CN108711608B - Three-dimensional net wall-shaped all-solid-state lithium ion battery cathode, preparation method and battery - Google Patents
Three-dimensional net wall-shaped all-solid-state lithium ion battery cathode, preparation method and battery Download PDFInfo
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Abstract
The invention discloses a honeycomb-like three-dimensional net wall-shaped all-solid-state thin film lithium ion battery cathode, a preparation method and an all-solid-state thin film lithium ion battery, wherein the all-solid-state thin film lithium ion battery cathode is formed by vertical wall-shaped Sb2S3The nano sheets are connected into a net to form an integral honeycomb-like film, wherein each sheet Sb is Sb2S3The thickness of the nanometer wall is 10nm-100nm, and the length is 0.5um-3 um. In the technical scheme of the invention, Sb with a honeycomb-like three-dimensional net wall-like structure2S3The performance is excellent, the capacity is high, the capacity retention rate is high in the circulation process, the preparation method of the vacuum thermal evaporation method requires simple equipment, the process is easy to realize, and the method can be used for continuous film coating and can be applied to industrialization.
Description
Technical Field
The invention relates to a honeycomb-like three-dimensional net wall-shaped all-solid-state thin film lithium ion battery cathode, a preparation method and an all-solid-state thin film lithium ion battery, and belongs to the technical field of lithium ion batteries.
Background
As one of the key development directions of the next generation lithium battery, the all-solid-state lithium battery has the advantages of safety, high energy and power, and the like, and is more and more favored by the academic and industrial circles. And can be classified into a polymer solid lithium battery, an inorganic solid lithium battery, and a composite solid lithium battery according to the properties of the electrolyte. The battery is mainly applied to the fields of large-scale energy storage, power automobiles, airplanes, aerospace, war industry and the like, and meanwhile, the all-solid-state lithium battery with the thin film is one of the hot spots of research in recent years. The all-solid-state thin-film lithium (ion) battery can be divided into an all-solid-state thin-film lithium battery (metal lithium is used as a negative electrode), an all-solid-state thin-film lithium ion battery (other non-lithium negative electrodes) and an all-solid-state thin-film lithium-free battery (a lithium thin film is formed in the charging and discharging process) according to the negative electrode, the application range of the all-solid-state thin-film lithium battery is limited due to the low melting point of the metal lithium, and the volume change of the lithium-free battery in the charging and discharging. Therefore, the all-solid-state thin film lithium ion battery adopting other substances with high theoretical specific capacity, strong thermal and chemical stability and cheap and easily-obtained materials as the negative electrode is expected to meet the development requirement in the future.
The transition metal sulfide as the negative electrode film has many advantages, the theoretical specific capacity of the transition metal sulfide is high (generally one time or several times of that of a carbon negative electrode material), the thermal and chemical stability is strong, the material is relatively cheap and easy to obtain, and the transition metal sulfide is an ideal negative electrode material of an all-solid-state film lithium ion battery. The antimony sulfide shows higher theoretical specific capacity (946mAh/g) when being used as a negative electrode, high temperature stability (melting point 550 ℃) and natural existence of sulfide ore, and is suitable for local material utilization and large-scale industrialization. However, antimony sulfide has the common defects of antimony-based materials, namely, a large volume effect is accompanied in the lithium extraction process, so that the materials collapse in the circulation process and fall off from a current collector, and the electrochemical activity is lost. Sb2S3The material is nanocrystallized orThe preparation of the three-dimensional microstructure is an effective method for solving the bottleneck of the commercial application of the microstructure. The literature reports that Sb with a rod-shaped nano structure, a flower-bunch-shaped microstructure, a micron strip-shaped structure and the like is prepared by a hydrothermal method, a microwave irradiation method, a high-energy ball milling method, a coprecipitation method and the like2S3The negative electrode is used in a conventional lithium ion battery. The patent application No. 201410616579.4 entitled "preparation method of spherical lamellar antimony sulfide film", prepares Sb with lamellar sphere by liquid phase deposition method2S3The film is applied to the field of solar electronic devices. The patent application number is 201710569803.2, the name is 'plane structure hybrid solar cell based on antimony trisulfide dense film', Sb is prepared under inert atmosphere2S3The precursor solution is coated on the electron transport layer in a spin mode, and then the solution is heated on a heating table to react to generate Sb2S3Repeating spin coating and heating to adjust thickness, and annealing at increased temperature to obtain Sb2S3And (4) crystallizing. The method for preparing the film has low deposition rate, higher equipment requirement and more complex process, and is not suitable for industrialized application. Although there are three-dimensional morphologies involved, it is not relevant to all-solid-state thin film lithium ion batteries, nor to addressing volume effects. The preparation of Sb by vacuum thermal evaporation method has been reported2S3Applied to solar cells, but prepared Sb2S3Most of the amorphous state is amorphous, and the nano-crystalline amorphous state has no nano-or three-dimensional appearance and has no popularization value.
Disclosure of Invention
The invention aims to overcome the defects of the conventional all-solid-state lithium ion battery cathode film and provide Sb with a honeycomb-like three-dimensional net wall-shaped structure, high capacity and good cycle performance2S3An anode and an all-solid-state lithium ion battery including the anode.
It is also an object of the present invention to provide Sb for preparing such 3D structures2S3The method for preparing the cathode has the advantages of high yield, low cost and controllable product, and is suitable for large-scale industrialization.
In order to achieve the purpose, the invention provides a honeycomb-like three-dimensional net wall-shaped full bodyThe solid-state thin-film lithium ion battery cathode is made of vertical wall-shaped Sb2S3The nano sheets are connected into a net to form an integral honeycomb-like film, wherein each sheet Sb is Sb2S3The thickness of the nanometer wall is 10nm-100nm, and the length is 0.5um-3 um.
In order to achieve the purpose, the invention provides a preparation method of the honeycomb-like three-dimensional net wall-shaped all-solid-state thin film lithium ion battery cathode, which is prepared from Sb2S3Is an evaporation source, a conductive current collector is a deposition substrate, and an evaporation chamber is vacuumized to 2 multiplied by 10-3And (4) below Pa, starting an evaporation power supply, gradually adjusting the current from 0 to 0.1-120A, evaporating for 1 s-5 h, and closing the evaporation power supply.
Preferably, the vacuum degree of the evaporation chamber is 1 × 10-3Pa～1×10-5Pa, the evaporation current is 1-100A, and the evaporation time is 10 s-60 min.
Preferably, the regulating speed of the current is 0.01-0.2A/s.
Preferably, Sb2S3The evaporation source is one or more of minerals, recovered products or finished products with the purity of more than 95 percent, and Sb2S3The physical appearance of the evaporation source is one or more of block shape or powder shape.
Preferably, the conductive current collector is a smooth and flat current collector comprising one or more of a stainless steel foil, a titanium foil, and a copper foil.
Preferably, the conductive current collector is a current collector with a 3D structure, and the current collector with the 3D structure includes one or more of stainless steel fiber wires, nickel foam, carbon cloth, carbon paper, and carbon nanotubes.
In order to achieve the above object, the all-solid-state thin film lithium ion battery provided by the present invention comprises a positive electrode, a negative electrode and a solid electrolyte interposed between the positive electrode and the negative electrode, wherein the negative electrode is the negative electrode as described above.
In the technical scheme of the invention, Sb prepared by adopting a vacuum thermal evaporation method2S3The film cathode has a three-dimensional net wall-shaped structure, is formed by connecting vertical wall-shaped nanosheets into nets, and is integrally honeycomb-likeIn the form of each sheet Sb2S3The thickness of the nanometer wall is 10nm-100nm, and the length is 0.5um-3 um. Due to the honeycomb-like three-dimensional net wall-shaped Sb2S3The negative electrode film is uniform and continuous, has large specific surface area, and can effectively solve the problem of Sb2S3The volume effect of the material in the lithium-releasing reaction is high, and the material has high capacity and good cycle performance. In the charging and discharging process, the first discharging specific capacity reaches 1266mAh/g under the multiplying power of 0.01V-3V and 0.1C, the first charging specific capacity reaches 849mAh/g, the first-turn coulombic efficiency reaches 67%, after five cycles of circulation under the multiplying power of 0.1C, the first-turn specific capacity is continuously circulated to 60 cycles under the multiplying power of 0.2C, the charging specific capacity is increased to 923mAh/g, the theoretical specific capacity reaches more than 97%, and the capacity retention rate is high.
The performances show that the Sb with the honeycomb-like three-dimensional net wall-like structure prepared by the vacuum thermal evaporation method2S3The lithium ion battery has the advantages of excellent performance, high capacity and high capacity retention rate in the circulation process, and is suitable for popularization and application in all-solid-state thin film lithium ion batteries. Meanwhile, the preparation method requires simple equipment, is easy to realize, can continuously coat the film and can be industrially applied.
Drawings
FIG. 1 is an XRD spectrum of a thin film anode obtained in example 1;
FIG. 2 is a scanning electron microscope image of the surface of the thin film negative electrode obtained in example 1;
FIG. 3 is a scanning electron micrograph of the surface of the negative electrode of the thin film obtained in example 1 on another scale;
FIG. 4 is a charge/discharge plateau curve of the thin film negative electrode obtained in example 1;
fig. 5 is a graph of the cycle rate performance of the thin film negative electrode obtained in example 1.
Detailed Description
The present invention will be described in further detail below with reference to the drawings and specific examples, but the present invention is not limited to the following examples.
Example 1
Antimony sulfide powder with purity of 99% is used as an evaporation source, a conductive current collector of a stainless steel foil is used as a deposition substrate, and an evaporation chamber is vacuumized to 1 x 10-4Pa, turning on the evaporation power supplyThe current was adjusted from 0 to 1.5A at 0.1A/s and the evaporation power was turned off after 10min of evaporation. Wherein, antimony sulfide powder is heated uniformly by slowly adjusting current, so as to obtain uniform Sb on the conductive current collector2S3A film.
Referring to FIG. 1, it can be confirmed by X-ray diffraction that the material prepared by the above method is pure Sb2S3And (4) crystals.
By determining the morphology through a scanning electron microscope, please refer to fig. 2 and 3, it can be seen that the thin film is formed by vertical walls Sb2S3The nano sheets are connected into a net and are integrally honeycomb-like, and each sheet of Sb2S3The thickness of the nanometer wall is 10 nm-20 nm, the length is 0.5 um-1 um, the specific surface area is large, and Sb can be effectively solved2S3Volume effect of material in the lithium deintercalation reaction.
The electrochemical performance test of the film cathode adopts a lithium sheet as a counter electrode and a reference electrode, and the electrolyte is 1M LiPF6+ EC/DEC/DMC (1:1:1, V/V/V), adopt Celgard 2032 diaphragm, assemble CR2032 button cell, the charging and discharging performance is confirmed by LAND test system, please refer to figure 5 for the performance of cycle multiplying power, please refer to figure 4 for the curve of charging and discharging platform, it can be found that, in the charging and discharging process, the first discharging specific capacity reaches 1266.9mAh/g under 0.01V-3V and 0.1C multiplying power, the first charging specific capacity reaches 849.5mAh/g, the first turn coulomb efficiency reaches 67.05%, after circulating for five turns under 0.1C multiplying power, continue circulating to 60 turns under 0.2C multiplying power and charge the specific capacity and rise to some extent, reach 923.2mAh/g, reach 97.6% of its theoretical specific capacity, have higher capacity retention ratio.
Example 2
Using stibnite as evaporation source, using the conductive current collector of titanium foil as deposition substrate, and vacuumizing the evaporation chamber to 0.8 × 10- 3Pa, turning on an evaporation power supply, regulating the current from 0 to 30A at the speed of 0.2A/s, and turning off the evaporation power supply after evaporation for 20 min.
The appearance is determined by a scanning electron microscope, and the fact that the film is formed by vertical wall-shaped Sb can be found2S3The nano sheets are connected into a net and are integrally honeycomb-like, and each sheet of Sb2S3The thickness of the nanometer wall is 30 nm-70 nm, and the length is 0.8 um-2 um.
The electrochemical performance test of the film cathode adopts a lithium sheet as a counter electrode and a reference electrode, and the electrolyte is 1M LiPF6+ EC/DEC/DMC (1:1:1, V/V/V), adopt Celgard 2032 diaphragm, assemble CR2032 button cell, the charging and discharging performance is confirmed by LAND test system, can find, in the course of charging and discharging under 0.01V-3V and 0.1C multiplying power first discharge specific capacity reach 1280.3mAh/g, first charge specific capacity reach 865.8mAh/g, first turn coulombic efficiency reach 67.62%, after circulating five rounds under 0.1C multiplying power, continue circulating to 60 rounds under 0.2C multiplying power and charge the specific capacity and rise, reach 920.8mAh/g, reach 97.3% of its theoretical specific capacity, there is higher capacity retention rate.
Example 3
With Sb2S3The recycled product is an evaporation source, the conductive current collector of the foamed nickel is a deposition substrate, and an evaporation chamber is vacuumized to 0.8 multiplied by 10-3Pa, turning on an evaporation power supply, regulating the current from 0 to 10A at the speed of 0.08A/s, and turning off the evaporation power supply after 50s of evaporation. In addition, Sb is2S3The impurities in the recovered product of (1) were not evaporated onto the deposition substrate under a current of 10A.
The appearance is determined by a scanning electron microscope, and the fact that the film is formed by vertical wall-shaped Sb can be found2S3The nano sheets are connected into a net and are integrally honeycomb-like, and each sheet of Sb2S3The thickness of the nanometer wall is 15 nm-30 nm, and the length is 1 um-2 um.
The electrochemical performance test of the film cathode adopts a lithium sheet as a counter electrode and a reference electrode, and the electrolyte is 1M LiPF6+ EC/DEC/DMC (1:1:1, V/V/V/V), adopt Celgard 2032 diaphragm, assemble CR2032 button cell, the charging and discharging performance is confirmed by LAND test system, can find, in the course of charging and discharging under 0.01V-3V and 0.1C multiplying power first discharge specific capacity reach 1268mAh/g, first charge specific capacity reach 870mAh/g, first circle coulombic efficiency reach 68.61%, after circulating five circles under 0.1C multiplying power, continue circulating to 60 circles under 0.2C multiplying power and charge specific capacity and rise, reach mA924 h/g, reach its theoretical97.67% of specific capacity, and has higher capacity retention rate.
The above embodiments are merely illustrative of the technical ideas and features of the present invention, and the purpose thereof is to enable those skilled in the art to understand the contents of the present invention and implement the present invention, and not to limit the protection scope of the present invention. All equivalent changes and modifications made according to the spirit of the present invention should be covered within the protection scope of the present invention.
Claims (8)
1. The honeycomb-like three-dimensional net wall-shaped all-solid-state thin film lithium ion battery cathode is characterized in that the cathode is vertical wall-shaped Sb2S3The nano sheets are connected into a net to form an integral honeycomb-like film, wherein each sheet Sb is Sb2S3The thickness of the nanometer wall is 10nm-100nm, and the length is 0.5um-3 um.
2. The preparation method of the honeycomb-like three-dimensional net wall-shaped all-solid-state thin film lithium ion battery cathode according to claim 1, characterized in that Sb is used2S3Is an evaporation source, a conductive current collector is a deposition substrate, and an evaporation chamber is vacuumized to 2 multiplied by 10-3And (4) below Pa, starting an evaporation power supply, gradually adjusting the current from 0 to 0.1-120A, evaporating for 1 s-5 h, and closing the evaporation power supply.
3. The method of claim 2, wherein the vacuum degree of the evaporation chamber is 1 x 10-3Pa～1×10-5Pa, the evaporation current is 1-100A, and the evaporation time is 10 s-60 min.
4. The method according to claim 2, wherein the current is adjusted at a rate of 0.01 to 0.2A/s.
5. The production method according to any one of claims 2 to 4, wherein Sb is2S3The evaporation source is one or more of minerals, recovered products or finished products with the purity of more than 95 percent, and Sb2S3Article of evaporation sourceThe physical appearance is one or more of block shape or powder shape.
6. The method of any one of claims 2-4, wherein the conductive current collector is a smooth, flat current collector comprising one of a stainless steel foil, a titanium foil, and a copper foil.
7. The method according to any one of claims 2 to 4, wherein the conductive current collector is a 3D structured current collector, and the 3D structured current collector comprises one of stainless steel fiber filament, nickel foam, carbon cloth, carbon paper, and carbon nanotube.
8. An all-solid-state thin-film lithium ion battery comprising a positive electrode, a negative electrode and a solid electrolyte interposed between the positive electrode and the negative electrode, wherein the negative electrode is the negative electrode of claim 1.
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| CN110380044B (en) * | 2019-08-22 | 2021-05-11 | 中南大学 | Preparation method of titanium dioxide/antimony sulfide porous composite cathode of lithium ion battery |
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| Facile synthesis of symmetric bundle-like Sb2S3 micron-structures and their application in lithiumion battery anodes;Zheng Yi,ect.;《ROYAL SOSIETY OF CHEMISTRY》;20160608;第7691-7692页 * |
| The influence of the post-deposition treatment on some physical properties of Sb2S3 thin films;N. Tigaˇu，ect.;《Journal of Non-Crystalline Solids》;20050323;第2-3节 * |
| Zheng Yi,ect..Facile synthesis of symmetric bundle-like Sb2S3 micron-structures and their application in lithiumion battery anodes.《ROYAL SOSIETY OF CHEMISTRY》.2016, * |
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