CN104477986B - 一种黑色二氧化钛纳米管的制备方法 - Google Patents
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- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 title claims abstract description 42
- 239000004408 titanium dioxide Substances 0.000 title claims abstract description 20
- 239000002071 nanotube Substances 0.000 title claims abstract description 16
- 238000002360 preparation method Methods 0.000 title claims abstract description 6
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000008367 deionised water Substances 0.000 claims abstract description 17
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 17
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000002127 nanobelt Substances 0.000 claims abstract description 11
- 238000007605 air drying Methods 0.000 claims abstract description 9
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 9
- 229910001220 stainless steel Inorganic materials 0.000 claims abstract description 9
- 239000010935 stainless steel Substances 0.000 claims abstract description 9
- 238000003756 stirring Methods 0.000 claims abstract description 9
- 239000000758 substrate Substances 0.000 claims abstract description 9
- 239000000843 powder Substances 0.000 claims abstract description 7
- NWZSZGALRFJKBT-KNIFDHDWSA-N (2s)-2,6-diaminohexanoic acid;(2s)-2-hydroxybutanedioic acid Chemical compound OC(=O)[C@@H](O)CC(O)=O.NCCCC[C@H](N)C(O)=O NWZSZGALRFJKBT-KNIFDHDWSA-N 0.000 claims abstract description 6
- IKDUDTNKRLTJSI-UHFFFAOYSA-N hydrazine monohydrate Substances O.NN IKDUDTNKRLTJSI-UHFFFAOYSA-N 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 239000012046 mixed solvent Substances 0.000 claims abstract description 5
- 238000001556 precipitation Methods 0.000 claims abstract description 5
- XJDNKRIXUMDJCW-UHFFFAOYSA-J titanium tetrachloride Chemical compound Cl[Ti](Cl)(Cl)Cl XJDNKRIXUMDJCW-UHFFFAOYSA-J 0.000 claims abstract description 5
- 238000005406 washing Methods 0.000 claims abstract description 5
- GRYLNZFGIOXLOG-UHFFFAOYSA-N Nitric acid Chemical compound O[N+]([O-])=O GRYLNZFGIOXLOG-UHFFFAOYSA-N 0.000 claims description 4
- APUPEJJSWDHEBO-UHFFFAOYSA-P ammonium molybdate Chemical compound [NH4+].[NH4+].[O-][Mo]([O-])(=O)=O APUPEJJSWDHEBO-UHFFFAOYSA-P 0.000 claims description 4
- 229940010552 ammonium molybdate Drugs 0.000 claims description 4
- 235000018660 ammonium molybdate Nutrition 0.000 claims description 4
- 239000011609 ammonium molybdate Substances 0.000 claims description 4
- 238000003760 magnetic stirring Methods 0.000 claims description 4
- 229910017604 nitric acid Inorganic materials 0.000 claims description 4
- 239000002244 precipitate Substances 0.000 claims description 4
- 238000000034 method Methods 0.000 abstract description 8
- 239000000463 material Substances 0.000 abstract description 4
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 abstract description 3
- 238000006555 catalytic reaction Methods 0.000 abstract description 3
- 229910001416 lithium ion Inorganic materials 0.000 abstract description 3
- 230000015572 biosynthetic process Effects 0.000 abstract 1
- 238000006243 chemical reaction Methods 0.000 abstract 1
- 239000002243 precursor Substances 0.000 abstract 1
- 238000003786 synthesis reaction Methods 0.000 abstract 1
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000013508 migration Methods 0.000 description 2
- 230000005012 migration Effects 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 238000000862 absorption spectrum Methods 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 239000003795 chemical substances by application Substances 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229910052755 nonmetal Inorganic materials 0.000 description 1
- 239000006250 one-dimensional material Substances 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000002829 reductive effect Effects 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G23/00—Compounds of titanium
- C01G23/04—Oxides; Hydroxides
- C01G23/047—Titanium dioxide
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Abstract
本发明公开了一种黑色二氧化钛纳米管的制备方法。将预先合成的0.1-0.5克MoO3纳米带粉体加入到10-30毫升去离子水与丙三醇的混合溶剂中，用磁力搅拌器搅拌0.5-1小时；此外，将0.5-2毫升四氯化钛加入到0.1-0.5毫升的水合肼中，用磁力搅拌器搅拌0.5-1小时；然后将含钛前躯体溶液加入到含MoO3的反应容器中，搅拌均匀后将其转入100毫升聚四氟乙烯衬底的不锈钢反应釜中，140-230℃水热反应12-16小时，过滤，将沉淀用无水乙醇洗涤3-6次后，常温干燥即得所述的黑色二氧化钛纳米管。本发明的优点在于：一方面，采用的前驱体是固体粉末，比较容易控制，另外利用该方法操作简便、成本低，并为锂离子电池，光催化，太阳电池等领域提供了新的材料。
Description
技术领域
本发明属于材料化学领域，特别涉及一种黑色二氧化钛纳米管的制备方法。
背景技术
二氧化钛已经广泛应用在锂离子电池，太阳电池，光催化等领域。传统白色二氧化钛吸收光谱主要在5%紫外线波段，且对可见光，近红外和远红外部分的吸收非常有限，这无疑限制了二氧化钛在光电领域方面的应用。此外，其本征电导率只有大约10-10S/cm，低的导电率不利于电子-空穴的传输和分离，进一步影响到二氧化钛在光电应用领域性能的发挥。
黑色二氧化钛已证明具有良好的宽光谱吸收，物理化学稳定性和提高载流子浓度和电子迁移性能，能够满足高效太阳能的需要。从大量文献和专利调研来看，获得黑色二氧化钛的途径主要有高温氢气还原、氢等离子法、铝还原法和二步非金属掺杂法。
纳米管作为一种特殊的一维材料，相比体材料，因其优越的单向导电性而广泛应用在能源和环境领域。利用简单有效的方法合成黑色二氧化钛纳米管无疑是一个巨大挑战。本发明利用MoO3纳米带作为牺牲模板，水合肼作为还原剂，利用Mo离子进行外向迁移掺杂，获得了一种黑色二氧化钛纳米管。
发明内容
本发明的目的在于提供一种工艺简单，成本低的黑色二氧化钛纳米管的制备方法，该法操作简便、成本低、耗能低，得到的产品纯度高，可以大规模合成。
具体步骤为：
（1）将0.1克钼酸铵在磁力搅拌下溶解于30毫升去离子水并加入6毫升分析纯硝酸，搅拌半小时后将上述混合均匀的溶液转入100毫升聚四氟乙烯衬底的不锈钢反应釜中，180℃水热反应24小时，过滤，将沉淀用去离子水洗涤3-6次后，常温干燥即得MoO3纳米带。
（2）将0.1-0.5克步骤（1）得到的MoO3纳米带粉体加入到10-30毫升去离子水与分析纯丙三醇的混合溶剂中，用磁力搅拌器搅拌0.5-1小时；去离子水与分析纯丙三醇的体积比为0.5-1：1-2。
（3）将0.5-2毫升分析纯四氯化钛加入到0.1-0.5毫升的分析纯水合肼中，用磁力搅拌器搅拌0.5-1小时。
（4）将步骤（3）得到的溶液加入到步骤（2）所得溶液中，搅拌均匀后将其转入100毫升聚四氟乙烯衬底的不锈钢反应釜中，140-230℃水热反应12-16小时，过滤，将沉淀用无水乙醇洗涤3-6次后，常温干燥即得管长为1-10微米，管外径为300-500纳米,管壁厚10-20纳米的黑色二氧化钛纳米管。
本发明的优点在于：一方面，采用的前驱体是固体粉末，比较容易控制，另外利用该方法操作简便、成本低，并为锂离子电池，光催化，太阳电池等领域提供了新的材料。
附图说明：
图1为本发明制备的黑色二氧化钛纳米管的X射线衍射花样图。
图2为本发明制备的MoO3纳米带的场发射扫描电镜照片。（a）低倍率场发射扫描电镜照片，（b）高倍率场发射扫描电镜照片。
图3为本发明制备的黑色二氧化钛纳米管的场发射扫描电镜照片。（a）-(b)低倍率场发射扫描电镜照片，（c）-（d）高倍率场发射扫描电镜照片。
具体实施方式
为了更好地理解本发明，下面结合实施例进一步阐明本发明的内容，但本
发明的内容不仅仅局限于下面的实施例。
实施例1：
（1）将0.1克钼酸铵在磁力搅拌下溶解于30毫升去离子水并加入6毫升分析纯硝酸，搅拌半小时后将上述混合均匀的溶液转入100毫升聚四氟乙烯衬底的不锈钢反应釜中，180℃水热反应24小时，过滤，将沉淀用去离子水洗涤3次后，常温干燥即得MoO3纳米带。
（2）将0.1克步骤（1）得到的MoO3纳米带粉体加入到10毫升去离子水与分析纯丙三醇的混合溶剂中，用磁力搅拌器搅拌0.5小时；去离子水与分析纯丙三醇的体积比为0.5：1。
（3）将0.5毫升分析纯四氯化钛加入到0.1毫升的分析纯水合肼中，用磁力搅拌器搅拌0.5小时。
（4）将步骤（3）得到的溶液加入到步骤（2）所得溶液中，搅拌均匀后将其转入100毫升聚四氟乙烯衬底的不锈钢反应釜中，140℃水热反应12小时，过滤，将沉淀用无水乙醇洗涤3次后，常温干燥即得管长为1-10微米，管外径为300-500纳米,管壁厚10-20纳米的黑色二氧化钛纳米管。
实施例2：
（1）将0.1克钼酸铵在磁力搅拌下溶解于30毫升去离子水并加入6毫升分析纯硝酸，搅拌半小时后将上述混合均匀的溶液转入100毫升聚四氟乙烯衬底的不锈钢反应釜中，180℃水热反应24小时，过滤，将沉淀用去离子水洗涤5次后，常温干燥即得MoO3纳米带。
（2）将0.5克步骤（1）得到的MoO3纳米带粉体加入到30毫升去离子水与分析纯丙三醇的混合溶剂中，用磁力搅拌器搅拌1小时；去离子水与分析纯丙三醇的体积比为1：2。
（3）将0.5毫升分析纯四氯化钛加入到0.1毫升的分析纯水合肼中，用磁力搅拌器搅拌0.5小时。
（4）将步骤（3）得到的溶液加入到步骤（2）所得溶液中，搅拌均匀后将其转入100毫升聚四氟乙烯衬底的不锈钢反应釜中，230℃水热反应16小时，过滤，将沉淀用无水乙醇洗涤6次后，常温干燥即得管长为1-10微米，管外径为300-500纳米,管壁厚10-20纳米的黑色二氧化钛纳米管。
Claims (1)
1.一种黑色二氧化钛纳米管的制备方法，其特征在于具体步骤为：
（1）将0.1克钼酸铵在磁力搅拌下溶解于30毫升去离子水并加入6毫升分析纯硝酸，搅拌半小时后将上述混合均匀的溶液转入100毫升聚四氟乙烯衬底的不锈钢反应釜中，180℃水热反应24小时，过滤，将沉淀用去离子水洗涤3-6次后，常温干燥即得MoO3纳米带；
（2）将0.1-0.5克步骤（1）得到的MoO3纳米带粉体加入到10-30毫升去离子水与分析纯丙三醇的混合溶剂中，用磁力搅拌器搅拌0.5-1小时；去离子水与分析纯丙三醇的体积比为0.5-1：1-2；
（3）将0.5-2毫升分析纯四氯化钛加入到0.1-0.5毫升的分析纯水合肼中，用磁力搅拌器搅拌0.5-1小时；
（4）将步骤（3）得到的溶液加入到步骤（2）所得溶液中，搅拌均匀后将其转入100毫升聚四氟乙烯衬底的不锈钢反应釜中，140-230℃水热反应12-16小时，过滤，将沉淀用无水乙醇洗涤3-6次后，常温干燥即得管长为1-10微米，管外径为300-500纳米,管壁厚10-20纳米的黑色二氧化钛纳米管。
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