CN114944288B - Flower-like bismuth trioxide, preparation method and application thereof, and prepared electrode - Google Patents
Flower-like bismuth trioxide, preparation method and application thereof, and prepared electrode Download PDFInfo
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- CN114944288B CN114944288B CN202210695062.3A CN202210695062A CN114944288B CN 114944288 B CN114944288 B CN 114944288B CN 202210695062 A CN202210695062 A CN 202210695062A CN 114944288 B CN114944288 B CN 114944288B
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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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
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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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- C—CHEMISTRY; METALLURGY
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- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention discloses flower-like bismuth trioxide, a preparation method and application thereof, and a prepared electrode. The flower-like bismuth trioxide is prepared into Bi by a solvothermal method 2 O 3 Introducing trace water in the process, for Bi 2 O 3 The microstructure and the crystallinity of the glass are adjusted and controlled. Compared with the prior conventional solvothermal method, the method not only realizes Bi by adding the green pollution-free trace water 2 O 3 The microcosmic morphology and the grain diameter can be regulated and controlled, and the obtained Bi 2 O 3 The sample has higher crystallinity, and the ultrathin nano-sheet with high crystallinity is assembledFlower-like Bi 2 O 3 The catalyst has higher specific surface area and can expose more electrochemical reaction sites; while the high crystallinity is helpful to improve the electron transfer efficiency and finally improve Bi 2 O 3 Is used for the capacitor performance of (a). In addition, the invention does not need to add any surfactant in the preparation process, thereby reducing the consumption of a large amount of water in the washing process and the problem of environmental pollution caused by the large amount of discharge of the surfactant.
Description
Technical Field
The invention belongs to the field of electrode materials, and particularly relates to flower-like bismuth trioxide, a preparation method and application thereof, and a prepared electrode.
Background
The super capacitor has the characteristics of high charging speed, high power density and good cycle stability, and becomes a potential energy storage device and a bridge for connecting the traditional capacitor and the lithium ion battery. However, the low energy density is currently limiting the large-scale application of supercapacitors. Pseudo-capacitance material Bi 2 O 3 The material has the characteristics of high theoretical capacity, reversible oxidation-reduction process, wide working potential window and environmental friendliness, is considered as a promising super-capacitor anode material, and can improve the problem of low energy density. Theoretically, an ideal capacitive material should have i) a high specific surface area exposing more electrochemically active sites; ii) excellent conductivity to accelerate electron transfer; iii) The porous structure promotes electrolyte diffusion. However, due to Bi 2 O 3 Poor conductivity and fewer electrochemically active sites on the surface result in lower actual capacitance. At present, bi is regulated and controlled by adding a surfactant in the preparation process 2 O 3 Is a common method for microstructure and morphology. However, since the surfactant is difficult to remove, a large amount of water is consumed in the washing process; in addition, the residual surfactant in the sample may decrease the conductivity of the electrode, affecting the electron transfer efficiency and the rate capability of the electrode. In addition, large amounts of surfactant are discharged to the environmentAnd (5) pollution. From the above, it can be seen that Bi is prepared by the alcohol thermal method at present 2 O 3 The electrode also has the problems of poor conductivity, insufficient surface active sites, environmental pollution caused by the application of the surfactant, and the like. Therefore, how to realize Bi by a new green and environment-friendly method 2 O 3 Morphology regulation and conductivity increase, and further capacitance increase become research hot spots.
Disclosure of Invention
The invention aims to solve the defects in the prior art and provides a trace water-regulated solvothermal method for preparing flower-like Bi assembled by ultrathin nano sheets 2 O 3 The new technology of (2) adopts the following technical scheme:
the preparation method of the flower-like bismuth trioxide comprises the following steps: bi (NO) 3 ) 3 ·5H 2 Adding O into glycol, stirring to form transparent solution, adding mixed solution of water and ethanol, and heating at 140-170deg.C for 5-8 hr to obtain the final product.
The invention prepares Bi by solvothermal method 2 O 3 Introducing trace water in the process, and utilizing trace water to make Bi 2 O 3 The microstructure and crystallinity of the glass are regulated and controlled. The inventor finds that introducing trace water in the alcohol heating process can accelerate the hydrolysis of the organic precursor, improve the crystallinity of the crystal grains and further achieve the purpose of morphology regulation. Bi prepared by the method 2 O 3 The morphology of the electrode material can be changed along with the change of the water volume, the crystallinity is continuously improved, and the improvement of the crystallinity is beneficial to increasing the conductivity of the electrode material and improving the transfer rate of electrons. The capacitance performance test result shows that Bi is added when a small amount of water is added 2 O 3 The capacitance of the alloy is obviously improved, and the optimal capacitance is Bi by the traditional solvothermal method 2 O 3 Capacitance of 5 times, which results mainly from exposing more electrochemically active sites and conductivity improvement.
Preferably, bi (NO 3 ) 3 ·5H 2 O: ethylene glycol: mixed solution = 1.96g:48mL:24mL.
The thickness of the prepared flower-shaped bismuth trioxide nano-sheet is 8-20nm, and the flower-shaped diameter is 3-10 mu m. Can be used as a negative electrode material of the super capacitor. The electrode prepared based on the flower-shaped bismuth trioxide comprises the following preparation processes: mixing flower-like bismuth trioxide, carbon black and PVDF uniformly, adding N-methyl pyrrolidone, grinding uniformly to form uniform slurry, coating the slurry on the surface of carbon cloth, and drying to obtain the electrode.
Wherein, the mass ratio of the flower-shaped bismuth trioxide, the carbon black and the PVDF is 8:1:1.
the beneficial effects of the invention are as follows:
(1) Compared with the prior conventional solvothermal method, the method not only realizes Bi by adding the green pollution-free trace water 2 O 3 The microcosmic appearance and the grain diameter can be regulated and controlled, and the microcosmic appearance and the crystallinity are changed along with the change of the water addition amount, thus obtaining the Bi 2 O 3 The sample has higher crystallinity, and the flower-like Bi assembled by the ultrathin nano-sheets with high crystallinity 2 O 3 The catalyst has higher specific surface area and can expose more electrochemical reaction sites; while the high crystallinity is helpful to improve the electron transfer efficiency and finally improve Bi 2 O 3 The capacitance of the capacitor is 5 times that of the sample prepared by the traditional solvothermal method.
(2) The invention solves the problem of Bi prepared by the traditional solvothermal method 2 O 3 Poor conductivity and fewer electrochemically active sites on the surface; meanwhile, any surfactant is not required to be added in the preparation process, so that the problems of pollution to the environment caused by consumption of a large amount of water and discharge of a large amount of surfactant in the washing process are reduced.
Drawings
FIG. 1 shows Bi under the addition of different volumes of water 2 O 3 Scanning electron microscope pictures of (2); a is added with 0mL; b is 6mL added; c is 12mL added, d is 24mL added;
FIG. 2 shows Bi under the addition of different volumes of water 2 O 3 An X-ray diffraction pattern of (2);
FIG. 3 shows Bi under the addition of different volumes of water 2 O 3 Is a GCD curve of (C).
Detailed Description
The conception and the technical effects produced by the present invention will be clearly and completely described below with reference to the embodiments and the drawings to fully understand the objects, aspects and effects of the present invention.
Example 1:
method for preparing flower-like Bi by solvothermal method 2 O 3 ：
Method for preparing flower-like Bi by solvothermal method 2 O 3 :48mL of ethylene glycol, 18mL of ethanol, and 6mL of deionized water were taken, and 1.96g of bismuth nitrate (Bi (NO) 3 ) 3 ·5H 2 O) was added to a beaker containing 48mL of ethylene glycol and magnetically stirred to form a clear solution. Adding a mixed solution of water and ethanol into the solution, and continuing magnetic stirring. Transferring the mixed solution into a 100mL reaction kettle liner, and heating in an oven at 160 ℃ for 5h to obtain flower-like Bi with high crystallinity 2 O 3 An electrode material.
Example 2:
method for preparing flower-like Bi by solvothermal method 2 O 3 ：
Method for preparing flower-like Bi by solvothermal method 2 O 3 :48mL of ethylene glycol, 12mL of ethanol, and 12mL of deionized water were taken, and 1.96g of bismuth nitrate (Bi (NO) 3 ) 3 ·5H 2 O) was added to a beaker containing 48mL of ethylene glycol and magnetically stirred to form a clear solution. Adding a mixed solution of water and ethanol into the solution, and continuing magnetic stirring. Transferring the mixed solution into a 100mL reaction kettle liner, and heating in an oven at 160 ℃ for 5h to obtain flower-like Bi with high crystallinity 2 O 3 An electrode material.
Example 3:
method for preparing flower-like Bi by solvothermal method 2 O 3 ：
Method for preparing flower-like Bi by solvothermal method 2 O 3 :48mL of ethylene glycol and 24mL of deionized water were taken, and 1.96g of bismuth nitrate (Bi (NO) 3 ) 3 ·5H 2 O) was added to a beaker containing 48mL of ethylene glycol and magnetically stirred to form a clear solution. Adding a mixed solution of water and ethanol into the solution, and continuing magnetic stirring. The mixed solution was transferred to a 100mL reactor liner at 160Heating in an oven at a temperature of below zero for 5h to obtain flower-like Bi with high crystallinity 2 O 3 An electrode material.
Example 4:
bi prepared by adding 0mL of deionized water (i.e., all ethanol added) and adding 24mL of deionized water (i.e., no ethanol added) was prepared in the same manner as in example 1 2 O 3 With the flower-like Bi obtained in examples 1-3 2 O 3 Testing was performed. The electron microscope photograph and the X-ray diffraction pattern are shown in fig. 1 and 2. As can be seen from FIG. 1, the addition of different volumes of water to Bi 2 O 3 The morphology has a significant impact. Along with the continuous increase of the water volume, bi 2 O 3 The morphology of (a) is changed from an irregular structure to a flower shape. As can be seen from FIG. 1 (a), bi is produced without adding water to the hydroalcoholic system 2 O 3 The structure is a random structure with lower crystallinity, and the surface is rough and uneven in appearance. FIG. 1 (b-d) shows Bi added with 6mL, 12mL and 24mL of water, respectively 2 O 3 Morphology, bi can be seen from SEM 2 O 3 The appearance is in a uniform flower sphere shape, the particle size is uniform, and the dispersibility is good. Meanwhile, from FIG. 1 (b-d), it can be seen that flower-ball-like Bi is formed after adding a trace amount of water 2 O 3 Is assembled by a large number of ultrathin nano sheet structures. The ultrathin sheet structure is beneficial to improving Bi 2 O 3 And the number of surface active sites is increased, thereby increasing the capacitance. In addition, the lamellar structure facilitates diffusion of electrolyte ions, increasing rate performance. From the XRD pattern of FIG. 2, it can be seen that with the addition of water, bi 2 O 3 The increase in diffraction peak intensity of (c) indicates that a small amount of water contributes to an increase in crystallinity thereof, which results from the fact that water accelerates the hydrolysis rate of the Bi intermediate to form large-particle Bi 2 O 3 . The high crystallinity is helpful to reduce the resistance, accelerate the electron transfer efficiency, and further improve the capacitance.
Preparation of working electrode: the Bi is prepared by 2 O 3 Bi as an electrode active material 2 O 3 With carbon black and polyvinylidene fluoride (PVDF) according to 8:1:1, adding proper amount of N-methyl pyrrolidone, grinding in a mortarGrinding uniformly to form uniform slurry; and then uniformly coating the slurry on the surface of the carbon cloth, drying at 60 ℃, and determining the quality of the electrode active material according to the difference of the front and back quality of the carbon cloth.
Electrochemical performance testing process:
to be coated with Bi 2 O 3 Carbon cloth of (2) is used as a working electrode, and a three-electrode system is constructed; before testing, electrode activation was first performed by 100 cycles of Cyclic Voltammetry (CV) in the potential window-1V-0V interval, then at 1Ag -1 Constant current charge and discharge (GCD) test is carried out under the charge and discharge current density, and the capacitance of the electrode material is calculated according to the curve discharge time. Based on the above test results, the effect of a trace amount of water on electrochemical performance was analyzed.
As a result, as shown in FIG. 3, the redox plateau of the GCD curve in FIG. 3 indicates Bi 2 O 3 Where the redox reaction occurs, further illustrating its pseudocapacitive behavior. Bi when 6mL of water was added 2 O 3 The electrode charge and discharge time is longest, and the current density is 1A g -1 When the capacitance reaches 889F g -1 Bi without adding water 2 O 3 Electrode and Bi with 12mL of water added 2 O 3 Electrode, bi added with 24mL of water 2 O 3 The charge and discharge time of the electrodes is not greatly different. Thus, bi was added with 6mL of water 2 O 3 Exhibits the best capacitance performance, which is mainly due to Bi added with 6mL of water 2 O 3 Ultra-thin nano-sheets appear in the electrode, and the sheet structure improves Bi 2 O 3 The number of surface active sites is increased, thereby increasing the capacitance.
The present invention is not limited to the above embodiments, but is merely preferred embodiments of the present invention, and the present invention should be construed as being limited to the above embodiments as long as the technical effects of the present invention are achieved by the same means. Various modifications and variations are possible in the technical solution and/or in the embodiments within the scope of the invention.
Claims (7)
1. The preparation method of the flower-like bismuth trioxide is characterized by comprising the following steps of: bi (NO) 3 ) 3 ·5H 2 Adding O into ethylene glycol, stirring to form a transparent solution, then adding a mixed solution of water and ethanol, and heating at 140-170 ℃ for 5-8h to obtain the bismuth trioxide; bi (NO) 3 ) 3 ·5H 2 O: ethylene glycol: mixed solution = 1.96g:48mL:24 And (3) mL.
2. A flower-like bismuth trioxide produced by the production method according to claim 1.
3. The flower-like bismuth trioxide according to claim 2, characterized in that the nanoplatelets thereof have a thickness of 8-20nm and a flower-like diameter of 3-10 μm.
4. Use of the flower-like bismuth trioxide according to claim 2 or 3 as a negative electrode material for supercapacitors.
5. An electrode prepared from the flower-like bismuth trioxide according to claim 2 or 3.
6. The electrode according to claim 5, wherein the preparation process is: mixing flower-like bismuth trioxide, carbon black and PVDF uniformly, adding N-methyl pyrrolidone, grinding uniformly to form uniform slurry, coating the slurry on the surface of carbon cloth, and drying to obtain the electrode.
7. The electrode of claim 6, wherein the mass ratio of flower-like bismuth trioxide, carbon black and PVDF is 8:1:1.
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