CN110808361A - Method for preparing lithium-sulfur battery cathode material based on bacterial cellulose - Google Patents
Method for preparing lithium-sulfur battery cathode material based on bacterial cellulose Download PDFInfo
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Abstract
The invention discloses a method for preparing a lithium-sulfur battery cathode material based on bacterial cellulose. Preparing a tin ion solution, and putting the BC aerogel and the tin ion solution into a reaction kettle according to the mass ratio of 1:1 to prepare BC-SnO2Calcining the main body material in the nitrogen atmosphere to combine the bacterial cellulose and the tin dioxide to form a three-dimensional composite material, and mixing the BC-SnO with the three-dimensional composite material2And finally, preparing the lithium-sulfur battery cathode material by using the three-dimensional material as a sulfur carrier.In the preparation process of the invention, SnO is uniformly combined on the surface of the bacterial cellulose2Natural interweaved network structure of nano particles and BC aerogel and SnO2The synergistic effect of the nano particles can better increase the loading capacity of sulfur so as to improve the volumetric specific capacity of the battery, the porous structure also effectively relieves the sulfur expansion phenomenon generated when the battery works, and simultaneously inhibits the shuttle effect of polysulfide. Effectively improves the theoretical specific capacity of the battery and forms stable cycle performance.
Description
Technical Field
The invention relates to the technical field of preparation of a lithium-sulfur battery positive electrode material and the field of preparation and application of bacterial cellulose.
Background
In recent years, among all available energy storage devices, lithium ion batteries have been dominant due to their efficient cleaning characteristics. However, the cost and energy density of lithium ion batteries still cannot meet the energy storage requirements of the market for electric vehicles and power supply networks, and people need energy storage devices with higher energy density. The theoretical capacity of the lithium-sulfur battery can reach 1675Amh/g, which is far beyond the lithium-ion battery used in the emergence stage, and the lithium-sulfur battery is widely considered as one candidate of the next-generation energy storage device. The failure of lithium-sulfur batteries to be put into practice on a large scale mainly results from the low area loading of sulfur and several obvious drawbacks of sulfur positive electrode materials, for example, the large volume expansion of sulfur leads to poor battery stability, and the inherent insulation property also causes very low conductivity of the positive electrode; the shuttling effect of polysulfides, as well as the deposition of insulating insoluble lithium disulfide and lithium sulfide on the cathode material, hinders the electrochemical reaction, resulting in cells exhibiting low coulombic efficiency and rapid capacity fade.
At present, the research method for improving the defects of the sulfur cathode material of the lithium-sulfur battery at home and abroad mainly comprises the following aspects: introducing a carbon-based substance to increase the conductivity of sulfur and inhibit the expansion phenomenon of sulfur; the polar metal oxide is utilized to form a high-strength chemical bond with polysulfide so as to reduce the shuttling effect of the polysulfide; conductive polymer additives, such as polypyrrole, polyaniline, polythiophene, etc., are added to improve the electrochemical performance of the lithium-sulfur battery due to their special morphology and conductivity. Among them, three-dimensional carbon nanomaterials, such as carbon aerogel, carbon nanotubes and graphene foam, have interconnected network structures, abundant pore structures, high conductivity, good chemical stability and excellent environmental compatibility, thus drawing much attention. However, the current mainstream methods for preparing 3D carbon nanomaterials inevitably have some disadvantages such as toxic and expensive precursor materials, complicated technical equipment requirements, and low productivity. Compared to these methods, the production of high performance 3D carbon-based materials with bacterial cellulose may overcome to some extent the several problems described above.
Disclosure of Invention
Aiming at the prior art, the invention provides a novel method for preparing a lithium-sulfur battery cathode material. Selecting bacterial cellulose as a substrate, and depositing a layer of SnO on the surface of the bacterial cellulose2Nanometer particles, and then the BC aerogel is carbonized to synthesize the three-dimensional BC-SnO with good electric conductivity2The main body material can load a large amount of sulfur to prepare the sulfur positive electrode BC-SnO of the lithium-sulfur battery2@ S. The electrode material prepared by the method can increase the capacity density of the battery, prevent the shuttle effect of polysulfide to a greater extent and relieve the potential safety hazard caused by the expansion phenomenon of sulfur of the battery in a long-time working state.
In order to solve the technical problems, the invention provides a method for preparing a lithium-sulfur battery cathode material based on bacterial cellulose, which comprises the following steps:
step one, preparing a tin ion solution: dissolving a certain amount of tin tetrachloride pentahydrate in a proper amount of ethanol water solution, and stirring to obtain a tin ion solution with the molar concentration of 1-10 mmol/L;
step two, preparing bacterial cellulose-stannic oxide (BC-SnO)2) Main material: placing the bacterial cellulose aerogel and the tin ion solution prepared in the first step into a reaction kettle according to the mass ratio of 1:1, stirring for 30min, sealing the container in a steel high-pressure kettle, and keeping the temperature in an electric furnace at 200 ℃ for 8 h; naturally cooling, collecting precipitate by vacuum filtration, washing with pure ethanol for 3-5 times, and drying to obtain BC-SnO2A host material;
step three, preparing bacterial cellulose-stannic oxide (BC-SnO)2) Three-dimensional material: the BC-SnO prepared in the second step2Sintering the main body material in nitrogen atmosphere to obtain BC-SnO2Sintering the three-dimensional material under the technological conditions that the calcining temperature is 450-650 ℃ and the heat preservation time is 1-2 h;
step four, preparing bacterial cellulose-stannic oxide-sulfur (BC-SnO)2@ S) active material: the BC-SnO prepared in the third step2Immersing the three-dimensional material into a proper amount of sulfur/carbon disulfide solution, keeping sealing for 3 hours, taking out the three-dimensional material from the solution, standing in air for 2 hours to completely volatilize carbon disulfide, then placing the three-dimensional material in a sealed high-pressure kettle, and keeping the temperature at 155 ℃ for 3 hours; cooling to room temperature to obtain the flexible BC-SnO2@ S active material;
step five, the BC-SnO prepared in the step four2The @ S active material, the conductive agent and the binding agent are sequentially dissolved into N-methyl pyrrolidone with a sufficient amount according to a mass ratio of 80:10:10, uniform suspension is obtained through continuous stirring, the suspension is used as slurry to be coated on aluminum foil, and the aluminum foil is dried to obtain the lithium-sulfur battery positive electrode material.
Further, in the preparation method of the present invention, preferably, the concentration of the tin ion solution prepared in the first step is 7.5 mmol/L.
In the third step, the calcining temperature is 550 ℃, and the heat preservation time is 2 hours.
The lithium-sulfur battery positive electrode material prepared by the preparation method is used for preparing a lithium-sulfur battery, the lithium-sulfur battery positive electrode material is cut into a wafer with the diameter of 12mm and used as the lithium-sulfur battery positive electrode material, and metal lithium is selected as a negative electrode and assembled into a button battery in a glove box.
Compared with the prior art, the invention has the beneficial effects that:
the innovation of the invention is that unlike graphene/carbon nano-tubes, the price of the bacterial cellulose is economic and low, and the hydroxyl in the structure can be combined with SnO more uniformly2Nanoparticles form BC-SnO with stable structure and uniform distribution2A sulfur positive electrode host material. In addition, the porous fibrous structure of the BC may also physically encapsulate polysulfides to inhibit their dissolution; SnO2The presence of the nanoparticles provides a rich set of electrochemically active sites for rapid diffusion and reaction, and also effectively prevents aggregation of the encapsulated electroactive nanoparticles, forming strong chemical bonds to the polysulfide through oxidation reactions. With no addition of SnO2Compared with the electrode material of the nano particles, the first discharge specific capacity of the battery is improved from 137.28mAh/g to 409.30mAh/g under the current density of 0.1A/g, and the nano particles show thatGood electrochemical performance improving capability.
Drawings
FIG. 1 shows BC-SnO obtained in example 2 of the present invention25000 times of scanning electron microscope pictures of the three-dimensional material;
FIG. 2 shows BC-SnO obtained in example 2 of the present invention250000 times of scanning electron microscope pictures of the three-dimensional material;
FIG. 3 shows BC-SnO obtained in example 2 of the present invention280000 times of scanning electron microscope pictures of the material;
FIG. 4 shows BC-SnO obtained in example 3 of the present invention250000 times of scanning electron microscope pictures of the material;
FIG. 5 shows BC-SnO obtained in example 3 of the present invention280000 times of scanning electron microscope pictures of materials.
Detailed Description
The invention will be further described with reference to the following figures and specific examples, which are not intended to limit the invention in any way.
The invention provides a method for preparing a lithium-sulfur battery cathode material based on bacterial cellulose, which mainly comprises the steps of mixing the Bacterial Cellulose (BC) with stannic oxide (SnO)2) And combining to form a three-dimensional composite material which is used as a sulfur carrier for a positive electrode of a lithium-sulfur battery.
The preparation method comprises the following steps: preparing tin ion solution with the concentration of 1 mmol-10 mmol; placing the bacterial cellulose aerogel and the tin ion solution into a reaction kettle according to the mass ratio of 1:1, stirring for 30min, sealing the container in a steel high-pressure kettle, and keeping the temperature in an electric furnace at 200 ℃ for 8 h; naturally cooling, collecting precipitate by vacuum filtration, washing with pure ethanol for 3-5 times, and drying to obtain BC-SnO2A host material; mixing BC-SnO2Sintering the main body material in nitrogen atmosphere to obtain BC-SnO2A three-dimensional material; mixing the BC-SnO2Immersing the three-dimensional material into a proper amount of sulfur/carbon disulfide solution, keeping sealing for 3 hours, taking out the three-dimensional material from the solution, standing in air for 2 hours to completely volatilize carbon disulfide, then placing the three-dimensional material in a sealed high-pressure kettle, and keeping the temperature at 155 ℃ for 3 hours; cooling to room temperature to obtain the flexible and binderless BC-SnO2@ S active material; will be provided withBC-SnO2The @ S positive electrode material, a conductive agent and a binder are sequentially dissolved into N-methylpyrrolidone according to the mass ratio of 80:10:10, uniform suspension is obtained through continuous stirring, the suspension is used as slurry to be coated on an aluminum foil, and the aluminum foil is dried to obtain the lithium-sulfur battery positive electrode material.
In the preparation structure of the invention, SnO is uniformly combined on the surface of the bacterial cellulose2Natural interweaved network structure of nano particles and bacterial cellulose aerogel and SnO2The synergistic effect of the nano particles can better increase the loading capacity of sulfur so as to improve the volumetric specific capacity of the battery, the porous structure also effectively relieves the sulfur expansion phenomenon generated when the battery works, and simultaneously inhibits the shuttle effect of polysulfide. The three-dimensional composite material improves the defects of the lithium-sulfur battery anode material in many aspects, effectively improves the theoretical specific capacity of the battery, forms stable cycle performance and provides more possibilities for the practical application of the lithium-sulfur battery.
Example 1, synthesis of bacterial cellulose aerogel.
Dissolving 2.5g glucose anhydride, 0.75g yeast extract, 1g lactopeptone and 1g sodium dihydrogen phosphate in 100mL ultrapure water under stirring; culturing bacterial cellulose by an acetobacter xylinum strain; the medium was adjusted to pH 5 using 30% acetic acid and sterilized at 115 ℃ for 30 minutes; culturing at 30 deg.C under static condition for 7 days; heating the bacterial cellulose in water bath at 80 ℃ for 5h by using high-purity water, repeating the heating and heating for three times, purifying and culturing the bacterial cellulose in 1 wt% sodium hydroxide solution for 30min, then repeatedly washing the bacterial cellulose by using ultrapure water until the pH value is 7, and storing the bacterial cellulose in a closed container containing tert-butyl alcohol at room temperature; the solvent-exchanged bacterial cellulose is placed in a freeze-dryer to release the organic solvent and produce a Bacterial Cellulose (BC) aerogel.
Example 2: a lithium sulfur battery was prepared by the following steps:
step one, preparing a tin ion solution with the concentration of 7.5 mmol: dissolving a certain amount of stannic chloride pentahydrate in 30ml of ethanol water solution (the volume ratio of ethanol to water is 3:5), and manually stirring to obtain a semitransparent or clear solution;
step two, preparing BC-SnO2A host material. Will be provided withThe 100mg mass of BC aerogel (prepared in example 1) and 100mg of the tin ion solution prepared in step one were placed in a 50mL reaction vessel, stirred for 30min, sealed in a steel autoclave and kept at 200 ℃ for 8h in an electric furnace. Naturally cooling, collecting precipitate by vacuum filtration, washing with pure ethanol for 5 times, and drying to obtain BC-SnO2A host material;
step three, preparing BC-SnO2A three-dimensional material. The BC-SnO obtained in the second step2Sintering the main material at 550 ℃ in an argon atmosphere, and preserving heat for 2 hours; the scanning electron microscope topography of the material is shown in fig. 1, fig. 2 and fig. 3.
Step four, preparing BC-SnO2@ S active Material: the prepared BC-SnO2The material was immersed in an appropriate amount of sulfur/carbon disulfide solution and kept sealed for 3 h. After the material was removed from the solution, it was allowed to stand in air for 2h to completely volatilize the carbon disulfide. In order to thoroughly penetrate sulfur into BC-SnO2In the pores of the material, BC-SnO is added2The @ S material was placed in a sealed autoclave and incubated at 155 ℃ for 3 h. After cooling to room temperature, a flexible and binder-free BC-SnO was obtained2@ S active material;
step five, preparing the lithium-sulfur battery anode material: 0.08g of BC-SnO prepared in the fourth step2And sequentially dissolving the @ S active material, 0.01g of conductive agent (Super-P) and 0.01g of binder (PVDF) into 0.52g of N-methylpyrrolidone, continuously stirring to obtain a uniform suspension, coating the uniform suspension on an aluminum foil as slurry, and drying to obtain the lithium-sulfur battery cathode material.
Step six, preparing the lithium-sulfur battery: and D, cutting the lithium-sulfur battery positive electrode material prepared in the fifth step into a wafer with the diameter of 12mm, selecting metal lithium as a negative electrode, and assembling the lithium-sulfur battery positive electrode material into a lithium-sulfur button battery in a glove box.
Example 3: a lithium sulfur battery was prepared, and the procedure of example 3 was the same except that the procedure of example 2 was changed to the procedure of step one and step three.
In the first step, the concentration of the tin ion solution is changed from 7.5mmol/L to 5.0 mmol/L; in the third step, the calcining temperature is changed from 550 ℃ to 650 ℃, and the BC-SnO obtained2FIG. 4 is a scanning electron microscope image of a three-dimensional materialAnd shown in fig. 5.
Example 4: a lithium sulfur battery was prepared and example 4 was identical to example 2 except for the third step. In step three, the calcination temperature was changed from 550 ℃ to 450 ℃.
Example 5: a lithium sulfur battery was prepared and example 5 was identical to example 2 except for the difference in step three. In the third step, the holding time for calcination was changed from 2h to 1.5 h.
Example 6: a lithium sulfur battery was prepared and example 6 was identical to example 2 except for the difference in step three. In the third step, the holding time for calcination was changed from 2h to 1 h.
In conclusion, the tin dioxide nanoparticles are deposited on the bacterial cellulose substrate, the synergistic effect between the tin dioxide nanoparticles and the bacterial cellulose substrate is utilized, the loading capacity of sulfur is greatly increased, the volume specific capacity of the battery is improved, the fibrous porous structure also effectively relieves the sulfur expansion phenomenon generated during the operation of the battery, and the shuttle effect of polysulfide is inhibited. The three-dimensional composite material improves the defects of the lithium-sulfur battery anode material in many aspects, can effectively improve the theoretical specific capacity of the battery, and forms stable cycle performance. The method is simple and convenient to operate and high in controllability, electrode materials with different conductivities can be obtained by changing the concentration of the tin ion solution, the calcining temperature and the heat preservation time, so that the charging and discharging specific capacity and the coulombic efficiency of the battery are influenced.
The present invention is not limited to the above-described embodiments, which are merely illustrative and not restrictive, and those skilled in the art can make many modifications without departing from the spirit and scope of the present invention.
Claims (4)
1. A method for preparing a lithium-sulfur battery cathode material based on bacterial cellulose is characterized by comprising the following steps:
step one, preparing a tin ion solution: dissolving a certain amount of tin tetrachloride pentahydrate in a proper amount of ethanol water solution, and stirring to obtain a tin ion solution with the molar concentration of 1-10 mmol/L;
step two, preparing a main body material: placing the bacterial cellulose aerogel and the tin ion solution prepared in the first step into a reaction kettle according to the mass ratio of 1:1, stirring for 30min, sealing the container in a steel high-pressure kettle, and keeping the temperature in an electric furnace at 200 ℃ for 8 h; naturally cooling, collecting precipitate by vacuum filtration, washing with pure ethanol for 3-5 times, and drying to obtain the bacterial cellulose-stannic oxide main material;
step three, preparing a bacterial cellulose-stannic oxide three-dimensional material: sintering the bacterial cellulose-stannic oxide main body material prepared in the step two in a nitrogen atmosphere to obtain a bacterial cellulose-stannic oxide three-dimensional material, wherein the sintering process conditions are that the calcining temperature is 450-650 ℃, and the heat preservation time is 1-2 hours;
step four, preparing the bacterial cellulose-stannic oxide-sulfur active material: immersing the bacterial cellulose-tin dioxide three-dimensional material prepared in the step three into a proper amount of sulfur/carbon disulfide solution, keeping sealing for 3 hours, taking out the material from the solution, standing in the air for 2 hours to completely volatilize carbon disulfide, then placing the material in a sealed high-pressure kettle, and keeping the temperature at 155 ℃ for 3 hours; cooling to room temperature to obtain the flexible bacterial cellulose-stannic oxide-sulfur active material;
and step five, sequentially dissolving the bacterial cellulose-stannic oxide-sulfur active material prepared in the step four, a conductive agent and a binder into a proper amount of N-methyl pyrrolidone according to the mass ratio of 8:1:1, continuously stirring to obtain a uniform suspension, coating the suspension serving as slurry on an aluminum foil, and drying to obtain the lithium-sulfur battery positive electrode material.
2. The method for preparing the positive electrode material of the lithium-sulfur battery based on the bacterial cellulose as claimed in claim 1, wherein the concentration of the tin ion solution prepared in the first step is 7.5 mmol/L.
3. The method for preparing the positive electrode material of the lithium-sulfur battery based on the bacterial cellulose as claimed in claim 1, wherein in the third step, the calcination temperature is 550 ℃ and the holding time is 2 hours.
4. A lithium-sulfur battery, characterized in that the positive electrode material of the lithium-sulfur battery prepared by the method of any one of claims 1 to 3 is cut into a disk having a diameter of 12mm and used as the positive electrode material of the lithium-sulfur battery, and metallic lithium is selected as the negative electrode and assembled into a button battery in a glove box.
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| CN112490449A (en) * | 2020-11-30 | 2021-03-12 | 胡冲丽 | Three-dimensional tubular molybdenum disulfide composite bacterial cellulose membrane electrode material and preparation method thereof |
| CN112768655A (en) * | 2021-01-11 | 2021-05-07 | 上海应用技术大学 | Preparation method of tin dioxide @ oxidized bacterial cellulose/reduced graphene oxide electrode material |
| CN113422056A (en) * | 2021-06-03 | 2021-09-21 | 江苏智泰新能源科技有限公司 | Composite positive electrode material with array structure and application |
| CN114094086B (en) * | 2021-11-20 | 2024-04-26 | 华北科技学院(中国煤矿安全技术培训中心) | Metal element doped alkali metal ion battery anode material and preparation method thereof |
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| CN113422056A (en) * | 2021-06-03 | 2021-09-21 | 江苏智泰新能源科技有限公司 | Composite positive electrode material with array structure and application |
| CN114094086B (en) * | 2021-11-20 | 2024-04-26 | 华北科技学院(中国煤矿安全技术培训中心) | Metal element doped alkali metal ion battery anode material and preparation method thereof |
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Application publication date: 20200218 |