CN116130620A - Modified sodium ion battery anode material and preparation method and application thereof - Google Patents

Modified sodium ion battery anode material and preparation method and application thereof Download PDF

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Publication number
CN116130620A
CN116130620A CN202211530953.XA CN202211530953A CN116130620A CN 116130620 A CN116130620 A CN 116130620A CN 202211530953 A CN202211530953 A CN 202211530953A CN 116130620 A CN116130620 A CN 116130620A
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China
Prior art keywords
ion battery
sodium ion
modified sodium
positive electrode
electrode material
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CN202211530953.XA
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Chinese (zh)
Inventor
邵俊华
孔东波
张利娟
龚国斌
李海杰
闫国锋
闫志卫
王郝为
王亚洲
郭飞
韩飞
宋东亮
施艳霞
李渠成
谢佳庆
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Hunan Farnlet New Energy Technology Co ltd
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Hunan Farnlet New Energy Technology Co ltd
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Priority to CN202211530953.XA priority Critical patent/CN116130620A/en
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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
    • 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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • 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
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • 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 relates to the technical field of batteries, and particularly discloses a modified sodium ion battery anode material, a preparation method and application thereof. The modified sodium ion battery anode material comprises a layered oxide and an indium-containing surface coating; wherein the chemical formula of the layered oxide is Na x Mn a B b Ni c O 2 Wherein x is more than 0.6 and less than 1.2, a is more than 0 and less than 0.6,0, b is more than 0 and less than or equal to c is more than or equal to 0.8, and a+b+c=1. The modified sodium ion battery anode material provided by the invention has good electrochemical performance.

Description

Modified sodium ion battery anode material and preparation method and application thereof
Technical Field
The invention relates to the technical field of batteries, in particular to a modified sodium ion battery positive electrode material, a preparation method and application thereof.
Background
In recent years, along with the continuous shortage of lithium resources, sodium ion batteries are expected to replace lithium ion batteries. Because sodium and lithium are in the same main group in the periodic table of elements, the sodium-lithium composite material has similar physicochemical properties, contains abundant sodium elements, is one of the most widely distributed elements on the earth, is easy to obtain and has low cost.
However, due to the larger ionic radius and electrochemical equivalent of sodium ions, the lithium ion battery has a larger gap from the lithium ion battery in energy density, power density and service life, and the battery can distort the crystal structure during charge and discharge cycles due to sodium ion extraction/intercalation, so that the capacity of the material is rapidly declined. Therefore, searching for a positive electrode material with a more stable structure and more favorable for sodium ion transmission is one of the important points in the current sodium ion battery research.
Manganese-based positive electrode materials have been widely studied for low cost and high safety, and have been widely used in aqueous and nonaqueous batteries. However, during electrochemical cycling, manganese is inevitably dissolved from the active material into the electrolyte, and this loss of manganese can lead to structural degradation and capacity fade of the electrode; on the other hand, manganese deposition on the negative side under electric field driving affects solid electrolyte interface stability. There is a need to find a corresponding strategy to inhibit the dissolution of manganese.
Disclosure of Invention
The present invention aims to solve at least one of the technical problems existing in the prior art. Therefore, the modified sodium ion battery anode material, the preparation method and the application thereof are beneficial to improving the cycle performance and the multiplying power performance of the material, and can improve the charge and discharge capacity, the specific capacity, the cycle stability and the service life of the sodium ion battery.
In a first aspect of the present invention, there is provided a modified sodium ion battery cathode material comprising:
layered oxide of the formula Na x Mn a B b Ni c O 2 Wherein x is more than 0.6 and less than 1.2, a is more than 0 and less than 0.9, b is more than 0 and less than 0.4, c is more than or equal to 0 and less than 0.8, and a+b+c=1;
and, an indium-containing surface coating.
According to the invention, two different modification methods of element doping and surface coating are adopted to modify the manganese-based positive electrode material, so that the relatively high specific capacity of the manganese-based positive electrode material is maintained, and the defects of poor stability, unsatisfactory multiplying power performance and the like of the manganese-based positive electrode material are overcome; therefore, the electrochemical performance of the manganese-based cathode material is remarkably improved.
The inert element boron doping can inhibit Jahn-Teller effect through doping, so that the capacity retention rate of the material is improved, manganese ions in the manganese-based positive electrode material can be effectively replaced, and the cycle performance and the rate performance of the layered positive electrode material are remarkably improved.
The interlayer effect of the surface coating avoids direct contact between the positive electrode material and the electrolyte, can effectively reduce side reaction on the surface and achieves the effect of inhibiting the growth of the positive electrode/electrolyte interface phase on the surface of the particles. The indium in the surface coating can effectively improve the discharge capacity and improve the cycle performance and the rate capability of the positive electrode material.
According to some embodiments of the invention, 0.4.ltoreq.a.ltoreq.0.8.
According to some embodiments of the invention, 0.1.ltoreq.b.ltoreq.0.3.
According to some embodiments of the invention, a: b=1 to 10:1, including but not limited to 1-9: 1. 1 to 8: 1. 1 to 7: 1. 1 to 6: 1. 1 to 5:1. 2-10: 1.2 to 9: 1.2 to 8: 1.2 to 7: 1.2 to 6: 1.2 to 5:1. 3-10: 1. 3 to 9: 1. 3-8: 1. 3 to 7: 1. 3 to 6: 1. 3 to 5:1.
according to some preferred embodiments of the invention, a: b=3 to 5:1.
too little boron doping amount does not obviously improve the cycle performance of the modified sodium ion battery anode material, but too high boron doping amount can cause certain capacity loss, and the electrochemical performance is poor instead.
According to some embodiments of the invention, 0.3.ltoreq.c.ltoreq.0.5.
Nickel can partially replace manganese element, so that the cycle stability and capacity of the positive electrode material are improved.
According to some embodiments of the invention, the indium-containing surface coating comprises In 2 O 3 。
In 2 O 3 Has strong inertia and electrolyte erosion resistance, can prevent the internal structure of the active material from deforming, the surface of the electrode material from peeling off, and the electrolyte from being consumed and decomposed in the electrochemical process. Thus, in 2 O 3 The electrochemical performance of the modified sodium ion battery anode material is obviously improved after coating. In addition, in 2 O 3 The coating can effectively inhibit the hygroscopicity of the surface of the material, and is beneficial to improving the stability of the material.
According to some embodiments of the invention, the indium-containing surface coating accounts for 1-10% of the mass of the modified sodium ion battery positive electrode material, including but not limited to 1-9%, 1-8%, 2-10%, 2-9%, 2-8%, 3-10%, 3-9%, 3-8%, 4-10%, 4-9%, 4-8%.
According to some preferred embodiments of the invention, the indium-containing surface coating comprises 4-8% by mass of the modified sodium ion battery cathode material.
In a second aspect of the present invention, a method for preparing the modified sodium ion battery positive electrode material is provided, comprising the following steps:
dispersing the layered oxide in an indium nitrate solution, precipitating indium, carrying out solid-liquid separation, taking the precipitate, drying and calcining.
According to some embodiments of the invention, the pH condition of the indium precipitate is 8-11.
According to some embodiments of the invention, an acid solution or an alkali solution is selected to adjust the pH;
further, the acid solution can be at least one of nitric acid solution and hydrochloric acid solution;
further, the alkali solution may be at least one of an aqueous ammonia solution and a sodium hydroxide solution.
According to some embodiments of the invention, the indium deposition time is 0.5h to 4h.
According to some embodiments of the invention, the molar concentration of the indium nitrate solution is 0.1 to 1.0mol/L.
According to some embodiments of the invention, the solid-liquid separation mode includes, but is not limited to, centrifugal separation and suction filtration separation; preferably by centrifugation.
According to some embodiments of the invention, the calcination temperature is 600-800 ℃.
According to some preferred embodiments of the invention, the calcination temperature is 600-700 ℃.
According to some embodiments of the invention, the calcination time is 2 to 4 hours.
In a third aspect of the invention, a sodium ion battery is provided, and the preparation raw materials of the sodium ion battery comprise the modified sodium ion battery anode material.
The beneficial effects are that:
the modified sodium ion battery anode material prepared by the invention is beneficial to improving the cycle performance and multiplying power performance of the material, and can improve the charge and discharge capacity, specific capacity and cycle stability of the sodium ion battery.
Additional features and advantages of the invention will be set forth in the description which follows, and in part will be obvious from the description, or may be learned by practice of the invention.
Detailed Description
The conception and the technical effects produced by the present invention will be clearly and completely described in conjunction with the embodiments below to fully understand the objects, features and effects of the present invention. It is apparent that the described embodiments are only some embodiments of the present invention, but not all embodiments, and that other embodiments obtained by those skilled in the art without inventive effort are within the scope of the present invention based on the embodiments of the present invention.
Unless defined otherwise, 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. The terminology used herein in the description of the invention is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention.
Examples
Example 1
The embodiment prepares a modified sodium ion battery anode material, which comprises the following specific processes:
the molar ratio is 0.375:0.25:0.2:0.05, accurately weighing Na with corresponding mass 2 CO 3 、Mn 2 O 3 、Ni 2 O 3 And B 2 O 3 Adding into a ball milling tank, adding grinding balls, introducing nitrogen, ball milling for 30h, heat treating at 900 ℃ for 12h, quenching to room temperature to obtain Na 0.75 Mn 0.5 Ni 0.4 B 0.1 O 2 。
Taking 100g of Na 0.75 Mn 0.5 Ni 0.4 B 0.1 O 2 Preparing into aqueous dispersion, adding 1.0mol/L indium nitrate solution, adjusting pH to 8.5 with ammonia water solution, stirring for 1 hr, collectingCollecting reaction liquid, centrifuging, and collecting precipitate.
Drying the precipitate, and calcining at 700 ℃ for 3 hours to obtain Na 0.75 Mn 0.5 Ni 0.4 B 0.1 O 2 With In 2 O 3 The mass ratio is 95:5, a modified sodium ion battery positive electrode material.
Example 2
The embodiment prepares a modified sodium ion battery anode material, which comprises the following specific processes:
preparation of Na by reference to the procedure in example 1 0.9 Mn 0.8 B 0.2 O 2 。
Taking 100g of Na 0.9 Mn 0.8 B 0.2 O 2 Preparing aqueous dispersion, adding 0.8mol/L indium nitrate solution, regulating pH of the reaction system to 8.0 with ammonia water solution, stirring for 1.5 hr, collecting the reaction solution, centrifuging, and collecting precipitate.
Drying the precipitate, and calcining at 600deg.C for 3 hr to obtain Na 0.9 Mn 0.8 B 0.2 O 2 With In 2 O 3 The mass ratio is 95:5, a modified sodium ion battery positive electrode material.
Example 3
The embodiment prepares a modified sodium ion battery anode material, which comprises the following specific processes:
preparation of Na by reference to the procedure in example 1 0.65 Mn 0.6 Ni 0.3 B 0.1 O 2 。
Taking 100g of Na 0.65 Mn 0.6 Ni 0.3 B 0.1 O 2 Preparing aqueous dispersion, adding 0.5mol/L indium nitrate solution, regulating pH of the reaction system to 10.5 with ammonia water solution, stirring for 0.5 hr, collecting the reaction solution, centrifuging, and collecting precipitate.
Drying the precipitate, and calcining at 680 deg.C for 2 hr to obtain Na 0.65 Mn 0.6 Ni 0.3 B 0.1 O 2 With In 2 O 3 The mass ratio is 90:10, a modified sodium ion battery positive electrode material.
Example 4
The embodiment prepares a modified sodium ion battery anode material, which comprises the following specific processes:
preparation of Na by reference to the procedure in example 1 0.7 Mn 0.4 Ni 0.3 B 0.3 O 2 。
Taking 100g of Na 0.7 Mn 0.4 Ni 0.3 B 0.3 O 2 Preparing aqueous dispersion, adding 0.6mol/L indium nitrate solution, regulating pH of the reaction system to 9 with ammonia water solution, stirring for 3.5 hr, collecting the reaction solution, centrifuging, and collecting precipitate.
Drying the precipitate, and calcining at 700 ℃ for 1.5h to obtain Na 0.7 Mn 0.4 Ni 0.3 B 0.3 O 2 With In 2 O 3 The mass ratio is 92:8, a modified sodium ion battery positive electrode material.
Example 5
The embodiment prepares a modified sodium ion battery anode material, which comprises the following specific processes:
preparation of Na by reference to the procedure in example 1 0.75 Mn 0.45 Ni 0.4 B 0.15 O 2 。
Taking 100g of Na 0.75 Mn 0.45 Ni 0.4 B 0.15 O 2 Preparing aqueous dispersion, adding 1mol/L indium nitrate solution, regulating pH of the reaction system to 6 with nitric acid solution, stirring for 2 hr, collecting the reaction solution, centrifuging, and collecting precipitate.
Drying the precipitate, and calcining at 800 ℃ for 1h to obtain Na 0.75 Mn 0.45 Ni 0.4 B 0.15 O 2 With In 2 O 3 The mass ratio is 94:6, a modified sodium ion battery positive electrode material.
Example 6
The embodiment prepares a modified sodium ion battery anode material, which comprises the following specific processes:
preparation of Na by reference to the procedure in example 1 0.85 Ni 0.45 Mn 0.45 B 0.1 O 2 。
Taking 100g of Na 0.85 Ni 0.45 Mn 0.45 B 0.1 O 2 PreparingForming aqueous dispersion, adding 1.0mol/L indium nitrate solution, adopting ammonia water solution to adjust the pH value of the reaction system to 9, stirring for 4 hours, collecting reaction liquid, centrifugally separating, and taking precipitate.
Drying the precipitate, and calcining at 800 ℃ for 4 hours to obtain Na 0.85 Ni 0.45 Mn 0.45 B 0.1 O 2 With In 2 O 3 The mass ratio is 95:5, a modified sodium ion battery positive electrode material.
Example 7
The embodiment prepares a modified sodium ion battery anode material, which comprises the following specific processes:
preparation of Na by reference to the procedure in example 1 0.75 Mn 0.5 Ni 0.4 B 0.1 O 2 。
Taking 100g of Na 0.75 Mn 0.5 Ni 0.4 B 0.1 O 2 Preparing aqueous dispersion, adding 4mol/L indium nitrate solution, regulating pH of the reaction system to 9 with ammonia water solution, stirring for 3 hr, collecting the reaction solution, centrifuging, and collecting precipitate.
Drying the precipitate, and calcining at 750deg.C for 3 hr to obtain Na 0.75 Mn 0.5 Ni 0.4 B 0.1 O 2 With In 2 O 3 The mass ratio is 80: 20.
Comparative example 1
A modified sodium ion battery cathode material was prepared with reference to the procedure of example 1, specifically differing from example 1 in that:
na is mixed with 0.75 Mn 0.5 Ni 0.4 B 0.1 O 2 Replaced by Na 0.7 MnO 2 。
Comparative example 2
A modified sodium ion battery cathode material was prepared with reference to the procedure of example 1, specifically differing from example 1 in that:
na is mixed with 0.75 Mn 0.5 Ni 0.4 B 0.1 O 2 Replaced by Na 0.75 Ni 0.5 Mn 0.5 O 2 。
Comparative example 3
A modified sodium ion battery cathode material was prepared with reference to the procedure of example 1, specifically differing from example 1 in that:
na is mixed with 0.75 Mn 0.5 Ni 0.4 B 0.1 O 2 Replaced by Na 0.7 Ni 0.5 B 0.5 O 2 。
Comparative example 4
A modified sodium ion battery cathode material was prepared with reference to the procedure of example 1, specifically differing from example 1 in that:
na is mixed with 0.75 Mn 0.5 Ni 0.4 B 0.1 O 2 Replaced by Na 0.65 Ni 0.5 Co 0.1 Mn 0.4 O 2 。
Comparative example 5
A modified sodium ion battery cathode material was prepared with reference to the procedure of example 1, specifically differing from example 1 in that:
na is mixed with 0.75 Mn 0.5 Ni 0.4 B 0.1 O 2 Replaced by Na 0.75 Ni 0.9 Mn 0.05 B 0.05 O 2 。
Comparative example 6
A layered oxide with the chemical formula of Na 0.75 Mn 0.5 Ni 0.4 B 0.1 O 2 。
Namely, the specific preparation steps are as follows: the molar ratio is 0.375:0.25:0.2:0.05, accurately weighing Na with corresponding mass 2 CO 3 、Mn 2 O 3 、Ni 2 O 3 And B 2 O 3 Adding into a ball milling tank, adding grinding balls, introducing nitrogen, ball milling for 30h, heat treating at 900 ℃ for 12h, quenching to room temperature to obtain Na 0.75 Mn 0.5 Ni 0.4 B 0.1 O 2 。
Test case
This test example uses the modified sodium ion battery positive electrode materials prepared in examples 1 to 7 and comparative examples 1 to 6 as positive electrode active materials, a button cell was prepared, and electrochemical properties of the button cell were tested, specifically:
according to the mass ratio of 7:2:1, weighing the anode material, the conductive carbon black and the polyvinylidene fluoride according to the proportion, fully grinding the anode material, the conductive carbon black and the polyvinylidene fluoride to uniformly mix the anode material, preparing the mixture into slurry, and coating the slurry on an aluminum foil. Drying for 8h at 80 ℃ by blowing, and drying for 12h by a vacuum oven to thoroughly remove the moisture in the sample wafer, wherein the temperature is kept at 120 ℃. The battery assembly needs to be completed in a glove box filled with high purity argon. Using a concentration of 1mol L -1 NaClO of (C) 4 Fluoroethylene carbonate: the mixed solution of propylene carbonate (2:98, v/v) is electrolyte. Sodium sheets are used as counter electrodes, and pure glass fiber filter paper Whatman GF/D is used as a diaphragm, and a button cell shell of model CR2032 is selected for testing.
The obtained button cell is subjected to electrochemical performance test within the range of 3.0-4.5V at 25 ℃ and current of 0.1 ℃.
The results of the performance tests are shown in table 1.
Table 1 results of electrochemical properties of the modified sodium-ion battery cathode materials obtained in examples 1 to 7 and comparative examples 1 to 6 corresponding to button cells
First week discharge capacity mAh/g Discharge capacity mAh/g after 100 times of circulation 100 week cycle retention (%)
Example 1 208.5 190.2 91.2
Example 2 200.4 176.9 88.3
Example 3 203.7 183.6 90.1
Example 4 204.2 185.3 90.7
Example 5 199.6 174.2 87.3
Example 6 206.0 187.5 91.0
Example 7 202.8 173.8 85.7
Comparative example 1 174.6 125.7 72.0
Comparative example 2 190.1 152.8 80.4
Comparative example 3 180.4 144.6 80.2
Comparative example 4 185.8 159.2 85.7
Comparative example 5 188.5 163.7 86.8
Comparative example 6 172.6 122.9 71.2
As can be seen from the test results of Table 1, the sodium ion battery cathode materials provided In examples 1 to 7 of the present invention were excellent In heat resistance due to In 2 O 3 The surface coating and boron, manganese or nickel element doping two different modification methods improve the electrochemical performance of the positive electrode material in the positive electrode of the sodium ion battery, and can maintain excellent cycle performance on the basis of ensuring the gram specific capacity of the first-week discharge.
The above-described embodiments of the present invention have been described in detail, but the present invention is not limited to the above-described embodiments, and various changes can be made within the knowledge of those skilled in the art without departing from the spirit of the present invention. Furthermore, embodiments of the invention and features of the embodiments may be combined with each other without conflict.

Claims (10)

1. The modified sodium ion battery positive electrode material is characterized by comprising the following components:
layered oxide of the formula Na x Mn a B b Ni c O 2 Wherein x is more than 0.6 and less than 1.2, a is more than 0 and less than 0.9, b is more than 0 and less than 0.4, c is more than or equal to 0 and less than 0.8, and a+b+c=1;
and, an indium-containing surface coating.
2. The modified sodium ion battery positive electrode material according to claim 1, wherein a is 0.4 or more and 0.8 or less.
3. The modified sodium ion battery positive electrode material according to claim 1, wherein b is 0.1.ltoreq.b.ltoreq.0.3.
4. The modified sodium ion battery positive electrode material according to claim 1, wherein c is 0.3.ltoreq.c.ltoreq.0.5.
5. The modified sodium ion battery positive electrode material of claim 1, wherein the indium-containing surface coating comprises In 2 O 3 。
6. The modified sodium ion battery positive electrode material according to claim 1, wherein the indium-containing surface coating accounts for 1-10% of the modified sodium ion battery positive electrode material by mass.
7. The method for preparing a modified sodium ion battery positive electrode material according to any one of claims 1 to 6, comprising the steps of:
dispersing the layered oxide in an indium nitrate solution, precipitating indium, carrying out solid-liquid separation, taking the precipitate, drying and calcining.
8. The method according to claim 7, wherein the pH condition of the indium precipitate is 8 to 11.
9. The method of claim 7, wherein the calcination temperature is 600-800 ℃;
and/or the calcination time is 2-4 h.
10. A sodium ion battery, characterized in that the preparation raw material of the sodium ion battery comprises the modified sodium ion battery positive electrode material of any one of claims 1 to 6.
CN202211530953.XA 2022-12-01 2022-12-01 Modified sodium ion battery anode material and preparation method and application thereof Pending CN116130620A (en)

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Publication Number Publication Date
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