CN101723313A - 一种制备纳米二氧化钛/碳纳米管复合材料的方法 - Google Patents
一种制备纳米二氧化钛/碳纳米管复合材料的方法 Download PDFInfo
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Abstract
本发明公开了一种纳米二氧化钛/碳纳米管复合材料的制备方法，其步骤为：取无机钛盐、碱金属碳酸盐、碳纳米管和去离子水加入到球磨罐中；在球磨罐中球磨充分混合反应；将混合反应后的产物在450～700℃，惰性气体保护下，退火至少1小时；将退火后的粉末水洗过滤，干燥研碎，得纳米二氧化钛/碳纳米管复合材料。本发明制备方法简单，成本低，产量高，易于工业化生产。制得的复合材料可望在传感器、催化剂和光电电池等领域广泛应用。
Description
技术领域
本发明涉及一种制备纳米二氧化钛/碳纳米管复合材料的方法，尤其是采用高能球磨制备纳米二氧化钛/碳纳米管复合材料的方法。
背景技术
碳纳米管(Cnts)具有的优异的机械、热学和电学性能，一直是国内外材料科学研究的热点。在碳纳米管表面接上具有某些碳纳米管本身不具备的性质的有机、无机或生物官能团，而可以大大拓展碳纳米管的应用领域。比如碳纳米管较大的比表面积和多孔结构，使其成为催化剂载体有力竞争者。最近，更发现碳纳米管具有选择性吸附一些有机物污染物的特性，例如，碳纳米管的吸附持久性有机污染物二恶英类的能力比目前工业用的活性炭吸附极强1030倍以上。近年来，在碳纳米管表面包覆一维纳米半导体晶成为研究的热门领域。TiO2作为一种宽禁带半导体，具有湿敏、光催化等功能，可以用于传感器、光分解水和光降解有机物以及太阳能电池等，锐钛矿型TiO2纳米粉体在光催化降解有机物方面性能更加突出。结合二者优点，制备氧化钛/碳纳米管复合材料可望应用领域十分广泛，如传感器、催化剂和光电电池等领域。目前已经有采用溶胶凝胶、溶剂热、沉淀法等方法制备二氧化钛/碳纳米管复合物。然而，采用这些方法，不但会用到一些有毒的溶剂、原料，且步骤也相对复杂。
发明内容
本发明的目的是提供一种方法简单、成本低廉、不需要有机溶剂、易于工业化的制备纳米二氧化钛/碳纳米管复合材料的方法。
本发明的制备纳米二氧化钛/碳纳米管复合材料的方法，采用的是高能球磨法，步骤如下：
1)取无机钛盐、碱金属碳酸盐、碳纳米管和去离子水加入到球磨罐中，其中，无机钛盐与碱金属碳酸盐的摩尔比为1∶1～1∶4，无机钛盐与碳纳米管的摩尔比为15∶1～15∶30，无机钛盐与去离子水的摩尔比为1∶10～1∶30；
2)球磨罐中的球与料的质量比为10∶1～20∶1，在200～450转/分钟转速下球磨，充分混合反应；
3)将混合反应后的产物在450～700℃，惰性气体保护下，退火至少1小时；
4)将退火后的粉末水洗过滤，干燥研碎，得纳米二氧化钛/碳纳米管复合材料。
本发明中，所说的无机钛盐可以是硫酸钛或硫酸氧钛。所说的碱金属碳酸盐可以是碳酸钠、碳酸氢钠、碳酸钾、碳酸氢钾或碳酸锂。所说的惰性气体是氮气或氩气。球磨时，球磨罐中球料的总体积占球磨罐体积的1/4～2/3。
本发明的有益效果在于：
本发明提供的制备纳米二氧化钛/碳纳米管复合材料的方法，以钛盐为钛源，成本较低，而且制备方法简单、产量高、易于工业化生产。制得的复合材料可望在传感器、催化剂和光电电池等领域广泛应用。
附图说明
图1为纳米二氧化钛/碳纳米管复合材料的扫描电镜图(SEM)；
图2为纳米二氧化钛/碳纳米管复合材料的X射线衍射图(XRD)；
图3为纳米二氧化钛/碳纳米管复合材料的热失重分析图(TG％/DTG)；
具体实施方式
为了更好的理解本发明，下面结合具体实施例进一步阐明本发明的内容，但本发明不仅仅局限于下面的实施例。
实施例1：
1)按摩尔比Ti(SO4)2∶Na2CO3∶H2O∶Cnts为1∶1∶10∶2称量取所需原料，加入到250ml的球磨罐中；
2)球磨罐中的球与料的质量比为20∶1，在300转/分钟转速下球磨，充分混合反应；
3)将混合反应后的产物在600℃，氮气保护下，退火1小时；
4)将退火后的粉末水洗过滤，干燥研碎，得纳米二氧化钛/碳纳米管复合材料。图1为该实施例所制得的纳米二氧化钛/碳纳米管复合材料的扫描电镜图(SEM)。图2为其X射线衍射图(XRD)，说明其中的二氧化钛为锐钛矿结构，由于碳纳米管峰与锐钛矿二氧化钛(101)晶面峰重合，XRD中看不到碳纳米管的衍射峰，但从SEM图中很明显看出有碳纳米管。
实施例2：
1)按摩尔比Ti(SO4)2∶NaHCO3∶H2O∶Cnts为1∶4∶15∶1称量取所需原料，加入250ml的球磨罐中；
2)球磨罐中的球与料的质量比为10∶1，在450转/分钟转速下球磨，充分混合反应；
3)将混合反应后的产物在700℃，氮气保护下，退火1小时；
4)将退火后的粉末水洗过滤，干燥研碎，得纳米二氧化钛/碳纳米管复合材料。
实施例3：
1)按摩尔比TiOSO4∶Na2CO3∶H2O∶Cnts为1∶1∶20∶2称量取所需原料，加入5L的球磨罐中；
2)球磨罐中的球与料的质量比为15∶1，在300转/分钟转速下球磨，充分混合反应；
3)将混合反应后的产物在650℃，氮气保护下，退火2小时；
4)将退火后的粉末水洗过滤，干燥研碎，得纳米二氧化钛/碳纳米管复合材料。图3为所制备的复合材料的热失重分析图(TG％/DTG)，其中400℃到650℃之间的失重为碳纳米管氧化所致。
实施例4：
1)按摩尔比Ti(SO4)2∶KHCO3∶H2O∶Cnts为1∶4∶30∶0.5称量取所需原料，加入250ml的球磨罐中；
2)球磨罐中的球与料的质量比为15∶1，在200转/分钟转速下球磨，充分混合反应；
3)将混合反应后的产物在550℃，氮气保护下，退火3小时；
4)将退火后的粉末水洗过滤，干燥研碎，得纳米二氧化钛/碳纳米管复合材料。
实施例5：
1)按摩尔比TiOSO4∶KHCO3∶H2O∶Cnts为1∶2∶15∶0.07称量取所需原料，加入5L的球磨罐中；
2)球磨罐中的球与料的质量比为15∶1，在250转/分钟转速下球磨，充分混合反应；
3)将混合反应后的产物在550℃，氮气保护下，退火3小时；
4)将退火后的粉末水洗过滤，干燥研碎，得纳米二氧化钛/碳纳米管复合材料。
实施例6：
1)按摩尔比TiOSO4∶Li2CO3∶H2O∶Cnts为1∶1∶25∶1.5称量取所需原料，加入250ml的球磨罐中；
2)球磨罐中的球与料的质量比为15∶1，在250转/分钟转速下球磨，充分混合反应；
3)将混合反应后的产物在450℃，氩气保护下，退火6小时；
4)将退火后的粉末水洗过滤，干燥研碎，得纳米二氧化钛/碳纳米管复合材料。
Claims (5)
1.一种制备纳米二氧化钛/碳纳米管复合材料的方法，其特征在于包括如下步骤：
1)取无机钛盐、碱金属碳酸盐、碳纳米管和去离子水加入到球磨罐中，其中，无机钛盐与碱金属碳酸盐的摩尔比为1∶1～1∶4，无机钛盐与碳纳米管的摩尔比为15∶1～15∶30，无机钛盐与去离子水的摩尔比为1∶10～1∶30；
2)球磨罐中的球与料的质量比为10∶1～20∶1，在200～450转/分钟转速下球磨，充分混合反应；
3)将混合反应后的产物在450～700℃，惰性气体保护下，退火至少1小时；
4)将退火后的粉末水洗过滤，干燥研碎，得纳米二氧化钛/碳纳米管复合材料。
2.根据权利要求1所述的制备纳米二氧化钛/碳纳米管复合材料的方法，其特征在于：所说的无机钛盐是硫酸钛或硫酸氧钛。
3.根据权利要求1所述的制备纳米二氧化钛/碳纳米管复合材料的方法，其特征在于：所说的碱金属碳酸盐是碳酸钠、碳酸氢钠、碳酸钾、碳酸氢钾或碳酸锂。
4.根据权利要求1所述的制备纳米二氧化钛/碳纳米管复合材料的方法，其特征在于：球磨罐中球料的总体积占球磨罐体积的1/4～2/3。
5.根据权利要求1所述的制备纳米二氧化钛/碳纳米管复合材料的方法，其特征在于：所说的惰性气体是氮气或氩气。
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101983764A (zh) * | 2010-09-17 | 2011-03-09 | 东莞市可迪环保科技有限公司 | 大面积有序皮芯结构二氧化钛纳米管薄膜光催化剂的制备方法及其应用 |
| CN102628115A (zh) * | 2012-04-01 | 2012-08-08 | 昆明理工大学 | 一种碳纳米管增强铜基复合材料的制备方法 |
| CN103804877A (zh) * | 2014-02-19 | 2014-05-21 | 江南大学 | 具有导电和光转换储能功能的聚合物材料的制备方法 |
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| CN100396373C (zh) * | 2006-06-22 | 2008-06-25 | 厦门大学 | 一种碳纳米管/二氧化钛复合光催化剂的制备方法 |
| CN101157521B (zh) * | 2007-09-20 | 2011-05-04 | 复旦大学 | 可见光活性的纳米二氧化钛复合薄膜材料及其制备方法 |
| CN101347725B (zh) * | 2008-08-19 | 2010-12-08 | 武汉大学 | 碳纳米管/二氧化钛纳米复合光催化剂及其用途 |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101983764A (zh) * | 2010-09-17 | 2011-03-09 | 东莞市可迪环保科技有限公司 | 大面积有序皮芯结构二氧化钛纳米管薄膜光催化剂的制备方法及其应用 |
| CN101983764B (zh) * | 2010-09-17 | 2012-08-29 | 东莞市可迪环保科技有限公司 | 大面积有序皮芯结构二氧化钛纳米管薄膜光催化剂的制备方法及其应用 |
| CN102628115A (zh) * | 2012-04-01 | 2012-08-08 | 昆明理工大学 | 一种碳纳米管增强铜基复合材料的制备方法 |
| CN102628115B (zh) * | 2012-04-01 | 2014-05-07 | 昆明理工大学 | 一种碳纳米管增强铜基复合材料的制备方法 |
| CN103804877A (zh) * | 2014-02-19 | 2014-05-21 | 江南大学 | 具有导电和光转换储能功能的聚合物材料的制备方法 |
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