CN108517696B - 一种图案化柔性导电石墨烯布的制备方法 - Google Patents
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Abstract
本发明公开一种图案化柔性导电石墨烯布的制备方法,该方法包括下述步骤:将布织物在三氯乙烯基硅烷类化合物溶液中浸泡处理为疏水;将图案模板固定在布织物表面后,采用等离子体处理将布织物上图案化的部分处理为亲水;然后去除图案模板,在布织物图案化部分表面成形氧化石墨烯膜,将所得布织物放入还原剂溶液中加热还原,然后用水浸泡、冲洗、晾干,得到图案化的柔性导电石墨烯布。本发明的制备方法操作简单,对设备、工艺要求不高,原料利用率高,成本低,可实现批量生产;而且,制得的图案化导电石墨烯布柔韧性好、导电性高,有望用于柔性电子、超级电容、可穿戴式传感等方面。
Description
技术领域
本发明涉及一种导电石墨烯织物的制备方法,特别涉及一种图案化柔性导电石墨烯布的制备方法,属于导电石墨烯材料制备技术领域。
背景技术
石墨烯作为一种新兴的二维材料最近几年在世界范围内掀起了热潮。它是一种蜂窝状的二维平面材料,其中每个碳原子具有一个s轨道和3个p轨道。一个s轨道和两个p轨道与其他碳原子形成刚性的σ键使石墨烯具有良好的机械强度,剩余的p轨道电子集合在一起组成大π键从而赋予石墨烯优良的性能。由于其具有良好的导电性,导热性,透光性,生物相容性,非常好的机械强度,使得它在各个领域引起人们的重视。尤其是石墨烯具有优良的机械性能及优异的导电性能,常温下石墨烯的电子迁移率可达15000cm2V-1S-1,使其在电子器件以及柔性电子器件方面极具应用前景。
图案化技术在大面积电子器件和柔性电路的实际应用中非常重要。目前,对于石墨图案化的加工方法包括掩膜版光刻法、印刷法、喷墨打印法和激光直写加工法。如Cong等人报道了采用聚苯乙烯纳米球在单层石墨烯上作为掩膜,然后利用O2反应离子刻蚀技术对石墨烯进行图案化处理,将未被保护的石墨烯薄膜刻蚀掉,在通过氯仿超声处理将聚苯乙烯纳米球移除掉,从而成功地在SiO2/Si基底上制作出周期性的石墨烯纳米阵列,石墨烯纳米阵列的尺寸可以通过改变聚苯乙烯纳米球的大小来调节,最小可精细到几十个纳米(J.Phys.Chem.C 2009,113:6529-6532.)。M.J.Allen等人采用PDMS(聚二甲基硅氧烷)作为印章,将石墨烯作为“油墨”粘附于印章之上,再利用PDMS与石墨烯之间的结合能要小于Si/SiO2基底与石墨烯之间的结合能这一思路,将图案化石墨烯薄膜“印”在了基底之上(Adv.Mater.2009,21:2098-2102.)。
但目前的这些技术在制备大面积的图案化的石墨烯材料时还存在耗时长、成本高等问题,不利于批量生产。
发明内容
发明目的:针对现有的图案化石墨烯材料制备方法存在的耗时长、成本高等问题,本发明提供一种图案化柔性导电石墨烯布的制备方法。
技术方案:本发明所述的一种图案化柔性导电石墨烯布的制备方法,包括如下步骤:
(1)将布织物在三氯乙烯基硅烷类化合物溶液中浸泡处理为疏水;
(2)将图案模板固定在布织物表面后,采用等离子体处理将布织物上图案化的部分处理为亲水;然后去除图案模板,在布织物图案化部分表面成形氧化石墨烯膜;
(3)将步骤(2)所得含有氧化石墨烯图案的布织物放入还原剂溶液中加热还原;
(4)将步骤(3)所得布织物用水浸泡、冲洗、晾干,得到图案化的柔性导电石墨烯布。
上述步骤(1)中,处理对象布织物为商品化的布,包括纱布、棉布、丝绸等柔性织物。浸泡处理的时间优选为1~5h,处理后布织物的接触角大于150°。
上述步骤(2)中,等离子体处理的时间可为1~10s。通过控制等离子体表面处理的时间,可以控制石墨烯薄膜图案的宽度,处理时间越长,石墨烯薄膜图案的宽度越宽。
优选的,步骤(2)中,在布织物图案化部分表面成形氧化石墨烯膜的方法为:将布织物放置在氧化石墨烯水溶液表面浸润5~100s,取出后在50~100℃下真空干燥成膜。
上述步骤(3)中,加热还原条件优选为:还原温度50~150℃,反应时间1~5h。还原剂溶液可水合肼溶液、抗坏血酸溶液等。
有益效果:与现有技术相比,本发明的优点在于:(1)本发明通过控制布织物表面的亲疏水图案就可实现相应的图案化石墨烯材料制备,制备方法操作简单,对设备、工艺要求不高,原料利用率高,成本低,可实现批量生产;而且,通过控制模板的图案,可以方便简单地获得具有不同图案的导电石墨烯布;(2)亲水的氧化石墨烯很容易紧密地吸附在亲水性的基底上,但还原氧化石墨烯由于亲水基团的还原而表现为疏水性,疏水的还原氧化石墨烯很容易从亲水性的基底上脱落下来,本发明首次提出采用具有微结构的布织物作为基底构建图案化的导电石墨烯,利用布织物的纤维状微结构提高石墨烯在基底上的吸附性能,有效解决了氧化石墨烯还原后容易从亲水基底上脱落的问题;(3)本发明制得的图案化导电石墨烯布柔韧性好、导电性高,有望用于柔性电子、超级电容、可穿戴式传感等方面。
附图说明
图1为实施例1制备的图案化柔性导电石墨烯布的图片;
图2为实施例2制备的图案化柔性导电石墨烯布的图片;
图3为实施例1制得的图案化柔性导电石墨烯布在不同放大倍数下的扫描电子显微镜图,其中,图3(a)中放大倍数为1000倍,图3(b)中放大倍数为5000倍;
图4为实施例1制得的图案化柔性导电石墨烯布的IV曲线。
具体实施方式
下面结合附图对本发明的技术方案作进一步说明。
实施例1条纹图案的柔性导电石墨烯布的制备
(1)将商品化的纱布织物在三氯乙烯基硅烷化合物溶液中浸泡1h,处理后布织物的接触角为153°;
(2)将条纹图案模板固定在布织物表面后进行等离子体处理1s,去除模板,将布织物浸泡在氧化石墨烯水溶液中浸润5s,取出后在50℃下真空干燥5h,得到图案化的石墨烯布;
(3)将制备的含有氧化石墨烯图案的布织物放入水合肼溶液中,在90℃油浴中加热3h,即得到图案化的柔性导电石墨烯布;
(4)将制备的柔性导电石墨烯布转移到纯水浸泡,冲洗,室温晾干,即得到条纹图案化的柔性导电石墨烯布,如图1,可以看到,石墨烯紧密地附着在布织物基底上;此外,从图3(a)和3(b)导电石墨烯布的扫描电子显微镜图也可以看出,石墨烯紧密地附着在布织物的纤维状微结构表面。测试制得的柔性导电石墨烯布的导电性能,如图4,可以看到,该条纹图案化柔性导电石墨烯布具有较高的导电性。
实施例2花型图案的柔性导电石墨烯布的制备
(1)将商品化的棉布织物在三氯乙烯基硅烷化合物溶液中浸泡2.5h,处理后布织物的接触角为156°;
(2)将花型图案模板固定在布织物表面后进行等离子体处理3s,去除模板,将布织物浸泡在氧化石墨烯水溶液中浸润50s,取出后在65℃下真空干燥3h,得到图案化的石墨烯布;
(3)将制备的含有氧化石墨烯图案的布织物放入水合肼溶液中,在50℃油浴中加热5h,即得到图案化的柔性导电石墨烯布;
(4)将制备的柔性导电石墨烯布转移到纯水浸泡,冲洗,室温晾干,即得到花型图案化的柔性导电石墨烯布,如图2,可以看到,本实施例中,石墨烯也紧密地附着在布织物基底上;制得的花型图案化柔性导电石墨烯布的导电性能与实施例1相近。
实施例3电路图案的柔性导电石墨烯布的制备
(1)将商品化的丝绸布织物在三氯乙烯基硅烷化合物溶液中浸泡5h,处理后布织物的接触角为159°;
(2)将电路图案模板固定在布织物表面后进行等离子体处理5s,去除模板,将布织物浸泡在氧化石墨烯水溶液中浸润100s,取出后在100℃下真空干燥1h,得到图案化的石墨烯布;
(3)将制备的含有氧化石墨烯图案的布织物放入抗坏血酸溶液中,在150℃油浴中加热1h,即得到电路图案化的柔性导电石墨烯布;
(4)将制备的柔性导电石墨烯布转移到纯水浸泡,冲洗,室温晾干,即得到电路图案的柔性导电石墨烯布;其导电性能与实施例1相近。
Claims (5)
1.一种图案化柔性导电石墨烯布的制备方法,其特征在于,包括如下步骤:
(1)将布织物在三氯乙烯基硅烷类化合物溶液中浸泡处理为疏水;所述浸泡处理时间为1~5h,处理后布织物的接触角大于150°;
(2)将图案模板固定在布织物表面后,采用等离子体处理将布织物上图案化的部分处理为亲水;然后去除图案模板,在布织物图案化部分表面成形氧化石墨烯膜;
(3)将步骤(2)所得含有氧化石墨烯图案的布织物放入还原剂溶液中加热还原;所述还原剂溶液为水合肼溶液或抗坏血酸溶液;
(4)将步骤(3)所得布织物用水浸泡、冲洗、晾干,得到图案化的柔性导电石墨烯布。
2.根据权利要求1所述的图案化柔性导电石墨烯布的制备方法,其特征在于,步骤(1)中,所述布织物为纱布、棉布或丝绸。
3.根据权利要求1所述的图案化柔性导电石墨烯布的制备方法,其特征在于,步骤(2)中,所述等离子体处理的时间为1~10s。
4.根据权利要求1所述的图案化柔性导电石墨烯布的制备方法,其特征在于,步骤(2)中,所述在布织物图案化部分表面成形氧化石墨烯膜的方法为:将布织物放置在氧化石墨烯水溶液表面浸润5~100s,取出后在50~100℃下真空干燥成膜。
5.根据权利要求1所述的图案化柔性导电石墨烯布的制备方法,其特征在于,步骤(3)中,所述加热还原条件为:还原温度50~150℃,反应时间1~5h。
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