CN105833858B - 一种二维碳膜包覆海胆状二氧化钛复合材料的制备方法 - Google Patents
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Abstract
本发明公开了一种二维碳膜包覆海胆状二氧化钛复合材料的制备方法，属于无机功能材料制备技术领域。其制备方法是通过一种两相界面的溶剂热方法，下层为酸催化剂水相溶液，上层为含有含碳有机物小分子和钛源的油相溶液，在油相和水相界面间自组装合成产物，经过过滤，水洗，干燥制得二维碳膜包覆海胆状二氧化钛复合材料。本发明的优点在于：1)在较低温度下(<200℃)通过两相界面法，在油相和水相界面间一步自组装合成二维碳膜包覆海胆状二氧化钛复合材料；2)用本发明提供的方法制备的合成二维碳膜包覆海胆状二氧化钛复合材料，海胆状二氧化钛的粒径均一，且碳膜包覆层为超薄碳膜。3)用本发明提供的方法条件温和、反应工艺简单、流程短，适合工业化生产。
Description
技术领域
本发明属于无机功能材料制备技术领域，特别涉及一种二维碳膜包覆海胆状二氧化钛复合材料的方法。
背景技术
二氧化钛作为一种典型氧化物材料，其光催化活性高，充放电电压高，无毒，稳定性和安全性好，在光催化、锂离子电池、超级电容器等领域有着重要的应用前景。由于材料的结构和形貌对其性能有很大影响，在微纳米尺度上构筑特殊形貌和结构，如科学家们已通过构筑多种特殊形貌的二氧化钛，如海胆状、空心球等大比表面积多级结构，提升了二氧化钛的光催化剂电化学性能。
除了通过在微纳米尺度构筑特殊形貌和结构来提升材料性能外，通过与功能材料复合进一步提升二氧化钛的性能成为今年来的研究热点。通过与碳材料复合可以有效提升二氧化钛的光催化和电化学性能。碳-二氧化钛复合材料不仅能够有效抑制电子-空穴复合，拓展光响应区间，又能赋予二氧化钛优异的吸附能力，大大提升二氧化钛的分散性。此外，由于碳材料具有高强度、热膨胀系数小、低电阻率、低密度等优越性能，碳-二氧化钛复合材料具有优异的导电性、锂离子传输性能及良好的循环寿命。通过制备碳包覆二氧化钛复合材料还可以有效改善二氧化钛粒子的分散性，进一步提升其性能。
综上所述，开发一种条件温和、工艺简单的以方法合成碳包覆二氧化钛复合材料具有重要的科学意义和实用价值，而现有的专利中也并没有通过一步法制备二维碳膜包覆海胆状二氧化钛复合材料的报道。
发明内容
本发明的目的在于提出一种条件温和、工艺简单易行、实验流程短的二维碳膜包覆海胆状二氧化钛复合材料的方法。通过一种两相界面的溶剂热方法，下层为酸催化剂水相溶液，上层为含有含碳有机物小分子和钛源的油相溶液，在油相和水相界面间自组装合成二维碳膜包覆海胆状二氧化钛复合材料，该过程简单、易控、高效，并且在密闭体系中可以有效地防止有毒物质的挥发。
本发明的技术方案是：首先将0.1～0.6g P123加入到5～60mL含碳有机物小分子中，在30～80℃搅拌1～3h后，加入0.1～10mmol钛源，继续在30～80℃搅拌1～3h，得到澄清的混合溶液(记为溶液A)。然后将上述混合溶液缓慢加入到含有1～20mL酸溶液(记为溶液B)中的反应釜，两种溶液在反应釜中出现分层现象，上层溶液为密度较大的溶液A，下层溶液为密度较小的溶液B。将反应釜密封，缓慢放入到120～200℃的烘箱中反应12～48h。当反应釜冷却到室温后，在溶液A和溶液B的两相界面间得到了产物。经过过滤，水洗，干燥制得二维碳膜包覆海胆状二氧化钛复合材料。
所述的含碳有机物小分子为正己烷、环己烷、甲苯、苯、二甲苯中的一种或两种以上。
所述的钛源为钛酸四丁脂、异丙醇钛、四氯化钛、三氯化钛中的一种或两种以上。
所述的酸溶液为盐酸或硫酸溶液中的一种。
本发明的优点在于：1)在较低温度下(<200℃)通过两相界面法，在油相和水相界面间一步自组装合成二维碳膜包覆海胆状二氧化钛复合材料；2)用本发明提供的方法制备的合成二维碳膜包覆海胆状二氧化钛复合材料，海胆状二氧化钛的粒径均一，且碳膜包覆层为超薄碳膜。3)用本发明提供的方法条件温和、反应工艺简单、流程短，适合工业化生产。
附图说明
图1为本发明实施案例1得到的超薄二维碳纳米材料的扫描电镜照片。
图2为本发明实施案例1得到的超薄二维碳纳米材料的XRD图。
具体实施方式
下面结合具体的实施方式对本发明的技术方案做进一步说明。
实施案例1
首先将0.2g P123加入到10mL环己烷中，在60℃搅拌2h后，加入0.6mmol钛酸四丁脂，继续在60℃搅拌2h，得到澄清的混合溶液(记为溶液A)。然后将上述混合溶液缓慢加入到含有5mL酸溶液(记为溶液B)中的反应釜，两种溶液在反应釜中出现分层现象，上层溶液为密度较大的溶液A，下层溶液为密度较小的溶液B。将反应釜密封，缓慢放入到160℃的烘箱中反应20h。当反应釜冷却到室温后，在溶液A和溶液B的两相界面间得到了产物。经过过滤，水洗，干燥制得二维碳膜包覆海胆状二氧化钛复合材料。产物的扫描电镜照片和XRD图如图1-2所示。
实施案例3
首先将0.2g P123加入到10mL环己烷中，在60℃搅拌2h后，加入0.6mmol异丙醇钛，继续在60℃搅拌2h，得到澄清的混合溶液(记为溶液A)。然后将上述混合溶液缓慢加入到含有5mL酸溶液(记为溶液B)中的反应釜，两种溶液在反应釜中出现分层现象，上层溶液为密度较大的溶液A，下层溶液为密度较小的溶液B。将反应釜密封，缓慢放入到160℃的烘箱中反应20h。当反应釜冷却到室温后，在溶液A和溶液B的两相界面间得到了产物。经过过滤，水洗，干燥制得二维碳膜包覆海胆状二氧化钛复合材料。
实施案例3
首先将0.1g P123加入到10mL正己烷中，在40℃搅拌2h后，加入1mmol钛酸四丁脂，继续在40℃搅拌2h，得到澄清的混合溶液(记为溶液A)。然后将上述混合溶液缓慢加入到含有5mL酸溶液(记为溶液B)中的反应釜，两种溶液在反应釜中出现分层现象，上层溶液为密度较大的溶液A，下层溶液为密度较小的溶液B。将反应釜密封，缓慢放入到180℃的烘箱中反应20h。当反应釜冷却到室温后，在溶液A和溶液B的两相界面间得到了产物。经过过滤，水洗，干燥制得二维碳膜包覆海胆状二氧化钛复合材料。
Claims (2)
1.一种二维碳膜包覆海胆状二氧化钛复合材料的制备方法，其特征在于首先将0.1～0.6g P123加入到5～60mL含碳有机物小分子中，在30～80℃搅拌1～3h后，加入0.1～10mmol钛源，继续在30～80℃搅拌1～3h，得到澄清的混合溶液A；然后将上述混合溶液A缓慢加入到含有1～20mL酸溶液B中的反应釜，两种溶液在反应釜中出现分层现象，上层溶液为密度较大的混合溶液A，下层溶液为密度较小的酸溶液B；将反应釜密封，缓慢放入到120～200℃的烘箱中反应12～48h；当反应釜冷却到室温后，在混合溶液A和酸溶液B的两相界面间得到了产物；经过过滤，水洗，干燥制得二维碳膜包覆海胆状二氧化钛复合材料；
所述的含碳有机物小分子为正己烷、环己烷、甲苯、苯、二甲苯中的一种或两种以上；
所述的酸溶液为盐酸或硫酸溶液中的一种。
2.如权利要求书1所述的一种二维碳膜包覆海胆状二氧化钛复合材料的制备方法，其特征在于所述的钛源为钛酸四丁脂、异丙醇钛、四氯化钛、三氯化钛中的一种或两种以上。
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