CN105504326A - 一种石墨烯叠层复合掺杂方法 - Google Patents
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Abstract
本发明提供一种石墨烯叠层复合掺杂方法,步骤如下:步骤一,配制氧化剂涂布液;步骤二,在目标基底表面涂布氧化剂溶液,并加热干燥形成氧化剂涂层;步骤三,将涂布有氧化剂的目标基底置于密闭容器中,加热到一定温度;步骤四,将导电高分子前驱体加热气化,与载气混合通入密闭容器,小分子前驱体吸附在氧化涂层上聚合形成掺杂涂层;步骤五,用去离子水浸泡掺杂涂层并烘干;步骤六,将石墨烯转移到带有掺杂涂层的目标基底。进一步,在上述石墨烯上重复上述步骤二至步骤五形成第二掺杂涂层。本发明在目标基底表面原位形成一层厚度均匀可控的掺杂涂层,掺杂效果均匀;此外,掺杂涂层本身稳定,转移后位于石墨烯与目标基底之间,掺杂效果稳定持久。
Description
技术领域
本发明属于石墨烯生产技术领域,尤其涉及一种石墨烯叠层复合掺杂方法。
背景技术
石墨烯是近十年发现的新型二维碳纳米材料,具有优异的力、热、光、电等方面性能。其中,极高的透过率及超高的载流子迁移率,使其可作为全新的透明导电材料而备受工业界关注。
目前,对于二维连续的石墨烯薄膜产品,电学性能是其核心关键性能。现有较为成熟的化学气相沉积法(CVD)制备的石墨烯薄膜方阻较高,不能直接使用,必须对其进行掺杂以降低方阻。当前主流掺杂方法大多是以小分子为掺杂剂,例如乙二胺、硝酸、氯金酸等,通过物理吸附使其附着在石墨烯表面达到掺杂目的。然而,物理吸附的小分子掺杂剂与石墨烯作用力弱,易迁移和挥发,放置过程中导致石墨烯方阻持续增加,严重限制了石墨烯的实际应用。
发明内容
本发明的目的就是为了克服上述背景技术的不足,提供一种石墨烯叠层复合掺杂方法,能够实现均匀、稳定、持久的掺杂效果。
本发明所涉及的一种石墨烯叠层复合方法,其步骤如下:
步骤一,配制氧化剂涂布液,其组成为氧化剂和惰性有机溶剂;其中氧化剂为对甲苯磺酸铁,用量范围为0.1~5%wt;惰性溶剂为乙醇、异丙醇、正丁醇、乳酸乙酯、乙二醇单乙醚、乙二醇单丁醚中的一种或几种;
步骤二,在目标基底001表面涂布氧化剂溶液,并加热干燥形成氧化剂涂层002,涂层厚度为1~30nm,形成由目标基底001、氧化剂涂层002依次组成的复合结构;
步骤三,将涂布有氧化剂涂层002的目标基底001置于密闭容器中加热,温度为50~130℃;
步骤四,将导电高分子前驱体加热气化,与载气混合通入密闭容器,小分子前驱体吸附在氧化剂涂层002上聚合形成第一掺杂涂层003,形成目标基底001/第一掺杂涂层003的复合结构;所述导电高分子前驱体为吡咯和3,4-乙撑二氧噻吩(EDOT);所述载气为氮气或氩气,载气用量体积百分比为80~99%;所述混合气体流量为10~100sccm,通气时间为20~60min;
步骤五,用去离子水浸泡第一掺杂涂层003并烘干;
步骤六,将石墨烯004转移到带有第一掺杂涂层003的目标基底001,得到由目标基底001/第一掺杂涂层003/石墨烯004依次组成的复合结构。
进一步,在所述由目标基底001/第一掺杂涂层003/石墨烯004依次组成的复合结构上重复上述步骤二至步骤五可形成第二掺杂涂层005,得到由目标基底001/第一掺杂涂层003/石墨烯004/第二掺杂涂层005依次组成的复合结构。进一步提升掺杂效果,同时对石墨烯起到一定封装保护效果。
本发明的有益效果是:采用气相氧化聚合方法,在目标基底表面原位形成一层厚度均匀的掺杂涂层,适合大面积生产;此外,掺杂涂层本身稳定,转移后位于石墨烯与目标基底之间,掺杂效果均匀稳定。
附图说明
图1为本发明一种石墨烯叠层复合掺杂方法的步骤流程图;
图2为本发明中所述目标基底/氧化剂涂层依次组成的复合结构示意图;
图3为本发明中所述目标基底/第一掺杂涂层的复合结构示意图;
图4为本发明中所述目标基底/第一掺杂涂层/石墨烯依次组成的复合结构示意图;
图5为本发明中所述目标基底/第一掺杂涂层/石墨烯/第二掺杂涂层依次组成的复合结构示意图;
附图中,各标号所代表的部件列表如下:
001为目标基底,002为氧化剂涂层,003为第一掺杂涂层,004为石墨烯,005为第二掺杂涂层。
具体实施方式
下面结合附图和实施例对本发明进一步说明。所举实例只用于解释本发明,并非用于限定本发明的范围。
实施例一
本实施例步骤如下:
步骤一,称取1.5g对甲苯磺酸铁溶于350g无水乙醇、600g乙二醇和450g乳酸乙酯组成的混合溶液,搅拌均匀后配成氧化剂涂布液;
步骤二,采用滚涂法将掺杂涂布液涂布于目标基底PET001,干燥后得到膜厚约30nm的氧化剂涂层002;
步骤三,将涂布有氧化剂涂层002的PET基底001置于密闭容器中,加热到60℃;
步骤四,将3,4-乙撑二氧噻吩小分子单体加热气化,以氩气为载气通入密闭容器中。氩气体积百分数为99%,流量为100sccm,通气40min后在目标基底PET001表面形成第一掺杂涂层003;
步骤五,将第一掺杂涂层003浸于去离子水浸洗,取出烘干;
步骤六,在第一掺杂层003上转移石墨烯004。
本实施例中,制备的石墨烯方阻均值为197±15欧方,140℃加热90min,并于室温下方阻30天后平均方阻为203±13欧方,掺杂效果均匀稳定。
实施例二
本实施例步骤如下:
步骤一,称取1g对甲苯磺酸铁溶于60g异丙醇、75g正丁醇和10g乙二醇单丁醚组成的混合溶剂,混合均匀后配成氧化剂涂布液;
步骤二,将掺杂涂布液涂布于光学级PET基底001,干燥后得到膜厚约10nm的氧化剂涂层002;
步骤三,将涂布有氧化剂涂层002的PET基底001置于密闭容器中,加热到90℃;
步骤四,将吡咯小分子单体加热气化,以氮气为载气通入密闭容器中。氮气体积百分数为95%,流量为50sccm,通气30min后在目标基底PET表面形成第一掺杂涂层003;
步骤五,将第一掺杂涂层003浸于去离子水浸洗,取出烘干;
步骤六,在第一掺杂层003上转移石墨烯004。
重复步骤二至步骤五,在已转移石墨烯004表面形成第二掺杂涂层005。
本实施例中,制备的石墨烯方阻均值为187±21欧方,140℃加热90min,并于室温下方阻30天后平均方阻为179±22欧方,掺杂效果均匀稳定。
实施例三
本实施例步骤如下:
步骤一,称取0.3g对甲苯磺酸铁溶于50g甲醇、60g异丙醇、170g正丁醇、8g乙二醇单甲醚和5g乙二醇单丁醚组成的混合溶剂,混合均匀后配成氧化剂涂布液;
步骤二,将掺杂涂布液涂布于光学级PET基底001,干燥后得到膜厚约5nm的氧化剂涂层002;
步骤三,将涂布有氧化剂涂层002的PET基底001置于密闭容器中,加热到50℃;
步骤四,将噻吩小分子单体加热气化,以氩气为载气通入密闭容器中。氩气体积百分数为90%,流量为30sccm,通气60min后在目标基底PET001表面形成第一掺杂涂层003;
步骤五,将第一掺杂涂层003浸于去离子水浸洗,取出烘干;
步骤六,在第一掺杂层003上转移石墨烯004。
本实施例中,制备的石墨烯方阻均值为226±19欧方,140℃加热90min,并于室温下方阻30天后平均方阻为223±17欧方,掺杂效果均匀稳定。
实施例四
本实施例步骤如下:
步骤一,称取2.0g对甲苯磺酸铁溶于1400g正丁醇,搅拌均匀后配成氧化剂涂布液;
步骤二,采用滚涂法将掺杂涂布液涂布于目标基底PET001,干燥后得到膜厚约1nm的氧化剂涂层002;
步骤三,将涂布有氧化剂涂层002的PET基底001置于密闭容器中,加热到130℃;
步骤四,将3,4-乙撑二氧噻吩小分子单体加热气化,以氮气为载气通入密闭容器中。氩气体积百分数为80%,流量为10sccm,通气20min后在目标基底PET001表面形成第一掺杂涂层003;
步骤五,将第一掺杂涂层003浸于去离子水浸洗,取出烘干;
步骤六,在第一掺杂层003上转移石墨烯004。
本实施例中,制备的石墨烯方阻均值为233±25欧方,140℃加热90min,并于室温下方阻30天后平均方阻为239±22欧方,掺杂效果均匀稳定。
实施例五
本实施例步骤如下:
步骤一,称取1.9g对甲苯磺酸铁溶于300g乙醇、500g异丙醇、600g正丁醇、10g乙二醇单丁醚组成的混合溶剂中,搅拌均匀后配成氧化剂涂布液;
步骤二,采用滚涂法将掺杂涂布液涂布于目标基底PET001,干燥后得到膜厚约20nm的氧化剂涂层002;
步骤三,将涂布有氧化剂涂层002的PET基底001置于密闭容器中,加热到100℃;
步骤四,将3,4-乙撑二氧噻吩小分子单体加热气化,以氮气为载气通入密闭容器中。氩气体积百分数为85%,流量为40sccm,通气60min后在目标基底PET001表面形成第一掺杂涂层003;
步骤五,将第一掺杂涂层003浸于去离子水浸洗,取出烘干;
步骤六,在第一掺杂层003上转移石墨烯004。
本实施例中,制备的石墨烯方阻均值为173±21欧方,140℃加热90min,并于室温下方阻30天后平均方阻为176±22欧方,掺杂效果均匀稳定。
以上所述仅为本发明的较佳实施例,并不用以限制本发明,凡在本发明的精神和原则之内,所作的任何修改、等同替换、改进等,均应包含在本发明的保护范围之内。
Claims (2)
1.一种石墨烯叠层复合掺杂方法,其特征在于,该方法步骤如下:
步骤一,配制氧化剂涂布液,其组成为氧化剂和惰性有机溶剂;其中氧化剂为对甲苯磺酸铁,用量范围为0.1~5%wt;惰性溶剂为乙醇、异丙醇、正丁醇、乳酸乙酯、乙二醇单乙醚、乙二醇单丁醚中的一种或几种;
步骤二,在目标基底(001)表面涂布氧化剂溶液,并加热干燥形成氧化剂涂层(002),涂层厚度为1~30nm,形成由目标基底(001)/氧化剂涂层(002)依次组成的复合结构;
步骤三,将涂布有氧化剂涂层(002)的目标基底(001)置于密闭容器中加热,温度为50~130℃;
步骤四,将导电高分子前驱体加热气化,与载气混合通入密闭容器,小分子前驱体吸附在氧化剂涂层(002)上聚合形成第一掺杂涂层(003),形成目标基底(001)/第一掺杂涂层(003)的复合结构;所述导电高分子前驱体为吡咯和3,4-乙撑二氧噻吩(EDOT);所述载气为氮气或氩气,载气用量体积百分比为80~99%;所述混合气体流量为10~100sccm,通气时间为20~60min;
步骤五,用去离子水浸泡第一掺杂涂层(003)并烘干;
步骤六,将石墨烯(004)转移到带有第一掺杂涂层(003)的目标基底(001),得到由目标基底(001)/第一掺杂涂层(003)/石墨烯(004)依次组成的复合结构。
2.根据权利要求1所述的一种石墨烯叠层复合掺杂方法,其特征在于,在所述由目标基底(001)/第一掺杂涂层(003)/石墨烯(004)依次组成的复合结构上重复上述步骤二至步骤五可形成第二掺杂涂层(005),得到由目标基底(001)/第一掺杂涂层(003)/石墨烯(004)/第二掺杂涂层(005)依次组成的复合结构。
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