CN109680314B - Preparation method of SnS nanotube film or SnS nanorod film - Google Patents
Preparation method of SnS nanotube film or SnS nanorod film Download PDFInfo
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- CN109680314B CN109680314B CN201910142133.5A CN201910142133A CN109680314B CN 109680314 B CN109680314 B CN 109680314B CN 201910142133 A CN201910142133 A CN 201910142133A CN 109680314 B CN109680314 B CN 109680314B
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Abstract
The invention discloses a preparation method of a SnS nanorod/tube film, wherein the deposition temperature is 10-18 ℃, and the humidity is not higher than 50%. Sequentially adding soluble stannous salt and thio compound into deionized water or organic solvent, stirring, adding citric acid or citrate, continuously stirring, adding acid, adjusting the pH value of the solution, and clarifying the solution; adding alkali to adjust the pH value of the solution to 1.5 to obtain a precursor solution; and then depositing in a precursor solution by using the FTO as a working electrode, a platinum wire as a counter electrode and an Ag/AgCl electrode as a reference electrode, intermittently stirring the solution in the deposition process, washing and drying the deposited SnS nano film by using deionized water, and controlling the deposition voltage to obtain the SnS nano rod/tube film. The preparation method is environment-friendly, simple to operate, can strictly control each step of operation, is low in cost of the used precursor material, and is beneficial to improving the photoelectric property of the prepared film.
Description
Technical Field
The invention relates to a preparation method of a semiconductor thin film material, in particular to a preparation method of a chalcogenide semiconductor thin film material, which is applied to the technical field of light absorption layer materials of thin film photovoltaic cells.
Background
With the gradual depletion of traditional fossil energy and the gradual increase of environmental pollution, people pay more attention to environmental protection awareness and sustainable development concept, and it is an important issue to find a renewable clean energy to replace the traditional fossil energy. Solar energy is one of ideal energy sources for human beings as a novel energy source which is inexhaustible, inexhaustible and nontoxic and pollution-free. Solar energy can be directly converted into electric energy by utilizing the photovoltaic effect, and the cost of the existing crystal silicon cell which uses more crystal silicon cells is higher, so that the development of a cheap, environment-friendly and efficient solar cell material becomes a research hotspot in recent years.
The chalcogenide semiconductor film has good application prospect in future photoelectric devices due to the unique photoelectric property thereof, particularly in high-efficiency low-cost thin-film solar cells, thereby drawing extensive attention and research interest of people. Among the many chalcogenide thin film materials, tin sulfide (SnS) thin film is one of the representative materials. The S and Sn elements forming the SnS are abundant on the earth. In general, its conductivity type is p-type due to the presence of Sn vacancies in the SnS. The optical direct band gap and the indirect band gap of the SnS are respectively 1.2-1.5 eV and 1.0-1.1 eV, and the SnS has good spectral matching with solar radiation, so the SnS is very suitable for being used as a light absorption layer in a solar cell. The theoretical photoelectric conversion efficiency is up to 25%. It is a novel thin film photovoltaic cell absorption layer material with great potential. The SnS film can be prepared by a chemical vapor transport method, a chemical deposition method, an electrodeposition method and the like, and the characteristics of the prepared material are to be further improved. Among the methods, the electrodeposition method has the advantages of simple process equipment, low cost, suitability for large-area preparation and the like, but the conventional electrodeposition method for preparing the chalcogenide compound semiconductor film usually requires higher temperature and vacuum equipment, has low utilization rate of raw materials, has higher cost for preparing chalcogenide compound semiconductor film materials, and needs to improve the quality because the cost for preparing large-area SnS thin film solar cells is not ideal.
Disclosure of Invention
In order to solve the problems of the prior art, the invention aims to overcome the defects in the prior art and provide a preparation method of a SnS nanotube film or a SnS nanorod film, which can be used for preparing a low-cost and high-quality SnS nanorod/tube film, and has the advantages of simple operation and low cost of used precursor materials.
In order to achieve the purpose, the invention adopts the following technical scheme:
a preparation method of a SnS nanotube film or a SnS nanorod film comprises the following steps:
a. firstly, regulating and controlling the deposition temperature to be 10-18 ℃, controlling the humidity to be not higher than 50%, under the conditions of the temperature and the humidity, sequentially adding 0.025-0.05 mol of soluble divalent tin salt and 0.025-0.05 mol of thio compound into a beaker containing 100-200 ml of deionized water or organic solvent, stirring for 1-2 minutes to obtain a mixed solution, then continuously adding 0.02-0.06 mol of citric acid or citrate into the mixed solution, and continuously stirring for 2-3 minutes; adding acid into the mixed solution to adjust the pH of the mixed solution to 0.6-0.8, and clarifying the mixed solution; adding alkali into the mixed solution, and adjusting the pH of the mixed solution to 1.5 to obtain an electrodeposition precursor solution;
b. depositing in the electrodeposition precursor solution prepared in the step a for 3-10 minutes by taking FTO as a working electrode, a platinum wire as a counter electrode and an Ag/AgCl electrode as a reference electrode, and controlling the deposition voltage to be-0.8V-1.1V; intermittently stirring the electro-deposition precursor solution in the deposition process, controlling the stirring speed to be 300-500 r/min, and then washing and drying the deposited SnS nano film by using deionized water;
in the step b, when the deposition voltage is controlled to be-0.8 to-0.9V, the SnS nanotube film is prepared; or when the deposition voltage is controlled to be-1.0 to-1.1V, the SnS nano-rod film is prepared.
In the step a, any one of stannous chloride, stannous sulfate and stannous acetate or a hydrate of the salt is used as the soluble stannous salt.
In a preferred embodiment of the present invention, in step a, the thio compound is any one salt or a hydrate of a salt of sodium thiosulfate, thioacetamide and thiourea.
In the step a, sulfuric acid, acetic acid or hydrochloric acid is used as the acid to be added when adjusting the pH of the mixed solution.
In the step a, when the pH value of the mixed solution is adjusted, the added alkali is NaOH, ammonia water or KOH.
In a preferred embodiment of the present invention, in step a, trisodium citrate or potassium citrate is used as the citrate.
In a preferred embodiment of the present invention, in the step a, the organic solvent is one or a mixture of two of alcohol and acetone.
In the step b, the deposition temperature is controlled to be 10-18 ℃, the humidity is controlled to be not higher than 50%, and the SnS nano-film is prepared by electrodeposition under the conditions of the temperature and the humidity.
In the step b, the electrodeposition precursor solution is intermittently stirred during the deposition process, and the interval time is not more than 250 s.
Compared with the prior art, the invention has the following obvious and prominent substantive characteristics and remarkable advantages:
1. the method requires that the deposition temperature is 10-18 ℃, the humidity is lower than 50%, the process conditions are mild, the preparation method of the SnS nanorod/tube film is simple, the experimental conditions can be strictly controlled, the cost of the used precursor material is low, the method is suitable for large-scale production, and the preparation process is green and environment-friendly;
2. the film prepared by the method is beneficial to improving the electron transmission performance, and can provide certain help for preparing high-performance film solar cell devices.
3. The method of the invention prepares the SnS nano-rod/tube on the FTO conductive glass substrate, can obtain the SnS with controllable stoichiometric ratio without expensive vacuum equipment and higher reaction temperature, has very high utilization rate of raw materials, and provides a brand-new idea for developing large-area SnS thin-film solar cells and reducing the preparation cost thereof.
Drawings
Fig. 1 is an X-ray diffraction pattern of the SnS nanotube film prepared in the first embodiment of the present invention.
Fig. 2 is a surface SEM image of the SnS nanotube film prepared in the first embodiment of the present invention.
Fig. 3 is a raman spectrum of the SnS nanotube film prepared in the first embodiment of the present invention.
FIG. 4 is an X-ray diffraction pattern of a SnS nanorod film prepared in example two of the present invention.
FIG. 5 is a surface SEM image of a SnS nanorod film prepared in example two of the present invention.
Fig. 6 is a raman spectrum of the SnS nanorod film prepared in example two of the present invention.
Detailed Description
The above-described scheme is further illustrated below with reference to specific embodiments, which are detailed below:
the first embodiment is as follows:
in this embodiment, referring to fig. 1 to 3, a method for preparing an SnS nanotube film includes the following steps:
a. firstly, regulating and controlling the deposition temperature to be 10-18 ℃, controlling the humidity to be lower than 50%, sequentially adding 0.025mol of stannous chloride dihydrate and 0.025mol of sodium thiosulfate pentahydrate into a beaker containing 100ml of deionized water under the conditions of the temperature and the humidity, stirring for 1-2 minutes for reaction to obtain a mixed solution, then continuously adding 0.04mol of trisodium citrate into the mixed solution, and continuously stirring for 2-3 minutes, wherein the solution is a yellow turbid solution; adding sulfuric acid into the mixed solution to adjust the pH value of the mixed solution to 0.8, so that the mixed solution is clarified; then adding NaOH into the mixed solution, and adjusting the pH of the mixed solution to 1.5 to obtain an electrodeposition precursor solution;
b. controlling the deposition temperature to be 10-18 ℃ and the humidity to be not higher than 50%, and carrying out electrodeposition to prepare the SnS nano film under the conditions of the temperature and the humidity, wherein the method specifically comprises the following steps:
the electrode clamp with the clean FTO is used as a working electrode, a platinum wire is used as a counter electrode, an Ag/AgCl electrode is used as a reference electrode, the prepared electro-deposition precursor solution with the pH value of 1.5 in the step a is deposited for 10 minutes, the deposition voltage is controlled to be-0.9V, the electro-deposition precursor solution is intermittently stirred in the deposition process, the stirring speed is controlled to be 300 revolutions per minute, the interval time is controlled to be 250s, and then the deposited SnS nano film is washed by deionized water and dried to obtain the SnS nano tube film.
Experimental test analysis:
the performance of the SnS nanotube film prepared in this example was tested, and fig. 1 is an XRD energy spectrum analysis of the SnS nanotube film deposited in this example at-0.9V. Diffraction angles of 22.01 degrees, 26.01 degrees, 31.53 degrees, 31.97 degrees, 39.33 degrees, 15.49 degrees and 66.37 degrees in the figure respectively correspond to diffraction peaks of (110), (120), (111), (040), (041), (002) and (152) in standard PDF cards JCPDS No.39-0354 of SnS. FIG. 2 is a surface SEM image of a SnS nanotube film deposited under-0.9V voltage in the present example. As can be seen from the surface diagram, the SnS film has a nanotube-like structure, and the nanotubes are relatively long. FIG. 3 is a Raman diffraction peak spectrum of the SnS nanotube film deposited under-0.9V voltage in the present example. In the figure at 94cm-1、155cm-1、181cm-1、216cm-1Has obvious diffraction peak, corresponding to SnS material. Raman diffraction shows that the prepared SnS nanotube film is relatively pure in phase and no other impurity phase is generated.
Example two:
this embodiment is substantially the same as the first embodiment, and is characterized in that:
in this embodiment, referring to fig. 4 to 6, a method for preparing an SnS nanorod film includes the following steps:
a. firstly, regulating and controlling the deposition temperature to be 10-18 ℃, controlling the humidity to be lower than 50%, sequentially adding 0.025mol of stannous chloride dihydrate and 0.025mol of sodium thiosulfate pentahydrate into a beaker containing 100ml of deionized water under the conditions of the temperature and the humidity, stirring for 1-2 minutes for reaction to obtain a mixed solution, then continuously adding 0.04mol of trisodium citrate into the mixed solution, and continuously stirring for 2-3 minutes, wherein the solution is a yellow turbid solution; adding sulfuric acid into the mixed solution to adjust the pH value of the mixed solution to 0.8, so that the mixed solution is clarified; then adding NaOH into the mixed solution, and adjusting the pH of the mixed solution to 1.5 to obtain an electrodeposition precursor solution;
b. controlling the deposition temperature to be 10-18 ℃ and the humidity to be not higher than 50%, and carrying out electrodeposition to prepare the SnS nano film under the conditions of the temperature and the humidity, wherein the method specifically comprises the following steps:
the electrode clamp with the clean FTO is used as a working electrode, a platinum wire is used as a counter electrode, an Ag/AgCl electrode is used as a reference electrode, the prepared electro-deposition precursor solution with the pH value of 1.5 in the step a is deposited for 10 minutes, the deposition voltage is controlled to be-1.1V, the electro-deposition precursor solution is intermittently stirred in the deposition process, the stirring speed is controlled to be 300 revolutions per minute, the interval time is 250s, and then the deposited SnS nano film is washed by deionized water and dried to obtain the SnS nano film.
Experimental test analysis:
the performance of the SnS nanorod film obtained in this example was tested, and fig. 4 is an XRD spectrum analysis of the SnS nanorod film deposited in this example at-1.1V. Diffraction angles of 22.01 degrees, 26.01 degrees and,31.53 degrees, 31.97 degrees, 39.33 degrees, 15.49 degrees and 66.37 degrees respectively correspond to diffraction peaks of (110), (120), (111), (040), (041), (002) and (152) in a standard PDF card JCPDS No.39-0354 of SnS. FIG. 5 is a surface SEM image of a SnS nanorod film deposited under a voltage of-1.1V in the embodiment. As seen from the surface diagram, the SnS film has a nanorod structure, is orderly arranged and has longer nanorods. FIG. 6 is a Raman diffraction peak spectrum of the SnS nanorod film deposited at the voltage of-1.1V in the embodiment. In the figure at 94cm-1、155cm-1、181cm-1、216cm-1Has obvious diffraction peak, corresponding to SnS material. The Raman diffraction shows that the prepared SnS nanorod film is relatively pure in phase and no other mixed phase is generated.
Example three:
this embodiment is substantially the same as the previous embodiment, and is characterized in that:
in this embodiment, a method for preparing an SnS nanotube film includes the following steps:
a. firstly, regulating and controlling the deposition temperature to be 10-18 ℃, controlling the humidity to be lower than 50%, sequentially adding 0.05mol of stannous sulfate and 0.05mol of thioacetamide into a beaker containing 200ml of deionized water under the conditions of the temperature and the humidity, stirring for 1-2 minutes for reaction to obtain a mixed solution, then continuously adding 0.06mol of potassium citrate into the mixed solution, and continuously stirring for 2-3 minutes, wherein the solution is a yellow turbid solution; then hydrochloric acid is added into the mixed solution to adjust the pH value of the mixed solution to 0.6, so that the mixed solution is clarified; adding KOH into the mixed solution, and adjusting the pH of the mixed solution to 1.5 to obtain an electrodeposition precursor solution;
b. controlling the deposition temperature to be 10-18 ℃ and the humidity to be not higher than 50%, and carrying out electrodeposition to prepare the SnS nano film under the conditions of the temperature and the humidity, wherein the method specifically comprises the following steps:
the electrode clamp with the clean FTO is used as a working electrode, a platinum wire is used as a counter electrode, an Ag/AgCl electrode is used as a reference electrode, the prepared electro-deposition precursor solution with the pH value of 1.5 in the step a is deposited for 10 minutes, the deposition voltage is controlled to be-0.8V, the electro-deposition precursor solution is intermittently stirred in the deposition process, the stirring speed is controlled to be 500 revolutions per minute, the interval time is 250s, and then the deposited SnS nano film is washed by deionized water and dried to obtain the SnS nano film.
Experimental test analysis:
the performance of the SnS nanotube film prepared by the embodiment is tested, the SnS film has a nanotube-shaped structure, is orderly arranged, and has longer nanotubes. The SnS nanotube film prepared by the embodiment is relatively pure, and no other impurity phase is generated. The method for preparing the SnS nanotube on the FTO conductive glass substrate has the advantages that the expensive vacuum equipment is not needed, the SnS with controllable stoichiometric ratio can be obtained without higher reaction temperature, and the utilization rate of raw materials is very high.
Example four:
this embodiment is substantially the same as the previous embodiment, and is characterized in that:
in this embodiment, a method for preparing an SnS nanorod film includes the following steps:
a. firstly, regulating and controlling the deposition temperature to be 10-18 ℃, controlling the humidity to be lower than 50%, sequentially adding 0.05mol of stannous acetate and 0.05mol of thiourea into a beaker containing 200ml of ethanol under the conditions of the temperature and the humidity, stirring for 1-2 minutes for reaction to obtain a mixed solution, then continuously adding 0.02mol of citric acid into the mixed solution, and continuously stirring for 2-3 minutes, wherein the solution is a yellow turbid solution; adding acetic acid into the mixed solution to adjust the pH value of the mixed solution to 0.6, so that the mixed solution is clarified; then adding ammonia water into the mixed solution, and adjusting the pH of the mixed solution to 1.5 to obtain an electrodeposition precursor solution;
b. controlling the deposition temperature to be 10-18 ℃ and the humidity to be not higher than 50%, and carrying out electrodeposition to prepare the SnS nano film under the conditions of the temperature and the humidity, wherein the method specifically comprises the following steps:
the electrode clamp with the clean FTO is used as a working electrode, a platinum wire is used as a counter electrode, an Ag/AgCl electrode is used as a reference electrode, the prepared electro-deposition precursor solution with the pH value of 1.5 in the step a is deposited for 10 minutes, the deposition voltage is controlled to be-1.0V, the electro-deposition precursor solution is intermittently stirred in the deposition process, the stirring speed is controlled to be 500 revolutions per minute, the interval time is 250s, and then the deposited SnS nano film is washed by deionized water and dried to obtain the SnS nano film.
Experimental test analysis:
the performance of the SnS nanorod film prepared in the embodiment is tested, the SnS nanorod film has a nanorod structure and is orderly arranged, and the nanorod is long. The SnS nanorod film prepared in the embodiment is relatively pure in phase, and no other mixed phase is generated. The method for preparing the SnS nanorods on the FTO conductive glass substrate does not need expensive vacuum equipment or higher reaction temperature, can obtain SnS with controllable stoichiometric ratio, and has very high utilization rate of raw materials.
In summary, in the method for preparing the SnS nanorod/nanotube film according to the embodiment of the invention, the deposition temperature is 10-18 ℃, and the humidity is lower than 50%. Firstly, sequentially adding soluble stannous salt and thio compound into deionized water or organic solvent, stirring and adding citric acid or citrate, continuously stirring and adding acid to adjust the pH value of the solution, so as to clarify the solution; then, alkali was added to adjust the pH of the solution to 1.5. And (2) depositing in a prepared solution with the pH value of 1.5 by using FTO as a working electrode, a platinum wire as a counter electrode and an Ag/AgCl electrode as a reference electrode, intermittently stirring the solution in the deposition process, and washing and drying the deposited SnS nano film by using deionized water. Wherein the SnS nano-tube film can be prepared under the deposition voltage of-0.8 to-0.9V, and the SnS nano-rod film can be prepared under the deposition voltage of-1.0 to-1.1V. The preparation method of the embodiment of the invention is environment-friendly, simple to operate, can strictly control each step of the operation, has low cost of the used precursor material, and is beneficial to improving the photoelectric property of the prepared film. According to the embodiment of the invention, the SnS nanorod/tube is manufactured on the FTO conductive glass substrate by adopting an electrodeposition method, expensive vacuum equipment is not needed, the SnS with controllable stoichiometric ratio can be obtained without higher reaction temperature, the utilization rate of raw materials is very high, and a brand-new thought is provided for researching and developing large-area SnS thin-film solar cells and reducing the preparation cost of the large-area SnS thin-film solar cells. The preparation method of the SnS nanorod/tube film in the embodiment of the invention is simple, the experimental conditions can be strictly controlled, the cost of the used precursor material is low, the method is suitable for large-scale production, and the preparation process is green and environment-friendly.
The embodiments of the present invention have been described with reference to the accompanying drawings, but the present invention is not limited to the embodiments, and various changes and modifications may be made according to the purpose of the invention, and any changes, modifications, substitutions, combinations or simplifications made according to the spirit and principle of the technical solution of the present invention shall be equivalent substitutions, as long as the purpose of the present invention is met, and the present invention shall fall within the protection scope of the present invention as long as the technical principle and inventive concept of the method for preparing the SnS nanotube film or the SnS nanorod film of the present invention are not departed from the technical principle and inventive concept of the method for preparing the SnS nanotube film or the SnS nanorod film of the.
Claims (9)
1. A preparation method of a SnS nanotube film or a SnS nanorod film is characterized by comprising the following steps:
a. firstly, regulating and controlling the deposition temperature to be 10-18 ℃, controlling the humidity to be not higher than 50%, under the conditions of the temperature and the humidity, sequentially adding 0.025-0.05 mol of soluble divalent tin salt and 0.025-0.05 mol of thio compound into a beaker containing 100-200 ml of deionized water or organic solvent, stirring for 1-2 minutes to obtain a mixed solution, then continuously adding 0.02-0.06 mol of citric acid or citrate into the mixed solution, and continuously stirring for 2-3 minutes; adding acid into the mixed solution to adjust the pH of the mixed solution to 0.6-0.8, and clarifying the mixed solution; adding alkali into the mixed solution, and adjusting the pH of the mixed solution to 1.5 to obtain an electrodeposition precursor solution;
b. depositing in the electrodeposition precursor solution prepared in the step a for 3-10 minutes by taking FTO as a working electrode, a platinum wire as a counter electrode and an Ag/AgCl electrode as a reference electrode, and controlling the deposition voltage to be-0.8V-1.1V; intermittently stirring the electro-deposition precursor solution in the deposition process, controlling the stirring speed to be 300-500 r/min, and then washing and drying the deposited SnS nano film by using deionized water;
in the step b, when the deposition voltage is controlled to be-0.8 to-0.9V, the SnS nanotube film is prepared; or when the deposition voltage is controlled to be-1.0 to-1.1V, the SnS nano-rod film is prepared.
2. The method for preparing the SnS nanotube film or the SnS nanorod film according to claim 1, wherein the method comprises the following steps: in the step a, any one of stannous chloride, stannous sulfate and stannous acetate or hydrate of the salt is adopted as the soluble stannous salt.
3. The method for preparing the SnS nanotube film or the SnS nanorod film according to claim 1, wherein the method comprises the following steps: in the step a, the thio compound adopts any one salt or hydrate of salt of sodium thiosulfate, thioacetamide and thiourea.
4. The method for preparing the SnS nanotube film or the SnS nanorod film according to claim 1, wherein the method comprises the following steps: in the step a, when the pH value of the mixed solution is adjusted, the added acid is sulfuric acid, acetic acid or hydrochloric acid.
5. The method for preparing the SnS nanotube film or the SnS nanorod film according to claim 1, wherein the method comprises the following steps: in the step a, when the pH value of the mixed solution is adjusted, NaOH, ammonia water or KOH is used as the added alkali.
6. The method for preparing the SnS nanotube film or the SnS nanorod film according to claim 1, wherein the method comprises the following steps: in the step a, trisodium citrate or potassium citrate is adopted as the citrate.
7. The method for preparing the SnS nanotube film or the SnS nanorod film according to claim 1, wherein the method comprises the following steps: in the step a, the organic solvent adopts any one of alcohol and acetone or a mixture of the two.
8. The method for preparing the SnS nanotube film or the SnS nanorod film according to claim 1, wherein the method comprises the following steps: in the step b, the deposition temperature is controlled to be 10-18 ℃, the humidity is controlled to be not higher than 50%, and the SnS nano film is prepared by electrodeposition under the conditions of the temperature and the humidity.
9. The method for preparing the SnS nanotube film or the SnS nanorod film according to claim 1, wherein the method comprises the following steps: in the step b, the electrodeposition precursor solution is intermittently stirred during the deposition process, and the interval time is not more than 250 s.
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| CN101724834B (en) * | 2009-12-14 | 2011-11-09 | 昆明理工大学 | Continuously self-catalyzed deposition chemical plating solution of tin and using method thereof |
| US9085829B2 (en) * | 2010-08-31 | 2015-07-21 | International Business Machines Corporation | Electrodeposition of thin-film cells containing non-toxic elements |
| CN102315333B (en) * | 2011-10-13 | 2014-07-30 | 南京大学 | Preparation of ZnSnS film and ZnSnS/SnS heterojunction, and application of solar cells |
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| CN108832094B (en) * | 2018-06-12 | 2021-05-04 | 陕西科技大学 | Method for preparing spherical tin sulfide/stannous sulfide lithium ion battery cathode material by one-step method |
| CN108923028B (en) * | 2018-06-29 | 2021-06-08 | 桑顿新能源科技(长沙)有限公司 | Multistage nano Sn-based material and preparation method thereof |
| CN109179489B (en) * | 2018-10-26 | 2020-07-24 | 浙江大学 | Preparation method, product and application of two-dimensional ultrathin stannous sulfide nanosheet |
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