，形成二氧化硅溶胶，直至该二氧化硅溶胶的旋转粘度达到预定的旋转粘度；
其中，正硅酸乙酯的摩尔数大于等于0.5而小于等于2；乙醇的摩尔数为大于等于2而小于等于12，摩尔数指的是1摩尔物质中所含基本单元的个数；
正硅酸乙酯作为硅源，水和乙醇作为溶剂，氨水作为催化剂；
所述预定的旋转粘度大于等于8MPa.s（毫帕·秒）而小于等于15MPa.s。
图2A、图2B、图2C、图2D、图2E是本发明一具体实施例所述的二氧化硅衬底上制备石墨烯透明导电薄膜的方法的工艺流程图。
首先，如图2A所示，在金属衬底201上制备石墨烯透明导电薄膜202，形成第一衬底；
然后，如图2B所示，在所述石墨烯透明导电薄膜202表面上制备二氧化硅溶胶层203；
如图2C所示，将表面制备有二氧化硅溶胶层203的第一衬底进行干燥处理，在该石墨烯透明导电薄膜202上形成二氧化硅衬底204，形成第二衬底；
如图2D所示，将所述第二衬底放置入装有金属刻蚀液的容器205中；
如图2E所示，待金属刻蚀液刻蚀掉该第二衬底包括的金属衬底201，将第二衬底从该容器205中取出后进行清洗，从而得到基于二氧化硅衬底204的石墨烯透明导电薄膜202。
在该具体实施例中，所述金属衬底可以采用铜箔衬底，本发明所述的基于二氧化硅衬底的石墨烯透明导电薄膜的制备方法的流程如下：
在温度1000℃以烷烃为碳源，以化学气象沉积法（CVD）为成碳方法，再铜箔衬底上制备出石墨烯透明导电薄膜；
将浓聚SiO2溶胶以旋涂或者浸润的方式制备在石墨烯透明导电薄膜表面；
于30℃～50℃的温度条件下，将表面依次制备有石墨烯透明导电薄膜和浓聚SiO2溶胶的铜箔衬底放置于真空干燥箱中，真空干燥3小时～7小时，最终从而得到基于二氧化硅衬底的石墨烯透明导电薄膜；
并将表面依次制备有石墨烯透明导电薄膜和SiO2衬底的铜箔衬底放置于铜刻蚀液中，将铜箔进行刻蚀去除，通常情况下该铜刻蚀液为三氯化铁溶液；
将刻蚀去除铜箔之后所得的二氧化硅-石墨烯衬底于去离子水中洗涤并干燥，最终可得到基于二氧化硅衬底的石墨烯透明导电薄膜。
以上说明对本发明而言只是说明性的，而非限制性的，本领域普通技术人员理解，在不脱离所附权利要求所限定的精神和范围的情况下，可做出许多修改、变化或等效，但都将落入本发明的保护范围内。

Claims (7)

1.一种基于二氧化硅衬底的石墨烯透明导电薄膜的制备方法，其特征在于，包括：在石墨烯透明导电薄膜上制备二氧化硅衬底，从而得到基于二氧化硅衬底的石墨烯透明导电薄膜。
2.如权利要求1所述的基于二氧化硅衬底的石墨烯透明导电薄膜的制备方法，其特征在于，具体包括：
石墨烯透明导电薄膜制备步骤：在金属衬底上制备石墨烯透明导电薄膜，以形成第一衬底；
二氧化硅衬底制备步骤：在所述石墨烯透明导电薄膜上制备二氧化硅衬底；
刻蚀步骤：刻蚀掉所述金属衬底，从而得到基于二氧化硅衬底的石墨烯透明导电薄膜。
3.如权利要求2所述的基于二氧化硅衬底的石墨烯透明导电薄膜的制备方法，其特征在于，所述二氧化硅衬底制备步骤具体包括：
二氧化硅溶胶层形成步骤：在所述石墨烯透明导电薄膜表面形成二氧化硅溶胶层；
干燥步骤：对表面形成有二氧化硅溶胶层的第一衬底进行干燥处理，以在该石墨烯透明导电薄膜上制备二氧化硅衬底。
4.如权利要求2所述的基于二氧化硅衬底的石墨烯透明导电薄膜的制备方法，其特征在于，二氧化硅溶胶层形成步骤进一步包括：将所述二氧化硅溶胶以旋涂的方式制备在石墨烯透明导电薄膜表面，以形成二氧化硅溶胶层，旋涂的旋转转速为100转/分至900转/分。
5.如权利要求2所述的基于二氧化硅衬底的石墨烯透明导电薄膜的制备方法，其特征在于，二氧化硅溶胶层形成步骤进一步包括：将所述二氧化硅溶胶以刮涂的方式制备在石墨烯透明导电薄膜表面，以形成二氧化硅溶胶层，刮涂速度为0.1厘米/秒～1厘米/秒。
6.如权利要求2所述的基于二氧化硅衬底的石墨烯透明导电薄膜的制备方法，其特征在于，二氧化硅溶胶层形成步骤进一步包括：将所述二氧化硅溶胶以浸润的方式制备在石墨烯透明导电薄膜表面，以形成二氧化硅溶胶层，浸润时间为10分钟～60分钟。
7.如权利要求3至6中任一权利要求所述的基于二氧化硅衬底的石墨烯透明导电薄膜的制备方法，其特征在于，形成于石墨烯透明导电薄膜表面的二氧化硅溶胶层的厚度为1微米至30微米。
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