CN105126796A - 一种氟掺杂片层状黑色二氧化钛纳米材料的制备方法 - Google Patents
一种氟掺杂片层状黑色二氧化钛纳米材料的制备方法 Download PDFInfo
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 57
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 27
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- KRHYYFGTRYWZRS-UHFFFAOYSA-N Fluorane Chemical compound F KRHYYFGTRYWZRS-UHFFFAOYSA-N 0.000 claims abstract description 20
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 238000006243 chemical reaction Methods 0.000 claims abstract description 8
- 238000001035 drying Methods 0.000 claims abstract description 7
- 230000001681 protective effect Effects 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 9
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims description 8
- 238000001354 calcination Methods 0.000 claims description 6
- 239000007789 gas Substances 0.000 claims description 6
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims description 4
- 229910052786 argon Inorganic materials 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 239000000706 filtrate Substances 0.000 claims description 4
- 239000001257 hydrogen Substances 0.000 claims description 4
- 229910052739 hydrogen Inorganic materials 0.000 claims description 4
- 230000007935 neutral effect Effects 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 4
- 238000002156 mixing Methods 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000007795 chemical reaction product Substances 0.000 abstract 2
- 230000010748 Photoabsorption Effects 0.000 abstract 1
- 230000005540 biological transmission Effects 0.000 abstract 1
- YHWCPXVTRSHPNY-UHFFFAOYSA-N butan-1-olate;titanium(4+) Chemical compound [Ti+4].CCCC[O-].CCCC[O-].CCCC[O-].CCCC[O-] YHWCPXVTRSHPNY-UHFFFAOYSA-N 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 239000011259 mixed solution Substances 0.000 abstract 1
- 239000000203 mixture Substances 0.000 abstract 1
- 239000000463 material Substances 0.000 description 6
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000003795 chemical substances by application Substances 0.000 description 3
- 230000031700 light absorption Effects 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 230000001699 photocatalysis Effects 0.000 description 3
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- 238000003786 synthesis reaction Methods 0.000 description 3
- 229910052719 titanium Inorganic materials 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- 229910010413 TiO 2 Inorganic materials 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 230000005518 electrochemistry Effects 0.000 description 2
- 230000003287 optical effect Effects 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000001228 spectrum Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000002389 environmental scanning electron microscopy Methods 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 239000007791 liquid phase Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000010189 synthetic method Methods 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
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Abstract
本发明公开了一种氟掺杂片层状黑色二氧化钛纳米材料的制备方法，属于纳米材料技术领域。包括步骤如下：1）首先配置好钛酸四正丁酯，正丙醇和氢氟酸混合体系，搅拌一段时间；2）将混合溶液转移至高压反应釜中，在一定温度下反应一段时间；3）将反应后的样品进行洗涤、干燥处理，然后在保护气氛下加热一段时间便可得到氟掺杂片层状黑色二氧化钛纳米材料。相比于商业化生产的二氧化钛P25，这种氟掺杂片层状黑色二氧化钛纳米材料具有更优异的光吸收和电子传输性能。
Description
技术领域
本发明属于纳米材料技术领域，特别涉及一种氟掺杂片层状黑色二氧化钛纳米材料的制备方法，该材料具有优异的光吸收和电化学性能，可作为催化剂应用于光催化，还可作为光阳极材料应用于染料敏化太阳电池中。
背景技术
二氧化钛（TiO2）是一种环境友好，化学性质稳定，价格较为低廉的半导体材料。由于其优异的电荷传输性能，在光照条件下催化性高等特点，在光电化学催化、染料敏化太阳能电池、钙钛矿电池，、锂离子电池等领域被广泛应用。然而，受限于二氧化钛是一种宽禁带半导体（~3eV），其可见光吸收和载流子传输与分离能力受到影响。因此，通过改善二氧化钛的电子能级结构，提高二氧化钛的光吸收与载流子传输与分离能力，对提高TiO2的性能极其重要。我们利用低温水热合成法，以钛酸四正丁酯为钛源，以正丙醇作为溶剂，以氢氟酸作为表面剂，制备了一种氟掺杂片层状黑色二氧化钛纳米材料。该二氧化钛材料在氟掺杂的作用下，产生了三价钛缺陷，电子能级结构得到了一定的改善，有利于电荷传输。黑色则意味着该材料可以吸收更多的太阳光，且片层状结构有利于提高比表面积，从而提高了该材料的光催化性能。
发明内容
本发明的目的是提出一种氟掺杂黑色片层状二氧化钛纳米材料。本发明提供的方法以钛酸四正丁酯为钛源，以正丙醇作为溶剂，以氢氟酸作为表面剂，采用简单的一步水热合成方法制备了氟掺杂片层状黑色二氧化钛纳米材料。具体的制备方法包括如下步骤：
（1）将20~30mL的正丙醇加入到烧杯中，随后加入1~3mL钛酸四正丁酯，搅拌均匀；
（2）往溶液中加入0.2~0.8mL的氢氟酸，然后搅拌1~3小时；
（3）将所得溶液转移至高压反应釜中，160~200℃下水热反应12~24小时；
（4）将反应后得到的沉淀用去离子水及无水乙醇洗涤至滤液为中性，然后进行干燥处理；
（5）将所得样品在保护气氛下进行400~450℃的煅烧，便可得到氟掺杂黑色片层状二氧化钛纳米材料。
所述步骤（1）中所加入的正丙醇为20~30mL,钛酸四正丁酯为1~3mL；
所述步骤（2）中所加入氢氟酸为0.2~0.8mL,搅拌时间为1~3小时；
所述步骤（3）中溶液在反应釜中的反应温度为160~200℃，反应时间为12~24小时；
所述步骤（4）中所得样品的干燥温度为50℃~60℃，干燥时间为12~20小时；
所述步骤（5）中所用保护气氛为氩气和氢气混合气，煅烧时间为2~4小时。
本发明的有益效果是通过以钛酸四正丁酯为钛源，以正丙醇作为溶剂，以氢氟酸作为表面剂，利用简单的水热法合成了一种氟掺杂片层状黑色二氧化钛纳米材料。水热合成的优势在于可以有效地进行液相控制、能耗相对较低、可控性好并且成本较低。利用本发明所提供的方法制备的TiO2纳米材料，在氟掺杂的作用下，能带结构发生了改变，大大增强了其性能。相对于商业用P25只能吸收紫外光，所合成的二氧化钛材料对紫外-可见-红外全光谱都有比较强的吸收，有利于提高其光催化性能。该材料可广泛应用于光电化学、钙钛矿电池和染料敏化电池等领域。
附图说明
图1是本发明实例1中合成的氟掺杂片层状黑色二氧化钛纳米材料与商业用P25的光吸收对比图。
图2是本发明实例1中合成的氟掺杂黑色片层状二氧化钛纳米材料与商业用P25的X射线电子能谱（XPS）F1s对比图。
图3是本发明实例1中合成的氟掺杂黑色片层状二氧化钛纳米材料的扫描电镜（SEM）图。
具体实施方式
本发明提出的一种制备松塔状TiO2纳米材料的方法可通过如下的方法实施，具体的制备方法包括如下步骤：
实施例1
（1）将25mL的正丙醇加入到烧杯中，随后加入2mL钛酸四正丁酯，搅拌均匀；
（2）往溶液中加入0.4mL的氢氟酸，然后搅拌2小时；
（3）将所得溶液转移至高压反应釜中，180℃下水热反应18小时；
（4）将反应后得到的沉淀用去离子水及无水乙醇洗涤至滤液为中性，然后进行干燥处理；
（5）将所得样品在氩气和氢气气氛下进行430℃的煅烧，便可得到氟掺杂片层状黑色二氧化钛纳米材料。
实施例2
（1）将20mL的正丙醇加入到烧杯中，随后加入1mL钛酸四正丁酯，搅拌均匀；
（2）往溶液中加入0.15mL的氢氟酸，然后搅拌1小时；
（3）将所得溶液转移至高压反应釜中，180℃下水热反应15小时；
（4）将反应后得到的沉淀用去离子水及无水乙醇洗涤至滤液为中性，然后进行干燥处理；
（5）将所得样品在氩气和氢气气氛下进行450℃的煅烧，便可得到氟掺杂黑色片层状二氧化钛纳米材料。
Claims (6)
1.一种氟掺杂黑色片层状二氧化钛纳米材料的制备方法，其特征在于，包括步骤如下：
（1）将20~30mL的正丙醇加入到烧杯中，随后加入1~3mL钛酸四正丁酯，搅拌均匀；
（2）往（1）中所得溶液加入0.2~0.8mL的氢氟酸，然后搅拌1~3小时；
（3）将（2）所得溶液转移至高压反应釜中，160~200℃下水热反应12~24小时；
（4）将（3）中反应后得到的沉淀用去离子水及无水乙醇洗涤至滤液为中性，然后进行干燥处理；
（5）将（4）所得样品在保护气氛下进行400~450℃煅烧一段时间，便可得到氟掺杂黑色片层状二氧化钛纳米材料。
2.根据权利要求1所述的一种氟掺杂黑色片层状二氧化钛纳米材料的制备方法，其特征在于，步骤（1）中所加入的正丙醇为20~30mL,钛酸四正丁酯为1~3mL。
3.根据权利要求1所述的一种氟掺杂黑色片层状二氧化钛纳米材料的制备方法，其特征在于，步骤（2）中所加入氢氟酸为0.2~0.8mL,搅拌时间为1~3小时。
4.根据权利要求1所述的一种氟掺杂黑色片层状二氧化钛纳米材料的制备方法，其特征在于，步骤（3）中溶液在反应釜中的反应温度为160~200℃，反应时间为12~24小时。
5.根据权利要求1所述的一种氟掺杂片层状黑色二氧化钛纳米材料的制备方法，其特征在于，步骤（4）中所得样品的干燥温度为50℃~60℃，干燥时间为12~20小时。
6.根据权利要求1所述的一种氟掺杂片层状黑色二氧化钛纳米材料的制备方法，其特征在于，步骤（5）中所用保护气氛为氩气和氢气混合气，煅烧时间为2~4小时。
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| CN107138161A (zh) * | 2017-07-17 | 2017-09-08 | 上海友兰科技有限公司 | 一种掺杂黑色二氧化钛的制备方法 |
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