CN111129489B - Graphene-based antimony sulfide negative electrode material and preparation method and application thereof - Google Patents
Graphene-based antimony sulfide negative electrode material and preparation method and application thereof Download PDFInfo
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Abstract
The invention relates to a graphene-based antimony sulfide negative electrode material and a preparation method and application thereof, wherein the preparation method comprises the following steps: (1) adding an antimony source into deionized water, uniformly stirring, adding ethylene glycol, and stirring to obtain a first solution; (2) adding sodium borohydride into the first solution obtained in the step (1), uniformly stirring, adding polyvinylpyrrolidone, and fully dissolving to obtain a second solution; (3) adding the second solution obtained in the step (2) into a hydrothermal kettle lining containing sulfur powder for hydrothermal reaction, carrying out solid-liquid separation after the reaction is finished, washing and drying to obtain Sb2S3(ii) a (4) Sb2S3And compounding with GO by a hydrothermal method, and freeze-drying to obtain the graphene-based antimony sulfide negative electrode material. Compared with the prior art, the invention has the advantages of simple process, mild conditions, low cost and the like, and shows excellent electrochemical performance as the cathode of the lithium ion battery.
Description
Technical Field
The invention belongs to the technical field of electrochemistry, relates to a negative electrode material, and particularly relates to a graphene-based antimony sulfide negative electrode material as well as a preparation method and application thereof.
Background
With the development and progress of the automobile industry, the continuous development problem of human beings faces huge challenges. The combustion of non-renewable fuels can release various exhaust gases, leading to various problems. Therefore, it is important to find renewable and sustainable energy storage devices. The rechargeable battery is economical, environment-friendly, high in power and long in service life, and compared with non-renewable energy, the rechargeable battery realizes continuous utilization of energy. Particularly, lithium ion batteries and sodium ion batteries have the advantages of high energy density, no memory effect, low maintenance cost, low self-discharge and low self-discharge effect and the like, and are one of the most promising electrochemical energy storage battery technologies at present. And becomes one of the most important rechargeable batteries.
Lithium Ion Batteries (LIBs) have played a very important role in the electronics and electrical industry for recent decades due to their excellent energy storage properties. However, the amount of lithium metal on earth is limited, and lithium ion batteries are expensive and require high production requirements. Meanwhile, the sodium ion battery is more in the field of vision of people due to the advantages of no over-discharge characteristic, low production cost, rich sodium reserve and the like. The cathode materials of the sodium ion batteries are transition metal-based inorganic materials (such as cobalt, nickel, manganese and the like) with small earth reserves, and the cathode materials of the materials have the defects of high raw material cost, poor conductivity and low capacity, and are one of the main bottlenecks in the development of the lithium ion batteries. In contrast, sulfur or selenium can alloy in the chalcogenide to form lithium chalcogenide, thereby improving the charging capability of the negative electrode, SnS2、SnSe2、Sb2S3And its carbon composite as a negative electrode material, and thus these electrodes are a combination of a lithium/sulfur cell and an element (whether tin or antimony) that also contributes to the ability of the lithium alloy to charge at lower potentials. However, the cycling stability of emerging high capacity sulfide electrodes remains a problem, and the lithiation process is accompanied by a large volume change, resulting in film cracking, deterioration of electrical integrity, gradual capacity fade, and shortened lifetime.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide the graphene-based antimony sulfide negative electrode material which has the advantages of simple preparation process, mild conditions, low cost and the like, high reversible capacity, very good cycle stability and rate capability and wide application prospect in the field of lithium ion batteries, and the preparation method and the application thereof.
Graphene is used as a superior two-dimensional conductive material, and is used as a substrate loaded with metal oxide, so that electron transfer can be effectively improved, polymerization can be prevented, a three-dimensional (3D) porous structure can be further constructed, and diffusion of electrons and ions in the whole electrode can be promoted. The graphene and the active negative electrode material are compounded, and the electrochemical performance of the electrode material is effectively improved through a synergistic effect. On the other hand, the composite material is obtained after three-dimensional assembly is carried out by utilizing the two-dimensional graphene, so that the contact between the composite material and the electrolyte can be greatly improved, and the electrochemical performance of the material can be further improved.
The establishment of the three-dimensional assembly method by using the metal sulfide and the graphene also opens up a new design idea for constructing other novel composite materials based on the high-performance three-dimensional graphene, and has profound significance for the development and practical application development of the high-performance sodium ion battery electrode.
The purpose of the invention can be realized by the following technical scheme:
the invention provides a preparation method of a graphene-based antimony sulfide negative electrode material, which comprises the following steps:
(1) adding an antimony source into deionized water, uniformly stirring, adding ethylene glycol, and stirring to obtain a first solution;
(2) adding sodium borohydride into the first solution obtained in the step (1), uniformly stirring, adding polyvinylpyrrolidone, and fully dissolving to obtain a second solution;
(3) adding the second solution obtained in the step (2) into a hydrothermal kettle lining containing sulfur powder for hydrothermal reaction, carrying out solid-liquid separation after the reaction is finished, washing and drying to obtain Sb2S3；
(4) Sb2S3Mixing with GO by hydrothermal method, and lyophilizing to obtain final productAnd the graphene-based antimony sulfide negative electrode material.
Preferably, in the step (1), the antimony source is SbCl3。
Preferably, in the step (1), the ratio of the antimony source to the deionized water is 1g: 100-140 mL.
Further preferably, in the step (1), the ratio of the antimony source to the deionized water is 1g:120 mL.
Preferably, in the step (1), the volume ratio of the ethylene glycol to the deionized water is 0.8-1.2: 1.
Further preferably, in the step (1), the volume ratio of the ethylene glycol to the deionized water is 1:1.
Preferably, in step (2), sodium borohydride is slowly added to the first solution obtained in step (1). Because the reaction can generate hydrogen and the reaction is violent, NaBH is added4It is advisable to add the solution slowly.
Preferably, in the step (2), the mass ratio of the sodium borohydride to the antimony source is 1-1.4: 1.
Further preferably, in the step (2), the mass ratio of the sodium borohydride to the antimony source is 1.2: 1.
Preferably, in the step (2), the viscosity average molecular weight of the polyvinylpyrrolidone is 280000-320000.
Further preferably, in the step (2), the viscosity average molecular weight of the polyvinylpyrrolidone is 300000.
Preferably, in the step (2), the mass ratio of the polyvinylpyrrolidone to the antimony source is 2.5-3.5: 1.
Preferably, in step (2), the mass ratio of polyvinylpyrrolidone to antimony source is 3: 1.
Preferably, in the step (3), the mass ratio of the sulfur powder to the antimony source is 1: 2-3.
Further preferably, in the step (3), the mass ratio of the sulfur powder to the antimony source is 1: 2.5.
Preferably, in the step (3), the sulfur powder is uniformly spread at the bottom of the lining of the hydrothermal kettle.
Preferably, in the step (3), the temperature of the hydrothermal reaction is 150-.
Further preferably, in the step (3), the temperature of the hydrothermal reaction is 160-200 ℃, and the reaction time is 12-24 h.
Preferably, in the step (3), the solid-liquid separation is performed by adopting a centrifugal separation mode, and the rotating speed during the centrifugal separation is performed by adopting a method of firstly high speed, then low speed and then high speed; the high-speed rotating speed is 7000rmp-8000 rmp; the low speed is 2000rmp-3000 rmp.
Preferably, in the step (3), the washing is performed by using deionized water.
Preferably, in the step (3), the drying is performed in a drying manner.
Preferably, in step (4), Sb2S3The mass ratio of the GO to the GO is 1: 0.8-1.2.
Further preferably, in the step (4), Sb2S3And GO is in a mass ratio of 1:1.
Preferably, in step (4), Sb2S3The conditions for compounding with GO by a hydrothermal method are as follows: the temperature is 160-200 ℃ and the time is 12-18 h.
Preferably, in step (4), the GO concentration is 3-5 mg/ml.
The invention also provides a two-dimensional carbide crystal-based antimony sulfide negative electrode material obtained by the preparation method.
Preferably, the Sb2S3 is in a rod-like structure, and is uniformly dispersed on a sheet structure of graphene in a three-dimensional porous structure formed after the GO is reduced.
The third aspect of the invention provides the application of the two-dimensional carbide crystal-based antimony sulfide negative electrode material in the aspect of a lithium ion battery negative electrode material.
Sb in the invention2S3And GO is compounded under the hydrothermal condition, and meanwhile, GO is reduced into RG (graphene) and self-assembled from a two-dimensional structure to form a three-dimensional structure Sb2S3Uniformly dispersed in the RG three-dimensional structure, and has the advantages of simple process, mild conditions, low cost and the like. The graphene-based antimony sulfide negative electrode material prepared by the invention has excellent electrochemical performance as a lithium ion battery negative electrode, and the electrochemical performance is 100 mA-g-1The capacity of the battery can reach 600 mAh.g under charging and discharging current-1At 4A · g-1The lower capacity is 150mAh g-1The excellent rate performance efficiency of the device is stabilized to be more than 90 percent. The method provides good experimental data and theoretical support for research and application of graphene, inorganic materials and metal sulfides in the field of electrochemistry
Compared with the prior art, the invention has the following beneficial effects:
1. the graphene-based antimony sulfide negative electrode material is prepared by a two-step hydrothermal method, and Sb is prepared by the hydrothermal method in the first step2S3After the material is obtained, Sb is obtained2S3The graphene is hydrothermally and uniformly mixed with graphene, so that the method is simple and safe, and the effect is good;
2. the invention takes antimony sulfide, sodium borohydride and the like as raw materials, and the raw materials are designable and have low cost;
3. the graphene-based antimony sulfide negative electrode material prepared by the method has high reversible capacity, very good cycle stability and rate capability, and has wide application prospect in the field of lithium ion batteries.
Drawings
FIG. 1 is an SEM topography of the graphene-based antimony sulfide negative electrode material obtained in example 1;
FIG. 2 is a cyclic XRD pattern of the antimony sulfide negative electrode material obtained in example 1 as a negative electrode material of a lithium ion battery;
FIG. 3 is a graph of the cycle performance of the graphene-based antimony sulfide negative electrode material and antimony sulfide negative electrode material obtained in example 1 as lithium ion battery negative electrode materials;
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
Step one, preparing an antimony sulfide material:
(1) 0.25g of SbCl3Adding the mixture into 30mL of deionized water and stirring the mixture evenly; then adding 30mL of glycol into the solution and stirring for 10 min;
(2) then 0.3g of sodium borohydride (NaBH)4) Slowly adding into the solution and stirringStirring, adding 0.75g polyvinylpyrrolidone (PVP) with molecular weight of 300000 into the solution to dissolve completely;
(3) finally, pouring the solution into a lining of a hydrothermal kettle containing sulfur powder for hydrothermal treatment, and keeping the temperature at 160-200 ℃ for 12-24 hours.
Step two, preparing the graphene-based antimony sulfide negative electrode material:
(1) washing the obtained solution with deionized water after the hydrothermal reaction is finished, and then drying to obtain Sb2S3Adding the obtained Sb2S3Performing hydrothermal reaction with GO again at 180 ℃ for 12h to obtain Sb2S3The method comprises the following steps of @ RG composite material, and finally freeze-drying to obtain the graphene-based antimony sulfide negative electrode material, wherein the morphology of the graphene-based antimony sulfide negative electrode material is shown in figure 1, and active material particles are uniformly dispersed in a three-dimensional structure of graphene; wherein Sb is added in the embodiment2S3The mass and dosage ratio of the active carbon to GO is 1:1.
(2) The obtained composite material is used as a negative electrode material of a lithium ion battery to assemble a lithium ion button type half battery, the composite material, carbon black (Super-P) and polyvinylidene fluoride (PVDF) are mixed according to the weight ratio of 7:2:1, then the mixture is uniformly coated on pure aluminum foil (99.6%) by a coating method to prepare a negative electrode, and a pure lithium sheet is used as a counter electrode. Electrochemical tests are carried out by utilizing the button type half cell, and the cycle performance diagram and the rate performance diagram are respectively shown in figures 2 and 3, so that the cycle performance and the rate performance are better, and the cycle life is longer.
The prepared graphene-based antimony sulfide negative electrode material has excellent electrochemical performance as a lithium ion battery negative electrode, and the electrochemical performance is 100 mA-g-1The capacity of the battery can reach 600 mAh.g under charging and discharging current-1At 4A · g-1The lower capacity is 150mAh g-1The excellent rate performance efficiency of the device is stabilized to be more than 90 percent.
Example 2
This example is substantially the same as example 1 except that in the first step (1), 25mL of deionized water was added.
Example 3
This example is substantially the same as example 1 except that in the first step (1), 35mL of deionized water was added.
Example 4
This example is substantially the same as example 1 except that in the first step (1), the amount of ethylene glycol added was 24 mL.
Example 5
This example is substantially the same as example 1 except that in the first step (1), the amount of ethylene glycol added was 36 mL.
Example 6
This example is substantially the same as example 1 except that in the first step (2), 0.25g of sodium borohydride was added.
Example 7
This example is substantially the same as example 1 except that in the first step (2), 0.35g of sodium borohydride was added.
Example 8
This example is substantially the same as example 1 except that in the first step (2), the viscosity average molecular weight of polyvinylpyrrolidone in this example was 280000.
Example 9
This example is substantially the same as example 1 except that in the first step (2), the viscosity average molecular weight of polyvinylpyrrolidone is 320000.
Example 10
This example is substantially the same as example 1 except that in the first step (2), polyvinylpyrrolidone was added in an amount of 0.625 g.
Example 11
This example is substantially the same as example 1 except that in the first step (2), polyvinylpyrrolidone was added in an amount of 0.875.
Example 12
This example is substantially the same as example 1, except that in the first step (3), 0.125g of sulfur powder was used.
Example 13
This example is substantially the same as example 1, except that in the first step (3), the amount of sulfur powder used was 0.833 g.
Example 14
This example is substantially the same as example 1, except that in the first step (3), the hydrothermal reaction temperature was 150 ℃ and the reaction time was 24 hours.
Example 15
This example is substantially the same as example 1, except that in the first step (3), the hydrothermal reaction temperature was 200 ℃ and the reaction time was 10 hours.
Example 16
This example is substantially the same as example 1, except that in the second step (1) in this example, Sb is added2S3The mass ratio of GO to GO is 1: 0.8.
Example 17
This example is substantially the same as example 1, except that in the second step (1) in this example, Sb is added2S3The mass ratio of GO to GO is 1: 1.2.
The embodiments described above are intended to facilitate the understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (8)
1. A preparation method of a graphene-based antimony sulfide negative electrode material is characterized by comprising the following steps:
(1) adding an antimony source into deionized water, uniformly stirring, adding ethylene glycol, and stirring to obtain a first solution;
(2) adding sodium borohydride into the first solution obtained in the step (1), uniformly stirring, adding polyvinylpyrrolidone, and fully dissolving to obtain a second solution;
(3) adding the second solution obtained in the step (2) into a hydrothermal kettle lining containing sulfur powder for hydrothermal reaction, carrying out solid-liquid separation after the reaction is finished, washing and drying to obtain Sb2S3；
(4) Sb2S3Compounding the graphene-based antimony sulfide anode material with GO in a mass ratio of 1:1 by a hydrothermal method, and freeze-drying to obtain the graphene-based antimony sulfide anode material, wherein active substance particles Sb in the material are Sb2S3The graphene is uniformly dispersed in a three-dimensional structure of graphene;
the viscosity average molecular weight of the polyvinylpyrrolidone is 280000-320000;
the mass ratio of the polyvinylpyrrolidone to the antimony source is 2.5-3.5: 1;
in the obtained graphene-based antimony sulfide negative electrode material, Sb2S3The graphene is in a rod-shaped structure and is uniformly dispersed on a three-dimensional porous graphene sheet structure formed after GO is reduced.
2. The method for preparing the graphene-based antimony sulfide negative electrode material as claimed in claim 1, wherein in the step (1), the antimony source is SbCl3；
The dosage ratio of the antimony source to the deionized water is 1g: 100-140 mL;
the volume ratio of the ethylene glycol to the deionized water is 0.8-1.2: 1.
3. The preparation method of the graphene-based antimony sulfide negative electrode material as claimed in claim 1, wherein in the step (2), sodium borohydride is slowly added into the first solution obtained in the step (1);
the mass ratio of the sodium borohydride to the antimony source is 1-1.4: 1.
4. The preparation method of the graphene-based antimony sulfide negative electrode material according to claim 1, wherein in the step (3), the mass ratio of the sulfur powder to the antimony source is 1: 2-3;
uniformly spreading sulfur powder at the bottom of the lining of the hydrothermal kettle;
the temperature of the hydrothermal reaction is 150-;
the solid-liquid separation adopts a centrifugal separation mode, and the rotating speed during the centrifugal separation adopts a method of firstly high speed, then low speed and then high speed; the high-speed rotating speed is 7000rmp-8000 rmp; the low-speed rotating speed is 2000rmp-3000 rmp;
washing with deionized water;
drying is carried out in a drying mode.
5. The method for preparing the graphene-based antimony sulfide negative electrode material as claimed in claim 1, wherein in the step (4), Sb is added2S3The conditions for compounding with GO by a hydrothermal method are as follows: the temperature is 160-200 ℃ and the time is 12-18 h;
the GO concentration is 3-5 mg/ml.
6. The graphene-based antimony sulfide negative electrode material obtained by the preparation method according to any one of claims 1 to 5.
7. The graphene-based antimony sulfide negative electrode material of claim 6, wherein Sb is Sb2S3The graphene is in a rod-shaped structure and is uniformly dispersed on a three-dimensional porous graphene sheet structure formed after GO is reduced.
8. The application of the graphene-based antimony sulfide negative electrode material as claimed in claim 6 in the aspect of negative electrode materials of lithium ion batteries.
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| CN112072107B (en) * | 2020-08-28 | 2022-07-05 | 中南大学 | Antimony sulfide-based composite material and preparation method and application thereof |
| CN112133909B (en) * | 2020-09-25 | 2021-09-21 | 中国科学院长春应用化学研究所 | Antimony sulfide-based negative electrode material for lithium ion battery and preparation method thereof |
| CN114669269B (en) * | 2022-02-15 | 2023-06-09 | 天津理工大学 | Cs (cell lines) + 、Sr 2+ Co-adsorption-separation dual-function ion exchanger and preparation method and application thereof |
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