LU504854B1 - Method for preparing high-nickel cathode material for lithium-ion batteries and high-nickel cathode material for lithium-ion batteries prepared therefrom - Google Patents

Method for preparing high-nickel cathode material for lithium-ion batteries and high-nickel cathode material for lithium-ion batteries prepared therefrom Download PDF

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LU504854B1
LU504854B1 LU504854A LU504854A LU504854B1 LU 504854 B1 LU504854 B1 LU 504854B1 LU 504854 A LU504854 A LU 504854A LU 504854 A LU504854 A LU 504854A LU 504854 B1 LU504854 B1 LU 504854B1
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lithium
cathode material
nickel
ion batteries
temperature
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LU504854A
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German (de)
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Xinpeng Wang
Jian Zhang
Lei Zhang
Yan He
Li Li
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Anhui Tianli Lithium Energy Co Ltd
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M10/00—Secondary cells; Manufacture thereof
    • H01M10/05—Accumulators with non-aqueous electrolyte
    • H01M10/052—Li-accumulators
    • H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
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    • C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
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    • C01—INORGANIC CHEMISTRY
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    • C01G53/00—Compounds of nickel
    • C01G53/40—Nickelates
    • C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
    • C01G53/44—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/50—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese
    • H01M4/505—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of manganese of mixed oxides or hydroxides containing manganese for inserting or intercalating light metals, e.g. LiMn2O4 or LiMn2OxFy
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
    • H01M4/00—Electrodes
    • H01M4/02—Electrodes composed of, or comprising, active material
    • H01M4/36—Selection of substances as active materials, active masses, active liquids
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
    • H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
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    • C01P2002/52—Solid solutions containing elements as dopants
    • C—CHEMISTRY; METALLURGY
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    • C01P2002/00—Crystal-structural characteristics
    • C01P2002/50—Solid solutions
    • C01P2002/52—Solid solutions containing elements as dopants
    • C01P2002/54—Solid solutions containing elements as dopants one element only
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
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    • C01P2004/45—Aggregated particles or particles with an intergrown morphology
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    • H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
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    • H01M2004/028—Positive electrodes
    • H—ELECTRICITY
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    • H01M4/00—Electrodes
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    • H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
    • H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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Abstract

The present application discloses a method for preparing a high-nickel cathode material for lithium-ion batteries and the high-nickel cathode material for lithium-ion batteries prepared therefrom, and specifically relates to the technical field of cathode materials for lithium-ion batteries. The method includes the following steps: (1) mixing a high-nickel ternary cathode material precursor, a lithium salt, a phosphorus-containing additive and a metal oxide additive; (2) loading mixed materials into a saggar, placing the saggar into a high-temperature and high-pressure device to conduct sintering, and after sintering, conducting natural cooling; and (3) grinding and sieving cooled materials to obtain the high-nickel cathode material for lithium-ion batteries. The present application has the beneficial effects of obtaining a high-nickel cathode material with a low residual lithium content, a low pH value and a low specific surface area by mixing the high-nickel ternary cathode material precursor, greatly simplifying process flows and reducing manufacturing costs.

Description

METHOD FOR PREPARING HIGH-NICKEL CATHODE MATERIAL FOR LUS04854
LITHIUM-ION BATTERIES AND HIGH-NICKEL CATHODE MATERIAL FOR
LITHIUM-ION BATTERIES PREPARED THEREFROM
TECHNICAL FIELD
[0001] The present application belongs to the technical field of cathode materials for lithium- ion batteries, and specifically discloses a method for preparing a high-nickel cathode material for lithium-ion batteries and the high-nickel cathode material for lithium-ion batteries prepared therefrom.
BACKGROUND
[0002] In recent years, with the high-speed development of the new energy automobile industry, demands for lithium-ion batteries grow rapidly. People’s demand for driving ranges of new energy automobiles has been on the rise. As the quantity demanded for high-energy- density lithium-ion batteries grows rapidly, a demand for high-nickel cathode materials grows at a high speed. A high-nickel ternary material has a characteristic of high capacity and also has certain disadvantages. Because of a higher nickel content, incomplete oxidation of bivalent nickel leads to serious Li'*/Ni** mixing, and lithium ions cannot migrate into structures so that a surface residual lithium content is higher and impacts material capacities.
[0003] At present, a preparation process of a high-nickel ternary cathode material is mainly a secondary sintering process, which comprises the following concrete flows: evenly mixing a precursor, a lithium salt and an additive, conducting primary high-temperature sintering in a kiln, crushing mixed materials, and conducting washing, drying, surface coating and secondary sintering. According to the method, residual lithium on material surfaces is removed mainly through washing. However, in the washing process, along with the removal of residual alkali, the migration of lithium ions inside the structures towards material surfaces leads to poor internal stability of the structures. A secondary sintering process means low-temperature sintering after boric acid coating. Although a pH value of materials can be controlled to be about 11.6. However, a specific surface area of the materials is generally more than 0.5 m”/g. This leads to a severe side reaction between the materials and an electrolyte, which has a strong impact on cycle performance of the materials. Moreover, manufacturing flows by the method are long, initial equipment investment is large, and manufacturing costs are very high. LU504854
[0004] The Chinese patent application document with the publication number
CN114933335A discloses a high-nickel ternary cathode material and a preparation method thereof. The preparation method comprises the following steps: Step 1, preparation of a precursor; Step 2, preparation of an oxidizing solution: weighing an oxidizing agent, dissolving the oxidizing agent into deionized water, and adding a water-soluble alkaline substance; Step 3, preparation of a modified precursor; and Step 4, mixing a lithium source with the modified precursor to prepare a cathode material. A corresponding cathode material and a lithium battery are also provided. A layer of intermediate product is formed on a surface layer of the precursor by adopting a pre-oxidation method to eliminate defects of crystals on an NCA surface layer, thereby remarkably improving stability and rate capabilities of batteries in a cycle process. But the patent does not involve a problem removing residual lithium on material surfaces.
SUMMARY
[0005] The technical problem that the present application is to solve is how to solve the problems of a high residual lithium content, a high pH value and a large specific surface area of an existing high-nickel cathode material.
[0006] The present application solves the technical problem by the following technological means:
[0007] a method for preparing a high-nickel cathode material for lithium-ion batteries, comprising the following steps:
[0008] (1) mixing a high-nickel ternary cathode material precursor, a lithium salt, a phosphorus-containing additive and a metal oxide additive, wherein a molar ratio of lithium in the lithium salt to nickel, cobalt and manganese in the high-nickel ternary cathode material precursor is 1.00-1.10; an added amount of the phosphorus-containing additive accounts for 0.1-1.5wt% of a mass of the high-nickel ternary cathode material precursor; an added amount of the metal oxide additive accounts for 0.1-0.5wt% of a mass of the high-nickel ternary cathode material precursor;
[0009] (2) loading materials mixed in Step (1) into a saggar, placing the saggar into a high- temperature and high-pressure device to conduct sintering, and after sintering, conducting natural cooling; and
[0010] (3) grinding and sieving materials cooled in Step (2) to obtain the high-nickel cathode material for lithium-ion batteries.
[0011] The present application has beneficial effects: mixing the high-nickel ternary cathode LU504854 material precursor, the lithium salt, the phosphorus-containing additive and the metal oxide additive in a specific proportion, by using a high-temperature and high-pressure gradient sintering technology and a crystal growth control technology and utilizing characteristics that phosphate ions and metal cations have large radii and are not easy to diffuse at a low temperature, fully oxidizing bivalent nickel to trivalent nickel under a low-temperature and high-pressure pure oxygen atmosphere to help lithium ions to migrate into structures and reduce lithium-nickel mixing and surface residual lithium, and continuing to heat up and conduct sintering to make primary particles of the materials directionally grow and simultaneously control a reaction speed of the material surface residual lithium and phosphate/metal ions to achieve the purpose of reducing and controlling material surface states, thereby obtaining the high-nickel cathode material with a low residual lithium content, a low pH value and a low specific surface area.
[0012] Preferably, the high-nickel ternary cathode material precursor has a chemical formula of Nix Co y Mn,Alixy, (OH), wherein 0.8<x<0.9, 0.05<y<0.15, 0.01<z<0.10, and 0.95<x+y+7z<0.99.
[0013] Preferably, the high-nickel ternary cathode material precursor is of a core-shell structure. An internal core is made of a high-nickel material, and an external shell is made of a low-nickel and high-manganese material, wherein a molar ratio of the nickel content in the high-nickel material is more than 85% and less than 96%, wherein a molar ratio of the nickel content in the low-nickel and high-manganese material is less than 60%, and a molar ratio of the manganese content in the low-nickel and high-manganese material is more than 20% and less than 60%.
[0014] Preferably, the high-nickel ternary cathode material precursor has a particle size D50 of 6-15 um.
[0015] Preferably, the lithium salt is a combination of one or two of lithium hydroxide, lithium oxalate, lithium dihydrogen phosphate and lithium phosphate.
[0016] Preferably, the phosphorus-containing additive is a combination of one or more of ammonium dihydrogen phosphate, phosphorus pentoxide, titanium phosphate, aluminum phosphate and phosphotungstic acid.
[0017] Preferably, metal ions in the metal oxide additive have radii of 60-80 pm.
[0018] Preferably, the metal oxide additive is a combination of one or more of zirconia, tungsten oxide, titanium oxide and strontium oxide.
[0019] Preferably, a high-temperature and high-pressure sintering device is a batch sintering LU504854 device, of which the maximum sintering temperature is 900 °C and an internal pressure of a kiln can be automatically adjusted from -10 Pato 500 Pa according to program settings.
[0020] Preferably, the sintering in Step (2) is conducted in an oxygen atmosphere furnace.
[0021] Preferably, a volume content of oxygen in the oxygen atmosphere furnace is greater than or equal to 90%, and the concentration of carbon dioxide is less than 50 ppm.
[0022] Preferably, the sintering in Step (2) refers to a gradient sintering: firstly low- temperature sintering first and secondly high-temperature sintering.
[0023] Preferably, the low-temperature sintering specifically comprises: heating up to 650- 780 °C at a heating rate of 1-3 °C/min under a pressure from -10 Pa to -5 Pa, and keeping a temperature for 4-10 h under a pressure from 50 Pa to 200 Pa in the temperature-keeping process.
[0024] Preferably, the high-temperature sintering specifically comprises: heating up to 750- 850 °C at a heating rate of 0.5-2 °C/min under a pressure from -10 Pa to -5 Pa, and keeping a temperature for 4-10 h under a pressure from 5 Pa to 50 Pa in the temperature-keeping process.
[0025] Preferably, the high-nickel cathode material with a low residual lithium content, a low pH value and a low specific surface area is obtained after the high-temperature and high- pressure gradient sintering is completed; a residual lithium content on surfaces of the high- nickel cathode material ranges from 500 ppm to 1200 ppm; a pH value of the high-nickel cathode material ranges from 11.30 to 11.70; the specific surface area of the high-nickel cathode material ranges from 0.15-0.35 m°/g.
[0026] The present application also provides a high-nickel cathode material for lithium-ion batteries prepared by adopting the method.
[0027] The present application has the advantages: (1) mixing the high-nickel ternary cathode material precursor, the lithium salt, the phosphorus-containing additive and the metal oxide additive in a specific proportion, by using the high-temperature and high-pressure gradient sintering technology and the crystal growth control technology and utilizing the characteristics that phosphate ions and metal cations have large radii and are not easy to diffuse at a low temperature, fully oxidizing bivalent nickel to trivalent nickel under a low-temperature and high-pressure pure oxygen atmosphere to help lithium ions to migrate into the structures and reduce lithium-nickel mixing and surface residual lithium, and continuing to heat up and conduct sintering to make primary particles of the materials directionally grow and simultaneously control the reaction speed of the material surface residual lithium and the phosphate/metal ions to achieve the purpose of reducing and LU504854 controlling the material surface states, thereby obtaining the high-nickel cathode material with the low residual lithium content, the low pH value and the low specific surface area. (2) The present application fundamentally solves the problems of a high residual lithium 5 content, a high pH value and a large specific surface area of the high-nickel cathode material, manufacturing process flows are shortened, and manufacturing costs are reduced. (3) Compared with existing technical solutions, the present application has obvious advantages that the problems of uncontrollable residual lithium and specific surface areas in industries are completely solved, process flows are greatly simplified, and manufacturing costs have an obvious advantage.
DESCRIPTION OF THE DRAWINGS
[0028] FIG. 1 is an electron micrograph image of a material prepared according to
Embodiment 1 of the present application.
[0029] FIG. 2 is an electrical performance diagram of the material prepared according to
Embodiment 1 of the present application.
[0030] FIG. 3 is an electron micrograph image of a material prepared according to
Embodiment 2 of the present application.
[0031] FIG. 4 is an electrical performance diagram of the material prepared according to
Embodiment 2 of the present application.
DESCRIPTION OF EMBODIMENTS
[0032] To make the object, technical solutions, and advantages of the embodiments of the present application clearer, the technical solution of the embodiments of the present application will be clearly described in conjunction with the embodiments of the present application, and it will be obvious that the described embodiments are part of the embodiments of the present application, but not all of them. Based on the embodiments of the present application, all other embodiments obtained by those skilled in the art without creative efforts shall fall within the scope of protection of this application.
[0033] Embodiment 1: LU504854
[0034] A method for preparing a high-nickel cathode material for lithium-ion batteries comprises the following steps:
[0035] (1) mixing a high-nickel ternary cathode material precursor, a lithium salt, a phosphorus-containing additive and a metal oxide additive, wherein the high-nickel ternary cathode material precursor is Nio.ss C00.083Mno.040Al0.027 (OH)2 , an internal core material is
NisoC00.07 Alo.03(OH)» ‚and a mass ratio is 90%; an external shell material is Nio.40C00.20
Mo 40(OH)2 , a mass ratio is 10%,and a particle size (D50) is 6 um; the lithium salt is a mixture of lithium hydroxide and lithium dihydrogen phosphate, wherein a mass ratio of lithium hydroxide is 96%; a molar ratio of lithium in the lithium salt to nickel, cobalt and manganese in the high-nickel ternary cathode material precursor is 1.04; the phosphorus-containing additive is phosphorus pentoxide; an added amount of the phosphorus-containing additive accounts for 0.5% of a mass of the high-nickel ternary cathode material precursor; the metal oxide additive is a mixture of zirconia and titanium oxide, wherein a mass ratio of zirconia to titanium oxide is 1:2, and an added amount of the metal oxide additive accounts for 0.3% of a mass of the high-nickel ternary cathode material precursor; the abovementioned materials are weighed in a proportion and placed into a 10 L of a high-speed mixer to be mixed for 60 min;
[0036] (2) loading materials mixed in Step (1) into a saggar, then placing the saggar into a high-temperature and high-pressure device to conduct sintering, and heating up to 700 °C at a heating rate of 1.5 °C/min under an internal pressure of -7 Pa in the device in the heating-up process; keeping a temperature for 6 h after the temperature reaches 700 °C under an internal pressure of 50 Pa in the device in the temperature-keeping process; heating up to 790 °C at a heating rate of 1.0 °C/min under an internal pressure of -5 Pa in the device in the heating-up process; keeping a temperature for 6 h after the temperature reaches 790 °C under an internal pressure of 10 Pa in the device in the temperature-keeping process; conducting natural cooling;
[0037] (3) grinding and sieving materials cooled in Step (2) to obtain the high-nickel cathode material for lithium-ion batteries.
[0038] Conduct tests on a residual lithium content, a pH value and a specific surface area of the material prepared according to the embodiment of the present application, wherein the residual lithium content is tested through acid-base titration, the pH value is tested through a pH meter, and the specific surface area is tested through a specific surface area tester, and testing results are shown as Table 1.
[0039] As shown in the electron micrograph image FIG. 1 of the material prepared according to the embodiment of the present application, it can be seen that primary particles on surfaces LU504854 are uniform, compactness of secondary spheres is good, and no obvious residual lithium is on the surfaces.
[0040] As shown in the electrical performance diagram FIG. 2 of the material prepared according to the embodiment of the present application, it can be seen that primary particles on surfaces are uniform, compactness of secondary spheres is good, and there is no obvious residual lithium on the surfaces.
[0041] Embodiment 2:
[0042] A method for preparing a high-nickel cathode material for lithium-ion batteries comprises the following steps:
[0043] (1) mixing a high-nickel ternary cathode material precursor, a lithium salt, a phosphorus-containing additive and a metal oxide additive, wherein the high-nickel ternary cathode material precursor is Nio.ss Co00.083Mno.040Al0.027 (OH)2 , an internal core material is
NigoC00.07 Alo.os(OH)2 ‚and a mass ratio is 90%; an external shell material is Nio40C00.20
Mng40(OH);, amass ratio is 10%,and a particle size (D50) is 10 um; the lithium salt is a mixture of lithium hydroxide and lithium dihydrogen phosphate, wherein a mass ratio of lithium hydroxide is 96%; a molar ratio of lithium in the lithium salt to nickel, cobalt and manganese in the high-nickel ternary cathode material precursor is 1.04; the phosphorus-containing additive is phosphorus pentoxide; an added amount of the phosphorus-containing additive accounts for 0.5% of a mass of the high-nickel ternary cathode material precursor; the metal oxide additive is a mixture of zirconia and titanium oxide, wherein a mass ratio of zirconia to titanium oxide is 1:2, and an added amount of the metal oxide additive accounts for 0.3% of a mass of the high-nickel ternary cathode material precursor; the abovementioned materials are weighed in a proportion and placed into a 10 L of a high-speed mixer to be mixed for 60 min;
[0044] (2) loading materials mixed in Step (1) into a saggar, then placing the saggar into a high-temperature and high-pressure device to conduct sintering, and heating up to 700 °C at a heating rate of 1.5 °C/min under an internal pressure of -7 Pa in the device in the heating-up process; keeping a temperature for 6 h after the temperature reaches 700 °C under an internal pressure of 50 Pa in the device in the temperature-keeping process; heating up to 790 °C at a heating rate of 1.0 °C/min under an internal pressure of -5 Pa in the device in the heating-up process; keeping a temperature for 6 h after the temperature reaches 790 °C under an internal pressure of 10 Pa in the device in the temperature-keeping process; conducting natural cooling;
[0045] (3) grinding and sieving materials cooled in Step (2) to obtain the high-nickel cathode material for lithium-ion batteries. LU504854
[0046] The difference between the embodiment and Embodiment 1 lies in: a particle size (D50) of the high-nickel ternary cathode material precursor in Step (1) is 10 um, and the other steps are the same as those in Embodiment 1.
[0047] Conduct tests on a residual lithium content, a pH value and a specific surface area of the material prepared according to the embodiment of the present application, wherein the residual lithium content is tested through acid-base titration, the pH value is tested through a pH meter, and the specific surface area is tested through a specific surface area tester, and testing results are shown as Table 1.
[0048] As shown in the electron micrograph image FIG. 3 of the material prepared according to the embodiment of the present application, it can be seen that primary particles on surfaces are uniform, compactness of secondary spheres is good, and no obvious residual lithium is on the surfaces.
[0049] As shown in the electrical performance diagram FIG. 4 of the material prepared according to the embodiment of the present application, it can be seen that primary particles on surfaces are uniform, compactness of secondary spheres is good, and there is no obvious residual lithium on the surfaces.
[0050] Embodiment 3:
[0051] The difference between the embodiment and Embodiment 1 lies in: a particle size (D50) of the high-nickel ternary cathode material precursor in Step (1) is 15 um, and the other steps are the same as those in Embodiment 1.
[0052] Conduct tests on a residual lithium content, a pH value and a specific surface area of the material prepared according to the embodiment of the present application, wherein the residual lithium content is tested through acid-base titration, the pH value is tested through a pH meter, and the specific surface area is tested through a specific surface area tester, and testing results are shown as Table 1.
[0053] Embodiment 4:
[0054] The difference between the embodiment and Embodiment 2 lies in: in Step (1), the molar ratio of lithium in the lithium salt to nickel, cobalt and manganese in the high-nickel ternary cathode material precursor is 1.02, and the other steps are the same as those in
Embodiment 2.
[0055] Conduct tests on a residual lithium content, a pH value and a specific surface area of LU504854 the material prepared according to the embodiment of the present application, wherein the residual lithium content is tested through acid-base titration, the pH value is tested through a pH meter, and the specific surface area is tested through a specific surface area tester, and testing results are shown as Table 1.
[0056] Embodiment 5:
[0057] The difference between the embodiment and Embodiment 2 lies in: in Step (1), the molar ratio of lithium in the lithium salt to nickel, cobalt and manganese in the high-nickel ternary cathode material precursor is 1.06, and the other steps are the same as those in
Embodiment 2.
[0058] Conduct tests on a residual lithium content, a pH value and a specific surface area of the material prepared according to the embodiment of the present application, wherein the residual lithium content is tested through acid-base titration, the pH value is tested through a pH meter, and the specific surface area is tested through a specific surface area tester, and testing results are shown as Table 1.
[0059] Embodiment 6:
[0060] The difference between the embodiment and Embodiment 2 lies in: “heating up to 700 °C at a heating rate of 1.5 °C/min and keeping the temperature for 6 h after the temperature reaches 700 °C” in Step (2) is changed to:
[0061] ‘heating up to 650 °C at a heating rate of 1.5 °C/min and keeping the temperature for 6 h after the temperature reaches 650 °C”, and the other steps are the same as those in
Embodiment 2.
[0062] Conduct tests on a residual lithium content, a pH value and a specific surface area of the material prepared according to the embodiment of the present application, wherein the residual lithium content is tested through acid-base titration, the pH value is tested through a pH meter, and the specific surface area is tested through a specific surface area tester, and testing results are shown as Table 1.
[0063] Embodiment 7:
[0064] The difference between the embodiment and Embodiment 2 lies in: “heating up to 700 °C at a heating rate of 1.5 °C/min and keeping the temperature for 6 h after the temperature reaches 700 °C” in Step (2) is changed to: LU504854
[0065] ‘heating up to 750 °C at a heating rate of 1.5 °C/min and keeping the temperature for 6 h after the temperature reaches 750 °C”, and the other steps are the same as those in
Embodiment 2.
[0066] Conduct tests on a residual lithium content, a pH value and a specific surface area of the material prepared according to the embodiment of the present application, wherein the residual lithium content is tested through acid-base titration, the pH value is tested through a pH meter, and the specific surface area is tested through a specific surface area tester, and testing results are shown as Table 1.
[0067] Embodiment 8:
[0068] The difference between the embodiment and Embodiment 2 lies in: “the high-nickel ternary cathode material precursor is Nig gs C0O0.083MN0.040Al0.027 (OH)», an internal core material is NiooCoo.07 Alo.os(OH)2, the mass ratio is 90%, an external shell material is Nio40C00.20
Mno40(OH)», and the mass ratio is 10%” in Step (1) is changed to:
[0069] “the high-nickel ternary cathode material precursor is Nio875 C00.0765MnN0020Al0.0285 (OH), the internal core material is NiggCoo.07 Alo.03(OH)», the mass ratio is 95%, an external shell material is Nio 40C00.20 Mng 40(OH)», and the mass ratio is 5%”, and the other steps are the same as those in Embodiment 2.
[0070] Conduct tests on a residual lithium content, a pH value and a specific surface area of the material prepared according to the embodiment of the present application, wherein the residual lithium content is tested through acid-base titration, the pH value is tested through a pH meter, and the specific surface area is tested through a specific surface area tester, and testing results are shown as Table 1.
[0071] Embodiment 9:
[0072] The difference between the embodiment and Embodiment 2 lies in: “the high-nickel ternary cathode material precursor is Nio.ss C0O0.083Mn0.040Al0.027 (OH)2, an internal core material is NisoC00.07 Alo.o3(OH)2, the mass ratio is 90%, an external shell material is Nio.40C00.20
Mno40(OH)», and the mass ratio is 10%” in Step (1) is changed to:
[0073] “the high-nickel ternary cathode material precursor is Niog2s C00.0895Mnoos0Alo 0255 (OH), the internal core material is Nt90C00.07 Aloo3(OH)z, the mass ratio is 85%, an external shell material is Nio40C00.20 Mno40(OH)2, and the mass ratio is 15%”, and the other steps are LU504854 the same as those in Embodiment 2.
[0074] Conduct tests on a residual lithium content, a pH value and a specific surface area of the material prepared according to the embodiment of the present application, wherein the residual lithium content is tested through acid-base titration, the pH value is tested through a pH meter, and the specific surface area is tested through a specific surface area tester, and testing results are shown as Table 1.
[0075] Embodiment 10:
[0076] The difference between the embodiment and Embodiment 2 lies in: “a mass ratio of lithium hydroxide is 96%” in Step (1) is changed to:
[0077] “a mass ratio of lithium hydroxide is 98%”, and the other steps are the same as those in Embodiment 2.
[0078] Conduct tests on a residual lithium content, a pH value and a specific surface area of the material prepared according to the embodiment of the present application, wherein the residual lithium content is tested through acid-base titration, the pH value is tested through a pH meter, and the specific surface area is tested through a specific surface area tester, and testing results are shown as Table 1.
[0079] Embodiment 11:
[0080] The difference between the embodiment and Embodiment 2 lies in: “the lithium salt is a mixture of lithium hydroxide and lithium dihydrogen phosphate, wherein a mass ratio of lithium hydroxide is 96%” in Step (1) is changed to:
[0081] “The lithium salt is lithium hydroxide”, and the other steps are the same as those in
Embodiment 2.
[0082] Conduct tests on a residual lithium content, a pH value and a specific surface area of the material prepared according to the embodiment of the present application, wherein the residual lithium content is tested through acid-base titration, the pH value is tested through a pH meter, and the specific surface area is tested through a specific surface area tester, and testing results are shown as Table 1.
[0083] Embodiment 12:
[0084] The difference between the embodiment and Embodiment 2 lies in: “keeping a temperature for 6 h after the temperature reaches 700 °C under an internal pressure of 50 Pa in LU504854 the device in the temperature-keeping process” in Step (2) is changed to:
[0085] “keeping a temperature for 6 h after the temperature reaches 700 °C under an internal pressure of 100 Pa in the device in the temperature-keeping process”, and the other steps are the same as those in Embodiment 2.
[0086] Conduct tests on a residual lithium content, a pH value and a specific surface area of the material prepared according to the embodiment of the present application, wherein the residual lithium content is tested through acid-base titration, the pH value is tested through a pH meter, and the specific surface area is tested through a specific surface area tester, and testing results are shown as Table 1.
[0087] Embodiment 13:
[0088] The difference between the embodiment and Embodiment 2 lies in: “keeping a temperature for 6 h after the temperature reaches 700 °C under an internal pressure of 50 Pa in the device in the temperature-keeping process” in Step (2) is changed to:
[0089] “keeping a temperature for 6 h after the temperature reaches 700 °C under an internal pressure of 150 Pa in the device in the temperature-keeping process”, and the other steps are the same as those in Embodiment 2.
[0090] Conduct tests on a residual lithium content, a pH value and a specific surface area of the material prepared according to the embodiment of the present application, wherein the residual lithium content is tested through acid-base titration, the pH value is tested through a pH meter, and the specific surface area is tested through a specific surface area tester, and testing results are shown as Table 1.
[0091] Embodiment 14:
[0092] The difference between the embodiment and Embodiment 2 lies in: in Step (1), the molar ratio of lithium in the lithium salt to nickel, cobalt and manganese in the high-nickel ternary cathode material precursor is 1.00, and the other steps are the same as those in
Embodiment 2.
[0093] Conduct tests on a residual lithium content, a pH value and a specific surface area of the material prepared according to the embodiment of the present application, wherein the residual lithium content is tested through acid-base titration, the pH value is tested through a pH meter, and the specific surface area is tested through a specific surface area tester, and testing LU504854 results are shown as Table 1.
[0094] Embodiment 15:
[0095] The difference between the embodiment and Embodiment 2 lies in: in Step (1), a molar ratio of lithium in the lithium salt to nickel, cobalt and manganese in the high-nickel ternary cathode material precursor is 1.10, and the other steps are the same as those in Embodiment 2.
[0096] Conduct tests on a residual lithium content, a pH value and a specific surface area of the material prepared according to the embodiment of the present application, wherein the residual lithium content is tested through acid-base titration, the pH value is tested through a pH meter, and the specific surface area is tested through a specific surface area tester, and testing results are shown as Table 1.
[0097] Embodiment 16:
[0098] The difference between the embodiment and Embodiment 2 lies in: in Step (1), “an added amount of the phosphorus-containing additive accounts for 0.5% of a mass of the high- nickel ternary cathode material precursor” is changed to:
[0099] “an added amount of the phosphorus-containing additive accounts for 0.1% of a mass of the high-nickel ternary cathode material precursor”, and the other steps are the same as those in Embodiment 2.
[0100] Conduct tests on a residual lithium content, a pH value and a specific surface area of the material prepared according to the embodiment of the present application, wherein the residual lithium content is tested through acid-base titration, the pH value is tested through a pH meter, and the specific surface area is tested through a specific surface area tester, and testing results are shown as Table 1.
[0101] Embodiment 17:
[0102] The difference between the embodiment and Embodiment 2 lies in: in Step (1), “an added amount of the phosphorus-containing additive accounts for 0.5% of a mass of the high- nickel ternary cathode material precursor” is changed to:
[0103] “an added amount of the phosphorus-containing additive accounts for 1.5% of a mass of the high-nickel ternary cathode material precursor”, and the other steps are the same as those in Embodiment 2.
[0104] Conduct tests on a residual lithium content, a pH value and a specific surface area of LU504854 the material prepared according to the embodiment of the present application, wherein the residual lithium content is tested through acid-base titration, the pH value is tested through a pH meter, and the specific surface area is tested through a specific surface area tester, and testing results are shown as Table 1.
[0105] Embodiment 18:
[0106] The difference between the embodiment and Embodiment 2 lies in: “the lithium salt is a mixture of lithium hydroxide and lithium dihydrogen phosphate, wherein a mass ratio of lithium hydroxide is 96%” in Step (1) is changed to:
[0107] “the lithium salt is a mixture of lithium oxalate and lithium phosphate, wherein a mass ratio of lithium phosphate is 96%”, and the other steps are the same as those in Embodiment 2.
[0108] Conduct tests on a residual lithium content, a pH value and a specific surface area of the material prepared according to the embodiment of the present application, wherein the residual lithium content is tested through acid-base titration, the pH value is tested through a pH meter, and the specific surface area is tested through a specific surface area tester, and testing results are shown as Table 1.
[0109] Embodiment 19:
[0110] The difference between the embodiment and Embodiment 2 lies in: in Step (1), “the phosphorus-containing additive is phosphorus pentoxide” is changed to:
[0111] “the phosphorus-containing additive is ammonium dihydrogen phosphate”, and the other steps are the same as those in Embodiment 2.
[0112] Conduct tests on a residual lithium content, a pH value and a specific surface area of the material prepared according to the embodiment of the present application, wherein the residual lithium content is tested through acid-base titration, the pH value is tested through a pH meter, and the specific surface area is tested through a specific surface area tester, and testing results are shown as Table 1.
[0113] Embodiment 20:
[0114] The difference between the embodiment and Embodiment 2 lies in: in Step (1), “the phosphorus-containing additive is phosphorus pentoxide” is changed to:
[0115] “the phosphorus-containing additive is a mixture of phosphorus pentoxide and ammonium dihydrogen phosphate, wherein a mass ratio of phosphorus pentoxide is 20%”, and LU504854 the other steps are the same as those in Embodiment 2.
[0116] Conduct tests on a residual lithium content, a pH value and a specific surface area of the material prepared according to the embodiment of the present application, wherein the residual lithium content is tested through acid-base titration, the pH value is tested through a pH meter, and the specific surface area is tested through a specific surface area tester, and testing results are shown as Table 1.
[0117] Embodiment 21:
[0118] The difference between the embodiment and Embodiment 2 lies in: in Step (1), “the phosphorus-containing additive is phosphorus pentoxide” is changed to:
[0119] “the phosphorus-containing additive is a mixture of titanium phosphate, aluminum phosphate and phosphotungstic acid, wherein mass ratios of titanium phosphate, aluminum phosphate and phosphotungstic acid are respectively 20%, 20%, 60%...”, and the other steps are the same as those in Embodiment 2.
[0120] Conduct tests on a residual lithium content, a pH value and a specific surface area of the material prepared according to the embodiment of the present application, wherein the residual lithium content is tested through acid-base titration, the pH value is tested through a pH meter, and the specific surface area is tested through a specific surface area tester, and testing results are shown as Table 1.
[0121] Embodiment 22:
[0122] The difference between the embodiment and Embodiment 2 lies in: in Step (1), “the metal oxide additive is a mixture of zirconia and titanium oxide, wherein a mass ratio of zirconia to titanium oxide is 1:2, and an added amount of the metal oxide additive accounts for 0.3% of a mass of the high-nickel ternary cathode material precursor,” is changed to:
[0123] “the metal oxide additive is tungsten oxide, wherein an added amount of tungsten oxide accounts for 0.1% of a mass of the high-nickel ternary cathode material precursor”, and the other steps are the same as those in Embodiment 2.
[0124] Conduct tests on a residual lithium content, a pH value and a specific surface area of the material prepared according to the embodiment of the present application, wherein the residual lithium content is tested through acid-base titration, the pH value is tested through a pH meter, and the specific surface area is tested through a specific surface area tester, and testing LU504854 results are shown as Table 1.
[0125] Embodiment 23:
[0126] The difference between the embodiment and Embodiment 2 lies in: in Step (1), “the metal oxide additive is a mixture of zirconia and titanium oxide, wherein a mass ratio of zirconia to titanium oxide is 1:2, and an added amount of the metal oxide additive accounts for 0.3% of a mass of the high-nickel ternary cathode material precursor,” is changed to:
[0127] “the metal oxide additive is a mixture of tungsten oxide, titanium oxide and strontium oxide, wherein mass ratios of tungsten oxide, titanium oxide and strontium oxide are respectively 0.1%, 0.1% and 0.1%, and an added amount of the metal oxide additive accounts for 0.5% of a mass of the high-nickel ternary cathode material precursor”, and the other steps are the same as those in Embodiment 2.
[0128] Conduct tests on a residual lithium content, a pH value and a specific surface area of the material prepared according to the embodiment of the present application, wherein the residual lithium content is tested through acid-base titration, the pH value is tested through a pH meter, and the specific surface area is tested through a specific surface area tester, and testing results are shown as Table 1.
[0129] Embodiment 24:
[0130] The difference between the embodiment and Embodiment 2 lies in: “heating up to 700 °C at a heating rate of 1.5 °C/min under an internal pressure of -7 Pa in the device in the heating-up process; keeping a temperature for 6 h after the temperature reaches 700 °C under an internal pressure of 50 Pa in the device in the temperature-keeping process; heating up to 790 °C at a heating rate of 1.0 °C/min under an internal pressure of -5 Pa in the device in the heating-up process; keeping a temperature for 6 h after the temperature reaches 790 °C under an internal pressure of 10 Pa in the device in the temperature-keeping process” in Step (2), is changed to:
[0131] “heating up to 650 °C at a heating rate of 1 °C/min under an internal pressure of -5 Pa in the device in the heating-up process; keeping a temperature for 10 h after the temperature reaches 650 °C under an internal pressure of 80 Pa in the device in the temperature-keeping process; heating up to 750 °C at a heating rate of 0.5 °C/min under an internal pressure of -8 Pa in the device in the heating-up process; keeping a temperature for 10 h after the temperature reaches 750 °C under an internal pressure of 5 Pa in the device in the temperature-keeping LU504854 process”, and the other steps are the same as those in Embodiment 2.
[0132] Conduct tests on a residual lithium content, a pH value and a specific surface area of the material prepared according to the embodiment of the present application, wherein the residual lithium content is tested through acid-base titration, the pH value is tested through a pH meter, and the specific surface area is tested through a specific surface area tester, and testing results are shown as Table 1.
[0133] Embodiment 25:
[0134] The difference between the embodiment and Embodiment 2 lies in: “heating up to 700 °C at a heating rate of 1.5 °C/min under an internal pressure of -7 Pa in the device in the heating-up process; keeping a temperature for 6 h after the temperature reaches 700 °C under an internal pressure of 50 Pa in the device in the temperature-keeping process; heating up to 790 °C at a heating rate of 1.0 °C/min under an internal pressure of -5 Pa in the device in the heating-up process; keeping a temperature for 6 h after the temperature reaches 790 °C under an internal pressure of 10 Pa in the device in the temperature-keeping process” in Step (2); is changed to:
[0135] “heating up to 780 °C at a heating rate of 3 °C/min under an internal pressure of -10
Pa in the device in the heating-up process; keeping a temperature for 4 h after the temperature reaches 780 °C under an internal pressure of 200 Pa in the device in the temperature-keeping process: heating up to 850 °C at a heating rate of 2 °C/min under an internal pressure of -10 Pa in the device in the heating-up process; keeping a temperature for 4 h after the temperature reaches 850 °C under an internal pressure of 50 Pa in the device in the temperature-keeping process”, and the other steps are the same as those in Embodiment 2.
[0136] Conduct tests on a residual lithium content, a pH value and a specific surface area of the material prepared according to the embodiment of the present application, wherein the residual lithium content is tested through acid-base titration, the pH value is tested through a pH meter, and the specific surface area is tested through a specific surface area tester, and testing results are shown as Table 1.
[0137] Table one is shown below:
Residual pH value Specific surface lithium area
Embodiment | 960 | ns | 016
TABLE 1
[0138] According to data in Table 1:
[0139] it can be seen by comparing schemes 1/2/3 that when particle sizes of precursors are different, after treatment by adopting the same technical solution, the bigger the particle size is, the lower the specific surface area of materials is, the higher the residual lithium content is, maybe when the particle size is too big, migration of lithium ions into the structures is difficult to cause relatively high surface residues, and that the pH value has no significant change is possibly caused by more residual lithium phosphate on the material surfaces;
[0140] it can be seen by comparing schemes 2/4/5 that when the lithium proportion differs, LU504854 residual lithium increases with the improvement of proportion coefficients, but the pH value and the specific surface area have no significant changes:
[0141] it can be seen by comparing schemes 2/6/7 that when the low-temperature sintering temperature differs, residual lithium and the pH value decrease firstly and then increase with the rising of the sintering temperature, and it may be mainly because bivalent nickel is mostly likely to be oxidized into trivalent nickel at the temperature, which is better for lithium ions to migrate into the structures;
[0142] it can be seen by comparing schemes 2/8/9 that when the nickel content differs, residual lithium and pH value increase with an increase in the nickel content, it may be mainly because shells are thin and the nickel content is high, it is hard to oxidize bivalent nickel into trivalent nickel, and this is not beneficial to lithium ions to migrate into the structures;
[0143] it can be seen by comparing schemes 2/10/11 that an increase in the usage amount of lithium hydroxide in the proportioning process has no obvious effect on residual lithium and the pH value:
[0144] it can be seen by comparing schemes 2/12/13 that during low-temperature sintering, residue alkali decreases with pressure application, it may be because increasing pressure is beneficial to oxidize bivalent nickel into trivalent nickel and better for lithium ions to migrate into the structures.
[0145] The applicant declares that the above 1s only the specific embodiment of the present application, but the scope of the present application is not limited thereto, and those skilled in the art can clearly understand that changes or substitutions that any person skilled in the art can easily think of within the technical scope of the present application should be covered by the protection scope and the disclosure scope of the present application.
[0146] The above embodiments are only used to illustrate the technical solutions of the present application, not to limit it; although the present application has been illustrated in detail by referring to the aforementioned embodiments, those of ordinary skill in the art should understand that: they can still make modification to the technical solution recorded in the aforementioned each embodiment, or make equivalent replacements to part of technical features thereof, but these modifications or replacements does not make the nature of the corresponding technical solution departing from the spirit and scope of the technical solution of each embodiment of the present application.

Claims (10)

WHAT IS CLAIMED IS: LUS04854
1. A method for preparing a high-nickel cathode material for lithium-ion batteries, comprising the following steps: (1) mixing a high-nickel ternary cathode material precursor, a lithtum salt, a phosphorus- containing additive and a metal oxide additive, wherein a molar ratio of lithium in the lithium salt to nickel, cobalt and manganese in the high-nickel ternary cathode material precursor 1s
1.00-1.10; an added amount of the phosphorus-containing additive accounts for 0.1-1.5wt% of a mass of the high-nickel ternary cathode material precursor; an added amount of the metal oxide additive accounts for 0.1-0.5wt% of a mass of the high-nickel ternary cathode material precursor; (2) loading materials mixed in Step (1) into a saggar, placing the saggar into a high- temperature and high-pressure device to conduct sintering, and after sintering, conducting natural cooling; and (3) grinding and sieving the materials cooled in Step (2) to obtain the high-nickel cathode material for lithium-ion batteries.
2. The method for preparing the high-nickel cathode material for lithium-ion batteries according to claim 1, wherein the high-nickel ternary cathode material precursor has a chemical formula of Nix Co y Mn; Al1-x-y-z (OH)2, wherein 0.8<x<0.9, 0.05<y<0.15, 0.01<z<0.10, and
0.95<x+y+z<0.99.
3. The method for preparing the high-nickel cathode material for lithium-ion batteries according to claim 1 or claim 2, wherein the high-nickel ternary cathode material precursor has a particle size D50 of 6-15 um.
4. The method for preparing the high-nickel cathode material for lithium-ion batteries according to claim 3, wherein the lithium salt is a combination of one or two of lithium hydroxide, lithium oxalate, lithium dihydrogen phosphate and lithium phosphate; the phosphorus-containing additive is a combination of one or more of ammonium dihydrogen phosphate, phosphorus pentoxide, titanium phosphate, aluminum phosphate and phosphotungstic acid.
5. The method for preparing the high-nickel cathode material for lithium-ion batteries according to claim 4, wherein metal ions in the metal oxide additive have radii of 60-80 pm. LU504854
6. The method for preparing the high-nickel cathode material for lithium-ion batteries according to claim 1, wherein the metal oxide additive is a combination of one or more of zirconia, tungsten oxide, titanium oxide and strontium oxide.
7. The method for preparing the high-nickel cathode material for lithium-ion batteries according to claim 1, wherein the sintering in Step (2) refers to a gradient sintering: firstly low- temperature sintering and secondly high-temperature sintering.
8. The method for preparing the high-nickel cathode material for lithium-ion batteries according to claim 7, wherein the low-temperature sintering specifically comprises: heating up to 650-780 °C at a heating rate of 1-3 °C/min under a pressure from -10 Pa to -5 Pa, and keeping a temperature for 4-10 h under a pressure from 50 Pa to 200 Pa in the temperature-keeping process.
9. The method for preparing the high-nickel cathode material for lithium-ion batteries according to claim 7, wherein the high-temperature sintering specifically comprises: heating up to 750-850 °C at a heating rate of 0.5-2 °C/min under a pressure from -10 Pa to -5 Pa, and keeping a temperature for 4-10 h under a pressure from 5 Pa to 50 Pa in the temperature-keeping process.
10. The high-nickel cathode material for lithium-ion batteries prepared by adopting the preparation method described according to any one of claims 1-9.
LU504854A 2022-10-21 2023-05-31 Method for preparing high-nickel cathode material for lithium-ion batteries and high-nickel cathode material for lithium-ion batteries prepared therefrom LU504854B1 (en)

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