CN112510197A - Sodium-ion battery negative electrode material and preparation method and application thereof - Google Patents
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Abstract
The invention relates to the technical field of sodium ion batteries, in particular to a sodium ion battery cathode material and a preparation method and application thereof. The method comprises the following steps: dissolving zinc source and tin source, mixing to obtain suspension, centrifuging, washing with water, and washing with alcohol to obtain white cubic ZnSn (OH)6Dispersing the carbon source and the carbon source in water, heating, stirring until the solution is black suspension, separating solid products, washing to obtain carbon-coated cubic ZnSn (OH)6Then dispersing the sulfur source and the sulfur into a solvent, then carrying out vulcanization treatment, separating out a solid product in the solvent after the vulcanization treatment is finished, and drying the solid product to obtain the sulfur-containing catalyst. The invention aims at the existing negative electrode material of the sodium-ion batteryThe problems of small reversible capacity, poor cycle performance and the like are solved, and the specific capacity and the cycle stability of the sodium ion battery can be remarkably improved by introducing carbon-coated cubic zinc tin sulfide as a negative active material to prepare a binary metal sulfide system.
Description
Technical Field
The invention relates to the technical field of sodium ion batteries, in particular to a sodium ion battery cathode material and a preparation method and application thereof.
Background
The information disclosed in this background of the invention is only for enhancement of understanding of the general background of the invention and is not necessarily to be taken as an acknowledgement or any form of suggestion that this information forms the prior art already known to a person skilled in the art.
With the increasing consumption of fossil energy and the increasing environmental pollution caused by the fossil energy, the development of clean energy has received more and more attention. However, new energy sources such as wind energy and solar energy are limited by time and regions and cannot be supplied continuously and stably. Therefore, the development of high performance energy storage technology is one of the current popular research directions. Sodium ion batteries are paid attention by researchers due to the characteristics of abundant reserves and low price, and are expected to replace commercial lithium ion batteries. Under the influence of the negative electrode material, the sodium ion battery cannot meet the high demand of the future society for energy density. The metal sulfide as the anode material of the redox mechanism has higher theoretical specific capacity and first-turn coulombic efficiency, and is an ideal anode material of a new-generation sodium-ion battery. However, the development of metal sulfide negative electrode materials is limited due to the huge volume change and poor conductivity during the charge and discharge processes.
Disclosure of Invention
The invention aims to solve the problems of small reversible capacity, poor cycle performance and the like of the current negative electrode material of the sodium-ion battery. Therefore, the invention provides a sodium-ion battery negative electrode material, and a preparation method and application thereof. The cathode material of the sodium ion battery is carbon-coated cubic zinc tin sulfide, and has the characteristics of high specific capacity and high stability.
In order to achieve the purpose, the invention discloses the following scheme:
first, a sodium ion battery negative electrode material is disclosed, which is composed of cubic zinc tin sulfide (ZnSnS)3) And a carbon coating layer coated on the surface of the zinc tin sulfide.
Secondly, a preparation method of the sodium-ion battery negative electrode material is disclosed, which comprises the following steps:
s1, fully dissolving a zinc source and a tin source, mixing, stirring to obtain a suspension, centrifuging, washing with water, and washing with alcohol to obtain white cubic ZnSn (OH)6；
S2, mixing the ZnSn (OH)6And a carbon source dispersed in water and heated, followed by stirringStirring until the solution is black suspension, separating solid product, washing to obtain carbon-coated cubic ZnSn (OH)6；
S3, coating the carbon with cubic ZnSn (OH)6And a sulfur source are dispersed in a solvent, sulfur element is vulcanized through a carbon coating layer, a solid product is separated out after the vulcanization is finished, and the carbon-coated cubic block zinc tin sulfide (ZnSnS) is obtained after the drying3)。
The invention further discloses an application of the sodium-ion battery negative electrode material and the preparation method thereof in the fields of sodium-ion batteries, lithium ion batteries, super capacitors, electrocatalysis and the like.
One of the characteristics of the cathode material of the invention is as follows: the multi-element composite material can effectively improve internal charge transmission and improve conductivity, so that the ZnS and SnS are combined to prepare a novel composite material consisting of two alloy materials so as to realize the aim of preparing the high-performance sodium-ion battery cathode material.
The anode material of the invention is characterized by the following two characteristics: due to large volume fluctuation in the charging and discharging process, pulverization of electrode materials and exfoliation of current collectors are caused, and rapid capacity attenuation and low capacity retention rate are finally caused. Therefore, the cathode material is in a cubic block shape, and the shape has a more stable structure, so that the aggregation and collapse of the active material can be effectively avoided, and the structural integrity in the circulation process is ensured.
The negative electrode material of the invention has the third characteristic that: the carbon-coated cubic massive zinc tin sulfide prepared by the invention has a stable and uniform structure, a microcrystalline boundary formed by zinc sulfide can provide a buffer area and effectively inhibit the volume expansion problem of tin sulfide in the charging and discharging processes through a binary metal zinc tin sulfide formed by atomic scale doping, the problem of poor electrical contact of the material due to the volume expansion can be solved by combining the cubic massive structure, and the cycling stability of the material is obviously improved; the coating by the carbon layer can provide good electrical conductivity to the bulk material.
The anode material of the invention has the four characteristics that: the conductivity is also a great obstacle for limiting the development of the sodium ion battery, and the conductivity of a material system can be obviously improved by coating the surface of the active material with a carbon layer, so that the electron transmission is accelerated, and the specific capacity of the battery is improved.
Compared with the prior art, the invention has the following beneficial effects:
(1) aiming at the problems of small reversible capacity, poor cycle performance and the like of the current sodium-ion battery cathode material, the invention introduces carbon-coated cubic zinc tin sulfide as a cathode active material. The system for preparing the binary metal sulfide is combined with a nano cubic structure, and the specific capacity and the cycling stability of the sodium ion battery can be remarkably improved through the treatment of coating the carbon layer.
(2) The preparation method designed by the invention has the advantages of simple required equipment, cheap and easily available raw materials, simple and controllable preparation parameters and high repeatability, and is beneficial to realizing large-scale batch preparation.
Drawings
The accompanying drawings, which are incorporated in and constitute a part of this specification, are included to provide a further understanding of the invention, and are incorporated in and constitute a part of this specification, illustrate exemplary embodiments of the invention and together with the description serve to explain the invention and not to limit the invention.
FIG. 1 shows ZnSn (OH) prepared in example 1 of the present invention6Scanning electron micrograph (c).
FIG. 2 is a scanning electron microscope image of cubic zinc tin sulfide prepared in example 1 of the present invention.
FIG. 3 is the charge-discharge curve diagram of the cubic zinc tin sulfide used as the cathode material of sodium ion battery in the first two cycles of the invention in example 1.
FIG. 4 is a discharge specific capacity cycle chart of cubic zinc tin sulfide used as a negative electrode material of a sodium ion battery, which is prepared in example 1 of the invention.
Detailed Description
It is to be noted that, unless otherwise specified, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs.
It is to be noted that the terminology used herein is for the purpose of describing particular embodiments only and is not intended to be limiting of exemplary embodiments according to the invention. As used herein, the singular forms "a", "an" and "the" are intended to include the plural forms as well, and it should be understood that when the terms "comprises" and/or "comprising" are used in this specification, they specify the presence of stated features, steps, operations, devices, components, and/or combinations thereof, unless the context clearly indicates otherwise.
As described above, although the metal sulfide as the redox mechanism type negative electrode material has higher theoretical specific capacity and first-turn coulombic efficiency, the metal sulfide is an ideal negative electrode material for the new generation of sodium ion batteries. However, the development of metal sulfide negative electrode materials is limited due to huge volume change and poor conductivity generated in the charging and discharging processes; therefore, the invention relates to a sodium ion battery negative electrode material and a preparation method thereof.
In some exemplary embodiments, the diameter of the sodium ion battery anode material is between 100 and 200 nm.
In some exemplary embodiments, the mass ratio of the carbon coating layer to the cubic zinc tin sulfide is 1 (0.5-2).
In some typical embodiments, the zinc source is one or more of zinc sulfate, zinc chloride, zinc acetate and zinc nitrate, and the tin source is one or more of potassium stannate, stannous chloride, stannic chloride and stannic oxalate;
in some typical embodiments, the carbon source is one or more of PAN, PVP, PPy, PDA, glucose;
in some typical embodiments, the sulfur source is one or more of thioacetamide, sublimed sulfur, thiourea, sulfur powder, thiopropionamide, ammonium sulfide.
In some exemplary embodiments, the S1 is specifically: dissolving zinc source and tin source in deionized water or anhydrous ethanol respectively, mixing after dissolving sufficiently, magnetically stirring for a certain time to obtain white suspension, centrifuging, washing with water, and washing with alcohol to obtain white cubic ZnSn (OH)6。
In some exemplary embodiments, the S2 is specifically: mixing ZnSn (OH)6Dispersing a carbon source in deionized water, heating, stirring in a magnetic stirrer until the solution is black suspension, centrifuging, washing with water, and washing with alcohol to obtain carbon-coated cubic ZnSn (OH)6。
In some exemplary embodiments, the S3 is specifically: coating cubic ZnSn (OH) with carbon6And a sulfur source is dispersed in deionized water or ethanol, vulcanization treatment is carried out in an oil bath pot through a cooling reflux device, and then the carbon-coated cubic zinc tin sulfide is obtained after centrifugal drying.
As a further technical scheme, the stirring time in the S1 is 1-24 hours, and the temperature during the stirring process is 10-50 ℃.
As a further technical scheme, ZnSn (OH) in S26And the molar ratio of the carbon source to the carbon source is 1: (0.5-2).
As a further technical scheme, the stirring time in the S2 is 1-24 hours, and the temperature during the stirring process is 20-100 ℃.
As a further technical scheme, the S3 adopts the structure that cubic ZnSn (OH) is coated with carbon6And the molar ratio of the sulfur source is: 1:(0.3-5).
As a further technical scheme, the stirring time in the S3 is 0.5-24 hours, and the oil bath temperature is 50-100 ℃.
The invention will now be further described with reference to the drawings and detailed description.
Example 1
A preparation method of a sodium-ion battery negative electrode material comprises the following steps:
(1) weighing 3g of potassium stannate, dissolving in 5mL of deionized water, weighing 2.88g of zinc sulfate, dissolving in 65mL of deionized water, mixing after fully dissolving, placing on a magnetic stirrer, stirring for 4 hours at 28 ℃ to obtain white suspension, centrifuging, washing with water, and washing with alcohol to obtain white cubic ZnSn (OH)6；
(2) 1g of ZnSn (OH) thus obtained was weighed out6And 0.5g of PPy are dispersed in 500mL of deionized water, the mixture is placed on a magnetic stirrer and stirred for 12 hours at the temperature of 80 ℃ until the solution is in a black suspension, and then the suspension is centrifuged, washed by water and washed by alcoholObtaining carbon-coated cubic ZnSn (OH)6；
(3) 100mg of carbon-coated cubic ZnSn (OH)6And 200mg of thioacetamide are dispersed in 100mL of ethanol, vulcanization treatment is carried out in an oil bath kettle at 90 ℃ for 2 hours by a cooling reflux device, and then centrifugal drying is carried out to obtain the carbon-coated cubic zinc tin sulfide (ZnSnS)3)。
Example 2
A preparation method of a sodium-ion battery negative electrode material comprises the following steps:
(1) weighing 3g of stannous chloride, dissolving the stannous chloride in 20mL of deionized water, weighing 3g of zinc nitrate, dissolving the zinc nitrate in 80mL of deionized water, mixing after fully dissolving, placing the mixture on a magnetic stirrer, stirring the mixture for 24 hours at 20 ℃ to obtain white suspension, and centrifuging, washing with water and washing with alcohol to obtain white cubic ZnSn (OH)6；
(2) 1g of ZnSn (OH) thus obtained was weighed out6And 0.3g of PVP are dispersed in 300mL of deionized water, the mixture is placed on a magnetic stirrer and stirred for 24 hours at the temperature of 20 ℃ until the solution is in a black suspension, and the solution is centrifuged, washed by water and alcohol to obtain carbon-coated cubic ZnSn (OH)6；
(3) 100mg of carbon-coated cubic ZnSn (OH)6And 30mg of thioacetamide are dispersed in 100mL of ethanol, vulcanization treatment is carried out in an oil bath kettle at 85 ℃ for 24 hours by a cooling reflux device, and then centrifugal drying is carried out to obtain the carbon-coated cubic zinc tin sulfide (ZnSnS)3)。
Example 3
A preparation method of a sodium-ion battery negative electrode material comprises the following steps:
(1) weighing 3g of stannous chloride, dissolving the stannous chloride in 20mL of deionized water, weighing 3g of zinc nitrate, dissolving the zinc nitrate in 80mL of deionized water, mixing after fully dissolving, placing the mixture on a magnetic stirrer, stirring the mixture for 1 hour at 50 ℃ to obtain white suspension, and centrifuging, washing with water and washing with alcohol to obtain white cubic ZnSn (OH)6；
(2) 1g of ZnSn (OH) thus obtained was weighed out6And 2g PVP dispersed in 300mL deionized water and placed under magnetic forceStirring for 1h at 100 ℃ on a stirrer until the solution is black suspension, centrifuging, washing with water, washing with alcohol to obtain carbon-coated cubic ZnSn (OH)6；
(3) 100mg of carbon-coated cubic ZnSn (OH)6And 500mg of thioacetamide are dispersed in 100mL of ethanol, vulcanization treatment is carried out in an oil bath kettle at 100 ℃ for 0.5 hour by a cooling reflux device, and then centrifugal drying is carried out to obtain the carbon-coated cubic zinc tin sulfide (ZnSnS)3)。
Performance testing
ZnSn (OH) prepared in example 16And the cubic zinc tin sulfide is taken as an example to test the micro morphology, the performance and the like, and the results are shown in figures 1-4.
FIG. 1 shows the ZnSn (OH)6The scanning electron microscope picture shows that the ZnSn (OH) which is not coated by carbon and is prepared by the invention6Is a cubic block structure with a diameter of about 100-200 nm. According to further research of the invention, the cubic block-shaped negative electrode material has a more stable structure, can effectively avoid aggregation and collapse of the active material, and ensures structural integrity in the circulation process.
FIG. 2 is a scanning electron micrograph of the cubic bulk ZnS, which is between about 100 and 200nm in diameter. It can be seen that under high voltage SEM, there is a nearly transparent carbon layer around the cubic zinc tin sulfide. Aiming at the problems of small reversible capacity, poor cycle performance and the like of the current sodium ion battery cathode material, the carbon-coated cubic zinc tin sulfide is introduced as a cathode active material, and the specific capacity and the cycle stability of the sodium ion battery can be remarkably improved through the treatment of carbon layer coating.
The first two-turn charge-discharge curve diagram of cubic zinc tin sulfide used as the cathode material of the sodium-ion battery in fig. 3 shows that: when the cubic blocky zinc tin sulfide prepared by the method is used as a negative electrode material of a sodium ion battery, the specific capacity is higher, and the first circle can reach 435 mAh.g-1The second turn can also reach 290mAh g-1。
Fig. 4 is a discharge specific capacity cycling diagram of cubic zinc tin sulfide used as a negative electrode material of a sodium ion battery, and it can be seen that: when the cubic zinc tin sulfide prepared by the method is used as a negative electrode material of a sodium ion battery, the cubic zinc tin sulfide has good cycling activity, the specific capacity of the battery is kept at a stable level after 50 cycles of charge and discharge, and the excellent stability and electrochemical cycling performance of the battery can be proved.
Any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the protection scope of the present invention. Although the embodiments of the present invention have been described with reference to the accompanying drawings, it is not intended to limit the scope of the present invention, and it should be understood by those skilled in the art that various modifications and variations can be made without inventive efforts by those skilled in the art based on the technical solution of the present invention.
Claims (10)
1. The negative electrode material of the sodium-ion battery is characterized by comprising cubic ZnSnS3And coating the ZnSnS3The carbon coating layer on the surface.
2. The negative electrode material of the sodium-ion battery as claimed in claim 1, wherein the diameter of the negative electrode material of the sodium-ion battery is between 100 nm and 200 nm.
3. The negative electrode material of the sodium-ion battery as claimed in claim 1, wherein the mass ratio of the carbon coating layer to the cubic zinc tin sulfide is as follows: 1: (0.5-2).
4. A preparation method of a sodium-ion battery negative electrode material is characterized by comprising the following steps:
s1, fully dissolving a zinc source and a tin source, mixing, stirring to obtain a suspension, centrifuging, washing with water, and washing with alcohol to obtain white cubic ZnSn (OH)6；
S2, mixing the ZnSn (OH)6And a carbon source dispersed in water and heated, then stirred to a solutionAfter the suspension liquid is black, solid products in the suspension liquid are separated out, and carbon-coated cubic ZnSn (OH) is obtained after the solid products are washed6；
S3, coating the carbon with cubic ZnSn (OH)6And a sulfur source are dispersed in a solvent, then vulcanization treatment is carried out, a solid product in the solvent is separated out after the vulcanization treatment is finished, and the carbon-coated cubic block zinc tin sulfide is obtained after drying.
5. The preparation method of claim 4, wherein the zinc source is one or more of zinc sulfate, zinc chloride, zinc acetate and zinc nitrate;
or; the tin source is one or more of potassium stannate, stannous chloride, stannic chloride and stannic oxalate;
or; the carbon source is one or more of PAN, PVP, PPy, PDA and glucose;
or; the sulfur source is one or more of thioacetamide, sublimed sulfur, thiourea, sulfur powder, thiopropionamide and ammonium sulfide.
6. The preparation method according to claim 4 or 5, wherein S1 specifically is: respectively dissolving a zinc source and a tin source in deionized water or absolute ethyl alcohol, mixing after fully dissolving, magnetically stirring for a certain time to obtain a white suspension, and performing centrifugation, water washing and alcohol washing to obtain white cubic ZnSn (OH) 6.
7. The preparation method according to claim 4 or 5, wherein S2 specifically is: mixing ZnSn (OH)6Dispersing a carbon source in deionized water, heating, stirring in a magnetic stirrer until the solution is black suspension, centrifuging, washing with water, and washing with alcohol to obtain carbon-coated cubic ZnSn (OH)6。
8. The preparation method according to claim 4 or 5, wherein S3 specifically is: coating cubic ZnSn (OH) with carbon6And a sulfur source are dispersed in deionized water or ethanol and pass through a cooling reflux deviceAnd carrying out vulcanization treatment in an oil bath pan, and then carrying out centrifugal drying to obtain the carbon-coated cubic zinc tin sulfide.
9. The method according to claim 4 or 5, wherein the stirring time in S1 is 1-24 hours, and the temperature during stirring is 10-50 ℃;
preferably, ZnSn (OH) in S26And the molar ratio of the carbon source to the carbon source is 1: (0.5-2);
preferably, the stirring time in the S2 is 1-24 hours, and the temperature during the stirring process is 20-100 ℃;
preferably, the carbon in S3 is coated with cubic ZnSn (OH)6And a sulfur source in a molar ratio of 1: (0.3-5);
preferably, the stirring time in the S3 is 0.5-24 hours, and the oil bath temperature is 50-100 ℃.
10. Use of the negative electrode material for sodium ion batteries according to any one of claims 1 to 3 and/or the negative electrode material prepared by the method according to any one of claims 4 to 9 in the fields of sodium ion batteries, lithium ion batteries, supercapacitors, electrocatalysis.
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| PCT/CN2020/096861 WO2021051908A1 (en) | 2019-09-16 | 2020-06-18 | Negative electrode material for sodium ion battery, preparation method therefor and use thereof |
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| CN113707861A (en) * | 2021-08-26 | 2021-11-26 | 合肥工业大学 | Nitrogen-doped carbon layer-coated cobalt oxide nanosheet and preparation method and energy storage application thereof |
| CN113851645A (en) * | 2021-08-30 | 2021-12-28 | 厦门大学 | Zinc sulfide/tin-carbon compound and preparation method and application thereof |
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| CN108039472A (en) * | 2017-12-11 | 2018-05-15 | 西北大学 | A kind of preparation method and application of the hollow micron cube composite material of carbon coating zinc metastannate |
| CN108288693B (en) * | 2017-12-22 | 2020-07-10 | 天津师范大学 | Zinc-tin bimetallic sulfide as negative electrode material of sodium-ion battery and preparation method and application thereof |
| CN109279647B (en) * | 2018-09-29 | 2020-12-01 | 中南大学 | Preparation method of cubic nano zinc tin sulfide as negative electrode material of sodium ion battery |
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| CN113707861A (en) * | 2021-08-26 | 2021-11-26 | 合肥工业大学 | Nitrogen-doped carbon layer-coated cobalt oxide nanosheet and preparation method and energy storage application thereof |
| CN113851645A (en) * | 2021-08-30 | 2021-12-28 | 厦门大学 | Zinc sulfide/tin-carbon compound and preparation method and application thereof |
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Application publication date: 20210316 |