CN106532071A - 一种制备n掺杂石墨烯包裹碳化铁电催化剂的方法 - Google Patents
一种制备n掺杂石墨烯包裹碳化铁电催化剂的方法 Download PDFInfo
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Abstract
本发明是一种制备N掺杂石墨烯包裹碳化铁电催化剂的方法。本发明的目的在于提供一种具有优异氧还原性能的Fe5C2@NG催化材料及其制备方法,以提升燃料电池中阴极的催化反应活性并且减少贵金属Pt的使用。本发明的制备N掺杂石墨烯包裹碳化铁电催化剂的方法是:以石墨化氮化碳(g‑C3N4)为碳源和氮源,加入二茂铁为铁源,混合均匀后在N2条件下煅烧,煅烧结束后用H2SO4处理,然后再次高温处理,即可得到Fe5C2@NG催化剂产品。采用本发明所制备的Fe5C2@NG催化剂产品,具有产品成本低、易控制、重复性好、可大规模生产等特点。
Description
技术领域
本发明属于N掺杂石墨烯包裹碳化铁(Fe5C2@NG)的二维纳米复合结构电催化剂制备技术领域,特别是提供了一种制备N掺杂石墨烯包裹碳化铁电催化剂的方法。
背景技术
燃料电池具有良好的能量转化效率,并且无二次污染以及反应条件温和等优势,被认为是相当有发展前景的一种化学电池,对于解决石油、天然气等能源不足问题提供了新的思路与途径。但是燃料电池所存在的缺点却是不可忽略的,首先燃料电池的成本很高,该不足主要源于贵金属Pt的大量使用;其次,稳定性不够,在使用过程中,由于Pt催化剂在体系中的催化活性会随着时间的增加而逐渐降低。因此寻找相对经济并且具有高效催化活性的催化剂已经成为了研究重点,其中石墨烯或石墨化碳具有良好的导电性以及催化活性,被广泛应用与燃料电池领域。
对于石墨烯基氧还原催化剂也有大量的报道,如专利CN104709900A公开了纳米石墨烯片的合成方法;专利CN104831307A公开合成了微纳石墨烯片的合成方法;《美国化学会志》杂志(2012年,134卷9082页)公开报道了石墨烯复合Fe3O4氧还原催化剂;《美国化学会志》杂志(2012年,134卷9082页)公开报道了石墨烯复合FePt合金氧还原电催化剂。但是通过这些方法合成催化剂往往需要很长的时间,操作比较繁复缺点。通过简单的煅烧方法制备合成高产、容易实现规模化生产而同时具备优异的氧还原性能的Fe5C2@NG材料的制备方法还没有被报道。
发明内容
本发明的目的在于提供一种具有优异氧还原性能的Fe5C2@NG催化材料及其制备方法,以提升燃料电池中阴极的催化反应活性并且减少贵金属Pt的使用。
本发明的技术方案是通过如下方式实现的:一种制备N掺杂石墨烯包裹碳化铁电催化剂的方法,以石墨化氮化碳(g-C3N4)为碳源和氮源,加入二茂铁为铁源,混合均匀后在N2条件下煅烧,煅烧结束后用H2SO4处理,然后再次高温处理,即可得到Fe5C2@NG催化剂。
在所述的一种制备N掺杂石墨烯包裹碳化铁电催化剂的方法中,制备Fe5C2@NG催化剂包含以下步骤:
⑴g-C3N4的制备:
称取5~15g三聚氰胺,放到坩埚中,并将坩埚用盖子盖住,然后将坩埚放入马弗炉里煅烧,煅烧温度为450~650℃,升温时间为1~3小时,保温时间为1~3小时,等马弗炉自然降温后即得到黄色块状粉末g-C3N4;
⑵Fe5C2@NG催化剂的制备:
取上述制备的g-C3N4 0.1~0.3g,放到研钵里,并称取二茂铁固体0.1~0.3g也放入研钵中,经研磨将固体混合均匀,然后将混合均匀的固体放入石英罐中,并用盖子盖紧,随后将石英罐放入到管式炉里煅烧,煅烧气氛为N2,煅烧温度为700~900℃,升温时间为1~3小时,保温时间为1~3小时,将产物分散到H2SO4溶液中,在室温中浸泡6~18小时,随后用蒸馏水和无水乙醇分别洗涤3次,60℃干燥箱中烘干,最后对用H2SO4处理过的产物进行二次煅烧,煅烧气氛为N2,煅烧温度为700~900℃,升温时间为1~3小时,保温时间为1~3小时。
在所述的一种制备N掺杂石墨烯包裹碳化铁电催化剂的方法中,在步骤⑵中所述的H2SO4其浓度为0.5~1.5M。
采用本发明所制备的Fe5C2@NG催化剂,具有产品成本低、易控制、重复性好、可大规模生产等特点。
附图说明
图1是荷兰飞利浦公司PW3040/60型X-射线衍射仪所测的实施例1中制备的g-C3N4以及实施例2中制备的Fe5C2@NG催化剂的X-射线衍射图,其中:横坐标X是衍射角度(2θ),纵坐标Y是相对衍射强度。
图2是日本日立公司S-4800型场发射扫描电子显微镜(FE-SEM)观测实施例2中制备的Fe5C2@NG催化剂的形貌图。
图3是日本电子株式会社JEM-2100F型透射电子显微镜(TEM)观测到的实施例2中制备的Fe5C2@NG催化剂内部结构像。
图4是是日本岛津Kratos AXIS Ultra DLD型X射线光电子能谱仪(XPS)测试得到的实施例2中制备的Fe5C2@NG催化剂的元素。
图5是美国Pine公司Gamry Instruments RDE710型旋转圆盘以及MetrohmPGSTAT101双恒电位仪测试Fe5C2@NG催化剂和商业化Pt/C电化学性能得到的线性伏安图。
图6是美国Pine公司Gamry Instruments RDE710型旋转圆盘以及MetrohmPGSTAT101双恒电位仪测试Fe5C2@NG催化剂和商业化Pt/C电化学性能得到的循环伏安图。
具体实施方式
下面通过实施例对本发明中Fe5C2@NG催化剂的制备方法做出进一步的具体说明。
实施例1
称取10g三聚氰胺,放到坩埚中,并将坩埚用盖子盖紧,然后将坩埚放入马弗炉里煅烧,煅烧温度为550℃,升温时间为2小时,保温时间为2小时,等马弗炉自然降温后即可得到黄色块状粉末g-C3N4。
取上述制备的g-C3N4 0.2g,放到研钵里,然后二茂铁固体0.2g也放入研钵中,经过一段时间的研磨将固体混合均匀,然后将混合均匀的固体放入石英罐中,并用盖子盖紧,随后将石英罐放入到管式炉里煅烧,煅烧气氛为N2,煅烧温度为700℃,升温时间为70分钟,保温时间为2小时,等管式炉自然降温后得到黑色的固体,将所得产物分散到1M的H2SO4溶液中,放在室温中浸泡12小时,随后用蒸馏水和无水乙醇分别洗涤3次,60℃干燥箱中烘干。最后对用H2SO4处理过的产物进行二次煅烧,煅烧气氛为N2,煅烧温度为700℃,升温时间为70分钟,保温时间为2小时,即可得到Fe5C2@NG-700(700指煅烧温度)催化剂。
实施例2
取上述制备的g-C3N4 0.2g,放到研钵里,然后二茂铁固体0.2g也放入研钵中,经过一段时间的研磨将固体混合均匀,然后将混合均匀的固体放入石英罐中,并用盖子盖紧,随后将石英罐放入到管式炉里煅烧,煅烧气氛为N2,煅烧温度为800℃,升温时间为70分钟,保温时间为2小时,等管式炉自然降温后得到黑色的固体,将所得产物分散到1M的H2SO4溶液中,放在室温中浸泡12小时,随后用蒸馏水和无水乙醇分别洗涤3次,60℃干燥箱中烘干。最后对用H2SO4处理过的产物进行二次煅烧,煅烧气氛为N2,煅烧温度为800℃,升温时间为80分钟,保温时间为2小时,即可得到Fe5C2@NG-800催化剂。
对于本实施例中制备的g-C3N4,Fe5C2@NG-800催化剂做X-射线衍射分析,结果如图1所示,其横坐标X是衍射角度(2θ),纵坐标Y是相对衍射强度,图中C3N4在27.5°的衍射峰与其层之间的堆积距离为0.326nm相符,该峰的指标为(002),Fe5C2@NG催化剂在26.1°处的射峰是碳的(002)面,而其他的峰则可指标化为(021)(-402)(312)等晶面,与国际标准粉末XRD衍射卡片中的JCPDS,20-0508相一致。
对于本实施例中制备的Fe5C2@NG-800催化剂做场发射扫描电镜分析,得到的电镜照片如图2所示,可以看出产物为片状结构。并且对该产物做透射电镜分析,得到的电镜照片如图3所示,从图3中可以看到,产物主要是石墨烯包裹纳米Fe5C2颗粒的薄片,并且纳米颗粒分散均匀。并且对本实施例中的产品做XPS分析,分析结果如图4所示,从图中可以看出我们制备的物质含有Fe,N,C,O等元素。
对于本实施例中制备的Fe5C2@NG-800催化剂做线性伏安分析以及循环伏安分析,得到的分析结果如图5(线性伏安)和图6(循环伏安)所示,可以看出在氧气饱和的电解液中我们制备得到的的Fe5C2@NG-800催化剂的氧还原性能与商业化的Pt/C有相似的性能,具有良好的应用前景。
实施例3
取上述制备的g-C3N4 0.2g,放到研钵里,然后二茂铁固体0.2g也放入研钵中,经过一段时间的研磨将固体混合均匀,然后将混合均匀的固体放入石英罐中,并用盖子盖紧,随后将石英罐放入到管式炉里煅烧,煅烧气氛为N2,煅烧温度为900℃,升温时间为90分钟,保温时间为2小时,等管式炉自然降温后得到黑色的固体,将所得产物分散到1M的H2SO4溶液中,放在室温中浸泡12小时,随后用蒸馏水和无水乙醇分别洗涤3次,60℃干燥箱中烘干。最后对用H2SO4处理过的产物进行二次煅烧,煅烧气氛为N2,煅烧温度为900℃,升温时间为90分钟,保温时间为2小时,即可得到Fe5C2@NG-900催化剂。
Claims (2)
1.一种制备N掺杂石墨烯包裹碳化铁电催化剂的方法,其特征在于以g-C3N4为碳源和氮源,二茂铁为铁源,通过管式炉高温煅烧得到相应的N掺杂石墨烯包裹碳化铁纳米复合物(Fe5C2@NG),其特征在于制备Fe5C2@NG的方法包括以下步骤:
⑴g-C3N4的制备:
称取5~15g三聚氰胺,放到坩埚中,并将坩埚用盖子盖住,然后将坩埚放入马弗炉里煅烧,煅烧温度为450~650℃,升温时间为1~3小时,保温时间为1~3小时,等马弗炉自然降温后即得到黄色块状粉末g-C3N4;
⑵Fe5C2@NG催化剂的制备:
取上述制备的g-C3N4 0.1~0.3g,放到研钵里,并称取二茂铁固体0.1~0.3g也放入研钵中,经研磨将固体混合均匀,然后将混合均匀的固体放入石英罐中,并用盖子盖紧,随后将石英罐放入到管式炉里煅烧,煅烧气氛为N2,煅烧温度为700~900℃,升温时间为1~3小时,保温时间为1~3小时,将产物分散到H2SO4溶液中,在室温中浸泡6~18小时,随后用蒸馏水和无水乙醇分别洗涤3次,60℃干燥箱中烘干,最后对用H2SO4处理过的产物进行二次煅烧,煅烧气氛为N2,煅烧温度为700~900℃,升温时间为1~3小时,保温时间为1~3小时。
2.根据权利要求1所述的一种制备N掺杂石墨烯包裹碳化铁电催化剂的方法,其特征在于步骤⑵中所述的H2SO4,其浓度为0.5~1.5M。
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