CN111628164A - Sodium ion battery positive electrode material and preparation method thereof - Google Patents
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Abstract
A positive electrode material of sodium ion battery and its preparation method, the general formula of the material is NaxNiyFezMn1‑y‑zO2X is 0.6-1, y is 0-0.3, and z is 0-0.3. The method comprises the following steps: fully dissolving soluble transition metal salt in deionized water to prepare a solution A, weighing anhydrous sodium carbonate and sodium hydroxide, and dissolving in the deionized water to prepare a solution B; respectively placing the two solutions in an oil bath, heating and stirring until the two solutions are dissolved, simultaneously heating to 60-90 ℃, then adding the solution B into the solution A, and adjusting the pH value; after the conditions are stable, reacting, aging, filtering, and drying in vacuum to obtain precursor solid powder; pre-burning the precursor solid powder; weighing excessive sodium compoundDissolving the product in a mixed solution of deionized water and absolute ethyl alcohol until the product is clear, adding a precursor until the deionized water and the absolute ethyl alcohol are completely volatilized, and performing vacuum drying; and sintering the obtained solid powder at high temperature to obtain the material.
Description
Technical Field
The invention belongs to the field of battery materials, and relates to a preparation technology of a sodium-ion battery anode material.
Background
Lithium ion batteries are widely used as important energy storage devices in the fields of portable electronic devices, electric vehicles and the like. In recent years, with the increasing demand of the market for lithium ion batteries, the shortage of lithium resources has become a first problem of future large-scale application of the lithium ion batteries. Therefore, the search for suitable energy storage materials that can replace lithium ion batteries is the key to solving the above problems. Compared with lithium resources, sodium resources are of great interest because of their advantages of abundant reserves, wide distribution, low cost, convenient development, etc. In addition, the physicochemical properties of sodium and lithium are similar, so that the problem caused by the shortage of lithium resources can be solved to a great extent by replacing lithium ion batteries with sodium ion batteries.
The positive electrode materials of the sodium ion battery comprise metal oxides, polyanions, organic compounds and the like, wherein the layered transition metal oxide material is widely concerned due to the advantages of high working voltage and high capacity, but the traditional preparation method widely used at present still has the following defects: the particle size, morphology and phase state of the particles of the material are difficult to control in the solid phase method preparation process, the agglomeration problem is serious due to the impact among the particles in the ball milling process, and the uniformity of the prepared material is poor; the sol-gel method has a relatively complex process, the preparation period is long, a large amount of organic raw materials are required to be consumed, and the method is not suitable for industrial production; although the co-precipitation method can obtain the cathode material with smooth surface, uniform particle size distribution and high tap density by controlling the reaction conditions, the pH value is difficult to accurately control in the process of preparing the precursor, and the uniform and complete precipitation of the transition metal cannot be ensured. At present, the method for preparing the cathode material with stable electrochemical performance and good crystallinity by optimizing a synthesis method is urgently needed to replace the lithium ion battery material.
The invention has the Chinese patent application number of CN201810326600.5 and is named as 'O3 type sodium ion battery layered positive electrode material, a preparation method and application thereof', and discloses the O3 type sodium ion battery layered positive electrode material, the preparation method and the application thereof, which are characterized in that metal oxide and a sodium source are mixed according to the stoichiometric ratio, are uniformly mixed and then are tableted, and then the temperature is programmed to 900 ℃, kept for a period of time and cooled to obtain the positive electrode material.
Many researches show that although the solid-phase method is simple and convenient in preparation process, agglomeration is easy to occur in the sintering process, so that the prepared material particles are not uniformly distributed, the morphology of the material is difficult to control, and the setting of the sintering temperature can also influence the phase state finally formed by the material, so that the layered cathode material prepared by the solid-phase method does not necessarily have excellent cycle performance.
The Chinese patent application No. CN201610061090.4, entitled "a sodium ion battery anode material and a preparation method and a use method thereof", discloses a sodium ion battery anode material and a preparation method and a use method thereof, and is characterized in that a mixed solution of a soluble manganese compound and a nickel compound is precipitated out through oxalate, hydrothermal reaction is carried out in a mixed solution of water and ethanol, and finally, the layered sodium nickel manganese oxide material is obtained through heat treatment.
The coprecipitation method is to precipitate soluble salt into a compound through a precipitator and obtain the anode material through high-temperature calcination. The coprecipitation method is difficult to control the experimental conditions accurately in the experimental operation process, and is difficult to obtain ideal data in the experimental scheme. In the future realization of sodium ion battery industrialization, if production equipment is not properly selected, proportion mismatching can be caused in the process of washing the coprecipitation compound, the stability of batch quality is difficult to control, and the cost is higher.
Disclosure of Invention
The invention aims to provide a sodium-ion battery positive electrode material and a preparation method thereof.
The invention relates to a positive electrode material of a sodium-ion battery and a preparation method thereof, wherein the positive electrode material of the sodium-ion battery comprises layered sodium iron nickel manganese oxide and has a chemical general formula of NaxNiyFezMn1-y-zO2Wherein x is 0.6-1, y is 0-0.3, and z is 0-0.3.
In the preparation method of the sodium ion battery cathode material, the precipitator adopted for preparing the precursor of the layered transition metal oxide is a mixed solution of sodium hydroxide and anhydrous sodium carbonate;
the preparation method comprises the following steps:
step (1) soluble transition metal salt is prepared according to the molecular formula NaxNiyFezMn1-y-zO2The chemical dosage ratio of the sodium carbonate and the sodium hydroxide are fully dissolved in deionized water to prepare a transition metal salt solution A with the required concentration, and the anhydrous sodium carbonate and the sodium hydroxide are weighed according to a certain proportion and dissolved in the deionized water to prepare a solution B or a precipitator B;
respectively placing the two solutions in an oil bath, heating and stirring until the two solutions are completely dissolved to be clear, taking the solution A as mother liquor, simultaneously heating to 60-90 ℃, then adding the solution B into the solution A at a certain speed, and adjusting the pH value to be a proper value required by precipitation;
after the conditions are stable, reacting for 6-10 h at a certain temperature, aging, performing suction filtration, and performing vacuum drying to obtain precursor solid powder;
pre-sintering the obtained precursor solid powder at 300-550 ℃ for 3-10 h;
weighing excessive sodium compounds according to a stoichiometric ratio, dissolving the excessive sodium compounds in a mixed solution of deionized water and absolute ethyl alcohol until the mixed solution is clear, adding a precursor, slowly stirring at about 50-90 ℃ until the deionized water and the absolute ethyl alcohol are completely volatilized, and drying in vacuum;
and (6) sintering the obtained solid powder at high temperature to obtain the final sodium-ion battery positive electrode material.
The invention prepares the uniform coprecipitation compound precursor of the nickel-manganese-iron by taking the mixed solution of sodium hydroxide and sodium carbonate as a precipitator, then transfers the precursor into ethanol solution to react with sodium salt, and then obtains the layered anode material through simple high-temperature reaction. The product can be applied to the anode material of the sodium-ion battery, and the precursor has a uniform structure and an accurate stoichiometric ratio, so that the material which is obviously superior to that obtained by the traditional method can be obtained.
Drawings
FIG. 1 shows a layered positive electrode material Na obtained in example 1 of the present invention0.67Mn0.65Fe0.2Ni0.15FIG. 2 shows an XRD spectrum of a layered positive electrode material Na obtained in example 1 of the present invention0.67Mn0.65Fe0.2Ni0.15FIG. 3 is a graph showing the first charge/discharge, and FIG. 1 shows a layered positive electrode material Na obtained in example 1 of the present invention0.67Mn0.65Fe0.2Ni0.15FIG. 4 is a graph showing the cycle characteristics of the layered positive electrode material Na obtained in example 1 of the present invention0.67Mn0.65Fe0.2Ni0.15Electron micrograph of (a).
Detailed Description
The invention relates to a positive electrode material of a sodium-ion battery and a preparation method thereof, wherein the positive electrode material of the sodium-ion battery comprises layered sodium iron nickel manganese oxide and has a chemical general formula of NaxNiyFezMn1-y-zO2Wherein x is 0.6-1, y is 0-0.3, and z is 0-0.3.
In the preparation method of the sodium ion battery cathode material, the precipitator adopted for preparing the precursor of the layered transition metal oxide is a mixed solution of sodium hydroxide and anhydrous sodium carbonate;
the preparation method comprises the following steps:
step (1) soluble transition metal salt is prepared according to the molecular formula NaxNiyFezMn1-y-zO2The chemical dosage ratio of the sodium carbonate and the sodium hydroxide are fully dissolved in deionized water to prepare a transition metal salt solution A with the required concentration, and the anhydrous sodium carbonate and the sodium hydroxide are weighed according to a certain proportion and dissolved in the deionized water to prepare a solution B or a precipitator B;
respectively placing the two solutions in an oil bath, heating and stirring until the two solutions are completely dissolved to be clear, taking the solution A as mother liquor, simultaneously heating to 60-90 ℃, then adding the solution B into the solution A at a certain speed, and adjusting the pH value to be a proper value required by precipitation;
after the conditions are stable, reacting for 6-10 h at a certain temperature, aging, performing suction filtration, and performing vacuum drying to obtain precursor solid powder;
pre-sintering the obtained precursor solid powder at 300-550 ℃ for 3-10 h;
weighing excessive sodium compounds according to a stoichiometric ratio, dissolving the excessive sodium compounds in a mixed solution of deionized water and absolute ethyl alcohol until the mixed solution is clear, adding a precursor, slowly stirring at about 50-90 ℃ until the deionized water and the absolute ethyl alcohol are completely volatilized, and drying in vacuum;
and (6) sintering the obtained solid powder at high temperature to obtain the final sodium-ion battery positive electrode material.
The invention mainly solves the technical problem of uneven precipitation of transition metal caused by the fact that the pH value is difficult to accurately control in the preparation process of a precursor by the traditional coprecipitation method. In the traditional coprecipitation method, sodium hydroxide or ammonia water is usually used as a precipitator, and the pH value is adjusted to ensure that transition metal ions are jointly precipitated to form an initial precursor material, so that the prepared anode material has poor dispersibility and low crystallinity. According to the invention, the mixed solution of sodium carbonate and sodium hydroxide is used as a precipitator, so that the transition metal ions can be more completely precipitated, the pH value is easy to control, and the cathode material with good dispersibility and excellent crystallinity is obtained.
In the preparation method of the sodium ion battery cathode material, in the step (1), the solution B or the precipitant B is used for preparing the precursor of the layered transition metal oxide, and the molar ratio of sodium hydroxide to anhydrous sodium carbonate is 0.1-2.
In the preparation method of the sodium-ion battery cathode material, the nickel compound in the step (1) is nickel acetate, or nickel nitrate, or nickel sulfate; the manganese compound is manganese acetate, or manganese nitrate, or manganese sulfate, and the iron compound is ferrous sulfate, or ferric nitrate.
In the preparation method of the positive electrode material of the sodium-ion battery, the compound in the step (5) is sodium acetate, or sodium nitrate, or sodium carbonate, or sodium hydroxide.
The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
Example 1
(1) 2.617 g of nickel nitrate hexahydrate and 4.848 g of ferric nitrate nonahydrate are weighed, 9.0641 ml of manganese nitrate solution is weighed, and 150 ml of deionized water is added to prepare a transition metal salt solution A;
(2) weighing 0.314 g of sodium hydroxide and 8 g of anhydrous sodium carbonate, and dissolving in 150 ml of deionized water to prepare a precipitator B;
(3) after the solution B of the solution A is completely dissolved to be clear, slowly dripping the solution B into the solution A, adjusting the pH value to be about 9, and reacting for 8 hours at 80 ℃;
(4) standing and aging for 24 h at room temperature, performing suction filtration, washing with 1000 ml of deionized water to remove impurities, and drying;
(5) presintering for 6 h at 450 ℃ to obtain precursor powder;
(6) weighing 4.9234 g of sodium acetate to be completely dissolved in a mixed solution of absolute ethyl alcohol and deionized water, adding the precursor powder obtained in the step (e), stirring at 70 ℃ until the solution is completely volatilized, and grinding after vacuum drying at 110 ℃ for 12 h;
(7) sintering at 850 ℃ for 10h to obtain the final layered positive electrode material Na of the sodium-ion battery0.67Mn0.65Fe0.2Ni0.15。
Example 2
(1) 3.942g of nickel sulfate hexahydrate, 7.998 g of ferric sulfate nonahydrate and 9.815g of manganese sulfate are weighed and added into 100ml of deionized water to prepare a transition metal salt solution A;
(2) weighing 0.314 g of sodium hydroxide and 8 g of anhydrous sodium carbonate, and dissolving in 150 ml of deionized water to prepare a precipitator B;
(3) after the solution B of the solution A is completely dissolved to be clear, slowly dripping the solution B into the solution A, adjusting the pH value to about 9, and reacting for 6 hours at 75 ℃;
(4) standing and aging for 24 h at room temperature, performing suction filtration, washing with 1000 ml of deionized water to remove impurities, and drying;
(5) presintering for 6 h at 450 ℃ to obtain precursor powder;
(6) weighing 9.573 g of sodium acetate to be completely dissolved in a mixed solution of absolute ethyl alcohol and deionized water, adding the precursor powder obtained in the step (e), stirring at 70 ℃ until the solution is completely volatilized, and grinding after vacuum drying at 110 ℃ for 12 h;
(7) sintering at 850 ℃ for 12 h to obtain the final layered positive electrode material Na of the sodium-ion battery0.67Mn0.65Fe0.2Ni0.15。
Claims (5)
1. A positive electrode material of a sodium-ion battery is characterized in that: the material comprises layered sodium iron nickel manganese oxide and has a chemical general formula of NaxNiyFezMn1-y-zO2Wherein x is 0.6-1, y is 0-0.3, and z is 0-0.3.
2. The method for preparing the positive electrode material of the sodium-ion battery according to claim 1, characterized in that: the precipitator used for preparing the precursor of the layered transition metal oxide is a mixed solution of sodium hydroxide and anhydrous sodium carbonate;
the preparation method comprises the following steps:
step (1) soluble transition metal salt is prepared according to the molecular formula NaxNiyFezMn1-y-zO2The chemical dosage ratio of the sodium carbonate and the sodium hydroxide are fully dissolved in deionized water to prepare a transition metal salt solution A with the required concentration, and the anhydrous sodium carbonate and the sodium hydroxide are weighed according to a certain proportion and dissolved in the deionized water to prepare a solution B or a precipitator B;
respectively placing the two solutions in an oil bath, heating and stirring until the two solutions are completely dissolved to be clear, taking the solution A as mother liquor, simultaneously heating to 60-90 ℃, then adding the solution B into the solution A at a certain speed, and adjusting the pH value to be a proper value required by precipitation;
after the conditions are stable, reacting for 6-10 h at a certain temperature, aging, performing suction filtration, and performing vacuum drying to obtain precursor solid powder;
pre-sintering the obtained precursor solid powder at 300-550 ℃ for 3-10 h;
weighing excessive sodium compounds according to a stoichiometric ratio, dissolving the excessive sodium compounds in a mixed solution of deionized water and absolute ethyl alcohol until the mixed solution is clear, adding a precursor, slowly stirring at about 50-90 ℃ until the deionized water and the absolute ethyl alcohol are completely volatilized, and drying in vacuum;
and (6) sintering the obtained solid powder at high temperature to obtain the final sodium-ion battery positive electrode material.
3. The method for preparing the positive electrode material of the sodium-ion battery according to claim 2, characterized in that: in the step (1), the molar ratio of the solution B or the precipitant B, the sodium hydroxide and the anhydrous sodium carbonate used for preparing the precursor of the layered transition metal oxide is 0.1-2.
4. The method for preparing the positive electrode material of the sodium-ion battery according to claim 2, characterized in that: in the step (1), the nickel compound is nickel acetate, or nickel nitrate, or nickel sulfate; the manganese compound is manganese acetate, or manganese nitrate, or manganese sulfate, and the iron compound is ferrous sulfate, or ferric nitrate.
5. The method for preparing the positive electrode material of the sodium-ion battery according to claim 2, characterized in that: the compound in the step (5) is sodium acetate, or sodium nitrate, or sodium carbonate, or sodium hydroxide.
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CN113889619A (en) * | 2021-09-26 | 2022-01-04 | 蜂巢能源科技有限公司 | Sodium-ion battery positive electrode material and preparation method and application thereof |
CN114956202A (en) * | 2022-04-28 | 2022-08-30 | 南通金通储能动力新材料有限公司 | Precursor of sodium ion positive electrode material, preparation method and positive electrode material |
CN115196691A (en) * | 2022-07-18 | 2022-10-18 | 宿迁市翔鹰新能源科技有限公司 | Nickel-iron-manganese ternary precursor for sodium ion battery and preparation method and application thereof |
CN115663173A (en) * | 2022-11-10 | 2023-01-31 | 赣州立探新能源科技有限公司 | Sodium-rich layered oxide material and preparation method and application thereof |
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CN113889619A (en) * | 2021-09-26 | 2022-01-04 | 蜂巢能源科技有限公司 | Sodium-ion battery positive electrode material and preparation method and application thereof |
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CN115650318A (en) * | 2022-11-16 | 2023-01-31 | 浙江吉利控股集团有限公司 | Doped P2 type layered sodium nickel manganese oxide cathode material and preparation method thereof |
CN115650318B (en) * | 2022-11-16 | 2024-03-01 | 浙江吉利控股集团有限公司 | Doped P2 type layered nickel sodium manganate positive electrode material and preparation method thereof |
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