CN110828820B - Positive electrode material of potassium ion battery and preparation method thereof - Google Patents
Positive electrode material of potassium ion battery and preparation method thereof Download PDFInfo
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Abstract
A potassium ion battery anode material and a preparation method thereof, wherein the chemical formula of the anode material is KxMyFezPO4Wherein x is more than or equal to 0 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 1, and z is more than or equal to 0 and less than or equal to 1; m is a transition metal ion. The preparation method comprises the following specific steps: dissolving ferric nitrate nonahydrate, polyvinylpyrrolidone (K30) and other transition metal nitrates in deionized water according to a certain proportion to prepare a mixed solution, then drying the mixed solution, grinding the mixed solution into powder, placing the powder in a tube furnace, heating and preserving heat in argon atmosphere, and then heating and preserving heat in oxygen atmosphere to obtain iron-based transition metal oxide nanoparticles; weighing iron-based transition metal oxide nanoparticles and dipotassium hydrogen phosphate according to a proportion, grinding and mixing uniformly, then placing the powder in a tubular furnace for heat treatment in a nitrogen atmosphere, cleaning the obtained powder with deionized water, and drying in vacuum to obtain KxFeMPO4And (3) a positive electrode material. The invention has low production cost and strong repeatability, and is suitable for large-scale preparation; the obtained anode material has the advantages of stable structure, excellent performance and wide application prospect.
Description
Technical Field
The invention belongs to the field of potassium ion batteries, and particularly relates to a potassium ion battery positive electrode material and a preparation method thereof.
Background
With the continuous development of economy and the continuous progress of science and technology, how to optimize the utilization rate of renewable energy sources (such as wind energy and solar energy) has become the focus of global attention. The solution is to store renewable energy using low cost and environmentally friendly rechargeable batteries. In the current energy storage devices, lithium ion batteries cannot meet the requirement of large-scale energy storage due to the rising cost. Therefore, there is a need to develop new low cost energy storage battery technologies.
Potassium ions have received attention from researchers in recent years due to their electrochemical principles similar to those of lithium ion batteries. The content of potassium element in the earth's crust is about 350 times that of lithium element, and potassium element has similar physical and chemical properties to lithium, so that potassium ion batteries will have great advantages as batteries for large-scale energy storage applications, and at the same time, K/K + has a standard redox potential closest to Li/Li + so that potassium ion batteries can exhibit high energy density. However, the large radius of potassium ions makes it challenging to find a framework material that is stable in the result of reversible intercalation and deintercalation of potassium ions. Polyanionic transition metal phosphates of the general formula KxMyM’zPO4Wherein A is an alkali metal such as Li, Na, K; m' and M are transition metals, such as Fe, Co, Ni, Mn). The structure has a three-dimensional space network structure, and can provide an effective channel for the storage of potassium ions.
Disclosure of Invention
The invention aims to provide a potassium ion battery anode material with excellent performance and low cost and a preparation method thereof.
In order to achieve the purpose, the invention adopts the technical scheme that:
a potassium ion battery positive electrode material is characterized in that: the chemical formula of the anode material is KxMyFezPO4Wherein x is 0-1, y is 0-1, z is 0-1, and M is transition metal ion (including Co)2+，Ni2+，Mn2+One or more of the above); the anode material has an open three-dimensional network structure and can reversibly store potassium ions.
The preparation method of the potassium ion battery positive electrode material comprises the following steps:
a. weighing ferric nitrate nonahydrate, polyvinylpyrrolidone (K30) and other transition metal nitrates according to the mass ratio, dissolving the weighed raw materials in deionized water, ultrasonically stirring to form a uniform solution, completely drying and grinding into powder;
b. transferring the ground powder into a crucible, then placing the crucible into a tube furnace, heating to 800-850 ℃ at a heating rate of 4-6 ℃/min in an argon gas atmosphere, and preserving heat for 1-2 h; then cooling to 350-400 ℃ at a cooling rate of 4-6 ℃/min, introducing oxygen, and keeping the temperature for 2-3 hours to obtain iron-based transition metal oxide nanoparticles;
c. weighing iron-based transition metal oxide nanoparticles and dipotassium hydrogen phosphate according to a mass ratio, grinding and uniformly mixing the mixture, placing the mixture in a tubular furnace, heating the mixture to 700-900 ℃ at a heating rate of 4-6 ℃/min in a nitrogen atmosphere, preserving heat for 10-15 hours, cleaning and drying the obtained powder in vacuum to obtain KxMyFezPO4And (3) a positive electrode material.
Further, in the step a, the other transition metal nitrate is one or more of cobalt nitrate, nickel nitrate and manganese nitrate.
Further, the mass ratio of the ferric nitrate nonahydrate, the other transition metal nitrates and the polyvinylpyrrolidone in the step a is (1.4-1.8): (0.1-1.0): 1; the drying temperature was 80 ℃.
Furthermore, the flow of the oxygen introduced in the step b is adjusted to make the volume content of the argon gas be 40-60% and the volume content of the oxygen gas be 40-60%.
Further, the mass ratio of the iron-based transition metal oxide nanoparticles to the dipotassium hydrogen phosphate in the step c is 1: (4-8).
Further, the precipitate formed by the reaction is separated by centrifugation or filtration in the step c, and then the precipitate is washed with water or anhydrous ethanol.
Furthermore, the shape of the positive electrode material obtained in the step c is a hollow structure.
Compared with the prior art, the invention has the beneficial effects that:
1) the shape of the anode material is a hollow structure, and the volume expansion in the process of potassium ion extraction and insertion can be effectively inhibited, so that the potassium ions can be stably and reversibly stored.
2) By regulating and controlling the reactant proportion and the components, the anode material with different components can be prepared.
3) The method is simple and easy to operate and has low cost.
Drawings
Fig. 1 is a low-magnification TEM photograph of the hollow-structure potassium ion battery positive electrode material prepared by the present invention.
Fig. 2 is a high-power TEM photograph of the hollow-structure potassium-ion battery positive electrode material prepared by the present invention.
Detailed Description
Example one
Weighing polyvinylpyrrolidone (K30), ferric nitrate nonahydrate and cobalt nitrate hexahydrate according to the mass ratio of 1:1.4:0.1, dissolving the mixture in deionized water, performing ultrasonic stirring to prepare a uniform solution, then placing the solution in a drying box, keeping the temperature at 80 ℃ until the solution is completely dried, grinding the solution into powder, transferring the powder into a crucible, placing the crucible in a tubular furnace, heating the crucible to 850 ℃ in an argon atmosphere at the heating rate of 5 ℃/min, keeping the temperature for 2h, cooling the tubular furnace to 400 ℃, introducing oxygen, keeping the temperature for 2h, adjusting the flow rate to ensure that the volume ratio of the oxygen is 50 percent and the volume ratio of the argon is 50 percent, cooling the furnace, and collecting the product to obtain the iron-cobalt oxide nano-particles with the hollow structure. Then weighing iron-cobalt oxide nanoparticles and dipotassium hydrogen phosphate according to the mass ratio of 1:4, grinding and mixing uniformly, heating the powder to 800 ℃ at the heating rate of 5 ℃/min in the nitrogen atmosphere, preserving heat for 10 hours, collecting the product after cooling in a furnace, respectively cleaning the product with deionized water and absolute ethyl alcohol for 3 times, and finally drying the product in a vacuum drying oven at 80 ℃ overnight to obtain the hollow-structure KxCoyFezPO4And (3) a positive electrode material.
Example two
Weighing polyvinylpyrrolidone (K30), ferric nitrate nonahydrate and cobalt nitrate hexahydrate in a mass ratio of 1:1.5:0.3, dissolving the mixture in deionized water, ultrasonically stirring to prepare a uniform solution, then placing the solution in a drying oven, and keeping the temperature at 80 ℃ until the solution is completely driedDrying, grinding into powder, transferring the powder into a crucible, placing the crucible into a tubular furnace, heating to 850 ℃ in an argon atmosphere at the heating rate of 5 ℃/min, preserving heat for 2h, introducing oxygen for preserving heat for 2h after the temperature of the tubular furnace is reduced to 400 ℃, adjusting the flow rate to enable the volume ratio of the oxygen to be 50% and the volume ratio of the argon to be 50%, cooling the furnace, and collecting the product to obtain the iron-cobalt oxide nano-particles with the hollow structures. Then weighing iron-cobalt oxide nanoparticles and dipotassium hydrogen phosphate according to the mass ratio of 1:4, grinding and mixing uniformly, heating the powder to 800 ℃ at the heating rate of 5 ℃/min in the nitrogen atmosphere, preserving heat for 10 hours, collecting the product after cooling in a furnace, respectively cleaning the product with deionized water and absolute ethyl alcohol for 3 times, and finally drying the product in a vacuum drying oven at 80 ℃ overnight to obtain the hollow-structure KxCoyFezPO4And (3) a positive electrode material.
EXAMPLE III
Weighing polyvinylpyrrolidone (K30), ferric nitrate nonahydrate and manganese nitrate hexahydrate according to the mass ratio of 1:1.4:0.1, dissolving the mixture in deionized water, performing ultrasonic stirring to prepare a uniform solution, then placing the solution in a drying box, keeping the temperature at 80 ℃ until the solution is completely dried, grinding the solution into powder, transferring the powder into a crucible, placing the crucible in a tubular furnace, heating the crucible to 850 ℃ in an argon atmosphere at the heating rate of 5 ℃/min, keeping the temperature for 2h, cooling the tubular furnace to 400 ℃, introducing oxygen, keeping the temperature for 2h, adjusting the flow rate to ensure that the volume ratio of the oxygen is 50 percent and the volume ratio of the argon is 50 percent, cooling the furnace, and collecting the product to obtain the iron-manganese oxide nano-particles with the hollow structure. Then weighing the iron-manganese oxide nanoparticles and the dipotassium hydrogen phosphate according to the mass ratio of 1:4, grinding and mixing uniformly, heating the powder to 800 ℃ at the heating rate of 5 ℃/min in the nitrogen atmosphere, preserving heat for 10 hours, collecting the product after cooling the furnace, respectively cleaning the product with deionized water and absolute ethyl alcohol for 3 times, and finally drying the product in a vacuum drying oven at 80 ℃ overnight to obtain the hollow-structure KxMnyFezPO4And (3) a positive electrode material.
Example four
Weighing polyvinylpyrrolidone (K30), ferric nitrate nonahydrate and manganese nitrate hexahydrate in a mass ratio of 1:1.5:0.3, dissolving the mixture in deionized water, and ultrasonically stirringPreparing a uniform solution, then placing the solution in a drying box, keeping the temperature at 80 ℃ until the solution is completely dried, grinding the solution into powder, transferring the powder into a crucible, placing the crucible in a tubular furnace, heating the crucible to 850 ℃ in an argon atmosphere at the heating rate of 5 ℃/min, keeping the temperature for 2h, introducing oxygen for keeping the temperature for 2h after the temperature of the tubular furnace is reduced to 400 ℃, adjusting the flow rate to ensure that the volume ratio of the oxygen is 50 percent and the volume ratio of the argon is 50 percent, cooling the furnace, and collecting the product to obtain the iron-manganese oxide nanoparticles with the hollow structure. Then weighing the iron-manganese oxide nanoparticles and the dipotassium hydrogen phosphate according to the mass ratio of 1:4, grinding and mixing uniformly, heating the powder to 800 ℃ at the heating rate of 5 ℃/min in the nitrogen atmosphere, preserving heat for 15 hours, collecting the product after cooling the furnace, respectively cleaning the product with deionized water and absolute ethyl alcohol for 3 times, and finally drying the product in a vacuum drying oven at 80 ℃ overnight to obtain the hollow-structure KxMnyFezPO4And (3) a positive electrode material.
The above embodiments are only intended to illustrate the technical solution of the present invention and not to limit the same, and it should be understood by those skilled in the art that the specific embodiments of the present invention can be modified or substituted with equivalents with reference to the above embodiments, and any modifications or equivalents without departing from the spirit and scope of the present invention are within the scope of the claims to be appended.
Claims (9)
1. A potassium ion battery positive electrode material is characterized in that: the chemical formula of the anode material is KxMyFezPO4Wherein x is more than or equal to 0 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 1, z is more than or equal to 0 and less than or equal to 1, and M is transition metal ions; the anode material has an open three-dimensional network structure and can reversibly store potassium ions.
2. The potassium-ion battery positive electrode material according to claim 1, characterized in that: m is Co2+，Ni2+，Mn2+One or more of (a).
3. A method for preparing a positive electrode material of a potassium-ion battery according to claim 1 or 2, comprising the steps of:
a. weighing ferric nitrate nonahydrate, polyvinylpyrrolidone K30 and other transition metal nitrates according to the mass ratio, dissolving the weighed raw materials in deionized water, ultrasonically stirring to form a uniform solution, completely drying and grinding into powder;
b. transferring the ground powder into a crucible, then placing the crucible into a tube furnace, heating to 800-850 ℃ at a heating rate of 4-6 ℃/min in an argon gas atmosphere, and preserving heat for 1-2 h; then cooling to 350-400 ℃ at a cooling rate of 4-6 ℃/min, introducing oxygen, and keeping the temperature for 2-3 hours to obtain iron-based transition metal oxide nanoparticles;
c. weighing iron-based transition metal oxide nanoparticles and dipotassium hydrogen phosphate according to a mass ratio, grinding and uniformly mixing the mixture, placing the mixture in a tubular furnace, heating the mixture to 700-900 ℃ at a heating rate of 4-6 ℃/min in a nitrogen atmosphere, preserving heat for 10-15 hours, cleaning and drying the obtained powder in vacuum to obtain KxMyFezPO4And (3) a positive electrode material.
4. The method for preparing the positive electrode material of the potassium ion battery according to claim 3, wherein the other transition metal nitrate in the step a is one or more of cobalt nitrate, nickel nitrate and manganese nitrate.
5. The method for preparing the positive electrode material of the potassium ion battery according to claim 3, wherein the mass ratio of the ferric nitrate nonahydrate to the other transition metal nitrates to the polyvinylpyrrolidone in the step a is (1.4-1.8): (0.1-1.0): 1; the drying temperature was 80 ℃.
6. The method for preparing the positive electrode material of the potassium ion battery according to claim 3, wherein after the oxygen is introduced in the step b, the volume content of the argon in the mixed gas is adjusted to 40-60%, and the volume content of the oxygen is adjusted to 40-60%.
7. The method for producing a positive electrode material for a potassium-ion battery according to claim 3, wherein the mass ratio of the iron-based transition metal oxide nanoparticles to the dipotassium hydrogen phosphate in the step c is 1: (4-8).
8. The method for preparing a positive electrode material for a potassium ion battery according to claim 3, wherein the precipitate formed by the reaction is separated by centrifugation or filtration in the step c, and then the precipitate is washed with water or absolute ethanol.
9. The method for preparing the positive electrode material of the potassium ion battery according to claim 3, wherein the shape of the positive electrode material obtained in the step c is a hollow structure.
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| JP6947259B1 (en) * | 2020-08-20 | 2021-10-13 | 住友大阪セメント株式会社 | Positive electrode material for alkali metal ion batteries, positive electrode and alkali metal ion batteries |
| CN112279510B (en) * | 2020-10-20 | 2022-09-06 | 宁波大学 | Glass state-doped potassium fast ion conductor K2O.4 SiO2 and preparation method thereof |
| CN113871586A (en) * | 2021-09-07 | 2021-12-31 | 武汉理工大学 | Controllable manganese-based layered oxide electrode material and preparation method and application thereof |
| CN114883522B (en) * | 2022-04-20 | 2024-05-28 | 南京邮电大学 | High-entropy-like multi-element layered transition metal oxide positive electrode material, and preparation method and application thereof |
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