CN116375109A - High-nickel ternary positive electrode material with core-shell structure and preparation method thereof - Google Patents

High-nickel ternary positive electrode material with core-shell structure and preparation method thereof Download PDF

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CN116375109A
CN116375109A CN202310384640.6A CN202310384640A CN116375109A CN 116375109 A CN116375109 A CN 116375109A CN 202310384640 A CN202310384640 A CN 202310384640A CN 116375109 A CN116375109 A CN 116375109A
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nickel
core
shell structure
salt
nickel ternary
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张彬
李阳
谭铁宁
朱高龙
邹昌武
范未峰
华剑锋
戴锋
李立国
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Yibin Libao New Materials Co Ltd
Sichuan New Energy Vehicle Innovation Center Co Ltd
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Sichuan New Energy Vehicle Innovation Center 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
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G51/00—Compounds of cobalt
    • C01G51/40—Cobaltates
    • C01G51/42—Cobaltates containing alkali metals, e.g. LiCoO2
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G53/00—Compounds of nickel
    • C01G53/40—Nickelates
    • C01G53/42—Nickelates containing alkali metals, e.g. LiNiO2
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • 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
    • C01G53/50—Nickelates containing alkali metals, e.g. LiNiO2 containing manganese of the type [MnO2]n-, e.g. Li(NixMn1-x)O2, Li(MyNixMn1-x-y)O2
    • 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
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
    • C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/028—Positive electrodes
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
    • Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
    • Y02E60/10—Energy storage using batteries

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention discloses a high-nickel ternary anode material with a core-shell structure and a preparation method thereof, wherein a nickel-rich compound is used as a core, and a low-nickel compound is used as a shell; the preparation method comprises the steps of taking a zeolite imidazole ester skeleton structure as an intermediate, depositing a layer of low-nickel hydroxide shell on a nickel-rich core in a liquid phase environment, and performing lithium mixing sintering to obtain the nickel-rich core-shell material with stable structure. According to the invention, ZIF-L is used as a sacrificial agent, and a layer of low-nickel shell layer is constructed on the surface of the nickel-rich positive electrode material under the hydrothermal condition by combining a metal salt solution, so that the cycle stability and the thermal stability of the nickel-rich material are improved.

Description

High-nickel ternary positive electrode material with core-shell structure and preparation method thereof
Technical Field
The invention belongs to the technical field of lithium ion battery anode materials, and particularly relates to a high-nickel ternary anode material with a core-shell structure and a preparation method thereof.
Background
Along with the aggravation of energy crisis and environmental pollution, the lithium ion battery becomes the main force army in the fields of electric automobiles and portable electronics because of the advantages of high energy density, good cycle life, no memory effect, relative environmental protection and the like. In the whole battery system, the positive electrode material plays a critical role, and relates to working voltage, specific capacity, power density, energy density, cycle life, safety and the like.
Lithium Nickelate (LNO) and its derivatives, such as lithium nickel cobalt manganese oxide (NCM) or lithium Nickel Cobalt Aluminate (NCA), can provide high specific capacity at an average voltage of 3.8Vvs Li/Li+ with only high nickel content>80%) of the layered nickel-rich NCA or NCM can be>Providing over 200mAh g at 3.8V operating voltage -1 Is a reversible capacity of (a). Therefore, in the battery industry, the development of nickel-rich layered cathode materials is critical. However, nickel-rich layered oxides also have some important drawbacks. Firstly, the problem of cation mixing and discharging is caused by Ni 2+ And Li (lithium) + Has a similar ionic radius, and thus Ni 2+ Li easy to migrate into lattice + The location, causing cation mixing. Second, too high a nickel content in the ternary material results in reduced mechanical stability, therebyResulting in cracking during battery cycling. Finally, as the Ni content increases, the thermal stability of the nickel-rich material in the delithiated state is also progressively poorer.
Disclosure of Invention
The invention aims to provide a preparation method of a high-nickel ternary cathode material with a core-shell structure and the high-nickel ternary cathode material with the core-shell structure, and aims to solve the problems. The invention is composed of a nickel-rich core with higher capacity and a low-nickel shell with good structural stability. The core-shell structure or concentration gradient structure particles with radial orientation grains on the surface reduce the strain among grains to a certain extent and improve the structural stability.
The invention is realized mainly by the following technical scheme:
the preparation method of the high-nickel ternary cathode material with the core-shell structure comprises the following steps:
step S1: mixing the nickel-rich precursor with lithium salt, and sintering in a first oxygen-containing atmosphere to obtain a sintered material;
step S2: dispersing the primary combustion material obtained in the step S1 into a dimethyl imidazole solution, slowly adding a metal salt solution into the dimethyl imidazole solution, uniformly stirring the mixture, and transferring the mixture into a hydrothermal reaction kettle for hydrothermal reaction; the concentration of the dimethyl imidazole solution is 1-4 mol/L, the concentration of the metal salt is 0.2-0.5 mol/L, the hydrothermal reaction temperature is 120-160 ℃, and the reaction time is 2-8 h;
step S3: and (3) sintering the material obtained in the step (S2) in a second oxygen-containing atmosphere to obtain the high-nickel ternary anode material with the core-shell structure.
The invention adopts a nickel-rich compound as a core and a low-nickel compound as a shell; a layer of low-nickel hydroxide shell is deposited on a nickel-rich core in a liquid phase environment by taking a zeolite imidazole ester skeleton structure (ZIF) as an intermediate, and then lithium mixing and sintering are carried out to obtain the nickel-rich core-shell material with stable structure. Preferably, in the step S2, stirring is carried out for 30-60min, and then the mixture is transferred into a hydrothermal reaction kettle for hydrothermal reaction.
In order to better realize the invention, the metal salt is any one or more of cobalt salt, nickel salt, manganese salt, ferric salt and cupric salt.
In order to better realize the invention, further, the mole percent of the cobalt salt is more than 30%.
In order to better realize the invention, further, the metal salt consists of nickel salt, cobalt salt and manganese salt, and the molar ratio is 1:1:1.
In order to better realize the invention, further, the metal salt consists of nickel salt, cobalt salt and manganese salt, and the molar ratio is 5:2:3.
In order to better realize the invention, the nickel-rich precursor is Ni x Co y Mn (1-x-y) (OH) 2 Wherein x is more than or equal to 0.7 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 0.3,1-x-y is more than or equal to 0.
To better practice the invention, further, the molar ratio of the nickel-rich precursor to the lithium source is 1: (1-1.06).
In order to better realize the invention, the sintering temperature in the step S1 is 650-900 ℃ and the sintering time is 5-15 h; the sintering temperature in the step S2 is 700-850 ℃ and the sintering time is 5-12 h.
In order to better realize the invention, further, the partial pressure of oxygen in the first oxygen-containing atmosphere and the second oxygen-containing atmosphere is 0.01-1 standard atmospheric pressure.
The high-nickel ternary anode material with the core-shell structure is prepared by adopting the method.
The beneficial effects of the invention are as follows:
most of the prior art adopts inorganic reaction, the thickness deposited on the surface layer of the particles is not uniform, the too thick area is not beneficial to the capacity exertion, and the too thin area can not play a role brought by the shell, so that the circulation performance is affected. According to the invention, ZIF-L is used as a sacrificial agent, and is easier to hydrolyze in a liquid phase environment to generate metal hydroxide, so that the metal hydroxide uniformly grows on the surface of the nickel-rich positive electrode to form a uniform core-shell structure. According to the invention, ZIF-L is used as a sacrificial agent, and a layer of low-nickel shell layer is constructed on the surface of the nickel-rich positive electrode material under the hydrothermal condition by combining a metal salt solution, so that the cycle stability and the thermal stability of the nickel-rich material are improved.
The high-nickel ternary positive electrode material modified by the low-nickel layer has high core-shell structure strength of radial oriented grains, reduces strain among grains to a certain extent, and reduces the amount of electrolyte entering the particle core due to microcracks. As the electrolyte is blocked from being directly contacted with the nickel-rich phase, the circulation stability and the thermal stability are greatly improved while the original specific capacity is basically maintained.
Drawings
FIG. 1 is a schematic diagram of a core-shell structure of the present invention;
fig. 2 is a plot of the surface scanning element profile of the high nickel ternary cathode material of core-shell structure in example 1.
Detailed Description
Example 1:
a preparation method of a high nickel ternary positive electrode material with a core-shell structure comprises the steps of firstly preparing Ni (OH) 2 Uniformly mixing the precursor and LiOH by a high-speed mixer according to the molar ratio of 1:1.06, then loading into a sagger, placing into an oxygen atmosphere furnace, heating to 500 ℃ at 5 ℃/min for 5h, heating to 650 ℃ at 2 ℃/min for 10h, and cooling to 300 ℃ at 2 ℃/min to obtain the burned material LiNiO 2 。
10g of LiNiO 2 Dispersing into 40mL of 2-MIM solution with concentration of 4mol/L, slowly adding 20mL of Co (NO) with concentration of 0.5mol/L 3 ) 2 Stirring the solution for 30min, transferring into a polytetrafluoroethylene hydrothermal reaction kettle, preserving heat for 8h at 120 ℃, and filtering, washing and drying to obtain the cobalt hydroxide shell coated high nickel anode material. Transferring into an oxygen atmosphere furnace, and sintering at 700 ℃ for 8 hours to obtain LiNiO 2 +LiCoO 2 High nickel ternary positive electrode material (LNO@LCO) with core-shell structure.
Example 2:
a process for preparing high-Ni ternary positive electrode material with core-shell structure includes such steps as preparing Ni from Ni 0.95 Co 0.02 Mn 0.03 (OH) 2 Uniformly mixing the precursor and LiOH by a high-speed mixer according to the mol ratio of 1:1.05, then loading into a sagger, placing into an oxygen atmosphere furnace, heating to 500 ℃ at 5 ℃/min, preserving heat for 5 hours, and then heating to 2 ℃/miHeating n to 720 ℃, preserving heat for 15h, and then cooling to 300 ℃ at 2 ℃/min to obtain a burned material LiNi 0.95 Co 0.02 Mn 0.03 O 2 。
10g of LiNi 0.95 Co 0.02 Mn 0.03 O 2 Dispersing into 40mL (concentration 1 mol/L) 2-MIM solution, and slowly adding 20mL of Co (NO) 3 ) 2 (concentration of 0.2 mol/L), ni (NO) 3 ) 2 (concentration of 0.2 mol/L) and Mn (NO) 3 ) 2 (concentration of 0.2 mol/L) solution, and Ni: co: mn in the molar ratio of 1:1:1, stirring for 60min, transferring into a polytetrafluoroethylene hydrothermal reaction kettle, preserving heat for 2h at 160 ℃, and filtering, washing and drying to obtain the cobalt hydroxide shell coated high-nickel anode material. Transferring into an oxygen atmosphere furnace, and sintering at 750deg.C for 8 hr to obtain LiNi 0.95 Co 0.02 Mn 0.03 O 2 +LiNi 0.33 Co 0.33 Mn 0.33 O 2 High nickel ternary positive electrode material (Ni95@NCM111) with core-shell structure.
Example 3:
a process for preparing high-Ni ternary positive electrode material with core-shell structure includes such steps as preparing Ni from Ni 0.7 Co 0.1 Mn 0.2 (OH) 2 Uniformly mixing the precursor and LiOH by a high-speed mixer according to the molar ratio of 1:1.03, then loading into a sagger, placing into an oxygen atmosphere furnace, heating to 500 ℃ at 5 ℃/min for 5h, heating to 900 ℃ at 2 ℃/min for 15h, and cooling to 300 ℃ at 2 ℃/min to obtain a burned material LiNi 0.7 Co 0.1 Mn 0.2 O 2 。
10g of LiNi 0.7 Co 0.1 Mn 0.2 O 2 Dispersing into 40mL of 2-MIM solution with concentration of 2mol/L, and slowly adding 20mL of Co (NO) 3 ) 2 (concentration of 0.3 mol/L), ni (NO) 3 ) 2 (concentration of 0.3 mol/L) and Mn (NO) 3 ) 2 (concentration of 0.3 mol/L) solution, and Ni: co: mn in a molar ratio of 5:2:3, stirring for 45min, transferring into a polytetrafluoroethylene hydrothermal reaction kettle, preserving heat for 4h at 140 ℃, and filtering, washing and drying to obtain the cobalt hydroxide shell coated high-nickel anode material. Then transferring the mixture into an oxygen atmosphere furnace,sintering for 8h at 850 ℃ to obtain LiNi 0.7 Co 0.1 Mn 0.2 O 2 +LiNi 0.5 Co 0.2 Mn 0.3 O 2 High nickel ternary positive electrode material (Ni70@NCM523) with core-shell structure.
Comparative example 1: first Ni (OH) 2 Uniformly mixing the precursor and LiOH by a high-speed mixer according to the molar ratio of 1:1.06, then loading into a sagger, placing into an oxygen atmosphere furnace, heating to 500 ℃ at 5 ℃/min for 5h, heating to 650 ℃ at 2 ℃/min for 10h, and cooling to 300 ℃ at 2 ℃/min to obtain the burned material LiNiO 2 (i.e., LNO).
Repairing and regenerating a positive electrode material, a conductive agent (Super P) and a binder (dissolved in NMP (N-methyl Pyrrolidone) (PVDF) according to the mass ratio of 90:5:5) according to the embodiment 1 to the comparative example 1, and weighing materials with corresponding mass in a stirring box; and placing the stirring box in a homogenizer with a set program, uniformly mixing the materials, uniformly coating the materials on an aluminum foil with the thickness of 16 mu m by a coating machine, controlling the coating thickness to be 0.25mm, and drying, cutting, weighing and editing to obtain the positive plate with the diameter of 14 mm. The negative electrode uses metallic lithium and LiPF 6 EC/EMC electrolyte and PE separator CR2032 button cell was assembled.
After the button cell was left for 10 hours, the button cell was set on a blue electric tester (CT 2001C) and charge-discharge cycle performance was measured. The test conditions of the lithium-rich manganese-based material were set as follows: the specific capacity and cycle performance of the positive electrode material were examined at 25℃for 2.7 to 4.3V at 1C/1C for 50 weeks after 3 weeks of activation of the button half cell at 0.1C/0.1C cycle, and the specific electrochemical properties are shown in Table 1.
As shown in FIG. 1, the structure of the invention is a nickel-rich core-low nickel shell, and as shown in FIG. 2, the invention successfully prepares particles with a concentration gradient structure, so that the strain among the particles is reduced to a certain extent, and the amount of electrolyte entering the particle core due to microcracks can be reduced. Analysis of example 1 and comparative example 1 revealed that the discharge capacity of the high nickel ternary cathode material of the core-shell structure was hardly changed, and the first charge and discharge efficiency, the 50-cycle performance and the thermal runaway temperature were significantly improved. And the high nickel ternary cathode material with the core-shell structure prepared in the embodiment 3 has relatively excellent performance. The invention can maintain original specific capacity, and improve circulation stability and thermal stability.
TABLE 1
Figure BDA0004173400080000041
The foregoing description is only a preferred embodiment of the present invention, and is not intended to limit the present invention in any way, and any simple modification, equivalent variation, etc. of the above embodiment according to the technical matter of the present invention fall within the scope of the present invention.

Claims (10)

1. The preparation method of the high-nickel ternary cathode material with the core-shell structure is characterized by comprising the following steps of:
step S1: mixing the nickel-rich precursor with lithium salt, and sintering in a first oxygen-containing atmosphere to obtain a sintered material;
step S2: dispersing the primary combustion material obtained in the step S1 into a dimethyl imidazole solution, slowly adding a metal salt solution into the dimethyl imidazole solution, uniformly stirring the mixture, and performing a hydrothermal reaction; the concentration of the dimethylimidazole solution is 1-4 mol/L, the concentration of the metal salt is 0.2-0.5 mol/L, the hydrothermal reaction temperature is 120-160 ℃, and the reaction time is 2-8 hours;
step S3: and (3) sintering the material obtained in the step (S2) in a second oxygen-containing atmosphere to obtain the high-nickel ternary anode material with the core-shell structure.
2. The preparation method of the high-nickel ternary cathode material with the core-shell structure, which is characterized in that the metal salt is any one or more of cobalt salt, nickel salt, manganese salt, ferric salt and cupric salt.
3. The method for preparing the high-nickel ternary cathode material with the core-shell structure according to claim 2, wherein the mole percentage of the cobalt salt is more than 30%.
4. The method for preparing the high-nickel ternary cathode material with the core-shell structure according to claim 3, wherein the metal salt consists of nickel salt, cobalt salt and manganese salt, and the molar ratio is 1:1:1.
5. The method for preparing the high-nickel ternary cathode material with the core-shell structure according to claim 3, wherein the metal salt consists of nickel salt, cobalt salt and manganese salt, and the molar ratio is 5:2:3.
6. The method for preparing a high-nickel ternary cathode material with a core-shell structure according to claim 1, wherein the nickel-rich precursor is Ni x Co y Mn (1-x-y) (OH) 2 Wherein x is more than or equal to 0.7 and less than or equal to 1, y is more than or equal to 0 and less than or equal to 0.3, and 1-x-y is more than or equal to 0.
7. The method for preparing the high-nickel ternary cathode material with the core-shell structure according to claim 6, wherein the molar ratio of the nickel-rich precursor to the lithium source is 1: (1-1.06).
8. The preparation method of the high-nickel ternary cathode material with the core-shell structure according to claim 1 or 6, wherein the sintering temperature in the step S1 is 650-900 ℃ and the sintering time is 5-15 h; the sintering temperature in the step S2 is 700-850 ℃ and the sintering time is 5-12 h.
9. The method for preparing the high-nickel ternary cathode material with the core-shell structure, according to claim 8, wherein the partial pressure of oxygen in the first oxygen-containing atmosphere and the second oxygen-containing atmosphere is 0.01-1 standard atmosphere.
10. A high nickel ternary cathode material with a core-shell structure, which is characterized by being prepared by the method of any one of claims 1-9.
CN202310384640.6A 2023-04-12 2023-04-12 High-nickel ternary positive electrode material with core-shell structure and preparation method thereof Pending CN116375109A (en)

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Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106099047A (en) * 2016-08-25 2016-11-09 深圳市贝特瑞纳米科技有限公司 A kind of surface coating method of electrode material and application thereof
CN115172756A (en) * 2022-09-06 2022-10-11 潍坊学院 Single crystal coated polycrystalline anode material with concentration gradient and preparation method thereof

Patent Citations (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN106099047A (en) * 2016-08-25 2016-11-09 深圳市贝特瑞纳米科技有限公司 A kind of surface coating method of electrode material and application thereof
CN115172756A (en) * 2022-09-06 2022-10-11 潍坊学院 Single crystal coated polycrystalline anode material with concentration gradient and preparation method thereof

Non-Patent Citations (1)

* Cited by examiner, † Cited by third party
Title
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