CN107245144A - 一种磷烯‑导电高分子复合材料的制备方法 - Google Patents
一种磷烯‑导电高分子复合材料的制备方法 Download PDFInfo
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Abstract
本发明公开了一种磷烯‑导电高分子复合材料的制备方法,包括:将磷烯涂覆于导电金属上制成磷烯电极;将导电高分子单体置于溶液中分散均匀,制得导电高分子电解液;将所述磷烯电极、参比电极和金属对电极置于所述导电高分子电解液中,并采用循环伏安法进行反应,从而制得磷烯‑导电高分子复合材料前驱体;将所述磷烯‑导电高分子复合材料前驱体置于pH值不高于5的溶液中浸泡0.1~72h,然后进行固液分离,并对固液分离得到的固体进行干燥,从而制得磷烯‑导电高分子复合材料。本发明不仅能够有效制备出兼具磷烯和导电高分子两者优点的磷烯‑导电高分子材料,而且操作简单、对设备要求低、产品质量好、产率高,十分适合进行规模化生产。
Description
技术领域
本发明涉及磷烯复合材料领域,尤其涉及一种磷烯-导电高分子复合材料的制备方法。
背景技术
磷烯材料是由单层磷原子紧密堆积成二维蜂窝状晶格结构的新型磷纳米材料,其特殊的微观稳定结构使其具有优异的电化学性能和热传导性能,因此磷烯材料在电子通信、交通运输等领域具有广阔应用前景。
磷烯材料因磷原子层间具有较强的范德华力和较大的比表面积,因此易于发生层叠现象而形成类似薄膜的片状结构,这种结构会导致比表面积大幅减小,从而会严重损失磷烯特有的吸附、导电、导热等优异性能。此外,磷烯较强的化学活性使其容易被氧气、水等物质侵蚀而失去原有性能。
在现有技术中,制备的磷烯材料比表面积较小,电化学性能较弱,另外对磷烯的层叠现象和容易被氧化侵蚀的缺点没有很好的处理方法,且没有出现磷烯-导电高分子复合材料及其合成方法。
发明内容
针对现有技术中的上述不足之处,本发明提供了一种磷烯-导电高分子复合材料的制备方法,不仅能够有效制备出兼具磷烯和导电高分子两者优点的磷烯-导电高分子材料,而且操作简单、对设备要求低、产品质量好、产率高,十分适合进行规模化生产。该磷烯-导电高分子材料具有良好的赝电容性能,不仅可以有效防止磷烯的片层堆叠,增大比表面积,而且可以有效抑制氧气和水对磷烯的侵蚀,保证磷烯的独特性能不被破坏,因此可广泛应用于电化学储能、电子通信等领域。
本发明的目的是通过以下技术方案实现的:
一种磷烯-导电高分子复合材料的制备方法,包括以下步骤:
步骤A、将磷烯涂覆于导电金属上制成磷烯电极;
步骤B、将导电高分子单体置于分散溶液中分散均匀,制得导电高分子电解液;
步骤C、将所述磷烯电极、参比电极和金属对电极置于所述导电高分子电解液中,并采用循环伏安法进行反应,电压范围为-1~1V、扫描速率为1~100mv/s、扫描次数为5~100次,从而制得磷烯-导电高分子复合材料前驱体;
步骤D、将所述磷烯-导电高分子复合材料前驱体置于pH值不高于5的溶液中浸泡0.1~72h,然后进行固液分离,并对固液分离得到的固体进行干燥,从而制得磷烯-导电高分子复合材料。
优选地,所述的导电金属为金、铂、银、铜、铁、镍、锌、锡、铅、不锈钢中的至少一种,并且所述导电金属的形状为片状、网状、棒状、丝状或泡沫状。
优选地,所述的导电高分子单体为苯胺、吡咯、吡啶、噻吩中的至少一种。
优选地,所述的分散溶液为水、甲醇、乙醇、丙醇、丙酮、四氢呋喃、四氯化碳、乙腈、乙醚、石油醚、戊烷、己烷、二硫化碳、二氯甲烷、二氯乙烷、三氯甲烷、三氯乙烷、乙酸乙酯、丁酮、苯、甲苯、二甲苯、环己烷、N,N-二甲基甲酰胺、甲醛、硫酸、盐酸、硝酸、乙酸、丙酸、氨水、水合肼、N-甲基吡咯烷酮中的至少一种。
优选地,所述的参比电极为标准氢电极、汞|氧化汞电极、汞|硫酸亚汞电极、饱和甘汞电极、银|氯化银电极中的至少一种。
由上述本发明提供的技术方案可以看出,本发明所提供的磷烯-导电高分子复合材料的制备方法将磷烯涂覆于导电金属上制成磷烯电极,并采用循环伏安法在磷烯电极上电化学聚合生成磷烯-导电高分子复合材料前驱体,然后去除所述磷烯-导电高分子复合材料前驱体中导电金属,从而即制得磷烯-导电高分子复合材料;该磷烯-导电高分子材料具有良好的赝电容性能,不仅可以有效防止磷烯的片层堆叠,而且可以有效抑制氧气和水对磷烯的侵蚀,保证磷烯的独特性能不被破坏,因此可广泛应用于电化学储能、电子通信等领域。本发明所提供的磷烯-导电高分子复合材料的制备方法操作简单、对设备要求低、产品质量好、产率高,十分适合进行规模化生产。
附图说明
为了更清楚地说明本发明实施例的技术方案,下面将对实施例描述中所需要使用的附图作简单地介绍,显而易见地,下面描述中的附图仅仅是本发明的一些实施例,对于本领域的普通技术人员来讲,在不付出创造性劳动的前提下,还可以根据这些附图获得其他附图。
图1为本发明实施例1所制备的氮掺杂磷烯的扫描电子显微镜照片。
具体实施方式
下面结合本发明实施例中的附图,对本发明实施例中的技术方案进行清楚、完整地描述,显然,所描述的实施例仅仅是本发明一部分实施例,而不是全部的实施例。基于本发明的实施例,本领域普通技术人员在没有做出创造性劳动前提下所获得的所有其他实施例,都属于本发明的保护范围。
下面对本发明所提供的磷烯-导电高分子复合材料的制备方法进行详细描述。
一种磷烯-导电高分子复合材料的制备方法,包括以下步骤:
步骤A、将磷烯涂覆于导电金属上制成磷烯电极。其中,所述的导电金属为金、铂、银、铜、铁、镍、锌、锡、铅、不锈钢中的至少一种,并且导电金属的形状可以为片状、网状、棒状、丝状或泡沫状。
步骤B、将导电高分子单体置于分散溶液中分散均匀,制得导电高分子电解液。其中,所述的导电高分子单体为苯胺、吡咯、吡啶、噻吩中的至少一种。所述的分散溶液为水、甲醇、乙醇、丙醇、丙酮、四氢呋喃、四氯化碳、乙腈、乙醚、石油醚、戊烷、己烷、二硫化碳、二氯甲烷、二氯乙烷、三氯甲烷、三氯乙烷、乙酸乙酯、丁酮、苯、甲苯、二甲苯、环己烷、N,N-二甲基甲酰胺、甲醛、硫酸、盐酸、硝酸、乙酸、丙酸、氨水、水合肼、N-甲基吡咯烷酮中的至少一种。
步骤C、将所述磷烯电极、参比电极和金属对电极置于所述导电高分子电解液中,并采用循环伏安法进行反应,电压范围为-1~1V、扫描速率为1~100mv/s、扫描次数为5~100次,从而制得磷烯-导电高分子复合材料前驱体。其中,所述的参比电极为标准氢电极、汞|氧化汞电极、汞|硫酸亚汞电极、饱和甘汞电极、银|氯化银电极中的至少一种。
步骤D、将所述磷烯-导电高分子复合材料前驱体置于pH值不高于5的溶液中浸泡0.1~72h,以去除所述磷烯-导电高分子复合材料前驱体中的导电金属,然后进行固液分离,并对固液分离得到的固体进行干燥,从而制得磷烯-导电高分子复合材料。
具体地,本发明所提供的磷烯-导电高分子复合材料的制备方法将磷烯涂覆于导电金属上制成磷烯电极,并采用循环伏安法在磷烯电极上电化学聚合生成磷烯-导电高分子复合材料前驱体,然后去除所述磷烯-导电高分子复合材料前驱体中导电金属,从而即制得磷烯-导电高分子复合材料;该磷烯-导电高分子材料具有良好的导电性、导热性、稳定性、柔性和赝电容性能,不仅可以有效防止磷烯的片层堆叠,而且可以有效抑制氧气和水对磷烯的侵蚀,保证磷烯的独特性能不被破坏,因此可广泛应用于电化学储能、电子通信等领域。本发明所提供的磷烯-导电高分子复合材料的制备方法操作简单、对设备要求低、产品质量好、产率高,十分适合进行规模化生产。
为了更加清晰地展现出本发明所提供的技术方案及所产生的技术效果,下面以具体实施例对本发明实施例所提供的磷烯-导电高分子复合材料的制备方法进行详细描述。
实施例1
一种磷烯-导电高分子复合材料的制备方法,包括以下步骤:
步骤a1、将磷烯涂覆于不锈钢网上制成磷烯电极。
步骤b1、将苯胺置于水中分散均匀,制得导电高分子电解液。
步骤c1、将所述磷烯电极、饱和甘汞电极(作为参比电极)和金箔对电极置于所述导电高分子电解液中,并采用循环伏安法进行反应,电压范围为-1~1V、扫描速率为2mv/s、扫描次数为5次,从而制得磷烯-导电高分子复合材料前驱体。
步骤d1、将所述磷烯-导电高分子复合材料前驱体置于pH值为0.001的盐酸溶液中浸泡0.5h,以去除所述磷烯-导电高分子复合材料前驱体中的不锈钢,然后进行固液分离,并对固液分离得到的固体进行干燥,从而制得如图1所示的磷烯-导电高分子复合材料。
具体地,现有技术中普通磷烯材料的比表面积约为60m2/g,而本发明实施例1所提供的磷烯-导电高分子复合材料的比表面积大于1000m2/g,并且赝电容性能远高于普通磷烯材料。
实施例2
一种磷烯-导电高分子复合材料的制备方法,包括以下步骤:
步骤a2、将磷烯涂覆于铜棒上制成磷烯电极。
步骤b2、将吡咯置于乙醇中分散均匀,制得导电高分子电解液。
步骤c2、将所述磷烯电极、汞|氧化汞电极(作为参比电极)和铂对电极置于所述导电高分子电解液中,并采用循环伏安法进行反应,电压范围为-0.7~1V、扫描速率为20mv/s、扫描次数为20次,从而制得磷烯-导电高分子复合材料前驱体。
步骤d2、将所述磷烯-导电高分子复合材料前驱体置于pH值为0.01的硫酸和乙腈的混合溶液中浸泡10h,以去除所述磷烯-导电高分子复合材料前驱体中的铜,然后进行固液分离,并对固液分离得到的固体进行干燥,从而制得磷烯-导电高分子复合材料。
实施例3
一种磷烯-导电高分子复合材料的制备方法,包括以下步骤:
步骤a3、将磷烯涂覆于锌棒上制成磷烯电极。
步骤b3、将吡咯置于乙醇中分散均匀,制得导电高分子电解液。
步骤c3、将所述磷烯电极、汞|氧化汞电极(作为参比电极)和铂对电极置于所述导电高分子电解液中,并采用循环伏安法进行反应,电压范围为-0.7~0.9V、扫描速率为20mv/s、扫描次数为20次,从而制得磷烯-导电高分子复合材料前驱体。
步骤d3、将所述磷烯-导电高分子复合材料前驱体置于pH值为0.1的硝酸溶液中浸泡10h,以去除所述磷烯-导电高分子复合材料前驱体中的锌,然后进行固液分离,并对固液分离得到的固体进行干燥,从而制得磷烯-导电高分子复合材料。
实施例4
一种磷烯-导电高分子复合材料的制备方法,包括以下步骤:
步骤a4、将磷烯涂覆于铝网上制成磷烯电极。
步骤b4、将吡啶置于二硫化碳中分散均匀,制得导电高分子电解液。
步骤c4、将所述磷烯电极、汞|硫酸亚汞电极(作为参比电极)和铝对电极置于所述导电高分子电解液中,并采用循环伏安法进行反应,电压范围为-0.5~0.8V、扫描速率为40mv/s、扫描次数为40次,从而制得磷烯-导电高分子复合材料前驱体。
步骤d4、将所述磷烯-导电高分子复合材料前驱体置于pH值为1的硝酸和石油醚溶液中浸泡24h,以去除所述磷烯-导电高分子复合材料前驱体中的铝,然后进行固液分离,并对固液分离得到的固体进行干燥,从而制得磷烯-导电高分子复合材料。
实施例5
一种磷烯-导电高分子复合材料的制备方法,包括以下步骤:
步骤a5、将磷烯涂覆于镍网上制成磷烯电极。
步骤b5、将吡啶置于二硫化碳中分散均匀,制得导电高分子电解液。
步骤c5、将所述磷烯电极、汞|硫酸亚汞电极(作为参比电极)和镍泡沫对电极置于所述导电高分子电解液中,并采用循环伏安法进行反应,电压范围为-0.5~0.8V、扫描速率为70mv/s、扫描次数为70次,从而制得磷烯-导电高分子复合材料前驱体。
步骤d5、将所述磷烯-导电高分子复合材料前驱体置于pH值为3的乙酸溶液中浸泡48h,以去除所述磷烯-导电高分子复合材料前驱体中的镍,然后进行固液分离,并对固液分离得到的固体进行干燥,从而制得磷烯-导电高分子复合材料。
实施例6
一种磷烯-导电高分子复合材料的制备方法,包括以下步骤:
步骤a6、将磷烯涂覆于铁丝上制成磷烯电极。
步骤b6、将噻吩和吡啶混合物置于N,N-二甲基甲酰胺中分散均匀,制得导电高分子电解液。
步骤c6、将所述磷烯电极、银|氯化银电极(作为参比电极)和铁棒对电极置于所述导电高分子电解液中,并采用循环伏安法进行反应,电压范围为-0.2~0.4V、扫描速率为100mv/s、扫描次数为100次,从而制得磷烯-导电高分子复合材料前驱体。
步骤d6、将所述磷烯-导电高分子复合材料前驱体置于pH值为5的丙酸溶液中浸泡72h,以去除所述磷烯-导电高分子复合材料前驱体中的铁,然后进行固液分离,并对固液分离得到的固体进行干燥,从而制得磷烯-导电高分子复合材料。
综上可见,本发明实施例不仅能够有效制备出兼具磷烯和导电高分子两者优点的磷烯-导电高分子材料,而且操作简单、对设备要求低、产品质量好、产率高,十分适合进行规模化生产。该磷烯-导电高分子材料具有良好的赝电容性能,不仅可以有效防止磷烯的片层堆叠,而且可以有效抑制氧气和水对磷烯的侵蚀,保证磷烯的独特性能不被破坏,因此可广泛应用于电化学储能、电子通信等领域。
以上所述,仅为本发明较佳的具体实施方式,但本发明的保护范围并不局限于此,任何熟悉本技术领域的技术人员在本发明披露的技术范围内,可轻易想到的变化或替换,都应涵盖在本发明的保护范围之内。因此,本发明的保护范围应该以权利要求书的保护范围为准。
Claims (6)
1.一种磷烯-导电高分子复合材料的制备方法,其特征在于,包括以下步骤:
步骤A、将磷烯涂覆于导电金属上制成磷烯电极;
步骤B、将导电高分子单体置于分散溶液中分散均匀,制得导电高分子电解液;
步骤C、将所述磷烯电极、参比电极和金属对电极置于所述导电高分子电解液中,并采用循环伏安法进行反应,电压范围为-1~1V、扫描速率为1~100mv/s、扫描次数为5~100次,从而制得磷烯-导电高分子复合材料前驱体;
步骤D、将所述磷烯-导电高分子复合材料前驱体置于pH值不高于5的溶液中浸泡0.1~72h,然后进行固液分离,并对固液分离得到的固体进行干燥,从而制得磷烯-导电高分子复合材料。
2.根据权利要求1所述的磷烯-导电高分子复合材料的制备方法,其特征在于,所述的导电金属为金、铂、银、铜、铁、镍、锌、锡、铅、不锈钢中的至少一种。
3.根据权利要求1或2所述的磷烯-导电高分子复合材料的制备方法,其特征在于,所述的导电金属的形状为片状、网状、棒状、丝状或泡沫状。
4.根据权利要求1或2所述的磷烯-导电高分子复合材料的制备方法,其特征在于,所述的导电高分子单体为苯胺、吡咯、吡啶、噻吩中的至少一种。
5.根据权利要求1或2所述的磷烯-导电高分子复合材料的制备方法,其特征在于,所述的分散溶液为水、甲醇、乙醇、丙醇、丙酮、四氢呋喃、四氯化碳、乙腈、乙醚、石油醚、戊烷、己烷、二硫化碳、二氯甲烷、二氯乙烷、三氯甲烷、三氯乙烷、乙酸乙酯、丁酮、苯、甲苯、二甲苯、环己烷、N,N-二甲基甲酰胺、甲醛、硫酸、盐酸、硝酸、乙酸、丙酸、氨水、水合肼、N-甲基吡咯烷酮中的至少一种。
6.根据权利要求1或2所述的磷烯-导电高分子复合材料的制备方法,其特征在于,所述的参比电极为标准氢电极、汞|氧化汞电极、汞|硫酸亚汞电极、饱和甘汞电极、银|氯化银电极中的至少一种。
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