CN111211324A - Borate lithium/sodium ion battery negative electrode material and preparation method thereof - Google Patents
Borate lithium/sodium ion battery negative electrode material and preparation method thereof Download PDFInfo
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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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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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
- 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
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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
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- 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 discloses a borate lithium/sodium ion battery cathode material and a preparation method thereof. The borate lithium/sodium ion battery cathode material is characterized in that the chemical formula of the borate lithium/sodium ion battery cathode material is Co3(BO3)2. Co of the invention3(BO3)2The material has wide raw material source, low cost, good safety performance and environmental protection, the preparation method has the characteristics of simple process flow, low equipment requirement, high product purity and the like, and the prepared Co has the characteristics of wide raw material source, low cost, high safety performance, environmental protection and the like3(BO3)2The material shows excellent electrochemical performance.
Description
Technical Field
The invention belongs to the field of lithium/sodium ion battery cathode materials, and relates to a borate lithium/sodium ion battery cathode material and a preparation method thereof.
Background
With the accelerated increase of energy demand, if fossil fuels are continuously consumed, resource exhaustion, environmental pollution and greenhouse effect increase inevitably. Therefore, renewable energy and clean energy such as wind power, solar power, tidal power, and the like are rapidly emerging. The lithium ion battery as an effective chemical power supply energy storage device has the advantages of high energy density, long cycle life, environmental friendliness and the like. Because of abundant sodium resources and the similarity of electrochemical properties between sodium and lithium, sodium-ion batteries have attracted extensive attention and made some progress in research in recent years. As commercial graphite is limited to a lower theoretical capacity, developing new anode materials is attracting increasing attention. Related research groups report that borate has good electrochemical performance as a negative electrode material of a lithium (sodium) ion battery.
The borate has wide application in daily life, can be used as a nonlinear optical material, a flame retardant, a ferroelectric, a ceramic material, an anti-wear material and a lubricating additive, and also has important application in the fields of catalysis, adsorption, ion exchange and the like. Borates are very diverse and can be classified as metaborates (BO) depending on the form of their boroxine complex anions2-) Pyroborate (B)4O10 2-) Pentaborate (B)5O10 2-) High borate (B)6O10 2-) And PO4 3-BO compared with other polyanionic compounds3 3-Has relatively small molar mass (58.8g/mol), so that the borate has relatively higher theoretical specific capacity as an electrode material of lithium ion batteries and sodium ion batteries.
When the polyanionic compound borate is used as the negative electrode material of the lithium (sodium) ion battery, the polyanionic compound borate has the advantages of high theoretical specific capacity, abundant reserves, environmental friendliness, wide resource distribution and the like. In the aspect of lithium ion batteries, Liu and the like adopt a hydrothermal method and a high-temperature pyrolysis method to prepare novel flower-shaped Ni3B2O6Nanostructured nickel borate without any template and surfactant, and the flower-like nanostructured material is used as lithium ionThe initial discharge capacity of the anode material of the sub-battery reaches 731.2mAh/g, the charge capacity is 423.6mAh/g, the first irreversible capacity is larger, and needs to be further improved (Solid State Sciences,37(2014) 131-. In the aspect of sodium ion batteries, Yang et al adopt a hydrothermal method to prepare Zn3B2O6And as a sodium ion battery cathode material, research results show that the material reaches 283.7mAh g after being cycled for 100 times in a sodium ion battery-1However, the specific capacity still needs to be improved. (Bulletin of the Chemical Society of Japan, 2018, 91(4), 548-553). We have also made constant attempts to develop new lithium (sodium) ion battery negative electrode materials. With the continuous and deep exploration of the energy storage of the lithium (sodium) ion battery, researchers are eagerly developing novel materials with excellent electrochemical properties such as high specific capacity and excellent rate performance and simple preparation method to meet the development requirement of the energy storage of the lithium (sodium) ion battery.
Disclosure of Invention
The technical problem to be solved by the invention is as follows: in order to overcome the problems of poor reversibility, low capacity and the like of the existing materials, a novel borate lithium/sodium ion battery anode material and a preparation method thereof are provided.
The invention solves the problems by the following technical scheme:
the borate lithium/sodium ion battery cathode material is characterized in that the chemical formula is Co3(BO3)2。
Preferably, it is orthorhombic, belonging to the Pnmn space group. The crystal structure is of the granular magnesium boron stone type.
The invention also provides a preparation method of the borate lithium/sodium ion battery negative electrode material, which is characterized by comprising the following steps: uniformly mixing a cobalt source and a boron source in a molar ratio of 3:2-3, sintering in an oxidizing atmosphere, and cooling to obtain the borate lithium/sodium ion battery cathode material.
Preferably, the cobalt source and the boron source contain cobalt and boron in a molar ratio of 3:2 to 3, preferably 3:2 to 2.5. If the cobalt source is not within the limits of the present invention, no pure phase product can be formed; if the boron source content is too high or too low, a pure phase of the desired product cannot be formed.
Preferably, the oxidizing atmosphere is under an air or oxygen atmosphere. Preferably under an air atmosphere.
Preferably, the mixing is performed by dry grinding or wet grinding for 2-4 h.
Preferably, the sintering step comprises heating to 800-1200 ℃ and keeping the temperature for 1-60 h. Furthermore, the sintering temperature is 800-. The sintering temperature is moderate, and if the temperature is too low, pure-phase Co cannot be prepared3(BO3)2Material, if the temperature is too high, Co produced3(BO3)2The particles of the material are too large, which is not beneficial to the contact of ion transmission and electrolyte and reduces the electrochemical performance of the material.
Preferably, the temperature rise rate of the sintering is controlled to be 1-20 ℃/min.
Preferably, the cobalt source is any one or a combination of several of cobaltosic oxide, cobalt oxalate, cobalt nitrate, cobalt sulfate or cobalt oxide.
Preferably, the boron source is selected from any one or a combination of a plurality of boron trioxide, boric acid, ammonia borate or phenylboronic acid.
The invention also provides a lithium/sodium ion battery which is characterized by comprising a working electrode, a counter electrode, electrolyte and a diaphragm, wherein the working electrode adopts the borate lithium/sodium ion battery cathode material.
Compared with the prior art, the invention has the beneficial effects that:
co prepared by the invention3(BO3)2The material has high specific capacity and rate capability, and is a lithium (sodium) ion battery cathode material with application potential. Co of the invention3(BO3)2The material has wide raw material source, low cost, good safety performance and environmental protection, the preparation method has the characteristics of simple process flow, low equipment requirement, high product purity and the like, and the prepared Co has the characteristics of wide raw material source, low cost, high safety performance, environmental protection and the like3(BO3)2The material shows excellent electrochemical performance.
Drawings
FIG. 1 shows Co prepared in example 13(BO3)2An XRD pattern of the material;
FIG. 2 shows Co prepared in example 13(BO3)2The first three times of charge and discharge curve chart as the lithium ion battery cathode material;
FIG. 3 shows Co prepared in example 13(BO3)2The lithium ion battery cathode material is taken as a cycle performance graph of the lithium ion battery cathode material under the current density of 100 mA/g.
FIG. 4 shows Co prepared in example 13(BO3)2The material is used as a multiplying power performance diagram of the lithium ion battery cathode material under different electric current densities.
FIG. 5 shows Co prepared in example 13(BO3)2The first three times of charge and discharge curve chart is taken as the negative electrode material of the sodium ion battery;
FIG. 6 shows Co prepared in example 13(BO3)2The cycle performance of the material is shown as a cycle performance chart of the negative electrode material of the sodium-ion battery under the current density of 100 mA/g.
FIG. 7 shows Co prepared in example 13(BO3)2The material is used as a rate performance graph of the negative electrode material of the sodium-ion battery under different current densities.
Detailed Description
In order to make the invention more comprehensible, preferred embodiments are described in detail below with reference to the accompanying drawings.
Each raw material used in the following examples is a commercially available product.
Cobalt nitrate in the following examples is a hexahydrate salt.
Example 1
Uniformly mixing 4.5g of cobalt nitrate and 0.7g of boric acid by dry grinding for 2h, heating to 900 ℃ at the speed of 5 ℃/min in a tube furnace under the air atmosphere condition, keeping the temperature for 48h, and naturally cooling to room temperature to obtain the borate lithium/sodium ion battery cathode material with the chemical formula of Co3(BO3)2. From the XRD pattern (FIG. 1), the patternExample 1, 900 ℃ preparation of Co3(BO3)2Material, with Co3(BO3)2The standard PDF cards are matched, and the components of the prepared material are pure-phase Co3(BO3)2It is an orthorhombic system belonging to the Pnmn space group, and has a crystal structure of a periclase type.
Use as lithium ion battery negative electrode: co synthesized by the method of the invention3(BO3)2The negative electrode material, the conductive carbon black and the binder carboxymethylcellulose sodium (CMC) (the mass ratio is 80:10:10) are added with a certain amount of deionized water to be uniformly mixed, coated on a copper foil, dried, punched into a negative electrode plate, and dried for 24 hours at 80 ℃. Taking metal lithium as a counter electrode; 1mol/L of LiPF dissolved in a mixed solution of Ethylene Carbonate (EC)/dimethyl carbonate (DMC) with a mass ratio of 1:16Salt solution is used as electrolyte; the button cell was assembled in an argon glove box with (Celgard 2400 polypropylene membrane) as separator. The electrochemical performance test is carried out by adopting a Wuhan blue electricity CT2001A type battery tester, and the charging and discharging voltage range is 0.01V-3.0V (vs. Li)+/Li). The test temperature was 25 ℃.
FIG. 2 shows Co3(BO3)2As shown in the graph of the previous three times of charge and discharge curves of the lithium ion battery cathode material, in the charge and discharge voltage range of 0.01-3.0V, an obvious discharge platform exists in the first discharge process, but the same platform does not exist in the second discharge process, which indicates that the material has structural evolution in the first charge and discharge process. In the three-time charging process, the shapes of the three charging curves are similar, and no obvious charging voltage platform appears. FIG. 3 is Co3(BO3)2As a cycle performance diagram of the lithium ion battery cathode material under the charge-discharge current density of 100mA/g, as shown in the figure, the first reversible capacity is 375.3mA/g, and after 90 cycles, Co is added3(BO3)2The capacity of the material is still 331.3mA/g, which shows that the material has high specific capacity and good lithium storage performance. FIG. 4 shows Co3(BO3)2As a multiplying power diagram of the lithium ion battery cathode material under different discharge currents, as shown in the figure, the multiplying power diagram is within the charge-discharge voltage range of 0.01-3.0V when dischargingWhen the electric current is increased to 200mA/g, 500mA/g, 1000mA/g and 2000mA/g, the capacities of the cobalt borate cathode are respectively maintained at 337.3mAh/g, 302.4mAh/g, 250.2mAh/g and 182.4 mAh/g. The material has excellent rate performance.
As a sodium ion battery negative electrode: co synthesized by the method of the invention3(BO3)2The negative electrode material, the conductive carbon black and the binder carboxymethylcellulose sodium (CMC) (the mass ratio is 80:10:10) are added with a certain amount of deionized water to be uniformly mixed, coated on a copper foil, dried, punched into a negative electrode plate, and dried for 24 hours at 80 ℃. Taking metallic sodium as a counter electrode; dissolving NaClO in a mixed solution of Ethylene Carbonate (EC) and dimethyl carbonate (DMC) with the mass ratio of 1:1 in 1mol/L4Salt solution is used as electrolyte; the button cell was assembled in an argon glove box with (Whatman glass fiber membrane) as the separator. The electrochemical performance test is carried out by adopting a Wuhan blue electricity CT2001A type battery tester, and the charging and discharging voltage range is 0.01V-3.0V (vs. Na)+Na). The test temperature was 25 ℃.
FIG. 5 shows Co3(BO3)2As shown in the graph of the previous three-time charge-discharge curve of the negative electrode material of the sodium-ion battery, in the charge-discharge voltage range of 0.01-3.0V, an obvious discharge platform exists in the first discharge process, but the same platform does not exist in the second discharge process, which indicates that the material has structural evolution in the first charge-discharge process. In the three-time charging process, the shapes of the three charging curves are similar, and no obvious charging voltage platform appears. FIG. 6 shows Co3(BO3)2As a cycle performance diagram of the negative electrode material of the sodium-ion battery under the charge-discharge current density of 100mA/g, as shown in the figure, the first reversible capacity is 374.1mA/g, and after 80 cycles, Co is added3(BO3)2The capacity of the material is still kept at 182.8mA/g, which shows that the material has high specific capacity and good sodium storage performance. FIG. 7 shows Co3(BO3)2As shown in the multiplying power diagram of the negative electrode material of the sodium ion battery under different discharge currents, when the discharge current is increased to 200mA/g, 500mA/g, 1000mA/g and 2000mA/g in the charge-discharge voltage range of 0.01-3.0V, the capacity of the cobalt borate negative electrode is respectively maintained to be 255.5mAh/g,190.0mAh/g, 152.0mAh/g and 116.6 mAh/g. The material has excellent rate performance.
Example 2
Grinding about 9g of cobalt nitrate and about 1.4g of boric acid by a dry method for 2h, uniformly mixing, heating to 900 ℃ at the speed of 3 ℃/min in a tube furnace under the condition of oxygen atmosphere, keeping the temperature for 48h, and naturally cooling to room temperature to obtain the borate lithium/sodium ion battery cathode material with the chemical formula of Co3(BO3)2。
Example 3
Uniformly mixing 4.5g of cobalt nitrate and 0.7g of boric acid by dry grinding for 2h, heating to 1100 ℃ at the speed of 3 ℃/min in a tube furnace under the air atmosphere condition, keeping the temperature for 48h, and naturally cooling to room temperature to obtain the borate lithium/sodium ion battery cathode material with the chemical formula of Co3(BO3)2。
Example 4
Uniformly mixing 4.5g of cobalt nitrate and 0.7g of boric acid by grinding, heating to 1200 ℃ at the speed of 5 ℃/min in a tube furnace under the air atmosphere condition, keeping the temperature for 55 hours, and naturally cooling to room temperature to obtain the borate lithium/sodium ion battery cathode material with the chemical formula of Co3(BO3)2。
Example 5
Uniformly mixing 8.8g of cobalt nitrate and 1.24g of boric acid by dry grinding for 4h, heating to 1200 ℃ at the speed of 3 ℃/min in a tube furnace under the air atmosphere condition, keeping the temperature for 48h, and naturally cooling to room temperature to obtain a product Co3(BO3)2A material.
Example 6
Taking cobaltosic oxide and boron trioxide, ensuring the molar ratio of cobalt to boron to be 3:2, grinding and mixing uniformly, heating to 950 ℃ at the speed of 1 min/DEG C in a tubular furnace in the air atmosphere, preserving heat for 60 hours, and naturally cooling to obtain the borate lithium/sodium ion battery cathode material with the chemical formula of Co3(BO3)2。
Example 7
Taking cobalt sulfate and ammonium borateThe molar ratio of cobalt to boron is ensured to be 3:2.5, the mixture is ground by a dry method for 2h and uniformly mixed, the temperature is raised to 1100 ℃ at the speed of 10 min/DEG C in a tube furnace under the air atmosphere, the temperature is kept for 20h, and the product Co is obtained after natural cooling3(BO3)2A material.
Example 8
Taking cobalt oxide and phenylboronic acid, ensuring that the molar ratio of cobalt to boron is 3:2.8, grinding by a dry method for 3 hours, uniformly mixing, heating to 1200 ℃ at the speed of 10 min/DEG C in a tube furnace in the air atmosphere, preserving heat for 48 hours, and naturally cooling to obtain the borate lithium/sodium ion battery cathode material with the chemical formula of Co3(BO3)2。
Example 9
Taking a mixture of cobalt nitrate and cobalt sulfate (the mass ratio of the cobalt nitrate to the cobalt sulfate is 1:1) and a mixture of boron trioxide and boric acid (the mass ratio of the cobalt to the boron is 1:1), ensuring that the molar ratio of the cobalt to the boron is 3:2.8, grinding by a dry method for 2h, uniformly mixing, heating to 900 ℃ in a tubular furnace at the speed of 10 min/DEG C in the air atmosphere, preserving heat for 40h, and naturally cooling to obtain the borate lithium/sodium ion battery cathode material, wherein the chemical formula of the borate lithium/sodium ion battery cathode material is Co3(BO3)2。
Claims (10)
1. The borate lithium/sodium ion battery cathode material is characterized in that the chemical formula is Co3(BO3)2。
2. The borate lithium/sodium ion battery negative electrode material of claim 1, which is orthorhombic and belongs to the Pnmn space group.
3. A method of preparing a borate lithium/sodium ion battery negative electrode material as claimed in claim 1 or 2, comprising: uniformly mixing a cobalt source and a boron source in a molar ratio of 3:2-3, sintering in an oxidizing atmosphere, and cooling to obtain the borate lithium/sodium ion battery cathode material.
4. The method of making a borate lithium/sodium ion battery anode material according to claim 3, wherein the molar ratio of the cobalt source to the boron source is 3:2 to 2.5.
5. The method of making a borate lithium/sodium ion battery anode material according to claim 3, wherein the oxidizing atmosphere is in an air or oxygen atmosphere.
6. The method for preparing the borate lithium/sodium ion battery negative electrode material as claimed in claim 3, wherein the mixing is performed by dry grinding or wet grinding for 2-4 h.
7. The method for preparing the borate lithium/sodium ion battery anode material as claimed in claim 3, wherein the sintering step comprises raising the temperature to 800-.
8. The method of making a borate lithium/sodium ion battery anode material according to claim 3, wherein the firing ramp rate is controlled to be 1-20 ℃/min.
9. The method for preparing the borate lithium/sodium ion battery cathode material as claimed in claim 3, wherein the cobalt source is any one or combination of cobaltosic oxide, cobalt oxalate, cobalt nitrate, cobalt sulfate or cobalt oxide; the boron source is selected from any one or combination of a plurality of boron trioxide, boric acid, ammonia borate or phenylboronic acid.
10. A lithium/sodium ion battery, which is characterized by comprising a working electrode, a counter electrode, an electrolyte and a diaphragm, wherein the working electrode adopts the borate lithium/sodium ion battery negative electrode material as claimed in claim 1 or 2.
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| CN114538459A (en) * | 2022-01-06 | 2022-05-27 | 上海电力大学 | Preparation method of borate lithium ion battery cathode material and lithium ion battery |
| CN114538459B (en) * | 2022-01-06 | 2024-05-10 | 上海电力大学 | Preparation method of borate lithium ion battery anode material and lithium ion battery |
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Application publication date: 20200529 |