CN101302036A - A kind of preparation method of doped titanium dioxide nanotube - Google Patents
A kind of preparation method of doped titanium dioxide nanotube 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 60
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- SOQBVABWOPYFQZ-UHFFFAOYSA-N oxygen(2-);titanium(4+) Chemical compound [O-2].[O-2].[Ti+4] SOQBVABWOPYFQZ-UHFFFAOYSA-N 0.000 description 8
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- 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 description 2
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Abstract
Description
【技术领域】 【Technical field】
本发明涉及一种掺杂二氧化钛纳米管的制备方法，属于纳米材料领域。The invention relates to a method for preparing doped titanium dioxide nanotubes, which belongs to the field of nanomaterials.
【背景技术】 【Background technique】
自从发现了碳纳米管具有韧性强、比表面积大、强度高等优异性能以来，人们展开了对各种物质的纳米管的广泛研究。同时，由于二氧化钛具有价格低廉、稳定性好等优点，二氧化钛纳米管在有机物降解，光电转换，光解水制氢，光传感器等方面的应用倍受世界科学家关注。Since the discovery that carbon nanotubes have excellent properties such as strong toughness, large specific surface area, and high strength, people have launched extensive research on nanotubes of various substances. At the same time, due to the advantages of low price and good stability of titanium dioxide, the application of titanium dioxide nanotubes in organic matter degradation, photoelectric conversion, hydrogen production by photolysis of water, and optical sensors has attracted the attention of scientists all over the world.
但是由于二氧化钛禁带宽度为3.2eV，只能吸收波长小于387nm的紫外光，而太阳光中大部分为可见光，紫外光的成分仅占5％。目前，太阳光利用率低成为阻碍二氧化钛应用的主要问题。近年为了提高二氧化钛的可见光利用率，单相或多相掺杂和复合调控技术被人们用来加强二氧化钛纳米粒子或薄膜对可见光的吸收。同时，掺杂元素形成的浅能级可以成为光生电子或空穴的捕获中心，有利于光生载流子分离，从而提高光量子效率。2001年，R.Asahi教授等制备出了N掺杂的高活性TiO2可见光催化剂，引发了非金属掺杂的热潮。2006年，In等制备出了B，N共掺杂高可见光活性的二氧化钛催化剂。Sn、Fe、In、P、S、C等其他元素掺杂二氧化钛也吸引了人们的极大兴趣。但是，由于二氧化钛纳米管的制备工艺比较复杂不利用掺杂或复合，因此关于掺杂或复合型纳米管的报道比较少。However, since titanium dioxide has a band gap of 3.2eV, it can only absorb ultraviolet light with a wavelength less than 387nm, and most of the sunlight is visible light, and the ultraviolet light only accounts for 5%. At present, the low utilization rate of sunlight has become the main problem hindering the application of titanium dioxide. In recent years, in order to improve the utilization rate of visible light of titanium dioxide, single-phase or multi-phase doping and compound regulation technology have been used to enhance the absorption of visible light by titanium dioxide nanoparticles or thin films. At the same time, the shallow energy level formed by doping elements can become the capture center of photogenerated electrons or holes, which is beneficial to the separation of photogenerated carriers, thereby improving the photon quantum efficiency. In 2001, Professor R.Asahi and others prepared N-doped highly active TiO 2 visible photocatalysts, which triggered an upsurge of non-metallic doping. In 2006, In et al. prepared B, N co-doped titanium dioxide catalyst with high visible light activity. TiO2 doped with other elements such as Sn, Fe, In, P, S, C, etc. has also attracted great interest. However, because the preparation process of titanium dioxide nanotubes is relatively complicated and does not use doping or compounding, there are relatively few reports on doped or compounded nanotubes.
本发明采用两步预合成法：先合成掺杂二氧化钛纳米颗粒，再将纳米颗粒通过水热法制成掺杂二氧化钛纳米管。该方法简单可行，制备出的纳米管管壁薄，管径小，比表面积大。但是水热法在强碱环境下对二氧化钛进行反应，不利于其他掺杂离子的存在，掺杂离子也不容易进入已经形成的二氧化钛晶格。因此，用水热法制可见光响应的掺杂纳米管一直是需要攻克的难题。The invention adopts a two-step pre-synthesis method: first synthesizing doped titanium dioxide nanometer particles, and then making the doped titanium dioxide nanometer tubes from the nanometer particles through a hydrothermal method. The method is simple and feasible, and the prepared nanotube has thin wall, small diameter and large specific surface area. However, the hydrothermal method reacts titanium dioxide in a strong alkaline environment, which is not conducive to the existence of other dopant ions, and the dopant ions are not easy to enter the formed titanium dioxide lattice. Therefore, the preparation of doped nanotubes responsive to visible light by hydrothermal method has always been a difficult problem to be overcome.
【发明内容】 【Content of invention】
本发明的主要目的是制备一种具有可见光响应的掺杂纳米管。采用预掺杂两步合成法，具体步骤如下：The main purpose of the present invention is to prepare a doped nanotube with visible light response. A pre-doped two-step synthesis method is adopted, and the specific steps are as follows:
1.用溶胶凝胶法或水解法等方法制备出掺杂的纳米二氧化钛粉末。掺杂量应比较大，而且应使掺杂原子进入二氧化钛晶格。1. Prepare doped nano-titanium dioxide powder by sol-gel method or hydrolysis method. The doping amount should be relatively large, and the dopant atoms should enter the titanium dioxide lattice.
2.钛酸盐纳米管的制备。将浓碱溶液与一定量的掺杂纳米二氧化钛粉末放入高压反应釜混合搅拌30min，然后加热到100℃以上反应20h左右，自然冷却。2. Preparation of titanate nanotubes. Put the concentrated alkali solution and a certain amount of doped nano-titanium dioxide powder into the high-pressure reactor, mix and stir for 30 minutes, then heat it to above 100°C for about 20 hours, and cool naturally.
3.将得到产物离心后倒去上层清液，用去离子水对沉淀洗涤至中性后，用稀盐酸浸泡30min左右，再次离心后对沉淀进行洗涤至中性。3. Centrifuge the obtained product and pour off the supernatant, wash the precipitate with deionized water until it is neutral, soak it in dilute hydrochloric acid for about 30 minutes, and then centrifuge again to wash the precipitate until it is neutral.
4.将中性产物烘干后，放入马弗炉400℃下煅烧2.5个小时，即得锐钛矿型可见光响应二氧化钛纳米管。4. After drying the neutral product, put it into a muffle furnace for calcination at 400° C. for 2.5 hours to obtain anatase-type visible light-responsive titanium dioxide nanotubes.
本发明采用两步预合成法制得的纳米管具有较强的可见光吸收，而且管壁薄，比表面积大，晶型好，掺杂量可控，而且本制备方法工艺简单，易于操作，适用于各种元素的掺杂。The nanotube prepared by the two-step pre-synthesis method in the present invention has strong visible light absorption, and the tube wall is thin, the specific surface area is large, the crystal form is good, and the doping amount is controllable. Moreover, the preparation method is simple in process and easy to operate, and is suitable for Doping of various elements.
【附图说明】 【Description of drawings】
图1实施例1中N掺杂TiO2纳米管的透射电子显微镜(TEM)图片。Fig. 1 Transmission electron microscope (TEM) picture of N - doped TiO nanotubes in Example 1.
图2所有实施例中产物的X射线衍射(XRD)图(与纯TiO2比较)The X-ray diffraction (XRD) pattern (with pure TiO 2 comparison) of product in Fig. 2 all embodiments
图3实施例1中N掺杂TiO2纳米管的紫外可见漫反射吸收图(与纯TiO2比较)The ultraviolet-visible diffuse reflection absorption figure (compared with pure TiO 2 ) of N-doped TiO 2 nanotubes in Fig. 3 embodiment 1
【具体实施方式】 【Detailed ways】
实施例1：In掺杂TiO2纳米管Example 1: In doped TiO nanotubes
1.采用溶胶-凝胶法制备In掺杂TiO2纳米粉末。取12ml钛酸四丁酯缓慢滴入混有40ml无水乙醇，2ml去离子水和1ml盐酸的烧杯中，搅拌半小时后，加入0.2ml三氯化铟滴入烧杯；得到透明溶胶，静置一段时间，凝胶后，于100℃恒温干燥10~12个小时，得到干凝胶；研磨后，450℃煅烧2.5小时后取出，得到In掺杂TiO2纳米粉末。1. Preparation of In-doped TiO2 nanopowders by sol-gel method. Take 12ml of tetrabutyl titanate and slowly drop it into a beaker mixed with 40ml of absolute ethanol, 2ml of deionized water and 1ml of hydrochloric acid. After stirring for half an hour, add 0.2ml of indium trichloride and drop it into the beaker; a transparent sol is obtained and left to stand After a period of time, after gelling, dry at a constant temperature of 100°C for 10-12 hours to obtain dry gel; after grinding, calcine at 450°C for 2.5 hours and take it out to obtain In-doped TiO 2 nanopowder.
2.将0.4g In掺杂TiO2纳米粉末与18ml 10mol/L的的NaOH溶液混合加入反应釜进行搅拌，半个小时后，将高压釜置于烘箱中加热到110℃，保温20h。2. Mix 0.4g of In-doped TiO 2 nanopowder with 18ml of 10mol/L NaOH solution and add it to the reactor for stirring. After half an hour, put the autoclave in an oven and heat it to 110°C and keep it warm for 20h.
3.将反应完的高压釜取出，待自然冷却后，离心，倒掉上层清液，将沉淀用去离子水洗直至中性，再用0.1mol/L盐酸浸泡半个小时，之后再次用去离子水将产物洗涤到中性。3. Take out the autoclave after the reaction, after cooling naturally, centrifuge, pour off the supernatant, wash the precipitate with deionized water until it is neutral, then soak it in 0.1mol/L hydrochloric acid for half an hour, and then use deionized water again Water washed the product to neutrality.
4.将所得产物平铺到表面皿中，放入烘箱中以100℃烘12h，取出烘干后的块体进行轻轻研磨。将研磨后的产物放入马弗炉以400℃温度下烧结2.5h，然后再经过再次轻轻研磨后即制得所需的TiO2纳米管。4. Spread the obtained product on a watch glass, put it in an oven and dry it at 100°C for 12 hours, take out the dried block and grind it lightly. The ground product was put into a muffle furnace for sintering at 400° C. for 2.5 h, and then lightly ground again to obtain the required TiO 2 nanotubes.
实施例2：N掺杂TiO2纳米管Example 2: N-doped TiO2 nanotubes
1.采用TiCl4水解法制备N掺杂TiO2纳米粉末。25％的氨水在剧烈搅拌下逐滴加入到200mL的浓度约为0.1molL-1的四氯化钛水溶液中，体系中立刻产生白色沉淀，当体系的pH值达到5.5时停止加入氨水。然后静置陈化24h，过滤，所得沉淀在70℃烘干，研磨成粉末，并在400℃烧结4小时。即得到N掺杂TiO2纳米粉末1. Preparation of N-doped TiO 2 nanopowders by TiCl 4 hydrolysis method. 25% ammonia water was added dropwise to 200 mL of titanium tetrachloride aqueous solution with a concentration of about 0.1 molL under vigorous stirring, and a white precipitate was formed in the system immediately, and the addition of ammonia water was stopped when the pH value of the system reached 5.5. Then it was left to age for 24 hours, filtered, and the obtained precipitate was dried at 70°C, ground into powder, and sintered at 400°C for 4 hours. That is, N-doped TiO 2 nanopowder is obtained
2.将0.4g N掺杂TiO2纳米粉末与18ml 10mol/L的的NaOH溶液混合加入反应釜进行搅拌，半个小时后，将高压釜置于烘箱中加热到110℃，保温20h。2. Mix 0.4g of N-doped TiO 2 nano powder and 18ml of 10mol/L NaOH solution into the reactor for stirring. After half an hour, heat the autoclave in an oven to 110°C and keep it warm for 20h.
3.将反应完的高压釜取出，待自然冷却后，离心，倒掉上层清液，将沉淀用去离子水洗直至中性，再用0.1mol/L盐酸浸泡半个小时，之后再次用去离子水将产物洗涤到中性。3. Take out the autoclave after the reaction, after cooling naturally, centrifuge, pour off the supernatant, wash the precipitate with deionized water until it is neutral, then soak it in 0.1mol/L hydrochloric acid for half an hour, and then use deionized water again Water washed the product to neutrality.
4.将所得产物平铺到表面皿中，放入烘箱中以100℃烘12h，取出烘干后的块体进行轻轻研磨。将研磨后的产物放入马弗炉以400℃温度下烧结2.5h，然后再经过再次轻轻研磨后即制得所需的TiO2纳米管。4. Spread the obtained product on a watch glass, put it into an oven and bake at 100°C for 12 hours, take out the dried block and grind it lightly. The ground product was put into a muffle furnace for sintering at 400° C. for 2.5 h, and then lightly ground again to obtain the required TiO 2 nanotubes.
实施例3：N、Sn双掺杂TiO2纳米管Embodiment 3: N, Sn double-doped TiO 2 nanotubes
1.采用溶胶-凝胶法制备N、Sn双掺杂TiO2纳米粉末。取12ml钛酸四丁酯缓慢滴入混有40ml无水乙醇，2ml去离子水和1ml盐酸的烧杯中，搅拌半小时后，加入0.2ml四氯化锡，再过半小时，加入3ml氨水，得到透明溶胶，静置一段时间，凝胶后，于100℃恒温干燥10~12个小时，得到干凝胶；研磨后，450℃煅烧2.5小时后取出，得到N、Sn双掺杂TiO2纳米粉末。1. N, Sn double-doped TiO 2 nanopowders were prepared by sol-gel method. Take 12ml of tetrabutyl titanate and slowly drop it into a beaker mixed with 40ml of absolute ethanol, 2ml of deionized water and 1ml of hydrochloric acid. After stirring for half an hour, add 0.2ml of tin tetrachloride, and after another half hour, add 3ml of ammonia water to obtain Transparent sol, let it stand for a period of time, after gelation, dry at 100°C for 10-12 hours to obtain xerogel; after grinding, take it out after calcination at 450°C for 2.5 hours, to obtain N, Sn double-doped TiO 2 nano powder .
2.将0.4g N、Sn双掺杂TiO2纳米粉末与18ml 10mol/L的的NaOH溶液混合加入反应釜进行搅拌，半个小时后，将高压釜置于烘箱中加热到110℃，保温20h。2. Mix 0.4g of N, Sn double-doped TiO 2 nanopowder with 18ml of 10mol/L NaOH solution and add to the reaction kettle for stirring. After half an hour, put the autoclave in an oven and heat it to 110°C and keep it warm for 20h .
3.将反应完的高压釜取出，待自然冷却后，离心，倒掉上层清液，将沉淀用去离子水洗直至中性，再用0.1mol/L盐酸浸泡半个小时，之后再次用去离子水将产物洗涤到中性。3. Take out the autoclave after the reaction, after cooling naturally, centrifuge, pour off the supernatant, wash the precipitate with deionized water until it is neutral, then soak it in 0.1mol/L hydrochloric acid for half an hour, and then use deionized water again Water washed the product to neutrality.
4.将所得产物平铺到表面皿中，放入烘箱中以100℃烘12h，取出烘干后的块体进行轻轻研磨。将研磨后的产物放入马弗炉以400℃温度下烧结2.5h，然后再经过再次轻轻研磨后即制得所需的TiO2纳米管。4. Spread the obtained product on a watch glass, put it into an oven and bake at 100°C for 12 hours, take out the dried block and grind it lightly. The ground product was put into a muffle furnace for sintering at 400° C. for 2.5 h, and then lightly ground again to obtain the required TiO 2 nanotubes.
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| MD4063C1 (en) * | 2010-02-18 | 2011-03-31 | Технический университет Молдовы | Method for producing nanotubes of titanium dioxide on a titanium substrate |
| CN102157732A (en) * | 2011-03-24 | 2011-08-17 | 河南大学 | Titanium dioxide/carbon composite nanotube and preparation and application thereof |
| CN102863046A (en) * | 2012-09-09 | 2013-01-09 | 桂林理工大学 | Application of Au/TiO2 Nanotube Arrays to Photocatalytic Degradation of Sugar Wastewater |
| WO2013139174A1 (en) * | 2012-03-19 | 2013-09-26 | The Hong Kong University Of Science And Technology | Incorporating metals, metal oxides and compounds on the inner and outer surfaces of nanotubes and between the walls of the nanotubes and preparation thereof |
| CN103531762A (en) * | 2013-10-23 | 2014-01-22 | 山东大学 | Preparation method of titanium dioxide nano tube doped with heterovalent metal salt |
| CN104084205A (en) * | 2014-07-24 | 2014-10-08 | 哈尔滨工业大学 | Preparation method and application of ferrum loaded titanium dioxide nanotube with catalytic oxidation activity |
| CN104722294A (en) * | 2015-02-15 | 2015-06-24 | 福建工程学院 | A Preparation Technology of Pt-TiO2 Nanotubes under Normal Pressure |
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| CN105800680A (en) * | 2016-03-14 | 2016-07-27 | 武汉理工大学 | Preparation method of titanium dioxide nanotube doped with transition metal |
| CN108187651A (en) * | 2017-12-28 | 2018-06-22 | 山东纳安环保科技有限公司 | A kind of preparation method and application for carrying zinc nano-titanium dioxide |
| CN108465461A (en) * | 2018-03-26 | 2018-08-31 | 江苏奥净嘉环保科技有限公司 | A kind of preparation method of photocatalysis air-cleaning material |
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| MD4063C1 (en) * | 2010-02-18 | 2011-03-31 | Технический университет Молдовы | Method for producing nanotubes of titanium dioxide on a titanium substrate |
| CN102157732A (en) * | 2011-03-24 | 2011-08-17 | 河南大学 | Titanium dioxide/carbon composite nanotube and preparation and application thereof |
| CN104350011A (en) * | 2012-03-19 | 2015-02-11 | 香港科技大学 | Method for doping metal, metal oxide and metal complex on inner surface and outer surface of nanotube and between nanotube layers and preparation method of nanotube |
| WO2013139174A1 (en) * | 2012-03-19 | 2013-09-26 | The Hong Kong University Of Science And Technology | Incorporating metals, metal oxides and compounds on the inner and outer surfaces of nanotubes and between the walls of the nanotubes and preparation thereof |
| US10238762B2 (en) | 2012-03-19 | 2019-03-26 | The Hong Kong University Of Science And Technology | Incorporating metals, metal oxides and compounds on the inner and outer surfaces of nanotubes and between the walls of the nanotubes and preparation thereof |
| CN104350011B (en) * | 2012-03-19 | 2016-09-28 | 香港科技大学 | Method for doping metal, metal oxide and metal complex on inner surface and outer surface of nanotube and interlayer of nanotube and nanotube |
| CN102863046A (en) * | 2012-09-09 | 2013-01-09 | 桂林理工大学 | Application of Au/TiO2 Nanotube Arrays to Photocatalytic Degradation of Sugar Wastewater |
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| CN104084205A (en) * | 2014-07-24 | 2014-10-08 | 哈尔滨工业大学 | Preparation method and application of ferrum loaded titanium dioxide nanotube with catalytic oxidation activity |
| CN104722294A (en) * | 2015-02-15 | 2015-06-24 | 福建工程学院 | A Preparation Technology of Pt-TiO2 Nanotubes under Normal Pressure |
| CN105271388A (en) * | 2015-10-10 | 2016-01-27 | 同济大学 | Preparation method of ultra-long TiO2 nanotubes with high specific surface area |
| CN105800680A (en) * | 2016-03-14 | 2016-07-27 | 武汉理工大学 | Preparation method of titanium dioxide nanotube doped with transition metal |
| CN108187651A (en) * | 2017-12-28 | 2018-06-22 | 山东纳安环保科技有限公司 | A kind of preparation method and application for carrying zinc nano-titanium dioxide |
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| CN112742414A (en) * | 2019-10-29 | 2021-05-04 | 中国石油化工股份有限公司 | Water-resistant and sulfur-resistant low-temperature SCR denitration catalyst and preparation method and application thereof |
| CN112742414B (en) * | 2019-10-29 | 2022-10-21 | 中国石油化工股份有限公司 | Water-resistant and sulfur-resistant low-temperature SCR denitration catalyst and preparation method and application thereof |
| CN111364051A (en) * | 2020-03-23 | 2020-07-03 | 江苏大学 | Method for doping In ions to titanium dioxide photoelectrode by flame |
| CN113368865A (en) * | 2021-06-08 | 2021-09-10 | 中国科学院山西煤炭化学研究所 | Denitration catalyst, preparation method thereof and waste gas denitration method |
| CN113368865B (en) * | 2021-06-08 | 2022-12-02 | 中国科学院山西煤炭化学研究所 | Denitration catalyst, preparation method thereof and waste gas denitration method |
| CN116159559A (en) * | 2022-12-16 | 2023-05-26 | 中国科学院福建物质结构研究所 | Preparation method and application of ruthenium-doped titania nanotube catalyst |
| CN116159559B (en) * | 2022-12-16 | 2024-07-23 | 中国科学院福建物质结构研究所 | Preparation method and application of ruthenium-doped titanium dioxide nanotube catalyst |
| CN117860704A (en) * | 2024-03-12 | 2024-04-12 | 天津医科大学总医院 | Nanocomposite Fe/TNT@NM and preparation method and application thereof |
| CN117860704B (en) * | 2024-03-12 | 2024-05-24 | 天津医科大学总医院 | A nanocomposite material Fe/TNT@NM and its preparation method and application |
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