CN113113576B - Bi/SnO x Composite electrode material of@C sodium ion battery and preparation method thereof - Google Patents

Bi/SnO x Composite electrode material of@C sodium ion battery and preparation method thereof Download PDF

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CN113113576B
CN113113576B CN202110224558.8A CN202110224558A CN113113576B CN 113113576 B CN113113576 B CN 113113576B CN 202110224558 A CN202110224558 A CN 202110224558A CN 113113576 B CN113113576 B CN 113113576B
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sno
electrode material
chloride
composite electrode
ion battery
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CN113113576A (en
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高林
苗世昌
杨学林
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China Three Gorges University CTGU
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/362—Composites
    • H01M4/366—Composites as layered products
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B22—CASTING; POWDER METALLURGY
    • B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
    • B22F9/00—Making metallic powder or suspensions thereof
    • B22F9/16—Making metallic powder or suspensions thereof using chemical processes
    • B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
    • B22F9/20—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from solid metal compounds
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
    • C01B32/00—Carbon; Compounds thereof
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/054—Accumulators with insertion or intercalation of metals other than lithium, e.g. with magnesium or aluminium
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

Abstract

The invention provides a Bi/SnO x The preparation method of the composite electrode material of the sodium ion battery at the temperature of C (x is one or more of 0, 1 and 2) comprises the specific process of synthesizing Bi/SnO x (x is one or more of 0, 1 and 2) ultrafine nano-particles and are coated in three-dimensional porous carbon. Bismuth chloride is used as bismuth source, stannous chloride is used as tin source, citric acid is used as carbon source, sodium chloride is used as template, and after dissolution, drying and high-temperature carbonization decomposition are carried out to obtain carbon-coated Bi/SnO x A composite material. The composite material prepared by the method has the characteristics of excellent cycling stability and high specific capacity when being used as a negative electrode material of a sodium ion battery. Such Bi/SnO x Material @ C at 1A g ‑1 After about 500 circles of current density, the current density still has 125 mAh g ‑1 Is a specific capacity of (a).

Description

Bi/SnO x Composite electrode material of@C sodium ion battery and preparation method thereof
Technical Field
The invention belongs to the field of negative electrode materials of sodium ion batteries, and in particular relates to a Bi/Sn-SnO with ultrafine nano particles 2 A preparation method of an @ C composite material belongs to the field of sodium ion battery anode materials.
Technical Field
The explosive growth of the renewable energy industry provides a great opportunity and challenge to the energy storage market. Sodium ion batteries are a more attractive energy storage device because they have similar electrochemical storage mechanisms and synthesis techniques as lithium ion batteries and are less costly. However, sodium ionsThe subcells have poor electrochemical stability and low energy density, and selecting appropriate electrode materials is an effective method of improving their electrochemical performance. For the negative electrode materials, such as carbon-based materials, alloy-type materials and conversion-type materials scientists have been widely explored. Elemental Bi and SnO x (x=0, 1 and 2) as a negative electrode material for sodium ion batteries, however, bi/Sn-SnO has been studied extensively 2 The @ C composite sodium ion battery anode material is studied remarkably.
Disclosure of Invention
The invention provides a Bi/SnO x Composite electrode material of@C sodium ion battery, bi/SnO in electrode material x The superfine nano particles are coated in the three-dimensional porous carbon, x is one or more of 0, 1 and 2, and the pore diameter of the 3D porous network is 100-400nm.
The Bi/SnO x X in the ultra-fine nano particles is 0, 1 and 2 at the same time, bi/SnO x The composite electrode material of the @ C sodium ion battery is Bi/Sn-SnO 2 @C in which Bi/Sn-SnO-SnO 2 The superfine nano particle composite material accounts for 20-90wt% and is Bi/Sn-SnO 2 The nanometer size ranges from 2 to 100 nm.
The Bi/SnO x X in the superfine nano particles is 0 and 1 at the same time, bi/SnO x The composite electrode material of the @ C sodium ion battery is Bi/Sn-SnO @ C, wherein the Bi/Sn-SnO ultrafine nano-particle composite material accounts for 20-90wt% and the nano-size range of Bi/Sn-SnO is 2-100 nm.
The Bi/SnO x X in the superfine nano particles is 1 and 2 at the same time, bi/SnO x The composite electrode material of the @ C sodium ion battery is Bi/SnO-SnO 2 @C in which Bi/SnO-SnO 2 The superfine nano particle composite material accounts for 20 to 90 weight percent, and the Bi/SnO-SnO is prepared 2 The nanometer size ranges from 2 to 100 nm.
The invention aims to obtain the bismuth nitrate-stannous chloride composite material with excellent electrochemical performance by taking bismuth nitrate and stannous chloride as raw materials, sodium chloride as a template and citric acid as a carbon source, dissolving and fully mixing the bismuth nitrate and stannous chloride with deionized water, drying, further annealing under the nitrogen condition, removing the sodium chloride with deionized water, and drying3D porous carbon nano Bi/SnO x @C (especially Bi/Sn-SnO 2 ) An ultrafine composite material. The raw materials involved in the invention are bismuth chloride, stannous chloride, citric acid and sodium chloride. In the preparation process of the material, bismuth chloride, stannous chloride, citric acid and sodium chloride are dissolved in deionized water and stirred, wherein the mass ratio of the bismuth chloride to the stannous chloride to the citric acid to the sodium chloride is 0.2-0.5:0.1-0.3:2-4:18-25, and after the bismuth chloride to the stannous chloride is dissolved, the solution is transferred into a culture dish and dried in an oven at 80 ℃. Then annealing the mixture in nitrogen at 500-700 ℃ and 2-12 h to obtain Bi/Sn-SnO of sodium chloride template 2 The alloy is filtered for multiple times to remove the sodium chloride template, and finally the nano Bi/Sn-SnO is obtained 2 Novel nanocomposite materials with ultrafine nanoparticles coated in 3D porous carbon.
The Bi/Sn-SnO 2 The superfine nano particles are coated in the three-dimensional porous carbon, and the pore diameter range of the 3D porous network is 100-400nm.
The nano Bi/Sn-SnO 2 The superfine nano particle composite material accounts for 20-90wt% and is Bi/Sn-SnO 2 The nanometer size ranges from 2 to 100 nm.
The nano Bi/SnO of the invention x The alloy anode material and the preparation method thereof have the following characteristics:
(1) The preparation method has the advantages of low preparation cost and simple operation. Preparing superfine Bi/SnO coated in porous carbon x Composite material of particles.
(2) The 3D carbon network improves the electron conductivity, bi/Sn-SnO 2 The @ C shows excellent cycling performance in sodium ion batteries.
Drawings
Figure 1 is an XRD pattern of samples prepared in examples 1, 2 and 3.
Fig. 2 is an SEM image and a corresponding element mapping image of the sample prepared in example 1, wherein a is an SEM image and B is a corresponding element mapping image.
Fig. 3 shows the first three charge and discharge curves of the sample prepared in example 1.
Fig. 4 is an SEM image of the sample prepared in example 2.
Fig. 5 is the first three charge and discharge curves of the sample prepared in example 2.
Fig. 6 is an SEM image of the sample prepared in example 3.
Fig. 7 is the first three charge and discharge curves of the sample prepared in example 3.
FIG. 8 is a graph showing the cycle performance of the samples prepared in examples 1, 2 and 3.
Detailed Description
Example 1
Dissolving bismuth chloride 0.329-g, stannous chloride 0.244g, citric acid 2.5g, and sodium chloride 20.642 g in deionized water 60 ml, stirring for 4-5 h, transferring the solution to a culture dish after dissolving, oven drying at 80deg.C, and mixing the above powder with N 2 At 8 ℃ for min under atmosphere -1 Annealing at 600 ℃ for 2 hours to obtain Bi/Sn-SnO 2 @ C composite. After the material is cooled to room temperature, the obtained material is filtered by deionized water for 2 to 3 times, sodium chloride is removed, and Bi/Sn-SnO is obtained after drying 2 @ C composite. FIG. 1 shows the Bi/Sn-SnO obtained 2 XRD pattern of @ C composite material, i.e. the composite material contains Sn, snO and SnO simultaneously 2 ，Bi/Sn-SnO-SnO 2 The superfine nano particle composite material accounts for 80 weight percent. It can be seen that Sn-SnO-SnO 2 Characteristic peaks of Bi and Bi. SEM characterization of the obtained Bi/Sn-SnO powder is shown in FIG. 2 2 The @ C composite material has a porous morphology. FIG. 3 shows that it is at 0.2A g -1 The first three circles of charge-discharge curves under the current density have the specific capacity of about 630 mAh g for the first time -1 . At 1A g -1 The charge and discharge test is carried out, and the material still has 125 mAh g after about 500 circles of circulation -1 The coulombic efficiency was about 98% and showed good electrochemical performance (fig. 7).
Example 2
The implementation method is the same as in example 1, and stannous chloride is not added, so that the Bi@C composite material is obtained. After the material is cooled to room temperature, the obtained material is filtered by deionized water for 2 to 3 times, sodium chloride is removed, and the superfine Bi particle material wrapped in porous carbon is obtained after drying, and the superfine Bi particle material is also porous (figure 4). Will beThe sodium ion half-cell is assembled as a cathode material and is 0.2A g -1 The charge and discharge test is carried out, the charge and discharge platform is obvious (figure 5), and the specific capacity of the initial discharge is about 800 mAh g -1 At 1A g -1 The specific capacity is less than 100 mAh g after 500 circles of circulation under the current density -1 (FIG. 7).
Example 3
The method is the same as in example 1, and Sn-SnO is obtained by adding only bismuth chloride 2 @ C composite. The sodium ion half cell was assembled at 0.2A g -1 The charge and discharge test is carried out, the charge and discharge platform is obvious (figure 6), and the first discharge capacity reaches 413 mAh g -1 . At 1A g -1 The specific capacity is about 20mAh g after 500 cycles under the current density -1 (FIG. 7).
Example 4
The method is the same as in example 1, except that the annealing temperature is 500℃to obtain Bi/Sn-SnO 2 @C composite material, assembled with a sodium ion half cell at 0.2 Ag -1 The charge and discharge test is carried out, the charge and discharge platform is obvious, and the first discharge capacity reaches 555mAh g -1 . At 1A g -1 The charge and discharge test is carried out, and 100 mAh g still exists after about 500 circles of circulation -1 Is a specific capacity of (a).
Example 5
The method is the same as in example 1, and the annealing temperature is 700 ℃ only, and Bi/Sn-SnO is obtained 2 @ C composite. The sodium ion half cell was assembled at 0.2A g -1 The charge and discharge test is carried out, the charge and discharge platform is obvious, and the first discharge capacity reaches 520mAh g -1 . At 1A g -1 The charge and discharge test is carried out, and the battery still has 82 mAh g after about 500 circles of circulation -1 Is a specific capacity of (a).
Example 6
The method was the same as in example 1 except that the mass of stannous chloride was 0.15g to give a Bi/Sn-SnO@C composite material, which was assembled into a sodium ion half cell at 0.2A g -1 The charge and discharge test is carried out, the charge and discharge platform is obvious, and the first discharge capacity reaches 410mAh g -1 . At 1A g -1 The charge and discharge test was performed under a condition of about 50After 0 cycles, the product has 120 mAh g -1 Is a specific capacity of (a).
Example 7
The method is the same as in example 1, except that the mass of stannous chloride is 0.30g, bi/SnO-SnO is obtained 2 @ C composite. The sodium ion half cell was assembled at 0.2A g -1 The charge and discharge test is carried out, the charge and discharge platform is obvious, and the first discharge capacity reaches 440mAh g -1 . At 1A g -1 The charge and discharge test is carried out, and the material still has 105mAh g after about 500 circles of circulation -1 Is a specific capacity of (a).

Claims (5)

1. Bi/SnO x The preparation method of the composite electrode material of the@C sodium ion battery is characterized by comprising the following steps of: weighing citric acid, sodium chloride, bismuth chloride and stannous chloride, dissolving in deionized water, continuously stirring until the citric acid, sodium chloride, bismuth chloride and stannous chloride are completely dissolved, drying, and then adding the mixture into N 2 Medium annealing, filtering with deionized water, removing sodium chloride, and preparing nano Bi/SnO x A @ C composite electrode material;
wherein the mass ratio of bismuth chloride to stannous chloride to citric acid to sodium chloride is 0.2-0.5:0.1-0.3:2-4:18-25;
Bi/SnO in the composite electrode material x The superfine nano particles are coated in the three-dimensional porous carbon, x is a plurality of 0, 1 and 2, but the pore diameter of the porous network which is not independently 0,3D is 100-400nm.
2. Bi/SnO according to claim 1 x The preparation method of the composite electrode material of the@C sodium ion battery is characterized by comprising the following steps of:
bismuth chloride, stannous chloride, citric acid and sodium chloride in a mass ratio of 0.329:0.244:2.5:20.642; obtaining nano Bi/SnO x Bi/SnO in the @ C composite electrode material x X in the ultra-fine nano particles is 0, 1 and 2 at the same time, bi/SnO x The composite electrode material of the @ C sodium ion battery is Bi/Sn-SnO 2 @C in which Bi/Sn-SnO-SnO 2 The superfine nano particle composite material accounts for 20-90wt% and is Bi/Sn-SnO 2 The nanometer size ranges from 2 to 100 nm.
3. Bi/SnO according to claim 1 x The preparation method of the composite electrode material of the@C sodium ion battery is characterized by comprising the following steps of:
bismuth chloride, stannous chloride, citric acid and sodium chloride in a mass ratio of 0.329:0.15:2.5:20.642; obtaining nano Bi/SnO x In the @ C composite electrode material, the Bi/SnO is x X in the superfine nano particles is 0 and 1 at the same time, bi/SnO x The composite electrode material of the @ C sodium ion battery is Bi/Sn-SnO @ C, wherein the Bi/Sn-SnO ultrafine nano-particle composite material accounts for 20-90wt% and the nano-size range of Bi/Sn-SnO is 2-100 nm.
4. Bi/SnO according to claim 1 x The preparation method of the composite electrode material of the@C sodium ion battery is characterized by comprising the following steps of:
bismuth chloride, stannous chloride, citric acid and sodium chloride in a mass ratio of 0.329:0.30:2.5:20.642; obtaining nano Bi/SnO x In the @ C composite electrode material, the Bi/SnO is x X in the superfine nano particles is 1 and 2 at the same time, bi/SnO x The composite electrode material of the @ C sodium ion battery is Bi/SnO-SnO 2 @C in which Bi/SnO-SnO 2 The superfine nano particle composite material accounts for 20 to 90 weight percent, and the Bi/SnO-SnO is prepared 2 The nanometer size ranges from 2 to 100 nm.
5. Bi/SnO according to claim 1 x The preparation method of the composite electrode material of the@C sodium ion battery is characterized by comprising the following steps of: annealing is carried out in nitrogen at 500-700 ℃ for 2-12 h.
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