CN115536063A - Nanometer flower-like bismuth sulfide, preparation method and application - Google Patents
Nanometer flower-like bismuth sulfide, preparation method and application Download PDFInfo
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- CN115536063A CN115536063A CN202211170708.2A CN202211170708A CN115536063A CN 115536063 A CN115536063 A CN 115536063A CN 202211170708 A CN202211170708 A CN 202211170708A CN 115536063 A CN115536063 A CN 115536063A
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- NNLOHLDVJGPUFR-UHFFFAOYSA-L calcium;3,4,5,6-tetrahydroxy-2-oxohexanoate Chemical compound [Ca+2].OCC(O)C(O)C(O)C(=O)C([O-])=O.OCC(O)C(O)C(O)C(=O)C([O-])=O NNLOHLDVJGPUFR-UHFFFAOYSA-L 0.000 title claims abstract description 36
- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims abstract description 54
- 239000002904 solvent Substances 0.000 claims abstract description 21
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 claims abstract description 18
- 238000009210 therapy by ultrasound Methods 0.000 claims abstract description 17
- FBXVOTBTGXARNA-UHFFFAOYSA-N bismuth;trinitrate;pentahydrate Chemical compound O.O.O.O.O.[Bi+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FBXVOTBTGXARNA-UHFFFAOYSA-N 0.000 claims abstract description 13
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 238000005406 washing Methods 0.000 claims abstract description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 5
- 238000000034 method Methods 0.000 claims description 12
- 238000005119 centrifugation Methods 0.000 claims description 5
- 241000207961 Sesamum Species 0.000 claims description 2
- 235000003434 Sesamum indicum Nutrition 0.000 claims description 2
- 239000003990 capacitor Substances 0.000 abstract description 4
- 241000222336 Ganoderma Species 0.000 abstract description 3
- 239000002086 nanomaterial Substances 0.000 abstract description 2
- 239000000463 material Substances 0.000 description 7
- 230000008569 process Effects 0.000 description 7
- 239000003795 chemical substances by application Substances 0.000 description 4
- 230000007547 defect Effects 0.000 description 3
- 239000007772 electrode material Substances 0.000 description 3
- 230000003321 amplification Effects 0.000 description 2
- 238000002484 cyclic voltammetry Methods 0.000 description 2
- 238000003199 nucleic acid amplification method Methods 0.000 description 2
- 230000008092 positive effect Effects 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000005234 chemical deposition Methods 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 230000001276 controlling effect Effects 0.000 description 1
- 239000013256 coordination polymer Substances 0.000 description 1
- 230000000875 corresponding effect Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000012360 testing method Methods 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L31/00—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L31/0248—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies
- H01L31/0256—Semiconductor devices sensitive to infrared radiation, light, electromagnetic radiation of shorter wavelength or corpuscular radiation and specially adapted either for the conversion of the energy of such radiation into electrical energy or for the control of electrical energy by such radiation; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by their semiconductor bodies characterised by the material
- H01L31/0264—Inorganic materials
- H01L31/032—Inorganic materials including, apart from doping materials or other impurities, only compounds not provided for in groups H01L31/0272 - H01L31/0312
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- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C01P2004/30—Particle morphology extending in three dimensions
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Abstract
The invention belongs to the technical field of nano materials, and discloses a nano flower-shaped bismuth sulfide, a preparation method and application thereof, wherein bismuth nitrate pentahydrate and thiourea are sequentially dissolved in 10-100 mL of N, N-dimethylformamide solvent according to the mass ratio of 1-4:1; grinding bismuth nitrate pentahydrate before dissolving; then carrying out ultrasonic treatment on the N, N-dimethylformamide solvent in which the bismuth nitrate pentahydrate and the thiourea are dissolved; the ultrasonic treatment is carried out by using a fresh Ganoderma cell pulverizer to perform ultrasonic treatment for 5-20min under the power of 100-500W; and finally, centrifuging the N, N-dimethylformamide solvent subjected to ultrasonic treatment at the rotating speed of 5000-8000, washing the N, N-dimethylformamide solvent for three times by using absolute ethyl alcohol, and drying the N, N-dimethylformamide solvent. The bismuth sulfide prepared by the invention has a nano flower-shaped structure, is uniform in size and good in dispersibility, and can be applied to the fields of photoelectric detectors, gas sensors, solar cells, super capacitors and the like.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a nano flower-shaped bismuth sulfide, a preparation method and application thereof.
Background
Currently, bismuth sulfide, which is a semiconductor material with a narrow band gap, attracts extensive research attention due to its special electronic structure, optical characteristics, and the like, and is widely used in the fields of photodetectors, gas sensors, solar cells, supercapacitors, and the like. And because the corresponding properties of the material are closely related to the shape of the material, including special factors such as size and shape, the controllable preparation of the shape and size of the material becomes an important way for regulating and controlling the properties of the material. At present, a plurality of preparation methods are applied to develop bismuth sulfide with special morphology, such as a hydrothermal method, a microwave method, a chemical deposition method and the like. However, most methods have the defects of low yield, template agent requirement, complex process, poor controllability and the like, and limit the application and popularization of the nano bismuth sulfide. Therefore, the development of a preparation method which is rapid and has good monodispersity has important practical significance.
Through the above analysis, the problems and defects of the prior art are as follows: the existing bismuth sulfide preparation method has the defects of low yield, template agent requirement, complex process, poor controllability and the like, and limits the application and popularization of the nano bismuth sulfide.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides a nano flower-shaped bismuth sulfide, a preparation method and application thereof.
The invention is realized in such a way that the preparation method of the nano flower-shaped bismuth sulfide comprises the following steps:
firstly, dissolving bismuth nitrate pentahydrate and thiourea in 10-100 mL of N, N-dimethylformamide solvent according to the mass ratio of 1-4:1;
step two, carrying out ultrasonic treatment on the N, N-dimethylformamide solvent in which the bismuth nitrate pentahydrate and the thiourea are dissolved;
and step three, centrifuging the N, N-dimethylformamide solvent after ultrasonic treatment, washing the N, N-dimethylformamide solvent for three times by using absolute ethyl alcohol, and drying the solvent.
Further, the bismuth nitrate pentahydrate in the first step is ground before being dissolved.
Further, the specific mode of the ultrasonic treatment in the second step is to use a new ganoderma cell crusher to perform ultrasonic treatment for 5-20min under the power of 100W-500W.
Further, the centrifugation in the third step adopts the centrifugation at the rotating speed of 5000-8000.
By combining the technical scheme and the technical problem to be solved, the technical scheme to be protected by the invention has the advantages and positive effects that:
the technical scheme to be protected by the invention has the advantages of simple process, no need of a template agent, no need of high temperature and high pressure, quick preparation and easy industrial amplification; the reagent used in the scheme of the invention has low cost and can be circulated for a plurality of times; and the prepared bismuth sulfide has high purity, uniform size and good monodispersity.
The technical scheme to be protected by the invention has the technical characteristics of quick preparation and no need of a template agent; the bismuth sulfide prepared by the invention has a nano flower-shaped structure, and has high purity, uniform size and good dispersibility.
The expected income and commercial value after the technical scheme of the invention is converted are as follows: the method can realize the rapid preparation of the nano bismuth sulfide with uniform size, does not need subsequent washing treatment, has simple scheme and process, is easy for industrial amplification, and has certain commercial value.
Drawings
FIG. 1 is a flow chart of a method for preparing nano flower-like bismuth sulfide provided by an embodiment of the invention;
FIG. 2 is a Scanning Electron Microscope (SEM) image of the product obtained in example 1 of the present invention;
FIG. 3 is an X-ray diffraction (SEM) pattern of a product obtained in example 1 of the present invention;
FIG. 4 is a graph of Cyclic Voltammetry (CV) of the product obtained in example 1 of the present invention used as an electrode material for a supercapacitor;
FIG. 5 is a graph of constant current charge and discharge (CP) of the product obtained in example 1 of the present invention as an electrode material for a supercapacitor;
FIG. 6 is a graph showing the specific capacity of the product obtained in example 1 of the present invention as an electrode material for a supercapacitor.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
This section is an illustrative example developed to explain the claims in order to enable those skilled in the art to fully understand how to implement the present invention.
As shown in fig. 1, the preparation method of nano flower-like bismuth sulfide provided by the embodiment of the present invention includes:
s101, dissolving bismuth nitrate pentahydrate and thiourea in 10-100 mL of N, N-dimethylformamide solvent in sequence according to the mass ratio of 1-4:1;
s102, carrying out ultrasonic treatment on the N, N-dimethylformamide solvent in which the bismuth nitrate pentahydrate and the thiourea are dissolved;
s103, centrifuging the N, N-dimethylformamide solvent after ultrasonic treatment, washing the N, N-dimethylformamide solvent for three times by using absolute ethyl alcohol, and drying the solvent.
In the embodiment of the present invention, the bismuth nitrate pentahydrate in step S101 is subjected to a grinding process before being dissolved.
The specific mode of the ultrasonic treatment in step S102 in the embodiment of the invention is to use a new sesame cell crusher to perform ultrasonic treatment for 5-20min under the power of 100W-500W.
In the embodiment of the invention, the centrifugation of the step S103 adopts the centrifugation with the rotating speed of 5000-8000.
Example 1
(1) 485mg of bismuth nitrate pentahydrate was first finely ground and dissolved in 30mL of N, N-dimethylformamide solvent, followed by dissolving 114mg of thiourea. (2) Then, carrying out ultrasonic treatment for 10min by using a new ganoderma cell crusher under the power of 500W. (3) And finally, centrifuging at the rotating speed of 7500, washing with absolute ethyl alcohol for three times, and drying. The bismuth sulfide prepared by the embodiment of the invention has a silicon nano flower-shaped structure; and has uniform size and good dispersibility. The morphology of the resulting product is shown in FIG. 2; the morphology of the resulting product is shown in FIG. 3; the obtained nano flower-like bismuth sulfide is successfully applied to the field of super capacitors, and the performances of the super capacitors are shown in figures 4-6.
In order to prove the creativity and the technical value of the technical scheme of the invention, the part is the application example of the technical scheme of the claims on specific products or related technologies.
The nano flower-shaped bismuth sulfide prepared by the preparation method of the nano flower-shaped bismuth sulfide provided by the embodiment of the invention can be applied to the fields of photoelectric detectors, gas sensors, solar cells, super capacitors and the like. As shown in FIGS. 4-6, the nano flower-like bismuth sulfide prepared according to example 1 can be successfully applied to the field of supercapacitors, and the specific capacity of the nano flower-like bismuth sulfide can reach 523.5F/g at a current density of 0.5A/g.
The embodiment of the invention achieves some positive effects in the process of research and development or use, and has great advantages compared with the prior art, and the following contents are described by combining data, diagrams and the like in the test process.
The nano flower-like bismuth sulfide prepared according to example 1 was successfully applied to the field of supercapacitors, as shown in FIG. 4, from which Bi in the CV curve can be seen 2 S 3 The redox peaks are quite obvious, the redox peaks are slightly shifted along with the increase of the scanning speed, and the response current of the redox peaks is correspondingly increased along with the increase of the scanning speed, which shows that the electrolyte is decomposed and generates a Faraday reaction when the material works under the working voltage window, and proves that the material has better reversibility; as shown in FIG. 5, the curve shape of the constant current charge-discharge curve was almost constant, indicating that Bi 2 S 3 The charge-discharge reversibility is good; under the current density of 0.5A/g, the specific capacity reaches 523.5F/g, and under the current density of 5A/g, the specific capacity still reaches 352.3F/g, which shows that the high-performance high-power-factor amplifier has better power-factor performance.
The above description is only for the purpose of illustrating the embodiments of the present invention, and the scope of the present invention should not be limited thereto, and any modifications, equivalents and improvements made by those skilled in the art within the technical scope of the present invention as disclosed in the present invention should be covered by the scope of the present invention.
Claims (10)
1. A preparation method of nano flower-shaped bismuth sulfide is characterized by comprising the following steps:
firstly, dissolving bismuth nitrate pentahydrate and thiourea in 10-100 mL of N, N-dimethylformamide solvent according to the mass ratio of 1-4:1;
step two, carrying out ultrasonic treatment on the N, N-dimethylformamide solvent in which the bismuth nitrate pentahydrate and the thiourea are dissolved;
and step three, centrifuging the N, N-dimethylformamide solvent after ultrasonic treatment, washing the N, N-dimethylformamide solvent for three times by using absolute ethyl alcohol, and drying the solvent.
2. The nano flower-like bismuth sulfide and the preparation method thereof according to claim 1, wherein the bismuth nitrate pentahydrate in the first step is ground before being dissolved.
3. The nano flower-like bismuth sulfide and the preparation method thereof according to claim 1, wherein the ultrasonic treatment in the second step is carried out by using a fresh sesame cell crusher at a power of 100W to 500W.
4. The nanoflower-shaped bismuth sulfide and the preparation method thereof according to claim 3, wherein the ultrasonic treatment time is 5-20min.
5. The nano flower-like bismuth sulfide and the preparation method thereof as claimed in claim 1, wherein the centrifugation of the third step is performed at 5000-8000 rpm.
6. A nano flower-like bismuth sulfide, characterized in that the nano flower-like bismuth sulfide is prepared by the method for preparing nano flower-like bismuth sulfide according to any one of claims 1 to 5.
7. A photodetector, characterized in that it is prepared using the nano flower-like bismuth sulfide of claim 6.
8. A gas sensor, wherein the gas sensor is prepared by using the nano flower-like bismuth sulfide according to claim 6.
9. A solar cell, characterized in that it is prepared using the nanoflower-shaped bismuth sulfide according to claim 6.
10. A supercapacitor, characterized in that it is produced using the nano flower-like bismuth sulfide of claim 6.
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| CN202211170708.2A CN115536063B (en) | 2022-09-23 | 2022-09-23 | Nanometer flower-shaped bismuth sulfide, preparation method and application |
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Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101492179A (en) * | 2009-03-10 | 2009-07-29 | 武汉理工大学 | Bismuth sulfide material and synthesis thereof |
| CN104226335A (en) * | 2014-09-19 | 2014-12-24 | 武汉工程大学 | Multilevel structure bismuth sulfide, preparation method and application thereof |
| CN104817111A (en) * | 2015-04-21 | 2015-08-05 | 南京邮电大学 | Room-temperature water phase preparation method of bismuth sulfide nanospheres |
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2022
- 2022-09-23 CN CN202211170708.2A patent/CN115536063B/en active Active
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101492179A (en) * | 2009-03-10 | 2009-07-29 | 武汉理工大学 | Bismuth sulfide material and synthesis thereof |
| CN104226335A (en) * | 2014-09-19 | 2014-12-24 | 武汉工程大学 | Multilevel structure bismuth sulfide, preparation method and application thereof |
| CN104817111A (en) * | 2015-04-21 | 2015-08-05 | 南京邮电大学 | Room-temperature water phase preparation method of bismuth sulfide nanospheres |
Non-Patent Citations (3)
| Title |
|---|
| JUAN LU ET AL.: "Microwave-assisted synthesis and characterization of 3D flower-like Bi2S3 superstructures", 《MATERIALS LETTERS》, vol. 61, pages 2883 - 2886 * |
| RONG HE ET AL.: "Preparation of Bi2S3 nanowhiskers and their morphologies", 《JOURNAL OF CRYSTAL GROWTH》, vol. 252, pages 505 - 510, XP004418392, DOI: 10.1016/S0022-0248(03)00968-0 * |
| 梁焕喜 等: "花状硫化铋纳米结构的制备及其光热特性研究", 《青岛科技大学学报（自然科学版）》, vol. 36, no. 6, pages 617 - 621 * |
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