CN111477864A - Preparation method and application of superfine metal bismuth nano material - Google Patents
Preparation method and application of superfine metal bismuth nano material Download PDFInfo
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- CN111477864A CN111477864A CN202010286700.7A CN202010286700A CN111477864A CN 111477864 A CN111477864 A CN 111477864A CN 202010286700 A CN202010286700 A CN 202010286700A CN 111477864 A CN111477864 A CN 111477864A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F1/00—Metallic powder; Treatment of metallic powder, e.g. to facilitate working or to improve properties
- B22F1/05—Metallic powder characterised by the size or surface area of the particles
- B22F1/054—Nanosized particles
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
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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
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/027—Negative electrodes
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a preparation method and application of a superfine metal bismuth nano material. The preparation method has the advantages of low cost of raw materials, extremely high synthesis efficiency, no surfactant, environmental protection, no pollution, low energy consumption and suitability for industrialization.
Description
Technical Field
The invention relates to a preparation method of a superfine metal bismuth nano material, belongs to the technical field of nano material preparation, and is mainly used as a negative electrode material of a potassium ion battery.
Background
With the increasing population of the world and the continuous development of modern industrialization, the human life and development also encounter two problems, namely environmental pollution and energy shortage, so the development and utilization of sustainable clean energy has stimulated the research interest of countries in the world. The development of rechargeable secondary battery technology is an important means to solve the above problems. Over the past few decades, lithium ion batteries have achieved unprecedented success in commercialization. With the continuous consumption of lithium resources, the cost of lithium ion batteries is gradually increased, thereby affecting the large-scale application of lithium ion batteries. Because potassium is close to the low standard oxidation-reduction potential (-2.93V vs. -3.04V) of lithium and the potassium resource reserves are abundant, potassium ion batteries are gradually developed and become the energy storage technology which is the most possible substitute for lithium ion batteries. Under the background, the nano material plays more and more important roles in the energy field due to the unique property of the nano material, wherein the alloy type nano material has the advantages of high conductivity, low cost, environmental friendliness, high chemical activity and the like, so that the material is widely concerned by scientists. More importantly, the superfine nano material is beneficial to the potassium ion battery to exert excellent performance. In view of this, the rapid and efficient preparation of an ultrafine nano-sized nanomaterial has a very important research significance for the application and development of potassium ion batteries.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provides a preparation method of an ultrafine metal bismuth nano material, which is mainly used as a negative electrode material of a potassium ion battery.
The technical purpose of the invention is realized by the following technical scheme.
A preparation method of an ultrafine metal bismuth nano material comprises the following steps:
step 1, cutting basswood into slices, placing the slices in a muffle furnace for calcination, wherein the calcination temperature is 250-260 ℃ and the calcination time is 4-6 hours, placing the slices in a tubular furnace in an inert protective atmosphere, preserving heat for 5-10 hours at 1000 +/-100 ℃, placing the slices in the muffle furnace at 300-350 ℃ for 1-3 hours, and cooling the slices to room temperature of 20-25 ℃ along with the furnace to obtain carbonized wood slices;
in step 1, basswood is cut into thin slices with a thickness of 100-500 nm.
In step 1, the muffle furnace is in an air atmosphere.
In step 1, the inert protective atmosphere is nitrogen, helium or argon.
In the step 1, the basswood is cut into slices and placed in a muffle furnace for calcination, the calcination temperature is 250-260 ℃, the calcination time is 5-6 hours, then the basswood is placed in a tubular furnace with inert protective atmosphere, the heat preservation is carried out for 6-8 hours under the condition of 1000 +/-50 ℃, and then the basswood is placed in the muffle furnace with 340-350 ℃ for the heat preservation for 2-3 hours.
in step 2, the bismuth salt is Bi (NO)3)3·5H2O, the concentration is 0.05-0.1 mol/L.
In step 2, the soaking temperature is 20-25 ℃ and the soaking time is 10-20 hours, preferably 12-15 hours.
In step 2, after the soaking, drying is performed at 50 to 60 ℃ for 10 to 20 hours, preferably 12 to 15 hours.
And 3, fixing two ends of the carbonized wood sheet loaded with the bismuth salt obtained in the step 2 on a conductive copper foil by using silver adhesive, connecting the conductive copper foil with a direct current power supply to form a closed loop, wherein the direction of an electric field is vertical to the direction of a channel in the wood, and performing rapid high-temperature thermal shock reaction by using the Joule heating principle to prepare the superfine metal bismuth nano material in the carbonized wood sheet.
In step 3, the voltage of the DC power supply is 1-50V, preferably 1-10V.
In step 3, the reaction time is in the order of seconds, for example, less than 5 seconds, preferably 0.1 to 1 second.
The invention belongs to the technical field of nano material preparation, and discloses a superfine metal bismuth nano material prepared by a high-temperature thermal shock method. The carbonized wood veneer is soaked in a bismuth salt solution, after the carbonized wood veneer is dried, two ends of the carbonized wood veneer are fixed on a conductive copper foil through silver glue, then the conductive copper foil is connected with a direct current power supply to form a closed loop, rapid high-temperature thermal shock reaction is carried out by utilizing the joule heating principle, and finally, the superfine metal bismuth nano material is prepared and can be used as a potassium ion battery cathode material. The preparation method has the advantages of low cost of raw materials, extremely high synthesis efficiency, no surfactant, environmental protection, no pollution, low energy consumption and suitability for industrialization.
Drawings
FIG. 1 is an SEM photograph of the ultrafine metallic bismuth nano-material prepared by the present invention.
FIG. 2 is an EDS-mapping spectrum of the ultra-fine metallic bismuth nano-material prepared by the present invention.
FIG. 3 is a cycle performance test curve diagram of the application of the superfine metallic bismuth nano-material prepared by the invention to a potassium ion battery cathode material.
Detailed Description
The technical scheme of the invention is further explained by combining specific examples.
Cutting basswood into 300nm slices, and placing in muffle furnaceCalcining at 260 deg.C for 6 hr, placing in Ar atmosphere tube furnace, holding at 1000 deg.C for 6 hr, holding at 350 deg.C in muffle furnace for 2 hr to obtain carbonized wood veneer, soaking the carbonized wood veneer in Bi (NO) with concentration of 0.05 mol/L3)3·5H2Soaking in O water solution for 12h, and drying in an oven at 50 deg.C for 12h to obtain supported Bi (NO)3)3The loading position is the surface of the carbonized wood veneer and the channel pipe. Will load Bi (NO)3)3The two ends of the carbonized wood sheet are fixed on the conductive copper foil by silver adhesive, the conductive copper foil is connected with a direct current power supply to form a closed loop, the direction of an electric field is vertical to the direction of a channel in the wood, the rapid high-temperature thermal shock reaction is carried out by utilizing the Joule heating principle, the reaction time is 1s, and the voltage is 10V (the Joule heating principle is that when energy is transferred to atoms of a conductor by conduction electrons in a collision mode, heat can be generated on a micro scale, namely when current passes through the carbonized wood sheet attached with bismuth salt, the resistance loss in the material can convert electric energy into heat energy to act on a precursor), and finally, the superfine metal bismuth nano material is prepared in the wood.
The superfine metallic bismuth nano material prepared by the invention is physically characterized by taking the superfine metallic bismuth nano material as an example. Scanning Electron Microscope (SEM) photographs, as shown in fig. 1, the wood vertical channels remained unobstructed after the high temperature reaction. On the section of the wood, the metal bismuth nanoparticles are uniformly dispersed on the wall of the channel tube, and the diameter of the bismuth nanoparticles is 25 +/-5 nm. Wood has an open and low-tortuosity structure that facilitates electrolyte penetration, thereby increasing the ion transport rate. The superfine metal bismuth nano-particles not only improve the specific surface area of the material, but also enhance the electrochemical activity of the material. The material with the structure can be directly applied to the negative electrode material of the potassium ion battery without any surfactant or binder. The EDS-mapping spectrum is shown in figure 2, bismuth is successfully detected, and the superfine metal bismuth nano material is successfully prepared; the bismuth element is uniformly distributed on the map, and further shows that the bismuth nanoparticles are uniformly dispersed on the wall of the wood.
The sample prepared in the example (carbonized wood veneer with uniformly dispersed bismuth nanoparticles) is directly used as a working electrode, and is assembled into a button cell in a glove box without adding conductive carbon black and a binder, wherein a diaphragm is glass fiber, a contrast electrode is a metal potassium sheet, and an electrolyte is KPF (potassium fluoride) with the concentration of 0.8M6EC/DEC (1: 1 by volume) solution of (D). The prepared button cell is placed in a blue cell test system for testing, wherein the charging and discharging interval is set to be 0.01V-3V, the current density is set to be 50mA/g, and the performance test is shown in figure 3. The cycle performance graph shows that the first discharge specific capacity of the prepared superfine metal bismuth nano material is 2.3mAh cm-2And the electrochemical performance is better when the charge and discharge test is carried out at room temperature and at the current density of 50 mA/g.
The preparation of the superfine metal bismuth nano material can be realized by adjusting the process parameters according to the content of the invention, and the test shows that the performance is basically consistent with that of the invention. The invention has been described in an illustrative manner, and it is to be understood that any simple variations, modifications or other equivalent changes which can be made by one skilled in the art without departing from the spirit of the invention fall within the scope of the invention.
Claims (10)
1. The preparation method of the superfine metal bismuth nano material is characterized by comprising the following steps of:
step 1, cutting basswood into slices, placing the slices in a muffle furnace for calcination, wherein the calcination temperature is 250-260 ℃ and the calcination time is 4-6 hours, placing the slices in a tubular furnace in an inert protective atmosphere, preserving heat for 5-10 hours at 1000 +/-100 ℃, placing the slices in the muffle furnace at 300-350 ℃ for 1-3 hours, and cooling the slices to room temperature of 20-25 ℃ along with the furnace to obtain carbonized wood slices;
step 2, soaking the carbonized wood veneer obtained in the step 1 into a bismuth salt aqueous solution so as to load bismuth salt on the carbonized wood veneer to obtain a carbonized wood veneer loaded with bismuth salt;
and 3, fixing two ends of the carbonized wood sheet loaded with the bismuth salt obtained in the step 2 on a conductive copper foil by using silver adhesive, connecting the conductive copper foil with a direct current power supply to form a closed loop, wherein the direction of an electric field is vertical to the direction of a channel in the wood, and performing rapid high-temperature thermal shock reaction by using the Joule heating principle to prepare the superfine metal bismuth nano material in the carbonized wood sheet.
2. The method of claim 1, wherein in the step 1, basswood is sliced to a thickness of 100 to 500 nm.
3. The method for preparing the ultrafine metallic bismuth nano-material according to claim 1, wherein in the step 1, the muffle furnace is in an air atmosphere; the inert protective atmosphere is nitrogen, helium or argon.
4. The method for preparing the ultra-fine metallic bismuth nano-material according to claim 1, wherein in the step 1, basswood is sliced and placed in a muffle furnace for calcination, the calcination temperature is 250-260 ℃ and the calcination time is 5-6 hours, then the basswood is placed in a tube furnace with an inert protective atmosphere, the heat preservation is carried out for 6-8 hours under the condition of 1000 +/-50 ℃, and then the heat preservation is carried out for 2-3 hours in the muffle furnace with the temperature of 340-350 ℃.
5. The method as claimed in claim 1, wherein in step 2, the bismuth salt is Bi (NO)3)3·5H2O, the concentration is 0.05-0.1 mol/L.
6. The method for preparing ultra-fine metallic bismuth nano-material according to claim 1, wherein in the step 2, the soaking temperature is 20-25 ℃ and the soaking time is 10-20 hours, preferably 12-15 hours.
7. The method of claim 1, wherein the voltage of the DC power supply in step 3 is 1-50V, preferably 1-10V.
8. The method as claimed in claim 1, wherein the reaction time in step 3 is in the order of seconds.
9. The method of claim 8, wherein the reaction time in step 3 is less than 5 seconds, preferably 0.1-1 s.
10. Use of the material obtained by the preparation method according to any one of claims 1 to 9 in the negative electrode material of a potassium ion battery.
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Cited By (7)
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| CN112404449A (en) * | 2020-10-23 | 2021-02-26 | 中国科学技术大学 | Device and method for continuously synthesizing powder material based on thermal shock |
| CN113247962A (en) * | 2021-06-26 | 2021-08-13 | 深圳中科精研科技有限公司 | Battery anode material and method for rapidly synthesizing battery anode material |
| CN113293406A (en) * | 2021-06-03 | 2021-08-24 | 中国科学技术大学 | Nano electro-catalyst, synthesis method, test electrode and preparation method |
| CN113353986A (en) * | 2021-07-08 | 2021-09-07 | 天津大学 | Rapid preparation method and application of lithium manganate cathode material |
| CN113526565A (en) * | 2021-07-09 | 2021-10-22 | 天津大学 | Method for rapidly synthesizing lithium cobaltate cathode material and application |
| CN113578222A (en) * | 2021-07-12 | 2021-11-02 | 浙江大学 | Nanocomposite synthesis device based on instantaneous high-temperature Joule heating method, preparation method and application |
| CN114823153A (en) * | 2022-04-24 | 2022-07-29 | 华星先进科学技术应用研究(天津)有限公司 | Flexible sodium ion capacitor electrode material |
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| CN114823153A (en) * | 2022-04-24 | 2022-07-29 | 华星先进科学技术应用研究(天津)有限公司 | Flexible sodium ion capacitor electrode material |
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