CN114084883B - 一种湿法浸泡和低温退火复合提高石墨烯性能的方法 - Google Patents
一种湿法浸泡和低温退火复合提高石墨烯性能的方法 Download PDFInfo
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Abstract
本发明一种湿法浸泡和低温退火复合提高石墨烯性能的方法,由以下步骤组成:将刻蚀掉生长基底的PMMA/石墨烯薄膜浸泡在甲酰胺溶液中,以增强石墨烯薄膜的亲水性;用目标衬底捞起PMMA/石墨烯,形成PMMA/石墨烯/目标衬底三明治结构;将PMMA/石墨烯/目标衬底浸泡在丙酮溶液中除去PMMA;采用低压低温气氛退火去除转移过程中石墨烯上残留的PMMA光刻胶,工艺中H2作为还原性气体,可与PMMA中的碳原子在高温下反应形成相应的碳氢化合物气体脱离石墨烯表面。该方法包含的两种处理工艺相辅相成、互不影响,既可较好的避免石墨烯表面褶皱的形成,又可高效去除石墨烯表面附着的PMMA残留物,获得完美性能的石墨烯薄膜,以实现石墨烯材料在微电子元器件及传感器中的广泛应用。
Description
技术领域
本发明属于半导体制备技术领域,更具体地,涉及一种湿法浸泡和低温退火复合提高石墨烯性能的方法。
背景技术
石墨烯是由单层碳原子蜂窝状排列构成的二维晶体,具有高导电率、迁移率、透光性及其他诸多优异性能。
CVD法作为当今制备石墨烯的主流方法,它不受衬底尺寸的限制,设备简单,可以大批量生产。石墨烯-PMMA自支撑技术是CVD法中石墨烯衬底转移的关键技术,能较稳定高效的完成石墨烯的衬底转移,且能基本保持其优良的性能。但是,石墨烯表面的疏水特性,使其不能与目标衬底完美贴合,在后续烘干处理时会有褶皱的形成,而褶皱的存在将吸附空气中的H2O、O2分子,进而降低石墨烯的电学性能;且PMMA湿法转移的石墨烯上会有光刻胶的残留,这些残胶将导致石墨烯产生显著的p型掺杂和引入大量的散射中心,而大大降低石墨烯的载流子迁移率。
甲酰胺湿法浸泡可提高石墨烯表面的亲水性,增强石墨烯与目标衬底的贴合性,以在后续烘干过程中,降低石墨烯表面褶皱的形成;而转移后的低温低压退火工艺中H2作为还原性气体,可与PMMA中的碳原子在高温下反应形成相应的碳氢化合物气体脱离石墨烯表面。此复合方法优化制备的石墨烯薄膜,实现了石墨烯材料在微电子元器件及传感器中的广泛应用。
发明内容
本发明的目的在于在传统石墨烯转移技术的基础上,提供一种湿法浸泡和低温退火复合提高石墨烯性能的方法,改善石墨烯与目标基底的结合状况,且消除残胶引起的石墨烯性能的退化,进而提高石墨烯薄膜的电学性能。
本发明的技术方案:
1.将刻蚀掉生长基底的PMMA/石墨烯薄膜浸泡在甲酰胺溶液中,以增强石墨烯薄膜的亲水性;
2.用目标衬底捞起PMMA/石墨烯,形成PMMA/石墨烯/目标衬底三明治结构,且在适宜的温度下处理,以除去水分;
3.将PMMA/石墨烯/目标衬底浸泡在丙酮溶液中除去PMMA;
4.采用低压低温气氛退火去除转移过程中石墨烯上残留的PMMA光刻胶。
优选的,所述的PMMA/石墨烯薄膜浸泡在甲酰胺溶液中5-30min,提高石墨烯表面的亲水性,增强后续石墨烯与目标衬底的贴合度。
优选的,所述的用目标衬底捞起PMMA/石墨烯,形成PMMA/石墨烯/目标衬底三明治结构,且在50-150℃温度下处理10-30min,以除去水分。
优选的,所述的PMMA/石墨烯/目标衬底浸泡在丙酮溶液中5-30min除去PMMA。
优选的,所述的低温低压退火包括以下步骤:
(1)将去除PMMA的石墨烯/目标衬底放入真空气氛管式炉;
(2)管式炉抽真空至0.1-1Pa,通入高纯惰性气体,赶走腔室内的空气;
(3)关闭惰性气体流量,待真空重新恢复至0.1-1Pa,通入高纯H2;
(4)设定加热程序,将目标基底缓慢加热,保持真空泵的抽速和步骤(3)中的H2流量不变;
(5)关闭加热程序,系统温度缓慢降至室温,关闭气体流量,关闭真空泵。
优选的,所述的管式炉抽真空至0.1-1Pa,通入高纯惰性气体,所述高纯惰性气体为Ar、N2、He,流量50-500sccm,时间5-20min,以赶走腔室内的空气。
优选的,所述的关闭惰性气体流量,待真空重新恢复至0.1-1Pa,通入高纯H2,流量5-100sccm,时间5-20min。
优选的,所述的设定加热程序,将目标衬底缓慢加热至100-500℃,加热速率1-5℃/min,保持真空泵的抽速和步骤(3)中的H2流量不变,时间10-120min。
总体而言,通过本发明所构思的技术方案具有以下优点:
1.使用甲酰胺湿法浸泡PMMA/石墨烯,再转移至目标衬底烘干后,石墨烯表面的褶皱明显减少;
2.使用低温低压退火工艺处理石墨烯薄膜,优化退火工艺,尽可能的减少了石墨烯表面PMMA的残留量,抑制了掺杂效应,提高了石墨烯的质量。
附图说明
图1是本发明的目标衬底上石墨烯薄膜湿法浸泡、转移与低温退火流程图。
具体实施方式
为了使本发明的目的、技术方案及优点更加清楚明白,以下结合附图及实施例,对本发明进行进一步详细说明。应当理解,此处所描述的具体实施例仅仅用以解释本发明,并不用于限定本发明。
参照图1,本发明给出如下实施例:
实施例1:
一种湿法浸泡和低温退火复合提高石墨烯性能的方法包括如下步骤:
(1)将刻蚀掉Cu基底的PMMA/石墨烯薄膜浸泡在甲酰胺溶液中10min,提高石墨烯表面的亲水性,增强后续石墨烯与衬底的贴合度;
(2)用SiO2/Si衬底捞起PMMA/石墨烯,形成PMMA/石墨烯/SiO2三明治结构,且在100℃温度下处理30min,以除去水分;
(3)将PMMA/石墨烯/SiO2/Si浸泡在丙酮溶液中15min除去PMMA;
(4)将去除PMMA的石墨烯/SiO2/Si衬底放入真空气氛管式炉;
(5)管式炉抽真空至0.1Pa,通入高纯(纯度>99.9%)Ar,流量100sccm,时间15min,赶走腔室内的空气;
(6)关闭惰性气体流量,待真空重新恢复至0.1Pa,通入高纯H2,流量10sccm,时间20min;
(7)设定加热程序,将衬底缓慢加热至200℃,加热速率2℃/min,保持真空泵的抽速和步骤(6)中的H2流量不变,时间100min;
(8)关闭加热程序,系统温度缓慢降至室温,关闭气体流量,关闭真空泵。
实施例2:
一种湿法浸泡和低温退火复合提高石墨烯性能的方法包括如下步骤:
(1)将刻蚀掉Cu基底的PMMA/石墨烯薄膜浸泡在甲酰胺溶液中20min,提高石墨烯表面的亲水性,增强后续石墨烯与衬底的贴合度;
(2)用SiO2/Si衬底捞起PMMA/石墨烯,形成PMMA/石墨烯/SiO2三明治结构,且在120℃温度下处理20min,以除去水分;
(3)将PMMA/石墨烯/SiO2/Si浸泡在丙酮溶液中10min除去PMMA;
(4)将去除PMMA的石墨烯/SiO2/Si衬底放入真空气氛管式炉;
(5)管式炉抽真空至0.5Pa,通入高纯(纯度>99.9%)N2,流量200sccm,时间10min,赶走腔室内的空气;
(6)关闭惰性气体流量,待真空重新恢复至0.5Pa,通入高纯H2,流量30sccm,时间15min;
(7)设定加热程序,将衬底缓慢加热至300℃,加热速率4℃/min,保持真空泵的抽速和步骤(6)中的H2流量不变,时间60min;
(8)关闭加热程序,系统温度缓慢降至室温,关闭气体流量,关闭真空泵。
实施例3:
一种湿法浸泡和低温退火复合提高石墨烯性能的方法包括如下步骤:
(1)将刻蚀掉Cu基底的PMMA/石墨烯薄膜浸泡在甲酰胺溶液中30min,提高石墨烯表面的亲水性,增强后续石墨烯与衬底的贴合度;
(2)用SiO2/Si衬底捞起PMMA/石墨烯,形成PMMA/石墨烯/SiO2三明治结构,且在150℃温度下处理15min,以除去水分;
(3)将PMMA/石墨烯/SiO2/Si浸泡在丙酮溶液中5min除去PMMA;
(4)将去除PMMA的石墨烯/SiO2/Si衬底放入真空气氛管式炉;
(5)管式炉抽真空至1Pa,通入高纯(纯度>99.9%)Ar,流量300sccm,时间5min,赶走腔室内的空气;
(6)关闭惰性气体流量,待真空重新恢复至1Pa,通入高纯H2,流量60sccm,时间15min;
(7)设定加热程序,将衬底缓慢加热至400℃,加热速率5℃/min,保持真空泵的抽速和步骤(6)中的H2流量不变,时间40min;
(8)关闭加热程序,系统温度缓慢降至室温,关闭气体流量,关闭真空泵。
以上所述仅为本发明较佳的具体实施例而已,并不用于限制本发明,任何熟悉本技术领域的技术人员在本发明揭露的技术范围内,根据本发明的技术方案及其发明构思加以等同替换或改变,都应涵盖在本发明的保护范围之内。
Claims (8)
1.一种湿法浸泡和低温退火复合提高石墨烯性能的方法,其特征在于,包括如下步骤:
(1)将刻蚀掉生长基底的PMMA/石墨烯薄膜浸泡在甲酰胺溶液中,以增强石墨烯薄膜的亲水性;
(2)用目标衬底捞起PMMA/石墨烯,形成PMMA/石墨烯/目标衬底三明治结构,目标衬底为SiO2/Si材质,且在适宜的温度下处理,以除去水分;
(3)将PMMA/石墨烯/目标衬底浸泡在丙酮溶液中除去PMMA;
(4)将去除PMMA的石墨烯/目标衬底放入真空气氛管式炉;
(5)管式炉抽真空至0.1-1 Pa,通入高纯惰性气体,赶走腔室内的空气;
(6)关闭惰性气体流量,待真空重新恢复至0.1-1 Pa,通入高纯H2;
(7)设定加热程序,将目标基底缓慢加热,保持真空泵的抽速和步骤(6)中的H2流量不变;
(8)关闭加热程序,系统温度缓慢降至室温,关闭气体流量,关闭真空泵。
2.如权利要求1所述的湿法浸泡和低温退火复合提高石墨烯性能的方法,其特征在于,所述的PMMA/石墨烯薄膜浸泡在甲酰胺溶液中,提高石墨烯表面的亲水性,增强后续石墨烯与目标衬底的贴合度。
3.如权利要求2所述的湿法浸泡和低温退火复合提高石墨烯性能的方法,其特征在于,所述的PMMA/石墨烯薄膜浸泡在甲酰胺溶液中,浸泡时间在为5-30 min。
4.如权利要求1所述的湿法浸泡和低温退火复合提高石墨烯性能的方法,其特征在于,所述的用目标衬底捞起PMMA/石墨烯,形成PMMA/石墨烯/目标衬底三明治结构,且在50-150℃温度下处理10-30 min,以除去水分。
5.如权利要求1所述的湿法浸泡和低温退火复合提高石墨烯性能的方法,其特征在于,所述的PMMA/石墨烯/目标衬底浸泡在丙酮溶液中5-30 min除去PMMA。
6.如权利要求1所述的湿法浸泡和低温退火复合提高石墨烯性能的方法,其特征在于,(5)管式炉抽真空至0.1-1 Pa,通入高纯惰性气体,所述高纯惰性气体为Ar、N2、He,流量50-500 sccm,时间5-20 min,以赶走腔室内的空气。
7.如权利要求1所述的湿法浸泡和低温退火复合提高石墨烯性能的方法,其特征在于,(6)关闭惰性气体流量,待真空重新恢复至0.1-1 Pa,通入高纯H2,流量5-100 sccm,时间5-20 min。
8.如权利要求1所述的湿法浸泡和低温退火复合提高石墨烯性能的方法,其特征在于,(7)设定加热程序,将目标衬底缓慢加热至100-500℃,加热速率1-5℃/min,保持真空泵的抽速和步骤(6)中的H2流量不变,时间10-120 min。
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