CN106365465B - Preparation method of a three-dimensional titanium dioxide-gold-carbon nitride ternary material - Google Patents
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Abstract
本发明涉及制备三维二氧化钛纳米棒‑金纳米‑氮化碳三元复合纳米材料的制备方法。碳化氮作为窄禁带半导体材料能够被可见光激发，增强对可见光的吸收，金纳米不仅能够促进电子传递，而且可以具有等离子体表面共振效应，能够增强光电转换效率。本方法所制备的三维树枝状二氧化钛纳米棒‑金纳米‑氮化碳三元复合纳米材料，能够增强对可见光的吸收改善光电转换效率，在光催化和太阳能电池等领域具有广泛的应用前景。
The invention relates to a preparation method for preparing a three-dimensional titanium dioxide nanorod-gold nano-carbon nitride ternary composite nanomaterial. Nitrogen carbide, as a narrow bandgap semiconductor material, can be excited by visible light and enhance the absorption of visible light. Gold nanometers can not only promote electron transfer, but also have a plasmon surface resonance effect, which can enhance photoelectric conversion efficiency. The three-dimensional dendritic titanium dioxide nanorod-gold nano-carbon nitride ternary composite nanomaterial prepared by the method can enhance the absorption of visible light and improve the photoelectric conversion efficiency, and has broad application prospects in the fields of photocatalysis and solar cells.
Description
技术领域technical field
本发明涉及纳米材料合成技术领域，更具体地说是一种在导电基底上制备三维树枝状二氧化钛纳米棒-金纳米-氮化碳三元复合材料的制备方法，并且改善光电性能。The invention relates to the technical field of nanomaterial synthesis, more specifically to a method for preparing a three-dimensional dendritic titanium dioxide nanorod-gold nanometer-carbon nitride ternary composite material on a conductive substrate, and improves the photoelectric performance.
背景技术Background technique
二氧化钛作为一种n型半导体材料，具有光催化性能好、稳定性高、价格便宜等优点，已经广泛应用于光电器件、太阳能电池、光催化、生物传感等领域。二氧化钛的光电性能与其形貌相关，与一维纳米材料相比，三维材料具有更大的表面积、电子传递速度快、增强光吸收效率，能够具有更好的光电响应。但二氧化钛具有3.2 eV禁带宽度，导致二氧化锑只能吸收紫外光，这限制了二氧化钛的广泛应用。染料敏化、半导体复合、掺杂、表面等离子体共振等方法已经被用来改善二氧化钛对可见光的响应，增强光电效率。As an n-type semiconductor material, titanium dioxide has the advantages of good photocatalytic performance, high stability and low price, and has been widely used in optoelectronic devices, solar cells, photocatalysis, biosensing and other fields. The photoelectric performance of titanium dioxide is related to its shape. Compared with one-dimensional nanomaterials, three-dimensional materials have larger surface area, faster electron transfer speed, enhanced light absorption efficiency, and better photoelectric response. However, titanium dioxide has a band gap of 3.2 eV, so antimony dioxide can only absorb ultraviolet light, which limits the wide application of titanium dioxide. Dye sensitization, semiconductor recombination, doping, surface plasmon resonance and other methods have been used to improve the response of TiO to visible light and enhance the photoelectric efficiency.
二氧化钛与窄禁带半导体复合形成异质结构，不仅能够促进电荷的分离而且能提高对可见光吸收效率。氮化碳作为一种窄禁带半导体材料，具有良好的化学稳定性，可以与二氧化钛复合改善其光电转换效率。然而，半导体异质结构之间存在电子传递慢，电子空穴容易复合等缺点，又限制了光电转换效率的提高。因此，加快异质结构界面之间电子传递的速度，降低电子空穴复合，能够进一步改善光电转换效率。金纳米颗粒具有良好的光学性能，同时具有良好的导电性，能够吸收特定波长的光，产生表面等离子体共振效应，与半导体材料复合能够极大地改善对可见光的吸收，增强光电转换效率。Titanium dioxide is compounded with narrow-bandgap semiconductors to form a heterostructure, which can not only promote the separation of charges but also improve the absorption efficiency of visible light. As a narrow bandgap semiconductor material, carbon nitride has good chemical stability and can be combined with titanium dioxide to improve its photoelectric conversion efficiency. However, there are disadvantages such as slow electron transfer between semiconductor heterostructures and easy electron-hole recombination, which limits the improvement of photoelectric conversion efficiency. Therefore, accelerating the speed of electron transfer between heterostructure interfaces and reducing electron-hole recombination can further improve the photoelectric conversion efficiency. Gold nanoparticles have good optical properties and good electrical conductivity. They can absorb light of specific wavelengths and produce surface plasmon resonance effects. Combining with semiconductor materials can greatly improve the absorption of visible light and enhance photoelectric conversion efficiency.
发明内容Contents of the invention
本发明提供了一种在导电基体上制备三维树枝状二氧化钛纳米棒-金纳米-氮化碳三元复合纳米材料的方法，三维树枝状二氧化钛相比零维、一维、二维二氧化钛，具有更大的表面积，同时能够提高电子传递速率，碳化氮能够增加对可见光的吸收，金纳米颗粒不仅可以促进电子从氮化碳向三维树枝状二氧化钛纳米棒传递，同时具有等离子体表面共振效率，吸收特定波长的光产生热电子，增强光电效率。The invention provides a method for preparing a three-dimensional dendritic titanium dioxide nanorod-gold nanometer-carbon nitride ternary composite nanomaterial on a conductive substrate. Compared with zero-dimensional, one-dimensional and two-dimensional titanium dioxide, the three-dimensional dendritic titanium dioxide has more Large surface area can increase the electron transfer rate at the same time. Carbonized nitrogen can increase the absorption of visible light. Gold nanoparticles can not only promote the transfer of electrons from carbon nitride to three-dimensional dendritic titanium dioxide nanorods, but also have plasmon surface resonance efficiency and specific absorption. The wavelength of light generates hot electrons, enhancing the photoelectric efficiency.
为了解决上述技术问题，本发明提供一种在导电基体上制备三维树枝状二氧化钛纳米棒-金纳米-氮化碳三元复合纳米材料改善光电性能的方法，该三元复合材料的制备方法为：In order to solve the above-mentioned technical problems, the present invention provides a method for preparing a three-dimensional dendritic titanium dioxide nanorod-gold nano-carbon nitride ternary composite nanomaterial on a conductive substrate to improve photoelectric performance. The preparation method of the ternary composite material is:
（1）利用导电玻璃作为基底（1 cm宽，5 cm长），利用水热法在导电玻璃表面合成三维树枝状的二氧化钛纳米棒；(1) Using conductive glass as a substrate (1 cm wide and 5 cm long), three-dimensional dendritic titanium dioxide nanorods were synthesized on the surface of conductive glass by hydrothermal method;
（2）在三维树枝状二氧化钛纳米棒表面修饰一层金纳米颗粒；(2) Decorate a layer of gold nanoparticles on the surface of three-dimensional dendritic titanium dioxide nanorods;
（3）在金纳米修饰的三维树枝状二氧化钛纳米棒表面修饰一层氮化碳。(3) A layer of carbon nitride was decorated on the surface of three-dimensional dendritic titanium dioxide nanorods decorated with gold nanoparticles.
本发明所述的导电玻璃为氟掺杂氧化锡导电玻璃（FTO）。The conductive glass described in the present invention is fluorine-doped tin oxide conductive glass (FTO).
本发明所述三维树枝状二氧化钛纳米棒的制备过程如下：首先将FTO导电玻璃切割成1 cm宽、5 cm长大小，分别用丙酮、乙醇和二次水超声清洗10 min，配置40 mL 6 M HCl溶液磁力搅拌10 min，随后加入0.8 mL钛酸四丁酯原液继续搅拌30 min，将4片FTO导电面向下放入50 mL高压釜内衬中，将上述制备的混合溶液转入高压釜内衬，将高压釜拧紧，放入预先升温至150 ℃的烘箱中反应4 h，反应完毕，将高压釜冷却至室温，取出FTO用二次水冲洗，即得到二氧化钛纳米棒；随后将1 mL 6 M HCl加入40 mL二次水中搅拌10 min，然后加入0.5 mL三氯化钛溶液继续搅拌10 min，将上述制备的含有二氧化钛纳米棒FTO导电面向下置于上述溶液中，用保鲜膜封口，置入80 ℃烘箱中反应40 min，反应完毕取出用二次水冲洗，置于450 ℃马弗炉中煅烧1 h，升温速率5 ℃/min，即可得到三维树枝状二氧化钛纳米棒。The preparation process of the three-dimensional dendritic titanium dioxide nanorods of the present invention is as follows: firstly, cut the FTO conductive glass into 1 cm wide and 5 cm long sizes, ultrasonically clean them with acetone, ethanol and secondary water for 10 min, and prepare 40 mL of 6 M Magnetically stir the HCl solution for 10 min, then add 0.8 mL of tetrabutyl titanate stock solution and continue to stir for 30 min, put 4 pieces of FTO with the conductive surface down into the lining of a 50 mL autoclave, and transfer the mixed solution prepared above into the autoclave Lining, tighten the autoclave, and put it into an oven heated to 150 °C to react for 4 h. After the reaction is completed, cool the autoclave to room temperature, take out the FTO and rinse it with secondary water to obtain titanium dioxide nanorods; then add 1 mL of 6 M HCl was added to 40 mL of secondary water and stirred for 10 min, then 0.5 mL of titanium trichloride solution was added and continued to stir for 10 min, the FTO containing titanium dioxide nanorods prepared above was placed in the above solution with the conductive surface down, sealed with plastic wrap, and placed Put it in an oven at 80 °C for 40 min, take it out after the reaction, wash it with secondary water, place it in a muffle furnace at 450 °C for 1 h, and heat up at a rate of 5 °C/min to obtain three-dimensional dendritic titanium dioxide nanorods.
本发明所述金纳米修饰三维树枝状二氧化钛纳米棒的制备过程如下：首先制备10mM HAuCl4水溶液，然后用10 mM的NaOH溶液调节HAuCl4 pH至4.5，随后将制备的三维树枝状二氧化钛纳米棒FTO进入该溶液3 h，然后用二次水冲洗，将上述FTO导电面向上至于马弗炉中，450℃下煅烧2 h，升温速率为10℃/min。反应完毕后即可得到金纳米修饰三维树枝状二氧化钛纳米棒。The preparation process of gold nano-modified three-dimensional dendritic titanium dioxide nanorods of the present invention is as follows: first prepare 10mM HAuCl 4 aqueous solution, then adjust HAuCl 4 pH to 4.5 with 10 mM NaOH solution, then the prepared three-dimensional dendritic titanium dioxide nanorods FTO Enter the solution for 3 hours, then rinse with secondary water, put the conductive surface of the above-mentioned FTO in the muffle furnace, and calcinate at 450°C for 2 hours, and the heating rate is 10°C/min. After the reaction is completed, the gold nanometer modified three-dimensional dendritic titanium dioxide nanorod can be obtained.
本发明所述三维树枝状二氧化钛纳米棒-金纳米-氮化碳三元复合纳米材料制备过程如下：首先将5 g尿素溶于50 mL二次水中超声10 min，然后将制备得到的金纳米修饰三维树枝状二氧化钛纳米棒浸入该溶液中24 h，随后二次水冲洗，导电面向上至于马弗炉中500x ℃下煅烧30 min，升温速率为5℃/min。反应完毕后即可得到三维树枝状二氧化钛纳米棒-金纳米-氮化碳三元复合纳米材料。The preparation process of the three-dimensional dendritic titanium dioxide nanorod-gold nano-carbon nitride ternary composite nanomaterial of the present invention is as follows: first, 5 g of urea is dissolved in 50 mL of secondary water and ultrasonicated for 10 min, and then the prepared gold nanometer is modified The three-dimensional dendritic titanium dioxide nanorods were immersed in the solution for 24 h, then rinsed with water for the second time, and then calcined at 500x ℃ for 30 min in a muffle furnace with the conductive surface up, and the heating rate was 5 ℃/min. After the reaction is completed, a three-dimensional dendritic titanium dioxide nanorod-gold nanometer-carbon nitride ternary composite nanomaterial can be obtained.
本发明的有益效果：Beneficial effects of the present invention:
（1）合成三维树枝状二氧化钛纳米棒，相比其他二氧化钛材料具有更大的表面积，有利于改善光吸收；(1) Synthesis of three-dimensional dendritic titanium dioxide nanorods, which has a larger surface area than other titanium dioxide materials, which is conducive to improving light absorption;
（2）三维树枝状二氧化钛纳米棒表面修饰氮化碳能够改善对可见光吸收；(2) Three-dimensional dendritic titanium dioxide nanorods surface modified carbon nitride can improve the absorption of visible light;
（3）金纳米能够加速电子从氮化碳向二氧化钛传递，同时金纳米表面等离子体共振效应能够增强光电转换效率。(3) Gold nanometers can accelerate the transfer of electrons from carbon nitride to titanium dioxide, and the surface plasmon resonance effect of gold nanometers can enhance the photoelectric conversion efficiency.
说明书附图Instructions attached
下面结合附图和具体实施方案对本发明作进一步详细描述Below in conjunction with accompanying drawing and specific embodiment the present invention will be described in further detail
图1为该三维树枝状二氧化钛纳米棒-金纳米-氮化碳三元复合纳米材料制备方法示意图。Fig. 1 is a schematic diagram of the preparation method of the three-dimensional dendritic titanium dioxide nanorod-gold nano-carbon nitride ternary composite nanomaterial.
具体实施方式Detailed ways
三维树枝状二氧化钛纳米棒-金纳米-氮化碳三元复合纳米材料制备方法Preparation method of three-dimensional dendritic titanium dioxide nanorod-gold nano-carbon nitride ternary composite nanomaterial
（1）三维树枝状二氧化钛纳米棒的制备：首先将FTO导电玻璃切割成1 cm宽、5 cm长大小，依次用丙酮、乙醇以及二次水超声清洗10 min，清洗完毕后用氮气干燥，配置40 mL6 M的HCl溶液磁力搅拌10 min，随后加入0.8 mL钛酸四丁酯原液继续搅拌30 min，将4片FTO导电面向下放入50 mL高压釜内衬中，将上述制备的混合溶液转入高压釜内衬，将高压釜拧紧，放入预先升温至150 ℃的烘箱中反应4 h，反应完毕，将高压釜冷却至室温，取出FTO用二次水冲洗，即得到二氧化钛纳米棒；随后将1 mL 6 M HCl加入40 mL二次水中搅拌10 min，然后加入0.5 mL三氯化钛溶液继续搅拌10 min，将上述制备的含有二氧化钛纳米棒FTO导电面向下置于上述溶液中，用保鲜膜封口，置入80 ℃烘箱中反应40 min，反应完毕取出用二次水冲洗，置于450 ℃马弗炉中煅烧1 h，升温速率5 ℃/min，即可得到三维树枝状二氧化钛纳米棒。(1) Preparation of three-dimensional dendritic titanium dioxide nanorods: First, cut the FTO conductive glass into 1 cm wide and 5 cm long sizes, and then ultrasonically clean them with acetone, ethanol, and secondary water for 10 min, and dry them with nitrogen after cleaning. 40 mL of 6 M HCl solution was magnetically stirred for 10 min, then 0.8 mL of tetrabutyl titanate stock solution was added and continued to stir for 30 min, and 4 pieces of FTO were placed in the lining of a 50 mL autoclave with the conductive surface down, and the mixed solution prepared above was transferred to put into the inner lining of the autoclave, tighten the autoclave, and put it into an oven heated to 150 °C to react for 4 h. After the reaction was completed, the autoclave was cooled to room temperature, and the FTO was taken out and rinsed with secondary water to obtain titanium dioxide nanorods; then Add 1 mL of 6 M HCl into 40 mL of secondary water and stir for 10 min, then add 0.5 mL of titanium trichloride solution and continue stirring for 10 min, place the FTO containing titanium dioxide nanorods prepared above with the conductive surface down in the above solution, and use fresh-keeping The film was sealed and placed in an oven at 80 °C for 40 min. After the reaction was completed, it was taken out and rinsed with secondary water. It was calcined in a muffle furnace at 450 °C for 1 h at a heating rate of 5 °C/min to obtain three-dimensional dendritic titanium dioxide nanorods. .
（2）金纳米修饰三维树枝状二氧化钛纳米棒的制备：首先制备10 mM HAuCl4水溶液，然后用10 mM的NaOH溶液调节HAuCl4 pH至4.5，随后将制备的三维树枝状二氧化钛纳米棒FTO进入该溶液3 h，然后用二次水冲洗，将上述FTO导电面向上至于马弗炉中，450℃下煅烧2 h，升温速率为10℃/min。反应完毕后即可得到金纳米修饰三维树枝状二氧化钛纳米棒。(2) Preparation of gold nano-modified three-dimensional dendritic titanium dioxide nanorods: firstly prepare 10 mM HAuCl 4 aqueous solution, then adjust the pH of HAuCl 4 to 4.5 with 10 mM NaOH solution, and then inject the prepared three-dimensional dendritic titanium dioxide nanorods FTO into the solution for 3 h, then rinsed with secondary water, put the conductive surface of the above-mentioned FTO up in the muffle furnace, and calcined at 450 °C for 2 h with a heating rate of 10 °C/min. After the reaction is completed, the gold nanometer modified three-dimensional dendritic titanium dioxide nanorod can be obtained.
（3）三维树枝状二氧化钛纳米棒-金纳米-氮化碳三元复合纳米材料制备过程如下：首先将5 g尿素溶于50 mL二次水中超声10 min，然后将制备得到的金纳米修饰三维树枝状二氧化钛纳米棒浸入该溶液中24 h，随后二次水冲洗，导电面向上至于马弗炉中500x℃下煅烧30 min，升温速率为5℃/min。反应完毕后即可得到三维树枝状二氧化钛纳米棒-金纳米-氮化碳三元复合纳米材料。(3) The preparation process of three-dimensional dendritic titanium dioxide nanorods-gold nano-carbon nitride ternary composite nanomaterials is as follows: firstly, 5 g of urea was dissolved in 50 mL of secondary water and ultrasonicated for 10 min, and then the prepared gold nanoparticles were modified into three-dimensional The dendritic titanium dioxide nanorods were immersed in the solution for 24 h, then rinsed with water for the second time, and then calcined at 500x°C for 30 min in a muffle furnace with the conductive surface up, and the heating rate was 5°C/min. After the reaction is completed, a three-dimensional dendritic titanium dioxide nanorod-gold nanometer-carbon nitride ternary composite nanomaterial can be obtained.
将所制得的样品进行SEM、XRD以及紫外分析，所用扫描电子显微镜型号为FEIQUANTA 3D FESEM，XRD粉末衍射仪型号为Rigaku DMAX-RB, Japan CuKα，紫外分光光度计型号为Varian Cary 5000。The prepared samples were subjected to SEM, XRD and UV analysis. The scanning electron microscope model used was FEIQUANTA 3D FESEM, the XRD powder diffractometer model was Rigaku DMAX-RB, Japan CuKα, and the UV spectrophotometer model was Varian Cary 5000.
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| CN107973341A (en) * | 2017-06-21 | 2018-05-01 | 济南大学 | A kind of preparation method of three-dimensional titanium dioxide nano material |
| CN107475745B (en) * | 2017-08-23 | 2018-12-25 | 黄河科技学院 | A kind of phosphorus doping nitridation carbon composite modified titanic oxide optoelectronic pole, preparation method and the application of gold modification |
| CN108845119A (en) * | 2018-04-13 | 2018-11-20 | 济南大学 | A kind of construction method of the photic electrochemical immunosensor based on carrier double regulation control strategy |
| CN108993572A (en) * | 2018-08-09 | 2018-12-14 | 中国地质大学（北京） | A kind of preparation method of Fe2O3 doping tungstic acid-nitridation carbon compound film |
| CN109292733B (en) * | 2018-09-20 | 2019-09-20 | 济南大学 | Preparation of Flexible Paper-Based Platinum Nanoparticles-Hibranched Titanium Dioxide Nanotubes Composite |
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| CN104399457A (en) * | 2014-12-26 | 2015-03-11 | 中国科学院广州地球化学研究所 | A kind of Au/TiO2/CFP ternary composite nano photocatalyst and its preparation method and application |
| CN104677892A (en) * | 2015-03-27 | 2015-06-03 | 济南大学 | Method for preparing electrochemiluminescence biological sensing interface based on loaded graphite phase carbon nitride and application thereof |
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