CN114759179A - Method for synthesizing anode material sodium iron phosphate for sodium ion battery - Google Patents
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Abstract
The invention discloses a method for synthesizing a sodium iron phosphate anode material for a sodium ion battery. The method realizes the solid-phase synthesis technology of the sodium iron phosphate anode material for industrial production for the first time, and mainly comprises the following steps of adding iron phosphate, a sodium source and a carbon source into a solvent according to a certain proportion for wet ball milling, and grinding the mixture to a particle size below a target particle size; then drying the ground slurry to obtain precursor powder; sintering the precursor powder at high temperature under the protection of inert atmosphere to obtain a sodium iron phosphate anode material; the method has the advantages of reasonable design, simple process and convenience for large-scale production, and the synthesized sodium iron phosphate cathode material has high gram volume and stable electrochemical performance and can be used as a preferred cathode material of a commercial sodium-ion battery in the future.
Description
Technical Field
The invention belongs to the technical field of batteries, and relates to a method for synthesizing a sodium iron phosphate anode material for a sodium ion battery.
Background
Lithium ion batteries are widely applied to the fields of electronic equipment, new energy steam, energy storage power stations and vehicles and the like as important energy storage devices, and lithium resources are used as core raw materials of the lithium ion batteries, so that the storage capacity is limited, the distribution is uneven, and the extraction is difficult. With the increasing demand of the energy storage market for lithium ion batteries, the shortage of lithium resources becomes the biggest problem in future large-scale application of lithium ion batteries. Therefore, finding a new energy storage device that can replace lithium ion batteries is the key to solving the above problems.
Compared with lithium resources, sodium resources have the advantages of abundant reserves, wide distribution, lower development cost and the like. In view of the resource advantages of sodium, the research of sodium ion batteries has been receiving much attention in recent years. Based on the association of lithium iron phosphate cathode materials of lithium ion batteries, the concept of sodium iron phosphate as a cathode material of sodium ion batteries has been proposed, but no clear technical route is provided for the synthesis. At present, few documents report that sodium iron phosphate is prepared by a sol-gel method or an electrochemical proton exchange method, and no industrial preparation technology from raw materials to finished materials exists. For example, in a method (CN105047913A) for preparing olivine-type sodium iron phosphate by an electrochemical method, lithium iron phosphate material is oxidized and delithiated by an electrochemical reduction method in a lithium-containing aqueous solution electrolyte to obtain olivine-type iron phosphate, and then the obtained iron phosphate is reduced and intercalated in a sodium-containing aqueous solution to obtain olivine-type sodium iron phosphate, which can simply and rapidly synthesize sodium iron phosphate, but is difficult to realize industrial production; for another example, a sodium iron phosphate composite material and a preparation method thereof (CN111056544A), a sol precursor of sodium iron phosphate is prepared by hydrothermal, and then olivine-type sodium iron phosphate is obtained by sintering, which is also unable to realize industrialization due to harsh hydrothermal conditions.
The invention provides a method for synthesizing sodium iron phosphate serving as a positive electrode material for a sodium ion battery, which defines a complete solid-phase synthesis technical route from raw materials to the sodium iron phosphate for the first time, is completely suitable for industrial production, and has feasibility for solving the problems by replacing lithium resources with sodium.
Disclosure of Invention
The invention aims to provide a method for synthesizing a sodium iron phosphate anode material for a sodium ion battery, which comprises the following specific scheme:
the invention synthesizes olivine type ferric sodium phosphate as the anode material for sodium ion battery by solid phase method, and the chemical formula is NaFePO4。
A method for synthesizing sodium iron phosphate serving as a positive electrode material for a sodium ion battery comprises the following steps:
(1) mixing iron phosphate, a sodium source and a carbon source according to a certain proportion;
(2) adding a solvent for wet grinding until the grain size is ground to a target grain size;
(3) after grinding to a target particle size, drying the ground fluid slurry at a certain temperature to obtain precursor powder;
(4) pre-sintering the obtained precursor powder for a certain time under the protection of inert atmosphere;
(5) then, continuously heating the pre-sintered material under the protection of the same inert atmosphere to perform high-temperature sintering treatment for a certain time;
(6) and finally, crushing, grinding and sieving the material sintered at high temperature to obtain the sodium iron phosphate cathode material.
The sodium source in the step (1) comprises at least one of sodium carbonate, sodium bicarbonate, sodium acetate, sodium benzoate or sodium ethoxide.
The carbon source in the step (1) comprises at least one of glucose, sucrose, polyethylene glycol, citric acid or polypropylene.
In the step (1), the molar ratio of the sodium source to the iron phosphate is (1.01-1.15): 1; the mass ratio of the carbon source to the iron phosphate is (0.1-0.3): 1.
the solvent adopted in the wet grinding in the step (2) comprises at least one of water, ethanol or ethylene glycol.
The target particle size of the wet grinding in the step (2) is 400-900 nm.
And (4) drying the slurry obtained in the step (3) in an air-blast drying oven at the drying temperature of 50-200 ℃ for 8-24 hours.
And (4) presintering at 300-450 ℃ under the protection of inert atmosphere, wherein the heating rate is 2-5 ℃/min, and the heat preservation time is 1-6 h.
And (5) after the pre-sintering in the step (5) is finished, heating to 500-800 ℃ for high-temperature calcination, wherein the heating rate is 5-10 ℃/min, and the heat preservation time is 8-15 h.
The complete scheme of the invention comprises the following steps:
(1) mixing iron phosphate and a sodium source according to a molar ratio of 1: (1.01-1.15) adding the mixture into a ball milling tank, and continuously adding a carbon source according to 10-30% of the mass of the ferric phosphate; then adding ball milling beads for dry ball milling, wherein the using amount of the ball milling beads is 20-100% of the volume of the powder material, the ball milling rotating speed is 100-300 rpm/min, and the ball milling time is 0.5-1 h;
(2) stopping ball milling after the step (1) is finished, and continuously adding a solvent for high-energy wet ball milling; the adding amount of the solvent is 50-200% of the mass of the ferric phosphate; the ball milling speed is 400-600 rpm/min, and the ball milling time is 4-12 h.
(3) Stopping ball milling after the step (2) is finished, collecting slurry with fluidity, and drying the slurry in an air-blast drying oven at the drying temperature of 50-200 ℃ for 8-24 h; then transferring the mixture into a ball milling tank again for ball milling and crushing, wherein the ball milling rotating speed is 100-300 rpm/min, and the ball milling time is 1-3 h, and finally obtaining a precursor powder material;
(4) presintering the precursor material at 300-450 ℃ under the protection of inert atmosphere, wherein the heating rate is 2-5 ℃/min, and the heat preservation time is 1-6 h;
(5) after the pre-sintering is finished, heating to 500-800 ℃ for high-temperature calcination, wherein the heating rate is 5-10 ℃/min, and the heat preservation time is 8-15 h;
(6) and collecting the sintered material, crushing and sieving to obtain the sodium iron phosphate cathode material.
When the positive electrode slurry is manufactured, mixing a sodium ferric phosphate positive electrode material, acetylene black and a binder polyvinylidene fluoride (PVDF) according to a mass ratio of 8: 1: 1, grinding and mixing, preparing slurry by taking N-methyl pyrrolidone (NMP) as a solvent, fully grinding and stirring to dissolve PVDF in NMP, then uniformly coating the slurry on an aluminum foil, drying at the temperature of 110 ℃ for more than 4h after drying, cutting the slurry into wafers for later use by a tablet machine, placing the electrode plates in a glove box under the protection of argon gas to be used as working electrodes, and assembling a metal sodium sheet as a counter electrode into a CR2032 button cell; the test voltage range is 2.5-4.2V.
The method for assembling the sodium-ion battery is characterized in that: in the process of assembling the sodium ion battery, the diaphragm is made of a glass fiber diaphragm or a polypropylene diaphragm, the electrolyte is a 1mol/L sodium perchlorate solution or a sodium hexafluorophosphate solution, and the solvent system is Ethylene Carbonate (EC), diethylene carbonate (DEC) and Propylene Carbonate (PC) which are prepared according to the mass percentages of 30%, 67% and 3%.
The olivine-phase sodium iron phosphate cathode material is prepared by the method. The method comprises two procedures of precursor preparation and precursor calcination. Firstly, mixing raw materials of ferric phosphate, a sodium source and a carbon source according to a certain proportion by a wet grinding process, then, carrying out wet grinding on the mixture until the mixture is below a nanometer level as a precursor material, and then, controlling parameters such as inert atmosphere, heating rate, pre-sintering temperature, pre-sintering time, calcining temperature and calcining time and the like in the calcining process to ensure that sodium ions and the ferric phosphate are fully diffused mutually under a high-temperature solid phase environment, and meanwhile, ferric iron with high valence state is reduced into ferrous iron, namely olivine type ferric sodium phosphate is generated. The invention also provides an evaluation method for assembling the button half-cell by using the sodium iron phosphate positive electrode material, wherein sodium metal is used as a negative electrode, and an electrolyte system and a diaphragm material which are suitable for sodium iron phosphate of the sodium ion battery are matched.
In short, the invention firstly provides a complete solid phase technical route for synthesizing the sodium iron phosphate (NaFePO3) cathode material of the sodium ion battery by taking the iron phosphate (FePO3) as the raw material, and the method has simple process and can be completely suitable for industrial production. And the invention can produce products with excellent effect and meeting the requirements through the improvement of working procedures (especially the control of grinding particle size, sintering time, temperature and heating rate).
Drawings
FIG. 1 shows NaFePO for sodium ion battery obtained in example 14SEM photograph of the positive electrode material.
FIG. 2 shows NaFePO for sodium ion battery obtained in example 14First charge-discharge curve diagram of the anode material.
FIG. 3 shows NaFePO for sodium ion battery obtained in example 14Cycle performance diagram of the positive electrode material.
Detailed Description
The present invention will be further illustrated by the following examples, but is not limited to the following examples.
Example 1
A method for synthesizing sodium iron phosphate serving as a positive electrode material for a sodium ion battery comprises the following steps:
150.82g of iron phosphate, 103.00g of sodium bicarbonate and 22.62g of glucose are weighed and added into a ball milling tank for dry ball milling mixing, the rotating speed is 300rpm/min, and the ball milling time is 1 h; then adding 300g of water for high-energy wet ball milling; the ball milling speed is 500rpm/min, and the ball milling time is 8 h; after wet ball milling is finished, collecting slurry with fluidity, and drying in an air-blast drying oven at 60 ℃ for 24 h; and collecting the materials after drying, then transferring the materials into a ball milling tank again for ball milling and crushing, wherein the ball milling rotation speed is 300rpm/min, and the ball milling time is 1.5h, and finally obtaining the precursor powder material.
And (2) putting the precursor powder material into a corundum sagger, compacting, transferring into a tube furnace for sintering, emptying air in the tube furnace by using high-purity nitrogen with the purity of 99.999%, and then keeping the high-purity nitrogen atmosphere for sintering. Firstly, heating to 350 ℃ for heat preservation and presintering for 4h, wherein the heating rate is 2 ℃/min; then heating to 700 ℃, keeping the temperature for 12 hours, and calcining at the heating rate of 5 ℃/min; and cooling to normal temperature after the calcination is finished.
And collecting the sintered material, sieving, and finally performing jet milling to obtain the sodium iron phosphate cathode material. The prepared sodium iron phosphate cathode material assembled button half-cell is subjected to capacity test, and the method comprises the following specific steps: mixing the synthesized sodium iron phosphate powder material with acetylene black and a binder polyvinylidene fluoride (PVDF) according to a mass ratio of 8: 1: 1, grinding the mixed mixture powder, and then mixing the mixture powder and the N-methyl pyrrolidone (NMP) according to a mass ratio of 4: 1, adding an NMP solvent, fully grinding and stirring to dissolve PVDF in NMP to obtain anode slurry; then, uniformly coating the positive electrode slurry on an aluminum foil by using a coating scraper with the thickness of 250 mu m, drying at 110 ℃ for more than 4h to obtain a positive electrode piece, and then cutting the positive electrode piece into a wafer for later use by using a sheet beating machine; the wafer pole piece is placed in a glove box protected by argon gas to be used as a working electrode, glass fiber is used as a diaphragm, a metal sodium sheet is used as a counter electrode to assemble a CR2032 button cell, and the electrolyte is sodium perchlorate electrolyte (1M NaClO)4And EC: DEC: PC-30: 67: 3 (mass ratio)), the test voltage range is 2.5-4.2V;
example 2
A method for synthesizing sodium iron phosphate serving as a positive electrode material for a sodium ion battery comprises the following steps:
150.82g of iron phosphate, 54.58g of sodium carbonate and 22.62g of glucose are weighed and added into a ball milling tank for dry ball milling mixing, the rotating speed is 300rpm/min, and the ball milling time is 1 h; then adding 120g of water for high-energy wet ball milling; the ball milling speed is 500rpm/min, and the ball milling time is 8 h; after wet ball milling is finished, collecting slurry with fluidity, and drying in an air-blast drying oven at 60 ℃ for 24 h; and collecting the materials after drying, then transferring the materials into a ball milling tank again for ball milling and crushing, wherein the ball milling rotation speed is 300rpm/min, and the ball milling time is 1.5h, and finally obtaining the precursor powder material.
The sintering step was carried out as in example 1. And collecting the sintered material, sieving, and finally performing jet milling to obtain the sodium iron phosphate cathode material. The cell assembly and testing procedure was as in example 1.
Example 3
A method for synthesizing sodium iron phosphate serving as a positive electrode material for a sodium ion battery comprises the following steps:
150.82g of iron phosphate, 84.46g of anhydrous sodium acetate and 15.08g of glucose are weighed and added into a ball milling tank for dry ball milling mixing, the rotating speed is 300rpm/min, and the ball milling time is 1 h; then adding 300g of water for high-energy wet ball milling; the ball milling speed is 500rpm/min, and the ball milling time is 8 h; after wet ball milling is finished, collecting slurry with fluidity, and drying in an air-blast drying oven at 60 ℃ for 24 h; and collecting the materials after drying, then transferring the materials into a ball milling tank again for ball milling and crushing, wherein the ball milling rotation speed is 300rpm/min, and the ball milling time is 1.5h, and finally obtaining the precursor powder material.
And (2) filling the precursor powder material into a corundum box, compacting, transferring into a tube furnace for sintering, emptying air in the tube furnace by using high-purity nitrogen with the purity of 99.999%, and then keeping the high-purity nitrogen atmosphere for sintering. Firstly, heating to 350 ℃ for heat preservation and presintering for 4 hours, wherein the heating rate is 2 ℃/min; then heating to 720 ℃, keeping the temperature for 12 hours, and calcining at the heating rate of 5 ℃/min; and cooling to normal temperature after the calcination is finished. And collecting the sintered material, sieving, and finally performing jet milling to obtain the sodium iron phosphate cathode material. The cell assembly and testing procedure was as in example 1.
Example 4
A method for synthesizing sodium iron phosphate serving as a positive electrode material for a sodium ion battery comprises the following steps:
150.82g of iron phosphate, 103.00g of sodium bicarbonate and 24.13g of sucrose are weighed and added into a ball milling tank for dry ball milling mixing, the rotating speed is 300rpm/min, and the ball milling time is 1 h; then adding 200g of water for high-energy wet ball milling; the ball milling speed is 500rpm/min, and the ball milling time is 8 h; after wet ball milling is finished, collecting slurry with fluidity, and drying in an air-blast drying oven at 60 ℃ for 24 h; and collecting the materials after drying, then transferring the materials into a ball milling tank again for ball milling and crushing, wherein the ball milling rotation speed is 300rpm/min, and the ball milling time is 1.5h, and finally obtaining the precursor powder material.
The sintering step was carried out as in example 1. And collecting the sintered material, sieving, and finally performing jet milling to obtain the sodium iron phosphate cathode material. The cell assembly and testing procedure was as in example 1.
Example 5
A method for synthesizing sodium iron phosphate serving as a positive electrode material for a sodium ion battery comprises the following steps:
150.82g of iron phosphate, 54.58g of sodium carbonate and 24.13g of cane sugar are weighed and added into a ball milling tank for dry ball milling and mixing, the rotating speed is 300rpm/min, and the ball milling time is 1 h; then adding 120g of water for high-energy wet ball milling; the ball milling speed is 500rpm/min, and the ball milling time is 8 hours; after wet ball milling is finished, collecting slurry with fluidity, and drying in an air-blast drying oven at 60 ℃ for 24 h; and collecting the materials after drying, then transferring the materials into a ball milling tank again for ball milling and crushing, wherein the ball milling rotation speed is 300rpm/min, and the ball milling time is 1.5h, and finally obtaining the precursor powder material.
The sintering step was carried out as in example 1. And collecting the sintered material, sieving, and finally performing jet milling to obtain the sodium iron phosphate cathode material. The cell assembly and testing procedure was as in example 1.
Example 6
A method for synthesizing sodium iron phosphate serving as a positive electrode material for a sodium ion battery comprises the following steps:
150.82g of iron phosphate, 84.46g of anhydrous sodium acetate and 24.13g of sucrose are weighed and added into a ball milling tank for dry ball milling mixing, the rotating speed is 300rpm/min, and the ball milling time is 1 h; then adding 300g of water for high-energy wet ball milling; the ball milling speed is 500rpm/min, and the ball milling time is 8 h; after wet ball milling is finished, collecting slurry with fluidity, and drying in an air-blast drying oven at 60 ℃ for 24 h; and collecting the materials after drying, then transferring the materials into a ball milling tank again for ball milling and crushing, wherein the ball milling rotation speed is 300rpm/min, and the ball milling time is 1.5h, and finally obtaining the precursor powder material.
The sintering step was carried out as in example 1. And collecting the sintered material, sieving, and finally performing jet milling to obtain the sodium iron phosphate cathode material. The cell assembly and testing procedure was the same as in example 1.
The effects of the embodiment are as follows:
table 1 physicochemical indexes achieved by sodium iron phosphate in each example
Table 2 electrochemical test results of sodium iron phosphate in each example.
The above-mentioned embodiments are only used for explaining the inventive concept of the present invention, and do not limit the protection of the claims of the present invention, and any insubstantial modifications of the present invention using this concept shall fall within the protection scope of the present invention.
Claims (9)
1. A method for synthesizing a sodium iron phosphate cathode material for a sodium ion battery is characterized by comprising the following steps:
(1) mixing iron phosphate, a sodium source and a carbon source according to a certain proportion;
(2) adding a solvent for wet grinding until the grain size is ground to a target grain size;
(3) after grinding to a target particle size, drying the ground fluid slurry at a certain temperature to obtain precursor powder;
(4) pre-sintering the obtained precursor powder for a certain time under the protection of inert atmosphere;
(5) then, continuously heating the pre-sintered material under the protection of the same inert atmosphere to perform high-temperature sintering treatment for a certain time;
(6) and finally, crushing, grinding and sieving the material sintered at high temperature to obtain the sodium iron phosphate anode material.
2. The method for synthesizing the sodium iron phosphate as the positive electrode material for the sodium ion battery, according to claim 1, is characterized in that: the sodium source in the step (1) comprises at least one of sodium carbonate, sodium bicarbonate, sodium acetate, sodium benzoate or sodium ethoxide.
3. The method for synthesizing the sodium iron phosphate as the positive electrode material for the sodium ion battery, according to claim 2, is characterized in that: the carbon source in the step (1) comprises at least one of glucose, sucrose, polyethylene glycol, citric acid or polypropylene.
4. The method for synthesizing the sodium iron phosphate as the positive electrode material for the sodium ion battery, according to claim 3, is characterized in that: in the step (1), the molar ratio of the sodium source to the iron phosphate is (1.01-1.15): 1; the mass ratio of the carbon source to the iron phosphate is (0.1-0.3): 1.
5. the method for synthesizing the sodium iron phosphate as the positive electrode material for the sodium ion battery, according to claim 1, is characterized in that: the solvent adopted in the wet grinding in the step (2) comprises at least one of water, ethanol or ethylene glycol.
6. The method for synthesizing the sodium iron phosphate as the positive electrode material for the sodium ion battery, according to claim 1, is characterized in that: the target particle size of the wet grinding in the step (2) is 400-900 nm.
7. The method for synthesizing the sodium iron phosphate as the positive electrode material for the sodium ion battery, according to claim 1, is characterized in that: and (4) drying the slurry obtained in the step (3) in a forced air drying oven at the drying temperature of 50-200 ℃ for 8-24 hours.
8. The method for synthesizing the sodium iron phosphate serving as the positive electrode material of the sodium-ion battery according to claim 1, wherein the method comprises the following steps: and (4) presintering at 300-450 ℃ under the protection of inert atmosphere, wherein the heating rate is 2-5 ℃/min, and the heat preservation time is 1-6 h.
9. The method for synthesizing the sodium iron phosphate as the positive electrode material for the sodium ion battery, according to claim 1, is characterized in that: and (5) after the pre-sintering in the step (5) is finished, heating to 500-800 ℃ for high-temperature calcination, wherein the heating rate is 5-10 ℃/min, and the heat preservation time is 8-15 h.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115924878A (en) * | 2023-01-15 | 2023-04-07 | 西安交通大学 | Positive electrode material sodium iron phosphate for sodium ion battery and preparation method thereof |
| CN116495716A (en) * | 2023-06-26 | 2023-07-28 | 南昌大学 | Method for preparing sodium ion battery anode material by using waste lithium iron phosphate |
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