CN107055516B - 一种石墨烯/二氧化锡量子点复合材料的制备方法 - Google Patents
一种石墨烯/二氧化锡量子点复合材料的制备方法 Download PDFInfo
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Abstract
本发明属于石墨烯‑金属氧化物复合材料制备技术领域，提交一种石墨烯/二氧化锡量子点复合材料的制备方法，室温下，将氧化石墨烯与四氯化锡溶入去离子水中后，加入水合肼，搅拌均匀后得到分散液，将分散液进行微波水热反应，产物清洗后得到石墨烯/二氧化锡量子点复合材料，制备得到的石墨烯/二氧化锡量子点复合材料能够应用于锂离子电池作负极材料。本发明的有益效果为，利用微波水热法，一步实现氧化石墨烯的还原与复合材料的制备，操作简单，制备迅速，有效避免氧化石墨烯的二次还原；二氧化锡量子点可以有效地避免石墨烯的二次堆积；二氧化锡量子点原位生长在石墨烯片上，能够提高复合材料的电学性质。
Description
技术领域
本发明涉及一种石墨烯/二氧化锡量子点复合材料的快速制备方法，属于石墨烯-金属氧化物复合材料制备技术领域。
背景技术
石墨烯是一种二维的碳材料，其具有优异的电荷传导性、良好的导热性、出色的力学性质与很大的比表面积，在很多领域表现出了极大的应用前景。二氧化锡是一种多功能的半导体氧化物材料，在气体传感，储能，光催化以及锂离子电池等方面受到广泛的关注。二氧化锡量子点比表面积高，具有尺寸效应和量子隧道效应，其性能相比宏观材料有很大提高。但是，单纯的量子点容易发生团聚，使材料的性能降低，大大限制了其应用。将石墨烯作为载体与二氧化锡纳米颗粒进行复合，这不仅可以抑制二氧化锡量子点的团聚，更会由于复合材料的协同效应而改善二氧化锡量子点在各个领域的应用效果。
目前，制备石墨烯-金属氧化物复合材料的方法有很多，但是有的方法过于繁琐，有的方法无法控制产物的形貌，还有的方法合成的复合材料不够均匀。本发明采用微波水热法，通过一步法制备了石墨烯/二氧化锡量子点复合材料。对材料的表征表明，二氧化锡颗粒的尺寸为2-3纳米，均匀分布在石墨烯片表面，具有很好的潜在应用。
发明内容
以利用复合材料的协同效应来改善材料特性出发，设计一种石墨烯/二氧化锡量子点复合材料的制备方法，该方法具有操作简单，制备快速，重复性良好等特点。
本发明采用以下技术方案：
一种石墨烯/二氧化锡量子点复合材料的制备方法，具体包括以下步骤：
1)室温下，将氧化石墨烯与四氯化锡按质量比为1:10～200溶入去离子水中，混合均匀得到混合溶液。
2)室温下，在混合溶液中加入水合肼，搅拌均匀后得到分散液。所述的氧化石墨烯与水合肼的质量比为1:20-100。
3)将分散液进行微波水热反应，所得的产物用清洗剂清洗后得到石墨烯/二氧化锡量子点复合材料，二氧化锡量子点尺寸均一，且均匀分布在石墨烯片的两侧。所述的微波水热反应温度为120-180℃，反应时间为5-120分钟；所述的清洗剂为去离子水、乙醇或二者混合溶液。
制备得到的石墨烯/二氧化锡量子点复合材料能够应用于锂离子电池作负极材料。
本发明的有益效果：本发明利用微波水热法，一步实现氧化石墨烯的还原与复合材料的制备，操作简单，制备迅速，有效避免了氧化石墨烯的二次还原；本方法制备的二氧化锡量子点尺寸较为均一，均匀分布在石墨烯片的两侧；二氧化锡量子点可以有效地避免石墨烯的二次堆积，与此同时，石墨烯又对二氧化锡量子点有固定作用，可以防止二氧化锡的团聚；二氧化锡量子点原位生长在石墨烯片上，接触良好，有利于二者的载流子交换，提高复合材料的电学性质；石墨烯/二氧化锡量子点复合材料结合了二者的优良性质，可以产生协同作用。因此，本发明制备的复合材料在传感器及锂离子电池等领域具有良好的应用前景。
附图说明
图1为石墨烯/二氧化锡量子点复合材料的X射线衍射谱图。
图2为石墨烯/二氧化锡量子点复合材料的透射电子显微镜图。
图3为石墨烯/二氧化锡量子点复合材料的制备机理示意图。
具体实施方式
下面结合附图对本发明的具体实施方式做进一步的陈述，根据以下实施例可以更好的理解本发明。
一种石墨烯/二氧化锡量子点复合材料的快速制备方法，具体步骤为：
将一定量氧化石墨烯超声分散于去离子水中；加入一定量的四氯化锡，混合均匀；加入一定量的水合肼，搅拌混合；将得到的液体转移到微波消解仪中进行微波水热反应便得到石墨烯/二氧化锡量子点复合材料。
实施例1
将10mg氧化石墨烯超声分散在50mL去离子水中；加入700mg SnCl4·H2O，搅拌10min；加入0.5mL浓度为80％的水合肼，继续搅拌10分钟；将上述溶液转入聚四氟乙烯内衬中，置于微波消解系统中进行反应，反应温度140℃，时间为60min。将产物离心收集并利用去离子水与乙醇多次清洗，得到石墨烯/二氧化锡量子点复合材料。
对产物进行X射线衍射图谱表征，结果如图1所示，可以看出谱图上所有的衍射峰均对应于四方相的二氧化锡，其JCPDS卡片编号为41-1445。从谱图上我们并没有观察到明显的石墨烯的衍射峰，这是由于石墨烯在复合材料中的含量较少且其衍射峰强度较低。
对产物进行透射电子显微镜表征，结果如图2所示，可以看出，二氧化锡的尺寸约为3nm，均匀分布在石墨烯片表面。
产物的形成机理示意图如图3所示，其形成机理如下：氧化石墨烯含有大量的带负电的含氧基团，如羧基、羟基等，当锡离子加入后，由于静电作用，锡离子将会和带负电的官能团结合。在微波水热的过程中，氧化石墨烯被还原成石墨烯，与此同时，二氧化锡量子点原位生长在石墨烯片上，最终得到石墨烯/二氧化锡量子点复合材料。
实施例2
将50mg氧化石墨烯超声分散在50mL去离子水中；向上述分散液中加入500mgSnCl4·H2O，搅拌10min；向得到的溶液中加入1mL浓度为80％的水合肼，继续搅拌10分钟；将上述溶液转入容积为100mL的聚四氟乙烯内衬中，置于微波消解系统中进行反应，反应温度160℃，时间为20min。
将产物离心收集并利用去离子水与乙醇多次清洗，得到石墨烯/二氧化锡量子点复合材料，其形貌与结构与实施例1类似。
除了上面的实施例子，还进行了其他实验，所得材料的形貌与结构也与实施例子类似，其中氧化石墨烯与水合肼的质量比为1:100、1:80及1:30；氧化石墨烯与四氯化锡的质量比为1:200、1:100及1:30；微波水热反应温度为120℃及180℃；微波水热反应时间为5min、90min及120min。
Claims (2)
1.一种石墨烯/二氧化锡量子点复合材料的制备方法，其特征在于，以下步骤：
1)室温下，将氧化石墨烯与四氯化锡溶入去离子水中，混合均匀得到混合溶液；所述的氧化石墨烯与四氯化锡按质量比为1:10～200；
2)室温下，在混合溶液中加入水合肼，搅拌均匀后得到分散液；所述的氧化石墨烯与水合肼的质量比为1:20-100；
3)将分散液进行微波水热反应5-120分钟，所得的产物用清洗剂清洗后得到石墨烯/二氧化锡量子点复合材料，二氧化锡量子点尺寸均一，且均匀分布在石墨烯片的两侧；所述的微波水热反应温度为120-180℃。
2.根据权利要求1所述的一种石墨烯/二氧化锡量子点复合材料的制备方法，其特征在于，所述的清洗剂为去离子水、乙醇或二者混合溶液。
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