CN111188021A - 一种石墨烯生长基底的预处理方法 - Google Patents
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Abstract
本发明公开了一种石墨烯生长基底的预处理方法，该方法以铜箔或铜镍合金箔作为基底，对其进行初步抛光，再将其置于管式炉内进行退火，退火后的基底从炉内取出，再次对其进行抛光，再将其置于加热台上加热氧化，即可完成预处理，预处理后的基底可用于石墨烯的化学气相沉积生长。该预处理方法可以降低铜或铜镍合金基底的粗糙度，提高基底纯度，降低基底表面的活性位点，最终达到降低石墨烯成核密度的效果，从而实现大单晶石墨烯以及大面积2‑5层范围内均匀厚度的少层石墨烯的制备。
Description
技术领域
本发明属于石墨烯制备技术领域，具体涉及一种石墨烯生长基底的预处理方法。
背景技术
二维材料石墨烯由于具有独特的光学、电学、机械性能等，在电子器件、光电子器件、储能器件、化学生物传感器等应用领域都发挥着巨大的作用。
化学气相沉积技术由于其具有的薄膜成份容易控制、重复性好、操作维护方便等优点被广泛应用于石墨烯的制备，但是化学气相沉积法制备的石墨烯薄膜往往表现为具有高密度晶界的多晶膜，其优异的物理性能在晶界上存在一定程度的降低，因此，降低石墨烯生长的成核密度，获得石墨烯大单晶及大面积的2-5层均匀厚度石墨烯薄膜非常有必要。
发明内容
针对上述现有技术的不足，本发明提供一种石墨烯生长基底的预处理方法，用以降低铜或铜镍合金基底上石墨烯成核密度的方法，实现石墨烯大单晶及大面积的2-5层均匀厚度石墨烯薄膜的制备。
为了实现上述发明目的，本发明采用以下技术手段：
先对铜箔或铜镍合金箔基底进行第一次电化学抛光，初步降低基底表面的粗糙度，再将其置于管式炉内进行退火，使基底内部的杂质析出到基底表面，退火后的铜基底从炉内取出后对其进行第二次电化学抛光，将基底表面的杂质除去，再将其置于加热台上加热氧化。最后将处理好的基底用于进行石墨烯的化学气相沉积生长。
进一步地，所述预处理中第一次电化学抛光和第二次电化学抛光的处理条件为：电压3-10V、抛光时间20-180秒；抛光液的成分包括磷酸、乙醇、异丙醇、去离子水、尿素。
进一步地，所述预处理中退火的条件为：退火时间0.5-12小时、退火温度1000℃-1050℃，退火气氛为氢气和氩气。
进一步地，所述预处理中加热氧化的条件为：加热温度100-180℃、加热时间1-30分钟。
进一步地，所述化学气相沉积的生长条件为：生长温度为1000℃-1050℃，生长时间为10-30分钟，采用流量为0.1-100sccm的甲烷作为碳源，采用流量为1-500sccm的氩气和流量为0.1-200sccm的氢气作为辅助气体。
有益效果：本发明提供了的石墨烯生长基底预处理方法，可以有效降低石墨烯成核密度，有利于石墨烯大单晶及大面积的2-5层均匀厚度石墨烯薄膜的制备。初次电化学抛光可降低基底的表面粗糙度，退火可以使基底内的杂质析出，再次抛光可去除基底表面杂质并降低基底粗糙度，加热氧化可降低基底表面的活性位点。
附图说明
图1为实施例1中未处理基底和处理后基底的原子力显微镜测试结果，(a)为未处理基底的原子力显微镜测试结果，(b)为处理后基底的原子力显微镜测试结果。
图2为实施例1中未处理基底和处理后基底上石墨烯生长的光学显微镜图像对比，(a)为未处理基底上石墨烯的生长情况，(b)为处理后基底上石墨烯的生长情况。
图3为实施例1中处理后基底上生长的石墨烯的扫描电子显微镜图像，(a)为处理后基底上生长的大单晶石墨烯，(b)为处理后基底上生长的大面积双层、三层石墨烯。
具体实施方式
以下实施例进一步说明本发明的内容，但不应理解为对本发明的限制。在不背离本发明精神和实质的情况下，对本发明方法、步骤或条件所作的修改或替换，均属于本发明的范围。实施例中未注明具体条件的实验方法及未说明配方的试剂均为按照本领域常规条件。
下面结合附图，对本发明提供的单晶石墨烯的制备方法的具体实施方式进行详细的说明。
实施例1
本发明提供了一种石墨烯生长基底的预处理方法，以铜箔为研究对象，对其进行初步抛光，再将其置于管式炉内进行退火，退火后的基底从炉内取出，再次对其进行抛光，再将其置于加热台上加热氧化，最后进行石墨烯的化学气相沉积生长。
首先对铜基底进行第一次电化学抛光，初步降低基底表面的粗糙度，电化学抛光的电压为10V，抛光时间为20-180秒，抛光液的成分为：磷酸100mL、乙醇100mL、异丙醇20mL、去离子水200mL、尿素2g。
将抛光后的铜基底置于管式炉内进行退火，使铜基底内部的杂质析出到基底表面，退火时间为0.5-12个小时，退火温度为1000℃-1050℃，退火气氛为氢气和氩气，氢气流量为0.1-200sccm，氩气的流量为1-500sccm。
将退火后的铜基底进行第二次电化学抛光，以去除析出在铜基底表面的杂质，同时提高基底表面的平整度，电化学抛光的条件同第一次电化学抛光。
将抛光后的铜基底置于加热台上，在空气环境中进行加热氧化，来减少铜基底表面的活性位点，加热温度为100-180℃，加热时间为1-30分钟。
全部处理结束后，将铜基底置于管式炉中进行石墨烯的化学气相沉积生长。
为了防止加热氧化的效果被减弱，在生长过程中的升温和退火中仅使用氩气气氛，氩气的流量为1-500sccm。
当石墨烯生长开始时，同时通入辅助气氛氢气和碳源甲烷，氢气流量为0.1-200sccm，甲烷流量为0.1-100sccm。
生长温度为1000℃-1050℃，生长时间为0.1-12小时。
图1为原子力显微镜的测试结果，未进行处理的基底(a)表面起伏很大，非常粗糙，而处理后的基底(b)表面更为平整，衬底的预处理有降低基底表面粗糙度的作用。
图2为未处理基底与处理后基底上生长的石墨烯光学显微镜图像，未进行处理的基底(a)上石墨烯成核密度很大，晶体尺寸很小，而处理后的基底(b)上石墨烯单晶分布比较稀疏，晶体尺寸较大。
在处理后的衬底上生长石墨烯，生长时间延长可以使石墨烯晶粒的尺寸增大。
在形核密度较低的前提下，合理调控生长温度、辅助气体与碳源的流量比例等条件也可以帮助增大石墨烯晶粒的尺寸。
图3是使用本发明提出的基底预处理方法，并合理调控石墨烯生长的实验参数后，制备出的大单晶石墨烯(a)和大面积双层、三层石墨烯等(b)。
Claims (5)
1.一种石墨烯生长基底的预处理方法，其特征在于：以铜箔或铜镍合金箔作为基底，首先对基底进行第一次抛光，再将其置于管式炉内进行退火，退火后的基底从管式炉内取出，对其进行第二次抛光，再将其置于加热台上加热氧化，即可完成预处理，预处理后的基底可用于进行石墨烯的化学气相沉积生长。
2.根据权利要求1所述的预处理方法，其特征在于：所述第一次电化学抛光和第二次电化学抛光的处理条件为：电压3-10V、抛光时间20-180秒；抛光液的成分包括磷酸、乙醇、异丙醇、去离子水、尿素。
3.根据权利要求1所述的预处理方法，其特征在于：所述退火的条件为：退火时间0.5-12小时、退火温度1000℃-1050℃，退火气氛为氢气和氩气。
4.根据权利要求1所述的预处理方法，其特征在于：所述加热氧化的条件为：加热温度100-180℃、加热时间1-30分钟。
5.根据权利要求1所述的预处理方法，其特征在于：所述化学气相沉积生长的条件为：生长温度为1000℃-1050℃，生长时间为10-30分钟，采用流量为0.1-100sccm的甲烷作为碳源，采用流量为1-500sccm的氩气，以流量为0.1-200sccm的氢气作为辅助气体。
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