CN115101723B - A method for preparing a negative electrode of a biomass sodium ion battery - Google Patents
A method for preparing a negative electrode of a biomass sodium ion battery Download PDFInfo
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- CN115101723B CN115101723B CN202210808277.1A CN202210808277A CN115101723B CN 115101723 B CN115101723 B CN 115101723B CN 202210808277 A CN202210808277 A CN 202210808277A CN 115101723 B CN115101723 B CN 115101723B
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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
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- H01M4/1393—Processes of manufacture of electrodes based on carbonaceous material, e.g. graphite-intercalation compounds or CFx
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Abstract
The invention provides a preparation method of a biomass sodium ion battery cathode, which comprises the following steps of S1, cleaning a natural biomass raw material with deionized water and alcohol through an ultrasonic cleaner to remove surface dust and pollutants soluble in water and alcohol, cleaning and then drying in a blast drying box, S2, soaking a material obtained in the step S1 in an acid solution, then washing with deionized water to be neutral, drying in a vacuum drying box, S3, mixing the material obtained in the step S2 with a crystal template, placing in a ark, calcining in a tubular furnace to carry out carbonization, wherein the temperature rising rate is 1-5 ℃ per minute, the carbonization temperature is 800-1600 ℃ under an inert atmosphere, the heat preservation time is 1-5 h, and rapidly cooling to room temperature after reaching the heat preservation time to obtain a final hard carbon material. The preparation method of the biomass sodium ion battery cathode provided by the invention can promote electron transfer kinetics, improve sodium ion diffusion rate and realize improvement of electrochemical performance.
Description
Technical Field
The invention relates to the technical field of sodium ion batteries, in particular to a preparation method of a biomass sodium ion battery cathode.
Background
Lithium ion batteries are widely used for research due to their high energy density and excellent cycle stability, however, their further development is limited due to lack of lithium resources and uneven global distribution, as well as high manufacturing costs. The sodium ion battery and the lithium ion battery have similar energy storage mechanisms, and the cathode material has certain commonality. And the sodium element is high in abundance and low in price, so that the sodium ion battery is expected to replace a lithium ion battery, and the sodium ion battery becomes one of the new-generation energy storage systems with excellent performance. However, sodium ion radiusRadius of specific lithium ionThis makes it difficult for sodium ions to intercalate into conventional lithium ion battery anode materials. Development of a negative electrode material with high sodium storage performance, high rate performance and excellent cycle life is a key to the trend of application of sodium ion batteries, so that it is important to improve the electric/ion transfer driving force of the negative electrode material and increase the number of active sites for storing sodium.
Carbon-based materials are considered one of the most promising negative electrode materials due to their considerable ion storage capacity, good electrical conductivity and excellent thermal/chemical stability. Soft carbon and hard carbon are two of the most common amorphous carbon-based materials on the market at present, wherein the hard carbon material is considered to be an ideal negative electrode material of a sodium ion battery due to low cost, non-toxicity, environmental protection and low sodium storage potential. The hard carbon material precursor sources are mainly divided into biomass-based, high-molecular and coal-based carbon materials. Biomass materials are the first choice for current commercial anode materials because of their richness, low cost, sustainability and economic advantages. However, poor rate capability and lower reversible capacity remain a major challenge for their commercial application. Hard carbon, also known as amorphous carbon, consists primarily of disordered structures with a partially randomly oriented graphite-like microcrystalline region. The existing biomass carbon conversion process focuses on changing the structure of the prepared hard carbon by changing the pyrolysis temperature, and researches show that the increase of the pyrolysis temperature is generally accompanied by the increase of graphitization degree, the increase of conductivity, the reduction of defects and the reduction of irreversible capacity loss, but the reduction of interlayer spacing is unavoidable, so that the sodium ion transmission capacity is reduced, the kinetics are slow, and finally, the negative electrode material is caused to show lower reversible sodium storage capacity and poorer cycle performance. Therefore, the above-described problems cannot be solved by merely changing the pyrolysis temperature.
In view of the above, it is necessary to provide a new process for solving the above technical problems.
Disclosure of Invention
The invention aims to solve the technical problem of providing a preparation method of a biomass sodium ion battery cathode, which adopts biomass with abundant resources and low cost as a raw material, realizes a unique fold structure by rapid cooling after carbonization, and realizes the increase of interlayer spacing and defects while ensuring high conductivity characteristics, thereby promoting electron transfer kinetics, improving sodium ion diffusion rate and realizing the improvement of electrochemical performance.
In order to solve the problems, the technical scheme of the invention is as follows:
the preparation method of the biomass sodium ion battery cathode comprises the following steps:
Step S1, cleaning natural biomass raw materials with deionized water and alcohol by an ultrasonic cleaner to remove surface dust and pollutants soluble in water and alcohol, and drying in a blast drying oven after cleaning;
Step S2, soaking the material obtained in the step S1 in an acid solution, washing with deionized water to be neutral, and drying in a vacuum drying oven;
Step S3, mixing the material obtained in the step S2 with a crystal template, placing the mixture in a square boat, and calcining the mixture in a tube furnace to carry out a carbonization process, wherein the carbonization process comprises the steps of heating the mixture at a temperature of between 1 and 5 ℃ per minute under an inert atmosphere, and keeping the temperature for 1 to 5 hours at a temperature of between 800 and 1600 ℃ and rapidly cooling the mixture to room temperature after the temperature is kept for the time to obtain a final hard carbon material;
The rapid cooling mode is water quenching or liquid nitrogen cooling, and after rapid cooling, the biomass derived hard carbon material has a unique fold structure and a larger interlayer spacing, and the porosity and defect number of the material are increased.
Further, in step S1, the natural biomass raw material includes at least one of plant petals, rhizomes, fruits, and animal hair.
Further, in step S2, the acid solution includes one or more of hydrochloric acid, nitric acid and sulfuric acid, the concentration of the acid is 0.1 m-3 m, and the soaking time is 5-12 h.
Further, in step S3, the crystal template is at least one of graphite, graphene, and graphene oxide.
Further, in step S3, the mixing manner of the material obtained in step S2 and the crystal template is one of ball milling and ultrasonic mixing.
Further, the inert atmosphere is argon or nitrogen.
Compared with the prior art, the preparation method of the biomass sodium ion battery cathode provided by the invention has the beneficial effects that:
According to the preparation method of the biomass sodium ion battery cathode provided by the invention, the biomass material is adopted to prepare the hard carbon material, so that the strategy of synthesizing the electrode material by using the biomass has important significance from the perspective of green and recoverability as the sodium ion battery cathode, and the biomass-derived carbon shows good electrochemical performance due to the fact that the carbon inherits unique natural morphology, structure and properties of biomass to a certain extent. The higher the carbonization temperature is, the higher the graphitization degree of the hard carbon material is, the conductivity is increased, the interlayer spacing and the defect number are reduced, but the carbonized carbon material with a fold structure can be obtained by rapid cooling, the interlayer spacing is increased, the defect number is increased while the high conductivity is ensured, and the effective sodium diffusion and embedding are facilitated, and the sodium ion interaction rate is improved. The fold structure can increase the contact area of the electrolyte, is beneficial to the intercalation of sodium ions, and the defects can provide more active sites, thereby effectively promoting ion diffusion and charge transfer.
According to the preparation method of the biomass sodium ion battery cathode, through rapid cooling, high conductivity is ensured, meanwhile, the interlayer spacing is increased, the electrolyte is rapidly permeated, ion transmission dynamics are improved, sodium ions are easier to embed, in addition, a carbon material derived from biomass has a porous structure, the electrolyte is effectively permeated in a circulating process, so that electron transfer dynamics are promoted, the sodium ion diffusion rate is improved, and electrochemical performance is synergistically improved in multiple aspects.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings required for the description of the embodiments will be briefly described below, and it is apparent that the drawings in the following description are only some embodiments of the present invention, and other drawings may be obtained according to these drawings without inventive effort for a person skilled in the art.
FIG. 1 is an SEM image of a hard carbon material obtained according to example 1;
FIG. 2 is a graph showing the cycle performance of the hard carbon material obtained in example 1 as a negative electrode material for sodium ion batteries at a current density of 50mA.g -1;
fig. 3 is a graph of GITT test of the hard carbon material obtained in example 1 as a negative electrode material for sodium ion battery and sodium ion diffusion coefficient during charge and discharge.
Detailed Description
In order to better understand the technical solution in the embodiments of the present invention and make the above objects, features and advantages of the present invention more obvious and understandable, the following detailed description of the present invention will be further described.
The endpoints and any values of the ranges disclosed herein are not limited to the precise range or value, and are understood to encompass values approaching those ranges or values. For numerical ranges, one or more new numerical ranges may be found between the endpoints of each range, between the endpoint of each range and the individual point value, and between the individual point value, in combination with each other, and should be considered as specifically disclosed herein.
The preparation method of the biomass sodium ion battery cathode comprises the following steps:
Step S1, cleaning natural biomass raw materials with deionized water and alcohol by an ultrasonic cleaner to remove surface dust and pollutants soluble in water and alcohol, and drying in a blast drying oven after cleaning;
Wherein the natural biomass raw material comprises at least one of plant petals, rhizomes, fruits and animal hair;
Step S2, soaking the material obtained in the step S1 in an acid solution, washing the material with deionized water for a plurality of times to neutrality, and drying the material in a vacuum drying oven;
wherein the acid solution comprises one or more of hydrochloric acid, nitric acid and sulfuric acid, the concentration of the acid is 0.1-3M, and the soaking time is 5-12 h;
The impregnation of the acid can remove part of pollutants, and the acid can effectively penetrate and strip the graphite structure of the sample in the impregnation process, so that the interlayer spacing is increased, and the intercalation/deintercalation of sodium ions is facilitated. Specifically, the acid concentration may be 0.1M, 0.5M, 0.8M, 1.0M, 1.5M, 2.0M, 2.5M or 3M, or other concentration values within the range, and the soaking time may be 5h, 6h, 7h, 8h, 9h, 10h, 11h or 12h, or other values within the range;
Step S3, mixing the material obtained in the step S2 with a crystal template, placing the mixture in a square boat, and calcining the mixture in a tube furnace to carry out a carbonization process, wherein the carbonization process comprises the steps of heating the mixture at a temperature of between 1 and 5 ℃ per minute under an inert atmosphere, and keeping the temperature for 1 to 5 hours at a temperature of between 800 and 1600 ℃ and rapidly cooling the mixture to room temperature after the temperature is kept for the time to obtain a final hard carbon material;
The biomass-derived hard carbon material has a unique fold structure and a larger interlayer spacing after being rapidly cooled, and the porosity and the defect number of the material are increased, so that the biomass-derived hard carbon material is favorable for containing more sodium ions and has higher reversible sodium storage capacity;
In the embodiment, the crystal template is at least one of graphite, graphene and graphene oxide, and the introduction of the crystal template can improve the ordering degree of the hard carbon material, and the mixing mode of the material and the crystal template is ball milling or ultrasonic mixing;
In this embodiment, the inert atmosphere is argon or nitrogen;
in this embodiment, the carbonization temperature may be 800 ℃, 900 ℃, 1000 ℃, 1100 ℃, 1200 ℃, 1300 ℃, 1400 ℃, 1500 ℃ or 1600 ℃, and may also be other temperature values within the range, the heating rate may be 1 ℃,2 ℃,3 ℃,4 ℃ or 5 ℃ or other values within the range, and the heat preservation time may be 1h, 2h, 3h or 4h or other values within the range.
The preparation method of the biomass sodium ion battery cathode is described in detail by specific examples.
Example 1
The preparation method of the biomass sodium ion battery cathode comprises the following steps:
step S1, cleaning osmanthus fragrans leaves with deionized water and alcohol through an ultrasonic cleaner, removing surface dust and pollutants soluble in water and alcohol, cleaning, and drying in a blast drying oven;
step S2, soaking the material obtained in the step S1 in 1M hydrochloric acid solution for 6 hours, washing with deionized water for several times to neutrality, and drying in a vacuum drying oven at 80 ℃ for 24 hours;
And S3, dispersing the material obtained in the step S2 and graphene oxide in an ethanol solution, centrifugally drying, placing in a ark, calcining in a tube furnace, and carbonizing at a temperature rising rate of 5 ℃ per minute, a carbonizing temperature of 1000 ℃ and a heat preservation time of 1-5 h in an argon atmosphere, and rapidly cooling to room temperature after reaching the heat preservation time to obtain the final hard carbon material.
Referring to fig. 1, which is an SEM image of a hard carbon material obtained in example 1, it can be seen from fig. 1 (a) that the hard carbon material prepared in example 1 has a porous structure, and fig. 1 (b) shows that the hard carbon material prepared by the present invention has a pleated structure, and the number of defects is increased, so that enough active sites are provided to absorb sodium ions, thereby promoting the increase of the diffusion rate of sodium ions, so as to improve the electrochemical performance.
The hard carbon material prepared in the example 1, acetylene black and PVP are mixed and ground according to the proportion of 8:1:1, and then NMP is dripped into the mixture after grinding, and the mixture is fully stirred (24 hours) to prepare the slurry. And coating the slurry on the copper foil surface, drying, stamping to prepare a pole piece, and assembling the button cell by taking the sodium piece as a counter electrode.
Referring to FIG. 2, the cycle performance curve of the hard carbon material obtained in example 1 as a negative electrode material of sodium ion battery at a current density of 50mA.g -1 is shown. As can be seen from FIG. 2, after 100 cycles, the specific capacity of the carbon material obtained by rapid cooling is 298.3 mAh.g -1, while the capacity of the carbon material obtained by natural cooling after 100 cycles is only 194.2 mAh.g -1.
Referring to fig. 3, a GITT test graph and a corresponding sodium ion diffusion coefficient during charge and discharge of the hard carbon material obtained in example 1 as a negative electrode material of a sodium ion battery are shown. As can be seen from fig. 3, the diffusion coefficient of the hard carbon material obtained by rapid cooling is higher than that of the hard carbon material obtained by natural cooling, and the result reflects that the rapid cooling makes the hard carbon material have higher ion diffusion driving force, so that the sodium storage performance of the hard carbon material is better than that of the hard carbon material obtained by natural cooling.
Compared with the prior art, the preparation method of the biomass sodium ion battery cathode provided by the invention has the beneficial effects that:
According to the preparation method of the biomass sodium ion battery cathode provided by the invention, the biomass material is adopted to prepare the hard carbon material, so that the strategy of synthesizing the electrode material by using the biomass has important significance from the perspective of green and recoverability as the sodium ion battery cathode, and the biomass-derived carbon shows good electrochemical performance due to the fact that the carbon inherits unique natural morphology, structure and properties of biomass to a certain extent. The higher the carbonization temperature is, the higher the graphitization degree of the hard carbon material is, the conductivity is increased, the interlayer spacing and the defect number are reduced, but the carbonized carbon material with a fold structure can be obtained by rapid cooling, the interlayer spacing is increased, the defect number is increased while the high conductivity is ensured, and the effective sodium diffusion and embedding are facilitated, and the sodium ion interaction rate is improved. The fold structure can increase the contact area of the electrolyte, is beneficial to the intercalation of sodium ions, and the defects can provide more active sites, thereby effectively promoting ion diffusion and charge transfer.
According to the preparation method of the biomass sodium ion battery cathode, through rapid cooling, high conductivity is ensured, meanwhile, the interlayer spacing is increased, the electrolyte is rapidly permeated, ion transmission dynamics are improved, sodium ions are easier to embed, in addition, a carbon material derived from biomass has a porous structure, the electrolyte is effectively permeated in a circulating process, so that electron transfer dynamics are promoted, the sodium ion diffusion rate is improved, and electrochemical performance is synergistically improved in multiple aspects.
The embodiments of the present invention have been described in detail above, but the present invention is not limited to the described embodiments. It will be apparent to those skilled in the art that various changes, modifications, substitutions and alterations can be made to these embodiments without departing from the principles and spirit of the invention.
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| JP2016056038A (en) * | 2014-09-05 | 2016-04-21 | トヨタ自動車株式会社 | Carbon material |
| CN107068997A (en) * | 2017-03-15 | 2017-08-18 | 刘金财 | A kind of hard carbon/graphite composite material based on the biological mass shell of carbon and preparation method thereof |
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| JP5838673B2 (en) * | 2011-09-09 | 2016-01-06 | 住友ベークライト株式会社 | Carbon material for lithium ion secondary battery, negative electrode material for lithium ion secondary battery, and lithium ion secondary battery |
| CN106876663B (en) * | 2015-12-12 | 2019-06-11 | 北京好风光储能技术有限公司 | A kind of electrode material carbon coating device and method |
| CN109301166A (en) * | 2018-09-27 | 2019-02-01 | 江苏双登富朗特新能源有限公司 | Fold graphene carbon-coated aluminum foils preparation method |
| CN109473649B (en) * | 2018-11-07 | 2022-03-15 | 哈尔滨理工大学 | A kind of composite negative electrode material for sodium ion battery and preparation method thereof |
| CN113548654A (en) * | 2021-06-10 | 2021-10-26 | 徐州浩华能源科技有限公司 | Method for preparing hard carbon material from biomass waste physalis pubescens fruit leaves and sodium ion battery |
| CN114171802B (en) * | 2021-12-08 | 2023-11-03 | 西安航空学院 | A lithium-ion battery with low-temperature performance and its preparation method |
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| JP2016056038A (en) * | 2014-09-05 | 2016-04-21 | トヨタ自動車株式会社 | Carbon material |
| CN107068997A (en) * | 2017-03-15 | 2017-08-18 | 刘金财 | A kind of hard carbon/graphite composite material based on the biological mass shell of carbon and preparation method thereof |
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