CN113213452B - 一种碳纳米管构成的三维有序大孔炭材料及其制备方法 - Google Patents

一种碳纳米管构成的三维有序大孔炭材料及其制备方法 Download PDF

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CN113213452B
CN113213452B CN202110658668.5A CN202110658668A CN113213452B CN 113213452 B CN113213452 B CN 113213452B CN 202110658668 A CN202110658668 A CN 202110658668A CN 113213452 B CN113213452 B CN 113213452B
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吉科猛
王疆
刘召召
刘心宇
吴梦倩
朱敏杰
陈明鸣
王成扬
刘帅
杜晓辉
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Abstract

一种碳纳米管构成的三维有序大孔炭材料及其制备方法，属于碳材料领域。本发明提供的由碳纳米管构成的三维有序大孔炭材料是利用硝酸镍溶液填充聚甲基丙烯酸甲酯微球模板，经在常压、惰性气氛中煅烧碳化，得到兼具碳纳米管一维结构和宏观三维有序大孔结构的纳米多孔炭材料。该材料宏观上具有三维双连续的有序蜂巢网络结构，大孔孔径分布均一，孔壁则由原位生成的、直径为亚纳米级别的碳纳米管交织构成。本发明所提供的材料制备方法简单，成本低廉，为所发明的上述新型炭材料的广泛功能化应用奠定了实用基础。

Description

一种碳纳米管构成的三维有序大孔炭材料及其制备方法
技术领域
本发明涉及一种碳纳米管构成的三维有序大孔炭材料及其制备方法，属于碳材料技术领域。
背景技术
多孔材料因其大的比表面积、高孔容和拓扑特性等特点，广泛应用于能量转换与储存、催化、传感等诸多领域。其中，多孔碳材料有高的比表面积之外，还具有优良的导电性和结构稳定性，已成为构建多种纳米复合材料的基础。近年来，很多新型的纳米多孔碳材料，如碳纳米管、有序介孔碳、三维大孔碳、多级孔碳等，已被成功制备并展现出优异的应用价值。三维有序大孔(3DOM)碳材料不仅具有通常多孔碳材料的一般特点，如比表面积大、导电性高等性质，而且还具有孔结构排列周期性强、孔尺寸均匀及整体结构三维有序等特点，在催化剂载体、电极材料及吸附净化等领域具有广阔的应用前景。纳米材料的可控合成和有效组装是纳米材料实用化的前提和保障。至今为止，尚无文献和专利报道过兼具碳纳米管一维结构和3DOM结构的纳米多孔炭材料及其制备方法。
发明内容
本发明的目的在于提供一种碳纳米管构成的3DOM炭材料及其制备方法。该材料制备过程简单，能够合成兼具碳纳米管一维结构和3DOM结构的纳米多孔炭材料，成本低廉、宏观结构规则有序。
一种碳纳米管构成的3DOM炭材料，其特征在于，该3DOM炭材料包括碳纳米管相互搭接形成具有3DOM结构的蜂巢网络结构，其中有序大孔的直径为270～360nm，纳米管的外径为8～20nm。
其中所述的炭材料是碳和其他物质的复合材料，而碳指的是纯碳。炭材料是碳和镍的复合。
本发明提供了一种碳纳米管构成的3DOM炭材料的制备方法，主要步骤包括：(1)将硝酸镍和柠檬酸固体粉末溶于去离子水溶液中，搅拌均匀作为前驱液，取排列规整的聚甲基丙烯酸甲酯PMMA微球构成的模板，浸渍到所述前驱液中，经真空抽滤、室温干燥后，得到前驱物；(2)将步骤(1)所得的前驱物置于管式炉中，在常压惰性气氛下煅烧进行碳化，即得到主要由碳纳米管构成的3DOM炭材料。
本发明优选的、所述硝酸镍和柠檬酸的摩尔比为2:1，硝酸镍和柠檬酸的浓度可根据需要调整，如采用硝酸镍的浓度为2mol/L、柠檬酸的浓度为1mol/L。
所述浸渍条件为室温下浸渍时间优选4h。
所述惰性气氛为氩气，所述煅烧碳化温度优选450～1000℃，反应时间为60min，从室温升至目标温度，升温速率为10℃/min，压力为常压，煅烧结束后自然降温。在本发明的一些实施例中，所述煅烧温度为450℃、600℃和1000℃。随着焙烧温度的升高，目标材料中金属镍组分的结晶度变强，纳米颗粒增大。另外，该金属镍组分可根据应用需要，用酸性试剂方便地进行刻蚀去除，得到碳纳米管构成的3DOM碳材料。
本发明提供的制备方法具有以下有益效果：
本发明提供的由碳纳米管构成的3DOM炭材料的制备方法，经过浸渍、惰性气氛煅烧等简单操作，即可得到兼具碳纳米管一维结构和3DOM结构的纳米多孔炭材料，其具有的三维双连续的蜂巢网络结构，孔径分布均一且高度有序，这些形貌结构特征为该材料后续的多功能化应用提供了基础。
利用D8-Focus型X射线衍射仪(XRD)、Regulus 8100型扫描电子显微镜(SEM)、JEMF200型高分辨电子投射显微镜(TEM)和LabRam HR Evolution型拉曼光谱仪(Raman)等仪器测定所得碳纳米管构成的3DOM炭材料的晶体结构、形貌、化学组分等物理性质。
附图说明
为了更清楚地说明本发明实施例，下面将对实施例描述中所需要使用的附图作简单地介绍。
图1是实施例1-3在不同煅烧温度下所制得的由碳纳米管构成3DOM炭材料的(a)XRD谱图、(b)Raman谱图，其中图(a)中的(I–III)和(b)中的(I–III)分别对应于450℃、600℃和1000℃温度下制备的样品。
图2是实施例1中于450℃制备的由碳纳米管构成的3DOM炭材料的SEM图(对应(a)–(c))、TEM图(对应(d)–(f))。
图3是实施例2中于600℃制备的由碳纳米管构成的3DOM炭材料的SEM图。
图4是实施例3中于1000℃制备的由碳纳米管构成的3DOM炭的SEM图。
具体实施方式
下面结合实施例对本发明做进一步地说明，但本发明并不限于以下实施例。
实施例1
将聚甲基丙烯酸甲酯PMMA微球模板于2mol/L的Ni(NO3)2·6H2O、1mol/L的柠檬酸和去离子水的混合溶液中浸渍4h，经真空抽滤和自然干燥后，将所得的固体物质置于流速为200sccm的氩气气氛中焙烧，从室温以10℃/min的速率升至450℃保持60min，自然降至室温，即得到由碳纳米管与金属镍纳米晶组装成的3DOM炭材料。具体地，该材料具有3DOM结构，孔壁由大量包裹单个Ni纳米晶的一维碳纳米管交织构成，Ni的晶粒尺寸为2～3nm，石墨化碳的层间距为0.34nm，3DOM结构的一级和二级孔径(即大孔的直径和联通大孔之间的窗口大小)分别为340～360nm和100～140nm，纳米管的外径为8～20nm，内径为2～5nm。
实施例2
将PMMA微球模板于2mol/L的Ni(NO3)2·6H2O、1mol/L的柠檬酸和去离子水的混合溶液中浸渍4h，经真空抽滤和自然干燥后，将所得的固体物质置于流速为200sccm的氩气气氛中焙烧，从室温以10℃/min的速率升至600℃保持60min，自然降至室温，即得到由碳纳米管与金属镍纳米晶组装成的3DOM炭材料。具体地，该材料具有3DOM结构，孔壁由大量包裹单个Ni纳米晶的一维碳纳米管交织构成，Ni的晶粒尺寸为3～4nm，石墨化碳的层间距为0.34nm，3DOM结构的一级和二级孔径分别为270～330nm和100～140nm，纳米管的直径为8～20nm。
实施例3
将PMMA微球模板于2mol/L的Ni(NO3)2·6H2O、1mol/L的柠檬酸和去离子水的混合溶液中浸渍4h，经真空抽滤和自然干燥后，将所得的固体物质置于流速为200sccm的氩气气氛中焙烧，从室温以10℃/min的速率升至1000℃保持60min，自然降至室温，即得到由碳纳米管与金属镍纳米晶组装成的3DOM炭材料。具体地，该材料具有3DOM结构，孔壁由大量包裹单个Ni纳米晶的一维碳纳米管交织构成，Ni的晶粒尺寸为22～27nm，石墨化碳的层间距为0.34nm，表面的纳米管近似成绒毛状，3DOM结构的一级和二级孔径分别为320～350nm和100～140nm。

Claims (6)

1.一种碳纳米管构成的3DOM炭材料，其特征在于，该3DOM炭材料为碳纳米管相互搭接形成具有3DOM结构的蜂巢网络结构，孔壁由大量包裹单个Ni纳米晶的一维碳纳米管交织构成，Ni的晶粒尺寸为2~4 nm，石墨化碳的层间距为0.34 nm，有序大孔的直径为270~360 nm，碳纳米管的外径为8~20 nm，内径为2~5 nm；炭材料是碳和镍的复合，碳指的是纯碳；
所述3DOM炭材料的制备方法包括以下步骤：
(1) 将硝酸镍和柠檬酸固体粉末溶于去离子水溶液中，搅拌均匀作为前驱液，取排列规整的聚甲基丙烯酸甲酯PMMA微球构成的模板，浸渍到所述前驱液中，经真空抽滤、室温干燥后，得到前驱物；(2) 将步骤(1)所得的前驱物置于管式炉中，在常压惰性气氛下煅烧进行碳化，即得到由碳纳米管构成的3DOM炭材料；所述惰性气氛为氩气，所述煅烧碳化温度为450~1000 ℃，反应时间为60 min，从室温升至目标温度，升温速率为10 ℃/min，压力为常压，煅烧结束后自然降温；
所述的硝酸镍和柠檬酸的摩尔比为2:1。
2.一种权利要求1所述的碳纳米管构成的3DOM炭材料的制备方法，其特征在于，包括如下步骤：(1) 将硝酸镍和柠檬酸固体粉末溶于去离子水溶液中，搅拌均匀作为前驱液，取排列规整的聚甲基丙烯酸甲酯PMMA微球构成的模板，浸渍到所述前驱液中，经真空抽滤、室温干燥后，得到前驱物；(2) 将步骤(1)所得的前驱物置于管式炉中，在常压惰性气氛下煅烧进行碳化，即得到由碳纳米管构成的3DOM炭材料；所述惰性气氛为氩气，所述煅烧碳化温度为450~1000 ℃，反应时间为60 min，从室温升至目标温度，升温速率为10 ℃/min，压力为常压，煅烧结束后自然降温。
3.按照权利要求2所述的方法，其特征在于，采用硝酸镍的浓度为2 mol/L、柠檬酸的浓度为1 mol/L。
4.按照权利要求2所述的方法，其特征在于，所述浸渍条件为室温下浸渍4 h。
5.按照权利要求2所述的方法，其特征在于，随着焙烧温度的升高，目标材料中金属镍组分的结晶度变强，纳米颗粒增大。
6.按照权利要求2所述的方法，其特征在于，该金属镍组分根据应用需要，用酸性试剂进行刻蚀去除，得到碳纳米管构成的3DOM碳材料。
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