CN115966687A - Layered sodium-ion battery positive electrode material and preparation method and application thereof - Google Patents
Layered sodium-ion battery positive electrode material and preparation method and application thereof Download PDFInfo
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Abstract
The invention provides a layered sodium-ion battery anode material and a preparation method and application thereof, wherein the chemical formula of the layered sodium-ion battery anode material is Na a Mg b Cu x Fe y Mn z O 2 Wherein a +2x, 3y, 4z, 2b, 4 is more than or equal to 0.85 and less than or equal to 0.95 of a, more than or equal to 0.05 and less than or equal to 0.1 of b, x>0，y>0，z>The valence of 0,Mn is +4, and the invention dopes a proper amount of magnesium in the sodium ion anode material, which can not only lead trivalent manganese in the materialCompletely oxidized into tetravalent manganese and can inhibit Mn at low potential 4+ Reduction of (2).
Description
Technical Field
The invention belongs to the technical field of sodium ion batteries, and relates to a layered sodium ion battery positive electrode material, and a preparation method and application thereof.
Background
One of the key challenges faced by the practical application of layered oxide positive electrode materials for sodium ion batteries is to improve the cycling stability of the material. Na (Na) + Radius of
Specific to Li + Radius>
Greater, na + Complex phase changes caused by the detachment and the embedding usually cause relatively poor cycle stability of the composite material, and meanwhile, the rate performance of the composite material is also influenced; therefore, it is very necessary to search for a positive electrode material for a sodium ion battery having a high rate and long cycle stability.
Element doping has been widely used to improve the electrochemical performance of transition metal oxide layered positive electrode materials. However, due to the differences in ionic radius, valence state and electrochemical activity, the mechanism of action and improvement of the introduction of the doping element is still not completely understood. Understanding how doping elements adjust crystal and electronic structures to improve electrochemical performance is very important for revealing structure-performance relationships and for reasonably designing high-performance cathode materials. Mg (Mg) 2+ Doping has proven to be an effective means for effectively improving the performance of the layered oxide cathode material.
CN115611319A discloses a sodium ion battery copper-iron-manganese-based positive electrode material and a preparation method thereof, the preparation method comprises the following steps: s1, dissolving a sodium source, a copper source, an iron source, a manganese source and a doping source M in deionized water, adding fuel, and uniformly stirring to obtain a mixed solution; s2, placing the mixed solution into a muffle furnace for self-propagating combustion, wherein the self-propagating combustion is to heat the muffle furnace to 300-500 ℃, then placing the mixed solution into the muffle furnace, and violently combusting the mixed solution in an oxygen-containing atmosphere for 1-60min to obtain a precursor; and S3, calcining the precursor at the temperature of 600-900 ℃ for 1-10h to obtain the material.
CN109817974A discloses a sodium ion nickel manganese magnesium iron quaternary anode material and a preparation method thereof, wherein the chemical molecular formula of the anode material is Na x Ni y Mn z Mg 0.9-y-z Fe 0.1 O 2 Wherein x is more than or equal to 1 and more than or equal to 0.67, y is more than or equal to 0.5 and more than or equal to 0.2, and z is more than or equal to 0.7 and more than or equal to 0.3.
In the above scheme, although doping with Mg can improve the performance, mg can be added when the Mg is added 2+ During doping, although the cycle stability is further improved, the specific discharge capacity is increased along with Mg 2+ Increase and decrease of doping amount, especially P 2 -Na 2/ 3 Mn 0.8 Mg 0.2 O 2 Only a specific discharge capacity of about 150mAh/g can be provided. But P is 2 -Na 2/3 Mn 0.72 Mg 0.28 O 2 Shows higher reversible capacity of 220mAh/g, and is deduced to be part O 2- The participation in electrochemical reaction contributes to partial capacity, and similar behavior exists in lithium-rich materials. But the cycling stability is poor, and the capacity is only 150mAh/g after 30 weeks of cycling, which is far from the requirement of application.
Disclosure of Invention
The invention aims to provide a layered sodium-ion battery positive electrode material and a preparation method and application thereof 4+ Reduction of (2).
In order to achieve the purpose, the invention adopts the following technical scheme:
in a first aspect, the invention provides a layered sodium-ion battery cathode material, the chemical formula of which is Na a Mg b Cu x Fe y Mn z O 2 Wherein a +2x +3y +4z + 2b=4and 0.85 a is not less than 0.95，0.05≤b≤0.1，x>0，y>0，z>The valence of 0,Mn is + 4.
In the layered sodium-ion battery anode material, the valence of a transition metal element Mn is +4, and low-valence Mg is used 2+ Substituted Mn 3+ High spin Mn due to charge compensation can be reduced 3+ And alleviate the Jahn-Teller effect, mg 2+ Doping can raise O 3 -P 3 Dynamic performance of phase transition process, and simultaneously restraining Mn at low potential 4+ While being Mg 2+ Improve Cu 3+ /Cu 2+ The electrochemical activity of the redox couple can improve the Na extraction and insertion quantity and the average reaction potential.
Preferably, the median particle diameter D50 of the layered sodium-ion battery positive electrode material is 5 to 15 μm, for example: 5 μm, 8 μm, 10 μm, 12 μm, 15 μm, or the like.
Preferably, the layered sodium-ion battery positive electrode material is O 3 A layered oxide positive electrode material.
In a second aspect, the present invention provides a method for preparing the layered sodium-ion battery positive electrode material according to the first aspect, wherein the preparation method comprises the following steps:
(1) Mixing a copper source, an iron source, a manganese source, a magnesium source and a solvent to obtain a mixed salt solution;
(2) Adding the mixed salt solution, a precipitator and a complexing agent into a reaction container for reaction to obtain a precursor;
(3) And mixing a sodium source with the obtained precursor, carrying out heat treatment, and rapidly cooling to obtain the layered sodium-ion battery anode material.
In the preparation method, for the Mn-containing layered oxide, the cooling speed is accelerated after sintering, which is beneficial to forming more Mn 3+ And the metastable phase with higher sodium content between layers improves the reversible capacity of the electrode material.
Preferably, the copper source of step (1) comprises any one of copper nitrate, copper acetate or copper sulfate or a combination of at least two thereof.
Preferably, the iron source comprises any one of ferric nitrate, ferric acetate, ferric citrate or ferrous sulfate or a combination of at least two of them.
Preferably, the manganese source comprises any one of manganese acetate, manganese nitrate or manganese sulphate or a combination of at least two thereof.
Preferably, the magnesium source comprises any one of magnesium sulfate, magnesium chloride or magnesium nitrate or a combination of at least two thereof.
Preferably, the total metal ion concentration of the mixed salt solution is 1.5 to 2mol/L, for example: 1.5mol/L, 1.6mol/L, 1.7mol/L, 1.8mol/L, 1.9mol/L or 2mol/L, etc.
Preferably, the precipitating agent comprises a sodium hydroxide solution.
Preferably, the mass concentration of the precipitant is 30 to 34%, for example: 30%, 31%, 32%, 33%, 34%, etc.
Preferably, the complexing agent comprises aqueous ammonia.
Preferably, the mass concentration of the complexing agent is 14 to 18%, for example: 14%, 15%, 16%, 17%, 18%, etc.
Preferably, the temperature of the reaction of step (2) is from 55 to 60 ℃, for example: 55 deg.C, 56 deg.C, 57 deg.C, 58 deg.C, 59 deg.C or 60 deg.C.
Preferably, the pH of the reaction is between 10 and 10.5, for example: 10. 10.1, 10.2, 10.3, 10.4, 10.5, etc.
Preferably, nitrogen is introduced and stirring is carried out during the reaction.
Preferably, the stirring speed is 200 to 300rpm, for example: 200rpm, 220rpm, 250rpm, 280rpm, 300rpm, or the like.
Preferably, the reaction is followed by an air-blast drying treatment.
Preferably, the powder tabletting treatment is performed on the mixed powder of the precursor and the sodium source before the heat treatment in the step (3).
Preferably, the sodium source comprises sodium carbonate sodium nitrate, sodium acetate, sodium citrate or a combination of any one or at least two of sodium carbonate.
Preferably, the temperature of the heat treatment is 800 to 900 ℃, for example: 800 deg.C, 820 deg.C, 850 deg.C, 880 deg.C or 900 deg.C.
Preferably, the heat treatment time is 12 to 18 hours, for example: 12h, 13h, 15h, 16h or 18h and the like.
In a third aspect, the present invention provides a positive electrode plate, which comprises the layered sodium-ion battery positive electrode material according to the first aspect.
In a fourth aspect, the invention provides a sodium-ion battery, which comprises the positive pole piece of the third aspect.
Compared with the prior art, the invention has the following beneficial effects:
(1) The invention uses low-price Mg 2+ Substituted Mn 3+ Can reduce Mn 3+ Jahn-Teller effect of (1), mg 2+ Doping can raise O 3 -P 3 Dynamic performance of phase transformation process, and simultaneously restraining Mn at low potential 4+ Reduction of (2) with Mg 2+ Improve Cu 3+ /Cu 2+ The electrochemical activity of the redox couple can improve the Na extraction and insertion quantity and the average reaction potential.
(2) Mg of the present invention 2+ Doping can reduce the structural and volume change of crystal lattice, inhibit the occurrence of irreversible phase change, and simultaneously Mg 2+ Doping can enlarge the interlayer spacing and not only contribute to Na + The diffusion of (a) improves rate capability and further mitigates lattice strain caused by sodium extraction and insertion.
(3) The battery prepared from the positive electrode material has a reversible specific capacity of over 114mAh/g at the first cycle of 0.2C, a capacity retention rate of over 85% at the cycle of 200 at the cycle of 0.2C, a capacity retention rate of over 72% at the cycle of 500 at the cycle of 1C and Na + The reversible stripping and embedding amount can reach more than 0.46.
Detailed Description
The technical solution of the present invention is further described below by way of specific embodiments. It should be understood by those skilled in the art that the examples are only for the understanding of the present invention and should not be construed as the specific limitations of the present invention.
Example 1
The embodiment provides a layered sodium-ion battery cathode material, and a preparation method of the layered sodium-ion battery cathode material comprises the following steps:
(1) Mixing CuSO 4 、Fe 2 (SO 4 ) 3 、Mn 2 (SO 4 ) 3 And MgSO 4 According to Mg: cu: fe: mixing the deionized water with a molar ratio of Mn = 0.08;
(2) Respectively adding the solution A, the solution B and the solution C into a crystallization reaction kettle, setting the temperature of continuous overflow reaction as 58 ℃, setting the stirring speed as 200rpm, maintaining the pH value at 10.2, introducing nitrogen during reaction, and drying the obtained material in an electric heating constant temperature air blast drying box at 60 ℃ for 12 hours to obtain a precursor;
(3) Na is mixed with 2 CO 3 Tabletting the powder which is uniformly mixed with the precursor powder in proportion, carrying out heat treatment in a muffle furnace at the air atmosphere of 850 ℃ for 16h, and then accelerating to cool to obtain the layered sodium-ion battery anode material, wherein the chemical formula of the anode material is Na 0.90 Mg 0.08 Cu 0.22 Fe 0.30 Mn 0.40 O 2 。
Example 2
The embodiment provides a layered sodium-ion battery cathode material, and a preparation method of the layered sodium-ion battery cathode material comprises the following steps:
(1) Mixing CuSO 4 、Fe 2 (SO 4 ) 3 、Mn 2 (SO 4 ) 3 And MgSO 4 According to Mg: cu: fe: mixing the solution with deionized water according to a molar ratio of Mn = 0.06;
(2) Respectively adding the solution A, the solution B and the solution C into a crystallization reaction kettle, setting the temperature of continuous overflow reaction as 59 ℃, setting the stirring speed as 250rpm, maintaining the pH value as 10.3, introducing nitrogen during the reaction, and drying the obtained material in an electric heating constant-temperature air blast drying oven at 60 ℃ for 12 hours to obtain a precursor;
(3) Mixing Na 2 CO 3 Tabletting the powder which is uniformly mixed with the precursor powder in proportion, carrying out heat treatment in a muffle furnace at the air atmosphere of 880 ℃ for 16h, and accelerating to cool to obtain the layered sodium-ion battery anode material, wherein the chemical formula of the anode material is Na 0.92 Mg 0.06 Cu 0.24 Fe 0.4 Mn 0.3 O 2 。
Example 3
The present example is different from example 1 only in that the molar ratio of magnesium ions in the material is controlled to be 0.03 (i.e., b = 0.03), and other conditions and parameters are exactly the same as those of example 1.
Example 4
This example is different from example 1 only in that the molar ratio of magnesium ions in the material is controlled to be 0.12 (i.e., b = 0.12), and other conditions and parameters are exactly the same as those in example 1.
Example 5
This example is different from example 1 only in that the temperature of the heat treatment in step (3) is 750 ℃, and other conditions and parameters are exactly the same as those of example 1.
Example 6
This example is different from example 1 only in that the temperature of the heat treatment in step (3) is 950 ℃, and other conditions and parameters are exactly the same as those of example 1.
Comparative example 1
The comparative example is different from example 1 only in that magnesium is not added, other conditions and parameters are completely the same as example 1, and the chemical formula of the cathode material is Na 0.90 Cu 0.22 Fe 0.30 Mn 0.48 O 2 。
And (4) performance testing:
the sodium ion positive electrode materials obtained in examples 1 to 6 and comparative example 1 were used as positive electrode active materials, metal sodium was used as a negative electrode, a glass fiber membrane was used as a separator, and 1M NaClO was used 4 Electrolyte of/EC/DMC/PC in argon glove boxAssembled into a button cell of the CR2032 type. The positive pole piece is an active substance, and the mass ratio of acetylene black to PVDF dissolved in NMP is 70:20:10, uniformly mixing, coating on an aluminum foil, and cutting into 8 x 8mm 2 And (5) placing the large and small pole pieces in a vacuum oven at 110 ℃ for 10h. The assembled button cell was placed on LAND for constant current charge and discharge testing, with the test results shown in Table 1:
TABLE 1
As can be seen from Table 1, in the case of the battery obtained in the embodiment 1-2, the reversible specific capacity at the first cycle of 0.2C of the battery prepared from the positive electrode material of the present invention can be more than 114mAh/g, the capacity retention rate at the cycle of 0.2C and 200 can be more than 85%, the capacity retention rate at the cycle of 1C and 500 can be more than 72%, and Na can be added + The reversible stripping and embedding amount can reach more than 0.46.
Compared with the embodiment 1 and the embodiment 3-4, the layered sodium-ion battery positive electrode material has the advantages that the doping amount of magnesium influences the performance of the layered sodium-ion battery positive electrode material, the doping amount of magnesium is controlled to be 0.05-0.1, the layered sodium-ion battery positive electrode material has good performance, if the doping amount of magnesium is too high, the capacity of the material is obviously reduced, the performance of the material is reduced, and if the doping amount of magnesium is too low, trivalent manganese cannot be effectively and completely oxidized into tetravalent manganese in the subsequent heat treatment process, and Mn is caused 3+ The Jahn-Teller effect of (1) occurs.
Compared with the examples 5 to 6, in the preparation process of the layered sodium-ion battery positive electrode material, the performance of the layered sodium-ion battery positive electrode material is influenced by the heat treatment temperature, the performance of the layered sodium-ion battery positive electrode material prepared by controlling the heat treatment temperature to be 800-900 ℃ is better, if the heat treatment temperature is too high, the oxidation degree of the material is too high, the material is cracked, the safety performance of the material is reduced, and if the heat treatment temperature is too low, trivalent manganese cannot be completely oxidized into tetravalent manganese, and Mn is caused 3+ The Jahn-Teller effect of (1) occurs.
As can be seen from comparison of example 1 with comparative example 1, the present invention uses low-priced Mg 2+ Substituted Mn 3+ Can reduce Mn 3+ Jahn-Teller effect of (1), mg 2+ Doping can raise O 3 -P 3 Dynamic performance of phase transition process, and simultaneously restraining Mn at low potential 4 + Reduction of (2) with Mg 2+ Improve Cu 3+ /Cu 2+ The electrochemical activity of the redox couple can improve the Na extraction and insertion quantity and the average reaction potential.
Mg 2+ Doping with P-O 3 -Na 0.90 Mg 0.08 Cu 0.22 Fe 0.30 Mn 0.40 O 2 Crystal structure and electrochemical performance are affected. In the voltage range of 2.4-3.9V, O 3 -Na 0.90 Mg 0.08 Cu 0.22 Fe 0.30 Mn 0.40 O 2 Corresponding to 0.42 Na + Reversible deintercalation and intercalation 3 -Na 0.90 Cu 0.22 Fe 0.30 Mn 0.48 O 2 Corresponding to 0.32 Na + Can be reversibly removed and inserted. In the voltage range of 2.4-4.0V, O 3 -Na 0.90 Mg 0.08 Cu 0.22 Fe 0.30 Mn 0.40 O 2 The reversible specific capacity is 116mAh/g and corresponds to 0.465 Na + Reversible pull-out and pull-in; and O is 3 -Na 0.90 Cu 0.22 Fe 0.30 Mn 0.48 O 2 The reversible specific capacity is only 90m Ah/g, corresponding to 0.36 Na + Reversible expulsion and insertion.
The applicant declares that the above description is only a specific embodiment of the present invention, but the scope of the present invention is not limited thereto, and it should be understood by those skilled in the art that any changes or substitutions that can be easily conceived by those skilled in the art within the technical scope of the present invention disclosed herein fall within the scope and disclosure of the present invention.
Claims (10)
1. The layered sodium-ion battery positive electrode material is characterized in that the chemical formula of the layered sodium-ion battery positive electrode material is Na a Mg b Cu x Fe y Mn z O 2 Wherein, a +2x, 3y, 4z +2b =4 and 0.85. Ltoreq. A.ltoreq.0.95, 0.05. Ltoreq. B.ltoreq.0.1, x>0，y>0，z>The valence of 0,Mn is + 4.
2. The layered sodium-ion battery positive electrode material according to claim 1, wherein the layered sodium-ion battery positive electrode material has a median particle diameter D50 of 5 to 15 μm.
3. The layered sodium-ion battery positive electrode material according to claim 1 or 2, wherein the layered sodium-ion battery positive electrode material is O 3 A layered oxide positive electrode material.
4. A method for preparing the layered sodium-ion battery positive electrode material according to any one of claims 1 to 3, wherein the preparation method comprises the following steps:
(1) Mixing a copper source, an iron source, a manganese source, a magnesium source and a solvent to obtain a mixed salt solution;
(2) Adding the mixed salt solution, a precipitator and a complexing agent into a reaction container for reaction to obtain a precursor;
(3) And mixing a sodium source with the obtained precursor, carrying out heat treatment, and rapidly cooling to obtain the layered sodium-ion battery anode material.
5. The method according to claim 4, wherein the copper source in the step (1) comprises any one of copper nitrate, copper acetate or copper sulfate or a combination of at least two thereof;
preferably, the iron source comprises any one of ferric nitrate, ferric acetate, ferric citrate or ferrous sulfate or a combination of at least two of them;
preferably, the manganese source comprises any one of manganese acetate, manganese nitrate or manganese sulphate or a combination of at least two thereof;
preferably, the magnesium source comprises any one of magnesium sulphate, magnesium chloride or magnesium nitrate, or a combination of at least two thereof;
preferably, the total metal ion concentration of the mixed salt solution is 1.5-2 mol/L.
6. The method according to claim 4 or 5, wherein the precipitant in the step (2) comprises a sodium hydroxide solution;
preferably, the mass concentration of the precipitant is 30-34%;
preferably, the complexing agent comprises aqueous ammonia;
preferably, the mass concentration of the complexing agent is 14-18%.
7. The method according to any one of claims 4 to 6, wherein the temperature of the reaction in the step (2) is 55 to 60 ℃;
preferably, the pH of the reaction is 10 to 10.5;
preferably, nitrogen is introduced and stirred during the reaction;
preferably, the stirring speed is 200-300 rpm;
preferably, the reaction is followed by a forced air drying process.
8. The production method according to any one of claims 4 to 7, wherein the powder mixture of the precursor and the sodium source is subjected to a powder tableting treatment before the heat treatment in step (3);
preferably, the sodium source comprises any one of sodium carbonate, sodium nitrate, sodium acetate, sodium citrate or sodium carbonate, or a combination of at least two thereof;
preferably, the temperature of the heat treatment is 800-900 ℃;
preferably, the time of the heat treatment is 12 to 18 hours.
9. A positive electrode sheet, characterized in that the positive electrode sheet comprises the layered sodium-ion battery positive electrode material according to any one of claims 1 to 3.
10. A sodium-ion battery comprising the positive electrode sheet according to claim 9.
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN117303466A (en) * | 2023-11-28 | 2023-12-29 | 广东省中科海钠科技有限责任公司 | Layered positive electrode material, preparation method thereof and positive electrode plate |
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