CN111446434A - Metaphosphate modified anode material and preparation method thereof - Google Patents
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Abstract
The invention belongs to the field of anode materials, and particularly relates to a metaphosphate modified anode material and a preparation method of the anode materialaNibCocMndRxO2Wherein a is more than or equal to 1.0 and less than or equal to 1.9, b is more than or equal to 0.5 and less than or equal to 0.95, c is more than or equal to 0.05 and less than or equal to 0.25, d is more than or equal to 0 and less than or equal to 0.3, x is more than or equal to 0 and less than or equal to 0.15, and b + c + d + x is 1, and metaphosphate is added for doping and cladding. The invention utilizes metaphosphate to dope and coat the ternary anode material, the metal cation and transition metal thereofThe cation can be coated on the surface of the material and can be embedded into the material structure, so that the cycle performance of the material can be improved, and the capacity of the material can be improved.
Description
Technical Field
The invention belongs to the field of anode materials, and particularly relates to a metaphosphate modified anode material and a preparation method of the anode material.
Background
In recent years, layered NCM ternary materials have been possible to replace L iCoO due to their high specific capacity, excellent cycling performance and excellent safety2Thus, the anode material becomes one of the hot spots of research in the industry. However, under the condition of high voltage, due to the aggravation of side reactions of the NCM ternary material and the electrolyte, the defects of fast capacity attenuation, reduced cycling stability and the like still exist, and the application of the NCM ternary material in the field of high-energy-density lithium ion batteries is limited. In order to further improve the rate capability and cycle performance of the ternary cathode material, especially the high nickel cathode material, it is usually necessary to perform doping and cladding during the synthesis of the ternary cathode material, so as to improve the rate capability and cycle performance of the material.
The surface residual alkali is L i existing on the surface of ternary material2O、LiOH、Li2CO3The residual on the surface of the ternary material is not favorable for the performance of the ternary material no matter how much, so that the surface impedance of the material/electrolyte is increased, the battery bulges and the electrochemical performance is reduced; and the viscosity of the slurry in the battery processing process is unstable directly, and even the pole piece coating cannot be carried out.
In the actual production process, because the lithium salt is volatilized in a certain amount in the high-temperature calcination process, the L i/M ratio is slightly improved in the actual batching process, and the lithium salt lost in the calcination process is compensated by using proper excess lithium salt, although the ratio of L i/M is optimized, trace L i is excessive, and once the lithium salt is mixed with H in the air2O and CO2Contact, L iOH and L i will form2CO3And the residual alkali amount on the surface of the material is increased. Too high a content of residual alkali on the surface of the positive electrode material may negatively affect the electrochemical performance, increase the irreversible capacity loss, and simultaneously decrease the cycle performance. In order to improve the cycle performance of the material, the material can be coated and reducedInfluence of residual alkali on the cycle performance of the material surface.
With respect to the positive electrode material for lithium ion batteries prepared by the conventional method, the capacity is still low and the cycle performance is not ideal, and therefore, improvements in the improvement of the capacity and cycle performance are required.
Disclosure of Invention
In order to solve the technical problems, the invention provides a metaphosphate modified anode material which can dope and coat the material and reduce the influence of the residual alkali on the cycle performance of the material surface, and the molecular formula of the anode material is L iaNibCocMndRxO2Wherein a is more than or equal to 1.0 and less than or equal to 1.9, b is more than or equal to 0.5 and less than or equal to 0.95, c is more than or equal to 0.05 and less than or equal to 0.25, d is more than or equal to 0 and less than or equal to 0.3, x is more than or equal to 0 and less than or equal to 0.15, and b + c + d + x is 1;
can be used as the anode material L iaNibCocMndRxO2Adding metaphosphate for doping coating.
In view of the problems mentioned in the background art, the surface of the ternary material can be modified by adding oxides or phosphates of magnesium, aluminum, titanium, zirconium, some rare earth metals and the like, so that the material is mechanically separated from the electrolyte, the side reaction of the material and the electrolyte is reduced, and the dissolution of metal ions is inhibited. The metaphosphate is doped and coated with the ternary cathode material, and metal cations and transition metal cations of the metaphosphate can be coated on the surface of the material and can be embedded into the structure of the material, so that the cycle performance of the material can be improved, and the capacity of the material can be improved.
In the actual production process, because the lithium salt is volatilized in a certain amount in the high-temperature calcination process, the L i/M ratio is slightly improved in the actual batching process, and the lithium salt lost in the calcination process is compensated by using proper excess lithium salt, although the ratio of L i/M is optimized, trace L i is excessive, and once the lithium salt is mixed with H in the air2O and CO2Contact, L iOH and L i will form2CO3And the residual alkali amount on the surface of the material is increased. Too high a content of residual alkali on the surface of the positive electrode material may negatively affect the electrochemical performance, increase the irreversible capacity loss, and simultaneously decrease the cycle performance. To improve the materialThe cycle performance can coat the material, and the influence of the residual alkali on the surface of the material on the cycle performance is reduced.
The metaphosphate is Al (PO)3)3、Ba(PO3)2、Ca(PO3)2、Mg(PO3)2、NaPO3、KPO3、LiPO3、Zn(PO3)2、Sr(PO3)2、Nd(PO3)3、Nb(PO3)5、La(PO3)3、Y(PO3)3At least one of (1).
The preparation method of the metaphosphate modified cathode material comprises the following steps:
(1) selecting a precursor of a lithium ion battery anode material according to a target product, mechanically mixing the precursor, lithium salt and metaphosphate in a mixer, and uniformly mixing until no white point appears visually;
(2) putting the uniformly mixed material in the step (1) into a sagger, and carrying out high-temperature calcination treatment in an oxygen atmosphere;
(3) cooling the fired material to below 100 ℃, taking out, crushing and sieving;
(4) placing the sieved material in a coating machine, and adding a trace amount of metaphosphate for coating treatment;
(5) putting the coated material into a muffle furnace, and carrying out heat preservation treatment in an oxygen atmosphere;
(6) and taking out the materials after the materials are cooled to below 100 ℃, and crushing and sieving the materials.
Preferably, (1) weighing a precursor, a lithium salt and a metaphosphate, wherein the molar ratio of the lithium salt to the precursor is 1.0-1.09, the molar ratio of the metaphosphate to the precursor is 0.001-0.15, mechanically mixing the precursor, the lithium salt and the metaphosphate in a mixer according to a certain mass ratio, and uniformly mixing until no white spot appears visually;
(2) putting the uniformly mixed materials into a sagger, and firing for 5-25 h at 715-935 ℃ in an oxygen atmosphere with the volume concentration of 21-100%;
(3) when the temperature is reduced to below 100 ℃, taking out the fired material, crushing by a crusher, and sieving;
(4) putting the sieved material into a mechanical fusion machine, and adding 0-0.3% of metaphosphate for coating;
(5) placing the coated material into an atmosphere muffle furnace, and sintering for 5-16 h at 300-800 ℃ in an oxygen atmosphere with the volume concentration of 21-100%;
(6) taking out the materials when the temperature is reduced to below 100 ℃, crushing and sieving.
Preferably, the preparation method of the metaphosphate modified cathode material comprises the following steps:
(1) weighing a precursor, lithium salt and metaphosphate, wherein the ratio of the lithium salt to the precursor is 1.0-1.09, the molar ratio of the metaphosphate to the precursor is 0.001-0.15, mechanically mixing the precursor, the lithium salt and the metaphosphate in a mixer according to a certain mass ratio, and uniformly mixing until no white point appears visually;
(2) putting the uniformly mixed materials into a sagger, putting the sagger into an atmosphere furnace, and firing the sagger for 5-25 hours at 715-935 ℃ in an oxygen atmosphere with the volume concentration of 21-100%;
(3) when the temperature is reduced to below 100 ℃, taking out the fired material, crushing the fired material by a crusher, and sieving the crushed material;
(4) loading the sieved material into a mechanical fusion machine, and adding 0-0.3% of metaphosphate for coating;
(5) placing the coated material into an atmosphere muffle furnace, and sintering for 5-16 h at 300-800 ℃ in an oxygen atmosphere with the volume concentration of 21-100%;
(6) taking out the materials when the temperature is reduced to below 100 ℃, and crushing and sieving the materials.
The method has the advantages that the anode material prepared by the method is doped when metaphosphate is used for preparing the ternary anode material so as to improve the capacity of the ternary anode material, and the material is coated, metal cations and transition metal cations can be coated on the surface of the material and can be embedded into the structure of the material during coating, so that the cycle performance of the material can be improved, and the capacity of the material can be improved.
The results demonstrate that the material obtained by the invention has excellent cycle performance and high capacity. Repeated verification and comparison of multiple experiments show that the 1C gram capacity of the doped coating material is improved by 2-7 mAh/g compared with that before modification when the 1C gram capacity of the doped coating material is exerted by 192-197 mAh/g; the capacity retention rate is more than 99.8% after 100 weeks of 1C charge-discharge circulation at normal temperature.
Drawings
FIG. 1 shows 1C charge-discharge cycle properties at room temperature for Y1, Y2, Y3, and Y4;
FIG. 2 shows the first charging and discharging curves of Y1, Y2, Y3 and Y4.
Detailed Description
In order that those skilled in the art will better understand the present invention, the inventors will further describe and illustrate the present invention by the following specific examples, but do not limit the present invention.
Example 1
Metaphosphate modified anode material Y1The preparation method comprises the following steps:
(1) selecting the precursor as Ni0.66Co0.12Mn0.12(OH)2Corresponding precursor, lithium carbonate and Y (PO) were weighed at L i/M1.05 and Y/M0.0053)3Mechanically mixing in a mixer until no white point is visible;
(2) putting the uniformly mixed materials into a sagger, and calcining for 12 hours at 915 ℃ in an oxygen atmosphere with the volume concentration of 99%;
(3) pulverizing the calcined material, sieving, adding Y (PO) in an amount of 0.15 wt% of the coating3)3Coating in a coating machine;
(4) and (3) placing the coated material in an atmosphere muffle furnace, preserving the heat for 7h at 650 ℃ in an oxygen atmosphere with the volume concentration of 21%, naturally cooling to below 100 ℃, taking out, crushing and sieving.
The percentage in the present invention is generally a mass percentage unless otherwise specified.
Example 2
Metaphosphate modified anode material Y2The preparation of (1) comprises the following stepsThe method comprises the following steps:
(1) selecting the precursor as Ni0.66Co0.12Mn0.12(OH)2Corresponding precursor, lithium carbonate and Y (PO) were weighed at L i/M1.05 and Y/M0.0053)3Mechanically mixing in a mixer until no white point is visible;
(2) and putting the uniformly mixed materials into a sagger, calcining for 12 hours at 915 ℃ in an oxygen atmosphere with the volume concentration of 99%, naturally cooling to be below 100 ℃, taking out, crushing and sieving.
Example 3
Metaphosphate modified anode material Y3The preparation method comprises the following steps:
(1) selecting the precursor as Ni0.66Co0.12Mn0.12(OH)2Weighing corresponding precursors and lithium carbonate according to L i/M of 1.05, and mechanically mixing in a mixer until no white spot appears visually;
(2) loading the uniformly mixed materials into a sagger, calcining for 12 hours at 915 ℃ in an oxygen atmosphere with the volume concentration of 99%, naturally cooling to be below 100 ℃, taking out, crushing and sieving;
(3) adding Y (PO) into the sieved material according to the coating amount of 0.15 wt%3)3Coating in a coating machine;
(4) and (3) putting the coated material into a sagger, preserving the heat for 7 hours at 650 ℃ in an oxygen atmosphere with the volume concentration of 21%, naturally cooling to below 100 ℃, taking out, crushing and sieving.
Example 4
Metaphosphate modified anode material Y4The preparation method comprises the following steps:
(1) selecting the precursor as Ni0.66Co0.12Mn0.12(OH)2Weighing corresponding precursors and lithium carbonate according to L i/M of 1.05, and mechanically mixing in a mixer until no white spot appears visually;
(2) and putting the uniformly mixed materials into a sagger, calcining for 12 hours at 915 ℃ in an oxygen atmosphere with the volume concentration of 99%, naturally cooling to be below 100 ℃, taking out, crushing and sieving.
The material Y prepared in the above 4 examples was mixed1、Y2、Y3、Y4Respectively mixing the above components with Super P and a binder PVDF according to a mass ratio of 92: 3: 5, uniformly mixing the mixture to be used as a positive electrode material, and using the metal lithium as a negative electrode to assemble the button cell. As shown in attached figures 1 and 2, an electrochemical test is carried out at 25 ℃, within a voltage range of 2.8-4.3V and under a multiplying power of 0.1C, and Y is1The discharge specific capacity reaches 192-197 mAh/g, and the capacity retention rate is maintained after 1C charge-discharge circulation for 100 weeks at normal temperature>99.8％；Y2Capacity retention rate after 100 weeks of 1C charge-discharge cycle at room temperature>97％；Y3Capacity retention rate after 100 weeks of 1C charge-discharge cycle at room temperature>99％；Y4Capacity retention rate after 100 weeks of 1C charge-discharge cycle at room temperature>92％。
The experiments prove that the material obtained by the invention has excellent cycle performance and high capacity. Repeated verification and comparison of multiple experiments show that the 0.1C gram capacity of the doped coating material is improved by 2-7 mAh/g compared with that before modification; the capacity retention rate is more than 99.8 percent after 100 weeks of 1C charge-discharge circulation at normal temperature, the capacity retention rate is higher, the circulation performance of the material is effectively improved, and the capacity of the material is also improved.
Claims (10)
1. The metaphosphate modified cathode material is characterized in that the cathode material L iaNibCocMndRxO2Wherein a is more than or equal to 1.0 and less than or equal to 1.9, b is more than or equal to 0.5 and less than or equal to 0.95, c is more than or equal to 0.05 and less than or equal to 0.25, d is more than or equal to 0 and less than or equal to 0.3, x is more than or equal to 0 and less than or equal to 0.15, and b + c + d + x is 1;
preferably, the positive electrode material L iaNibCocMndRxO2Adding metaphosphate for doping and coating.
2. The metaphosphate modified positive electrode material according to claim 1, wherein the metaphosphate is Al (PO)3)3、Ba(PO3)2、Ca(PO3)2、Mg(PO3)2、NaPO3、KPO3、LiPO3、Zn(PO3)2、Sr(PO3)2、Nd(PO3)3、Nb(PO3)5、La(PO3)3、Y(PO3)3At least one of (1).
3. The method for preparing a metaphosphate modified positive electrode material as defined in claim 1, comprising the steps of:
(1) selecting a precursor of a lithium ion battery anode material according to a target product, mechanically mixing the precursor and lithium salt in a mixer, and uniformly mixing until no white point appears visually;
(2) putting the uniformly mixed material in the step (1) into a sagger, and carrying out high-temperature calcination treatment in an oxygen atmosphere;
(3) after the fired material is cooled, taking out, crushing and sieving;
in the alternative, the first and second sets of the first,
(1) selecting a precursor of a lithium ion battery anode material according to a target product, mechanically mixing the precursor, lithium salt and metaphosphate in a mixer, and uniformly mixing until no white point appears visually;
(2) putting the uniformly mixed material in the step (1) into a sagger, and carrying out high-temperature calcination treatment in an oxygen atmosphere;
(3) after the fired material is cooled, taking out, crushing and sieving;
(4) placing the sieved material in a coating machine, and adding metaphosphate for coating treatment;
(5) putting the coated material into an atmosphere muffle furnace, and carrying out heat preservation treatment in an oxygen atmosphere;
(6) and after the materials are cooled, taking out the materials, crushing and sieving the materials.
4. The method according to claim 1, wherein the step of preparing the metaphosphate modified positive electrode material,
(1) weighing a precursor and lithium salt, mechanically mixing in a mixer, and uniformly mixing until no white point appears visually; the molar ratio of the lithium salt to the precursor is 1.0-1.09;
or (1) weighing a precursor, a lithium salt and a metaphosphate, wherein the molar ratio of the lithium salt to the precursor is 1.0-1.09, and the molar ratio of the metaphosphate to the precursor is 0.001-0.15, mechanically mixing in a mixer until no white spot appears visually.
5. The method for preparing a metaphosphate modified cathode material according to claim 1, wherein (2) the uniformly mixed materials are put into a sagger and fired at 715-935 ℃ for 5-25 hours in an oxygen atmosphere with a volume concentration of 21-100%.
6. The method for producing a metaphosphate modified positive electrode material as defined in claim 1, wherein (3) when the temperature is lowered to 100 ℃ or lower, the fired material is taken out, pulverized by a pulverizer, and sieved.
7. The preparation method of the metaphosphate modified cathode material of claim 1, wherein (4) the sieved material is put into a mechanical fusion machine, and 0-0.3% metaphosphate is added for coating.
8. The method for preparing a metaphosphate modified cathode material according to claim 1, wherein (5) the coated material is placed in an atmosphere furnace, and sintered at 300-800 ℃ for 5-16 hours in an oxygen atmosphere with a volume concentration of 21-100%.
9. The method according to claim 1, wherein (6) when the temperature is lowered to 100 ℃ or below, the fired material is taken out, pulverized in a pulverizer, and sieved.
10. The method for preparing a metaphosphate modified positive electrode material as defined in claim 1, comprising the steps of:
(1) weighing the raw materials, and mechanically mixing the precursor and the lithium salt in a mixer; the molar ratio of the lithium salt to the precursor is 1.0-1.09;
(2) putting the uniformly mixed materials into a sagger, putting the sagger into an atmosphere furnace, and firing the sagger for 5-25 hours at 715-935 ℃ in an oxygen atmosphere with the volume concentration of 21-100%;
(3) when the temperature is reduced to below 100 ℃, taking out the fired material, crushing by a crusher, and sieving;
in the alternative, the first and second sets of the first,
(1) weighing the raw materials, and mechanically mixing the precursor, the lithium salt and the metaphosphate in a mixer; wherein the molar ratio of the lithium salt to the precursor is 1.0-1.09, and the molar ratio of the metaphosphate to the precursor is 0.001-0.15;
(2) putting the uniformly mixed materials into a sagger, putting the sagger into an atmosphere furnace, and firing the sagger for 5-25 hours at 715-935 ℃ in an oxygen atmosphere with the volume concentration of 21-100%;
(3) when the temperature is reduced to below 100 ℃, taking out the fired material, crushing by a crusher, and sieving;
(4) putting the sieved material into a mechanical fusion machine, and adding 0-0.3% of metaphosphate for coating;
(5) placing the coated material in an atmosphere muffle furnace, and sintering at 300-800 ℃ for 5-16 h in an oxygen atmosphere with the volume concentration of 21-100%;
(6) when the temperature is reduced to below 100 ℃, the burnt material is taken out, crushed in a crusher and sieved.
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Cited By (7)
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| CN112038612A (en) * | 2020-09-16 | 2020-12-04 | 长沙理工大学 | Boron-doped & phosphite-coated nickel-based positive electrode material for lithium ion all-solid-state battery and preparation method thereof |
| CN113224310A (en) * | 2021-05-12 | 2021-08-06 | 桂林电子科技大学 | By using Al (PO)3)3Coating NCM811 cathode material and preparation method thereof |
| CN113314700A (en) * | 2021-05-11 | 2021-08-27 | 电子科技大学 | Dual-action modified high-nickel positive electrode material of lithium ion battery and preparation method of dual-action modified high-nickel positive electrode material |
| CN113346055A (en) * | 2021-05-11 | 2021-09-03 | 电子科技大学 | Composite phosphate coated high-nickel anode material of lithium ion battery and preparation method thereof |
| CN113488620A (en) * | 2021-06-28 | 2021-10-08 | 恒大新能源技术(深圳)有限公司 | Ternary positive electrode precursor and preparation method thereof, ternary positive electrode material and preparation method thereof, and lithium ion battery |
| CN113629240A (en) * | 2021-07-30 | 2021-11-09 | 江苏翔鹰新能源科技有限公司 | Single crystal lithium nickel cobalt manganese oxide positive electrode material and preparation method and application thereof |
| CN113745500A (en) * | 2021-08-03 | 2021-12-03 | 湖北融通高科先进材料有限公司 | Preparation method of high-nickel ternary cathode material |
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