CN108017084B - preparation method of titanium dioxide/copper sulfide core shell - Google Patents
preparation method of titanium dioxide/copper sulfide core shell Download PDFInfo
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Abstract
A preparation method of a titanium dioxide/copper sulfide core shell comprises the following steps: (1) adding titanium dioxide P25 powder into a sodium hydroxide solution, stirring, carrying out hydrothermal reaction on a product, carrying out solid-liquid separation on the reacted product, washing, drying, grinding and calcining to obtain a titanium dioxide nanorod; (2) and (2) adding the titanium dioxide nanorods obtained in the step (1) into a 3-mercaptopropionic acid solution, stirring, adding a copper source, stirring again, adding a sulfur source, continuously stirring, performing solid-liquid separation on the product, washing, drying and grinding to obtain the titanium dioxide/copper sulfide core-shell product. Compared with a pure nanorod structure, the titanium dioxide/copper sulfide core-shell structure prepared by the invention can increase the specific surface area and improve the electron mobility.
Description
Technical Field
The invention belongs to the technical field of synthesis of nano materials, and particularly relates to a preparation method of a titanium dioxide/copper sulfide core shell.
background
The titanium dioxide (TiO 2) is an important multifunctional inorganic material, and has the advantages of no toxicity, low cost, higher chemical stability and the like, unique photocatalytic performance, excellent color effect, ultraviolet shielding and other functions, and has wide application prospects in the fields of catalyst carriers, ultraviolet-resistant absorbers, functional ceramics, gas-sensitive sensing devices and the like.
In recent years, titanium dioxide/copper sulfide with different morphologies is reported successively, but reports on titanium dioxide/copper sulfide core shells are extremely rare. Compared with other morphologies, the titanium dioxide/copper sulfide core shell has higher specific surface area and faster electron mobility, so that the titanium dioxide/copper sulfide core shell has great application potential in the fields of photocatalysis, dye-sensitized solar cells, sensors and the like.
Yu and the like firstly use acetic acid as a solvent, tetrabutyl titanate as a titanium source, and prepare uniform TiO 2 nanospheres by a hydrothermal method, then use L-cysteine as an inducer, sodium sulfide as a sulfur source, and copper nitrate as a copper source, and obtain a titanium dioxide/copper sulfide composite material (Shuyan Yu, Jincheng Liu, Yan Zhou, et al. ACS Sustainable Chem. Eng,2017,5(2): 1347-1357) by the hydrothermal method.
CN107051545A discloses a nano titanium dioxide/copper sulfide nano composite material, a titanium dioxide nanowire prepared by a hydrothermal method is used as a reaction substrate, a composite structure of a copper sulfide nanosheet and the titanium dioxide nanowire is successfully prepared by a secondary hydrothermal method at 100 ℃ for 10h, and the influence of hydrothermal temperature and hydrothermal time on the photocatalytic performance of the composite structure is explored, but the copper sulfide coated titanium dioxide synthesized by the method is not uniform, so that the performance of the final product is influenced.
disclosure of Invention
therefore, one of the purposes of the invention is to provide a preparation method of titanium dioxide/copper sulfide core shell. The titanium dioxide/copper sulfide core shell prepared by the invention has an obvious shell layer. Compared with a pure nanorod structure, the core-shell structure can increase the specific surface area and improve the electron mobility.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a titanium dioxide/copper sulfide core shell comprises the following steps:
(1) Adding titanium dioxide P25 powder into a sodium hydroxide solution, stirring, carrying out hydrothermal reaction on a product, carrying out solid-liquid separation on the reacted product, washing, drying, grinding and calcining to obtain a titanium dioxide nanorod;
(2) And (2) adding the titanium dioxide nanorods obtained in the step (1) into a 3-mercaptopropionic acid solution, stirring, adding a copper source, stirring again, adding a sulfur source, continuously stirring, performing solid-liquid separation on the product, washing, drying and grinding to obtain the titanium dioxide/copper sulfide core-shell product.
Preferably, the molar volume ratio mmol/mL of the titanium dioxide P25 and the sodium hydroxide solution in the step (1) is 1:10-20, for example, 1:12, 1:15, 1:17, 1:19, etc., preferably 1: 14.
preferably, the concentration of the sodium hydroxide solution is 8-12mol/L, such as 9mol/L, 11mol/L, etc., preferably 10 mol/L.
Preferably, the temperature of the hydrothermal reaction is 100-240 ℃, preferably 120 ℃, and the time is 10-24h, preferably 10 h. The hydrothermal method is a commonly used method for preparing nano materials, and generally generates a small amount of impurities, while the hydrothermal reaction does not generate impurities in the method. Therefore, the product prepared by the method has higher purity, so that the product has better performance in application.
Preferably, the calcination is carried out at a temperature of 500-600 deg.C, preferably 500 deg.C, for a period of 2-4 hours, preferably 2 hours. The invention has the advantages of low calcination temperature, short calcination time and reduced energy consumption.
Preferably, the drying temperature is 40-80 ℃, the drying time is 12-24h, the product after the hydrothermal reaction is amorphous, the product after the hydrothermal reaction is dried under the condition, the change of the crystal form of the product cannot be influenced, an amorphous precursor before calcination can be formed, and preparation is made for the calcined crystal form change, preferably 12 h.
preferably, the nanorods obtained in step (1) have an average size of 80-120nm, preferably 100 nm.
Preferably, the copper source in step (2) is copper nitrate and the sulfur source is sodium thiosulfate.
Preferably, the molar ratio of the titanium dioxide nanorods obtained in step (1) to the copper source is 1.5-2.5:1, such as 1.7:1, 1.9:1, 2.1:1, 2.4:1, etc., preferably 2:1, and the molar ratio of the copper source to the sulfur source is 0.5-2:1, such as 0.7:1, 0.9:1, 1.2:1, 1.5:1, 1.8:1, etc., preferably 1: 1.
Preferably, the copper source is added and then stirred for 2-5h, the solution is uniformly mixed by stirring under the conditions, and meanwhile, the copper source and the titanium dioxide can be better combined by proper stirring time, so that a foundation is laid for the formation of titanium dioxide/copper sulfide, and the stirring time is preferably 3 h.
Preferably, the solution is stirred for 2 to 5 hours after the sulfur source is added, the solution is uniformly mixed by stirring under the conditions, and meanwhile, the copper source and the titanium dioxide can be better combined by proper stirring time, so that a foundation is laid for the formation of titanium dioxide/copper sulfide, and the stirring time is preferably 3 hours.
preferably, the drying temperature is 40-80 ℃ and the drying time is 12-24 h.
The solid-liquid separation in the present invention can be carried out by a conventional method such as filtration, centrifugation or the like, and preferably, centrifugation. The separated solid matter may be washed with distilled water.
The titanium dioxide/copper sulfide core-shell prepared by the method has the average diameter of about 100 nm.
The invention has the following beneficial effects:
1. The titanium dioxide/copper sulfide core shell prepared by the invention has an obvious shell layer. Compared with a pure nanorod structure, the core-shell structure can increase the specific surface area and improve the electron mobility.
2. The product is amorphous after drying, so calcination is required to effect the conversion of the crystalline form. The invention has the advantages of relatively low calcining temperature, short calcining time and reduced energy consumption. The hydrothermal method is a commonly used method for preparing nano materials, and generally generates a small amount of impurities or even a large amount of impurities, while the hydrothermal reaction does not generate impurities in the method. Therefore, the product prepared by the method has higher purity, so that the product has better performance in application.
3. according to the invention, P25, copper nitrate and sodium thiosulfate are used as raw materials, and 3-mercaptopropionic acid is used as an inducer to prepare the titanium dioxide/copper sulfide core-shell, wherein the average diameter of the titanium dioxide/copper sulfide core-shell is about 100 nm.
4. The proportion of P25 to the copper nitrate and sodium thiosulfate is necessary for realizing the invention, and when the proportion of P25 to the copper nitrate and sodium thiosulfate is larger, the shell thickness is reduced. When the proportion of P25, copper nitrate and sodium thiosulfate is reduced, the product does not have the shape disclosed in the invention, and the product prepared according to the proportion disclosed by the invention is regular in shape, uniform and good in dispersity, and can be used in the fields of catalyst carriers, ultraviolet-resistant absorbers, functional ceramics, gas-sensitive sensing devices and the like.
Detailed Description
For the purpose of facilitating an understanding of the present invention, the present invention will now be described by way of examples. It should be understood by those skilled in the art that the examples are only for the purpose of facilitating understanding of the present invention and should not be construed as specifically limiting the present invention.
Example 1
(1) 5.71mmol of P25 were added to 80mL of sodium hydroxide solution (10M), stirred at room temperature for 2h, the reaction medium was then transferred to a reaction vessel, heated at 120 ℃ for 10h, the white precipitate solution obtained after cooling was centrifuged and the precipitate obtained was washed repeatedly with distilled water. And drying the obtained precipitate at 40 ℃ for 12h, grinding the dried precipitate, and calcining the ground precipitate at 500 ℃ for 2h to obtain the titanium dioxide nano-rod with the diameter of about 100 nm.
(2) 1.4mmol of titanium dioxide nanorods are dissolved in 20 mu L of 3-mercaptopropionic acid and 100mL of distilled water solution, stirred at room temperature for 2h, then 0.7mmol of copper nitrate is added, stirred for 3h, then 0.7mmol of sodium thiosulfate is added, the obtained white precipitate solution is centrifuged after continuous stirring for 3h, and the obtained precipitate is repeatedly washed with distilled water. The resulting precipitate was dried at 40 ℃ for 12h and ground to obtain a titanium dioxide/copper sulfide core shell.
Example 2
(1) 5.71mmol of P25 were added to 80mL of sodium hydroxide solution (10M), stirred at room temperature for 2h, the reaction medium was then transferred to a reaction vessel, heated at 100 ℃ for 10h, the white precipitate solution obtained after cooling was centrifuged and the precipitate obtained was washed repeatedly with distilled water. And drying the obtained precipitate at 40 ℃ for 12h, grinding the dried precipitate, and calcining the ground precipitate at 500 ℃ for 2h to obtain the titanium dioxide nano-rod with the diameter of about 100 nm.
(2) 1.4mmol of titanium dioxide nanorods are dissolved in 20 mu L of 3-mercaptopropionic acid and 100mL of distilled water solution, stirred at room temperature for 2h, then 0.7mmol of copper nitrate is added, stirred for 3h, then 0.7mmol of sodium thiosulfate is added, the obtained white precipitate solution is centrifuged after continuous stirring for 3h, and the obtained precipitate is repeatedly washed with distilled water. The resulting precipitate was dried at 40 ℃ for 12h and ground to obtain a titanium dioxide/copper sulfide core shell.
Example 3
(1) 5.71mmol of P25 were added to 80mL of sodium hydroxide solution (10M), stirred at room temperature for 2h, the reaction medium was then transferred to a reaction vessel, heated at 150 ℃ for 10h, the white precipitate solution obtained after cooling was centrifuged and the precipitate obtained was washed repeatedly with distilled water. And drying the obtained precipitate at 40 ℃ for 12h, grinding the dried precipitate, and calcining the ground precipitate at 500 ℃ for 2h to obtain the titanium dioxide nano-rod with the diameter of about 100 nm.
(2) 1.4mmol of titanium dioxide nanorods are dissolved in 20 mu L of 3-mercaptopropionic acid and 100mL of distilled water solution, stirred at room temperature for 2h, then 0.7mmol of copper nitrate is added, stirred for 3h, then 0.7mmol of sodium thiosulfate is added, the obtained white precipitate solution is centrifuged after continuous stirring for 3h, and the obtained precipitate is repeatedly washed with distilled water. The resulting precipitate was dried at 40 ℃ for 12h and ground to obtain a titanium dioxide/copper sulfide core shell.
Example 4
(1) 5.71mmol of P25 were added to 80mL of sodium hydroxide solution (10M), stirred at room temperature for 2h, the reaction medium was then transferred to a reaction vessel, heated at 120 ℃ for 10h, the white precipitate solution obtained after cooling was centrifuged and the precipitate obtained was washed repeatedly with distilled water. And drying the obtained precipitate at 40 ℃ for 12h, grinding the dried precipitate, and calcining the ground precipitate at 400 ℃ for 2h to obtain the titanium dioxide nano-rod with the diameter of about 100 nm.
(2) 1.4mmol of titanium dioxide nanorods are dissolved in 20 mu L of 3-mercaptopropionic acid and 100mL of distilled water solution, stirred at room temperature for 2h, then 0.7mmol of copper nitrate is added, stirred for 3h, then 0.7mmol of sodium thiosulfate is added, the obtained white precipitate solution is centrifuged after continuous stirring for 3h, and the obtained precipitate is repeatedly washed with distilled water. The resulting precipitate was dried at 40 ℃ for 12h and ground to obtain a titanium dioxide/copper sulfide core shell.
Example 5
(1) 5.71mmol of P25 were added to 80mL of sodium hydroxide solution (10M), stirred at room temperature for 2h, the reaction medium was then transferred to a reaction vessel, heated at 120 ℃ for 10h, the white precipitate solution obtained after cooling was centrifuged and the precipitate obtained was washed repeatedly with distilled water. And drying the obtained precipitate at 40 ℃ for 12h, grinding the dried precipitate, and calcining the ground precipitate at 600 ℃ for 2h to obtain the titanium dioxide nano-rod with the diameter of about 100 nm.
(2) 1.4mmol of titanium dioxide nanorods are dissolved in 20 mu L of 3-mercaptopropionic acid and 100mL of distilled water solution, stirred at room temperature for 2h, then 0.7mmol of copper nitrate is added, stirred for 3h, then 0.7mmol of sodium thiosulfate is added, the obtained white precipitate solution is centrifuged after continuous stirring for 3h, and the obtained precipitate is repeatedly washed with distilled water. The resulting precipitate was dried at 40 ℃ for 12h and ground to obtain a titanium dioxide/copper sulfide core shell.
Example 6
(1) 5.71mmol of P25 were added to 80mL of sodium hydroxide solution (10M), stirred at room temperature for 2h, the reaction medium was then transferred to a reaction vessel, heated at 120 ℃ for 10h, the white precipitate solution obtained after cooling was centrifuged and the precipitate obtained was washed repeatedly with distilled water. And drying the obtained precipitate at 80 ℃ for 20h, grinding the dried precipitate, and calcining the ground precipitate at 600 ℃ for 2h to obtain the titanium dioxide nano-rod with the diameter of about 100 nm.
(2) 1.4mmol of titanium dioxide nanorods are dissolved in 20 mu L of 3-mercaptopropionic acid and 100mL of distilled water solution, stirred at room temperature for 2h, then 0.7mmol of copper nitrate is added, stirred for 3h, then 0.7mmol of sodium thiosulfate is added, the obtained white precipitate solution is centrifuged after continuous stirring for 3h, and the obtained precipitate is repeatedly washed with distilled water. And drying the obtained precipitate at 60 ℃ for 20h, and grinding to obtain the titanium dioxide/copper sulfide core shell.
The titanium dioxide/copper sulfide core-shell composite materials prepared in the above examples 1 to 6 were subjected to electrochemical performance tests, and the capacitance performance thereof was studied. The cyclic voltammetry and constant-current charge and discharge tests in the electrochemical method are adopted to research the super-capacitance performance of the material, including the specific capacitance and the cyclic stability of the material. It can be seen from the cyclic voltammetry curve that the curve shows very good reversibility, the graph surrounded by the curve is similar to a rectangle, and the maximum specific capacitance of the titanium dioxide/copper sulfide core-shell nanocomposite prepared in the above examples 1-6 is calculated to be between 402 and 445F/g, which is far larger than that of the current commercial carbon-based cathode material. Also, the constant current charge-discharge curve shows very good reversibility and capacitance. After ten thousand cycles of charge and discharge, the capacitance value still keeps more than 80 percent of the original capacitance value. In conclusion, the titanium dioxide/copper sulfide core-shell nano composite material has very good super-capacitance performance and has great prospect in the aspect of energy storage.
Comparative example 1
Same as example 1, except that the amount of titanium dioxide nanorods was 2.8mmol, and the amount of sodium thiosulfate was 0.2 mmol.
The electrochemical performance test of the materials obtained by the method is that the maximum specific capacitance is 302F/g, and the capacitance value is 70 percent of the original capacitance value after ten thousand cycles of cyclic charge and discharge.
Comparative example 2
the same as example 1 except that the drying temperature in step (1) was 100 ℃.
The electrochemical performance test of the materials obtained by the method is that the maximum specific capacitance is 338F/g, and the capacitance value is 73 percent of the original capacitance value after ten thousand cycles of cyclic charge and discharge.
It should be understood that the above examples are only for clarity of illustration and are not intended to limit the embodiments. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. And obvious variations or modifications therefrom are within the scope of the invention.
Claims (6)
1. A preparation method of a titanium dioxide/copper sulfide core-shell structure comprises the following steps:
(1) Adding 5.71mmol P25 into 80mL10M sodium hydroxide solution, stirring at room temperature for 2h, transferring the reaction medium into a reaction kettle, heating at 120 ℃ for 10h, cooling, centrifuging the obtained white precipitate, and repeatedly washing the obtained precipitate with distilled water; drying the obtained precipitate at 40 ℃ for 12h, grinding the dried precipitate, and calcining at 500 ℃ for 2h to obtain a titanium dioxide nanorod with the diameter of 100 nm;
(2) Adding 1.4mmol of titanium dioxide nanorods into 20 mu L of 3-mercaptopropionic acid and 100mL of distilled water solution, stirring for 2h at room temperature, then adding 0.7mmol of copper nitrate, stirring for 3h, then adding 0.7mmol of sodium thiosulfate, continuously stirring for 3h, centrifuging the obtained white precipitate, and repeatedly washing the obtained precipitate with distilled water; and drying the obtained precipitate at 40 ℃ for 12h, and grinding to obtain the titanium dioxide/copper sulfide core-shell structure.
2. A preparation method of a titanium dioxide/copper sulfide core-shell structure comprises the following steps:
(1) Adding 5.71mmol P25 into 80mL10M sodium hydroxide solution, stirring at room temperature for 2h, transferring the reaction medium into a reaction kettle, heating at 100 ℃ for 10h, cooling, centrifuging the obtained white precipitate, and repeatedly washing the obtained precipitate with distilled water; drying the obtained precipitate at 40 ℃ for 12h, grinding the dried precipitate, and calcining at 500 ℃ for 2h to obtain a titanium dioxide nanorod with the diameter of 100 nm;
(2) Adding 1.4mmol of titanium dioxide nanorods into 20 mu L of 3-mercaptopropionic acid and 100mL of distilled water solution, stirring for 2h at room temperature, then adding 0.7mmol of copper nitrate, stirring for 3h, then adding 0.7mmol of sodium thiosulfate, continuously stirring for 3h, centrifuging the obtained white precipitate, and repeatedly washing the obtained precipitate with distilled water; and drying the obtained precipitate at 40 ℃ for 12h, and grinding to obtain the titanium dioxide/copper sulfide core-shell structure.
3. A preparation method of a titanium dioxide/copper sulfide core-shell structure comprises the following steps:
(1) adding 5.71mmol P25 into 80mL10M sodium hydroxide solution, stirring at room temperature for 2h, transferring the reaction medium into a reaction kettle, heating at 150 ℃ for 10h, cooling, centrifuging the obtained white precipitate, and repeatedly washing the obtained precipitate with distilled water; drying the obtained precipitate at 40 ℃ for 12h, grinding the dried precipitate, and calcining at 500 ℃ for 2h to obtain a titanium dioxide nanorod with the diameter of 100 nm;
(2) Adding 1.4mmol of titanium dioxide nanorods into 20 mu L of 3-mercaptopropionic acid and 100mL of distilled water solution, stirring for 2h at room temperature, then adding 0.7mmol of copper nitrate, stirring for 3h, then adding 0.7mmol of sodium thiosulfate, continuously stirring for 3h, centrifuging the obtained white precipitate, and repeatedly washing the obtained precipitate with distilled water; and drying the obtained precipitate at 40 ℃ for 12h, and grinding to obtain the titanium dioxide/copper sulfide core-shell structure.
4. A preparation method of a titanium dioxide/copper sulfide core-shell structure comprises the following steps:
(1) Adding 5.71mmol P25 into 80mL10M sodium hydroxide solution, stirring at room temperature for 2h, transferring the reaction medium into a reaction kettle, heating at 120 ℃ for 10h, cooling, centrifuging the obtained white precipitate, and repeatedly washing the obtained precipitate with distilled water; drying the obtained precipitate at 40 ℃ for 12h, grinding the dried precipitate, and calcining at 400 ℃ for 2h to obtain a titanium dioxide nanorod with the diameter of 100 nm;
(2) Adding 1.4mmol of titanium dioxide nanorods into 20 mu L of 3-mercaptopropionic acid and 100mL of distilled water solution, stirring for 2h at room temperature, then adding 0.7mmol of copper nitrate, stirring for 3h, then adding 0.7mmol of sodium thiosulfate, continuously stirring for 3h, centrifuging the obtained white precipitate, and repeatedly washing the obtained precipitate with distilled water; and drying the obtained precipitate at 40 ℃ for 12h, and grinding to obtain the titanium dioxide/copper sulfide core-shell structure.
5. A preparation method of a titanium dioxide/copper sulfide core-shell structure comprises the following steps:
(1) adding 5.71mmol P25 into 80mL10M sodium hydroxide solution, stirring at room temperature for 2h, transferring the reaction medium into a reaction kettle, heating at 120 ℃ for 10h, cooling, centrifuging the obtained white precipitate, and repeatedly washing the obtained precipitate with distilled water; drying the obtained precipitate at 40 ℃ for 12h, grinding the dried precipitate, and calcining at 600 ℃ for 2h to obtain a titanium dioxide nanorod with the diameter of 100 nm;
(2) Adding 1.4mmol of titanium dioxide nanorods into 20 mu L of 3-mercaptopropionic acid and 100mL of distilled water solution, stirring for 2h at room temperature, then adding 0.7mmol of copper nitrate, stirring for 3h, then adding 0.7mmol of sodium thiosulfate, continuously stirring for 3h, centrifuging the obtained white precipitate, and repeatedly washing the obtained precipitate with distilled water; and drying the obtained precipitate at 40 ℃ for 12h, and grinding to obtain the titanium dioxide/copper sulfide core-shell structure.
6. A preparation method of a titanium dioxide/copper sulfide core-shell structure comprises the following steps:
(1) Adding 5.71mmol P25 into 80mL10M sodium hydroxide solution, stirring at room temperature for 2h, transferring the reaction medium into a reaction kettle, heating at 120 ℃ for 10h, cooling, centrifuging the obtained white precipitate, and repeatedly washing the obtained precipitate with distilled water; drying the obtained precipitate at 80 ℃ for 20h, grinding the dried precipitate, and calcining at 600 ℃ for 2h to obtain a titanium dioxide nanorod with the diameter of 100 nm;
(2) adding 1.4mmol of titanium dioxide nanorods into 20 mu L of 3-mercaptopropionic acid and 100mL of distilled water solution, stirring for 2h at room temperature, then adding 0.7mmol of copper nitrate, stirring for 3h, then adding 0.7mmol of sodium thiosulfate, continuously stirring for 3h, centrifuging the obtained white precipitate, and repeatedly washing the obtained precipitate with distilled water; and drying the obtained precipitate at 60 ℃ for 20h, and grinding to obtain the titanium dioxide/copper sulfide core-shell structure.
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