CN105932321A - Doped micro-scale single-crystal ternary positive electrode material and preparation method thereof - Google Patents

Doped micro-scale single-crystal ternary positive electrode material and preparation method thereof Download PDF

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CN105932321A
CN105932321A CN201610443127.XA CN201610443127A CN105932321A CN 105932321 A CN105932321 A CN 105932321A CN 201610443127 A CN201610443127 A CN 201610443127A CN 105932321 A CN105932321 A CN 105932321A
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cathode material
tertiary cathode
lithium
doping type
micron order
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陈人杰
魏磊
吴锋
李丽
王萌
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Beijing Institute of Technology BIT
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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
    • 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
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • 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
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/388—Halogens
    • 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
    • H01M4/481—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mercury
    • 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
    • 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

Abstract

The invention relates to a doped micro-scale single-crystal ternary positive electrode material and a preparation method thereof, and belongs to the technical field of lithium-ion battery materials. The particle sizes of the ternary positive electrode material are 1-8 microns and the compaction density is 3.6-4.3g/cm<3>; and a proper amount of metal ions and fluoride ions are doped, so that the cycle performance of the ternary positive electrode material is obviously improved. The preparation method of the ternary positive electrode material comprises the following steps: firstly, crushing a ternary precursor in a ball mill tank; adding a lithium salt, an M-containing compound and a fluoride to the ball mill tank; mixing the lithium salt, the M-containing compound and the fluoride evenly; and putting the mixture into an oxygen atmosphere and carrying out constant-temperature calcination at 800-1200 DEG C for 10-20 hours to obtain the ternary positive electrode material.

Description

A kind of doping type micron order monocrystalline tertiary cathode material and preparation method thereof
Technical field
The present invention relates to a kind of doping type micron order monocrystalline tertiary cathode material and preparation method thereof, be specifically related to A kind of tertiary cathode material LiNixCoyMnzM1-x-y-zO2-nFnAnd preparation method thereof, belong to lithium ion battery material Material technical field.
Background technology
Compared with other secondary cell, lithium ion battery has that specific energy is high, volume is little, light weight and circulation The advantages such as performance length, have been widely used in notebook computer, digital camera, mobile device etc. portable In electronic equipment.Due to LiCoO2Materials theory finite capacity, and Co element is poisonous, scarcity of resources, Expensive, so hinder its development in electrokinetic cell field always.As LiCoO2Positive electrode replaces The LiNi of Dai PinxCoyMnzO2(0 < x, y, z < 1) tertiary cathode material have high power capacity, security performance good, Advantage with low cost, becomes one of focus of everybody research.But, the most traditional ternary material is general Being all by the spherical second particle of the spherical of the least particle aggregation or class, this pattern not only can make material In the nipping process prepare electrode slice, it is susceptible to second particle crush, and causes its compacted density relatively low (typically at 3.5g/cm3Left and right), thus significantly limit ternary material in high energy density cells Application.
Summary of the invention
For defect present in prior art, it is an object of the invention to provide a kind of doping type micron order list Brilliant tertiary cathode material and preparation method thereof, is doped with appropriate gold in tertiary cathode material of the present invention Belong to ion and fluorion, and there is good chemical property；By the optimization of sintering process, preparation Tertiary cathode material has higher compacted density.
It is an object of the invention to be achieved through the following technical solutions.
A kind of doping type micron order monocrystalline tertiary cathode material, the chemical formula of described tertiary cathode material is LiNixCoyMnzM1-x-y-zO2-nFn；Wherein, 0 < x < 1,0 < y < 1,0 < z < 1,0 < n < 0.5, M be Al, More than one in Mg or Ti.
The grain diameter of doping type micron order monocrystalline tertiary cathode material is 1～8 μm.
A kind of preparation method of doping type micron order monocrystalline tertiary cathode material as described in the present invention, described system Preparation Method specifically comprises the following steps that
Ternary precursor is added in ball grinder by step 1., ball mill pulverizing 1～6h under 100～600r/min；So After again lithium salts, compound containing M and fluoride are added in ball grinder, ball milling under 100～600r/min Batch mixing 1～6h, the mixture being uniformly mixed；
Mixture is placed in oxygen atmosphere by step 2., is then heated to the heating rate of 0.1～5 DEG C/min 800～1200 DEG C, again with the rate of temperature fall cooling of 0.1～5 DEG C/min after calcining at constant temperature 10～20h, obtain described Tertiary cathode material；
Described ternary precursor is the hydroxide containing Ni, Co and Mn or oxide；
In step 1, ternary precursor is 1:1.03～1.13 with the mol ratio of lithium salts.
More than one in the preferred lithium nitrate of described lithium salts, Quilonorm (SKB), lithium carbonate or Lithium hydrate.
The described preferred aluminum nitrate of the compound containing M, aluminium acetate, aluminium oxide, aluminium hydroxide, magnesium nitrate, second More than one in acid magnesium, magnesium oxide, magnesium hydroxide, titanium oxide, titanium hydroxide or butyl titanate.
More than one in described fluoride preferred fluorinated lithium, Afluon (Asta) or aluminium fluoride.
Beneficial effect:
(1) in doping type micron order monocrystalline tertiary cathode material of the present invention, by the appropriate gold that adulterates Belong to ion and fluorion, hence it is evident that improve the cycle performance of tertiary cathode material；Joined by regulation and control sintering process Number, the tertiary cathode material obtained has higher compacted density, and compacted density is 3.6～4.3g/cm3。
(2) preparation method technique of the present invention is simple, the good product consistency of preparation, is suitable for extensive Produce.
Accompanying drawing explanation
Fig. 1 is scanning electron microscope (SEM) figure of the tertiary cathode material of preparation in embodiment 1.
Fig. 2 is X-ray diffraction (XRD) figure of the tertiary cathode material of preparation in embodiment 2.
Fig. 3 be in embodiment 3 tertiary cathode material of preparation at 25 DEG C, the first charge-discharge of test under 0.5C Curve chart.
Fig. 4 be in embodiment 4 tertiary cathode material of preparation at 25 DEG C, the cycle performance curve of test under 1C Figure.
Detailed description of the invention
Below in conjunction with detailed description of the invention, the present invention will be further described.
In following example:
Ball mill: vertical semicircle planetary ball mill XQM-2A Changsha Tian Chuan powder company limited；
Scanning electron microscope: FEI Co. of Quanata200f type scanning electron microscope Holland；
X-ray diffractometer: Ultima IV-185 type X-ray diffractometer Rigaku company；
The assembling of lithium ion battery: the tertiary cathode material for preparing in embodiment, acetylene black, poly-inclined fluorine Ethylene is mixed by the mass ratio of 8:1:1, is coated on aluminium foil by the slurry of mix homogeneously, is then placed in The vacuum drying oven of 100 DEG C is dried, dried aluminium foil is carried out roll-in, cut-parts, the aluminium foil cut out As positive electrical pole piece；Metal lithium sheet is as negative electricity pole piece, and barrier film is Celgard barrier film；In electrolyte, Solvent be volume ratio be the dimethyl carbonate of 1:1:1, diethyl carbonate, ethylene carbonate mixed solution, lithium salts LiPF for 1mol/L6；In the glove box of full argon, it is assembled into CR2025 type button cell；Will system After the lithium ion battery got ready shelves 24h, then carry out on Land test system (Wuhan Jin Nuo company) Electrochemical property test.
Embodiment 1
Step 1. is by 45.8050g Ni0.5Co0.2Mn0.3(OH)2Add in ball grinder, ball milling under 400r/min Pulverize 1h；The most again 17.1840g lithium carbonate, 18.7600g aluminum nitrate and 1.2970g lithium fluoride are added In ball grinder, ball mill mixing 6h under 200r/min, the mixture being uniformly mixed；
Mixture is placed in the tube furnace of oxygen atmosphere by step 2., then adds with the heating rate of 0.1 DEG C/min Heat, to 900 DEG C, again with the rate of temperature fall cooling of 0.6 DEG C/min after calcining at constant temperature 10h, obtains doping type micron Level monocrystalline tertiary cathode material.
It will be seen that tertiary cathode material prepared by the present embodiment is particle diameter exists from the SEM figure of Fig. 1 Granule between 1～4 μm, dispersibility is preferable.XRD figure from the tertiary cathode material prepared by the present embodiment In it will be seen that XRD spectra does not has obvious dephasign peak and peak type sharp-pointed, illustrate that this material has higher Degree of crystallinity, for monocrystalline phase.Tablet machine is utilized to be compacted by the tertiary cathode material prepared by the present embodiment, pressure Solid area is 1.32cm2, pressure is 2000kg, then compacted density is 4.3g/cm3。
Tertiary cathode material prepared by the present embodiment is assembled into CR2025 type button cell, then exists 25 DEG C, carry out performance test under 0.5C charge-discharge magnification, discharge capacity is 170.3mAh/g first, the 40th The discharge capacity of circle is 167.5mAh/g.
Embodiment 2
Step 1. is by 42.8780g Ni1/3Co1/3Mn1/3(OH)2Add in ball grinder, ball milling under 500r/min Pulverize 2h；The most again 11.9573g Lithium hydrate, 17.0180g butyl titanate and 6.2302g are fluorinated Magnesium adds in ball grinder, ball mill mixing 3h under 500r/min, the mixture being uniformly mixed；
Mixture is placed in the tube furnace of oxygen atmosphere by step 2., then adds with the heating rate of 3.5 DEG C/min Heat, to 1000 DEG C, again with the rate of temperature fall cooling of 0.1 DEG C/min after calcining at constant temperature 15h, obtains doping type micron Level monocrystalline tertiary cathode material.
It is known that this tertiary cathode material from the SEM figure of the tertiary cathode material prepared by this enforcement Grain diameter is 2～5 μm.Can from the XRD figure of the tertiary cathode material prepared by Fig. 2 the present embodiment Go out, XRD spectra do not have obvious dephasign peak and peak type sharp-pointed, illustrate that this material has higher degree of crystallinity, For monocrystalline phase.Utilizing tablet machine to be compacted by the tertiary cathode material prepared by the present embodiment, compaction area is 1.32 cm2, pressure is 2000kg, then compacted density is 4.1g/cm3。
Tertiary cathode material prepared by the present embodiment is assembled into CR2025 type button cell, then exists 25 DEG C, carry out performance test under 0.5C charge-discharge magnification, discharge capacity is 175.3mAh/g first, the 40th The discharge capacity of circle is 170.1mAh/g.
Embodiment 3
Step 1. is by 44.9900g Ni0.6Co0.2Mn0.2O2Add in ball grinder, ball mill pulverizing under 500r/min 3h；The most again 9.5800g Lithium hydrate, 9.2185g magnesium nitrate and 3.8910g lithium fluoride are added ball milling In tank, ball mill mixing 1h under 500r/min, the mixture being uniformly mixed；
Mixture is placed in the tube furnace of oxygen atmosphere by step 2., then heats with the heating rate of 5 DEG C/min To 1200 DEG C, again with the rate of temperature fall cooling of 5 DEG C/min after calcining at constant temperature 20h, obtain doping type micron order Monocrystalline tertiary cathode material.
It is known that this tertiary cathode material from the SEM figure of the tertiary cathode material prepared by this enforcement Grain diameter is 4～8 μm.From the XRD figure of the tertiary cathode material prepared by the present embodiment it will be seen that XRD spectra does not has obvious dephasign peak and peak type sharp-pointed, illustrate that this material has higher degree of crystallinity, for Monocrystalline phase.Utilizing tablet machine to be compacted by the tertiary cathode material prepared by the present embodiment, compaction area is 1.32 cm2, pressure is 2000kg, then compacted density is 3.6g/cm3。
Tertiary cathode material prepared by the present embodiment is assembled into CR2025 type button cell, then exists 25 DEG C, carry out performance test under 0.5C charge-discharge magnification, discharge capacity is 177.5mAh/g first, refers to figure 3；The discharge capacity of the 40th circle is 175.1mAh/g.
Embodiment 4
Step 1. is by 44.8050g Ni0.5Co0.2Mn0.3O2Add in ball grinder, ball mill pulverizing under 600r/min 1.5h；The most again 20.3198g lithium carbonate, 10.7230g magnesium acetate and 4.1990g aluminium fluoride are added ball milling In tank, ball mill mixing 5h under 600r/min, the mixture being uniformly mixed；
Mixture is placed in the tube furnace of oxygen atmosphere by step 2., then heats with the heating rate of 2 DEG C/min To 950 DEG C, again with the rate of temperature fall cooling of 3 DEG C/min after calcining at constant temperature 11h, obtain doping type micron order list Brilliant tertiary cathode material.
It is known that this tertiary cathode material from the SEM figure of the tertiary cathode material prepared by this enforcement Grain diameter is 3～7 μm.From the XRD figure of the tertiary cathode material prepared by the present embodiment it will be seen that XRD spectra does not has obvious dephasign peak and peak type sharp-pointed, illustrate that this material has higher degree of crystallinity, for Monocrystalline phase.Utilizing tablet machine to be compacted by the tertiary cathode material prepared by the present embodiment, compaction area is 1.32 cm2, pressure is 2000kg, then compacted density is 3.9g/cm3。
Tertiary cathode material prepared by the present embodiment is assembled into CR2025 type button cell, then exists 25 DEG C, carry out performance test under 1C charge-discharge magnification, discharge capacity is 168.5mAh/g first；40th circle Discharge capacity be 163.7mAh/g, capability retention is 97.2%, refers to Fig. 4.
In sum, these are only presently preferred embodiments of the present invention, be not intended to limit the guarantor of the present invention Protect scope.All within the spirit and principles in the present invention, any modification, equivalent substitution and improvement etc. made, Should be included within the scope of the present invention.

Claims (6)

1. a doping type micron order monocrystalline tertiary cathode material, it is characterised in that: described tertiary cathode material Chemical formula be LiNixCoyMnzM1-x-y-zO2-nFn；Wherein, 0 < x < 1,0 < y < 1,0 < z < 1,0 < n < 0.5, M is more than one in Al, Mg or Ti.
A kind of doping type micron order monocrystalline tertiary cathode material the most according to claim 1, its feature exists In: the grain diameter of doping type micron order monocrystalline tertiary cathode material is 1～8 μm.
3. the preparation side of a doping type micron order monocrystalline tertiary cathode material as claimed in claim 1 or 2 Method, it is characterised in that: described preparation method specifically comprises the following steps that
Ternary precursor is added in ball grinder by step 1., ball mill pulverizing 1～6h under 100～600r/min；So After again lithium salts, compound containing M and fluoride are added in ball grinder, ball milling under 100～600r/min Batch mixing 1～6h, the mixture being uniformly mixed；
Mixture is placed in oxygen atmosphere by step 2., is then heated to the heating rate of 0.1～5 DEG C/min 800～1200 DEG C, again with the rate of temperature fall cooling of 0.1～5 DEG C/min after calcining at constant temperature 10～20h, obtain described Tertiary cathode material；
Described ternary precursor is the hydroxide containing Ni, Co and Mn or oxide；
In step 1, ternary precursor is 1:1.03～1.13 with the mol ratio of lithium salts.
The preparation side of a kind of doping type micron order monocrystalline tertiary cathode material the most according to claim 3 Method, it is characterised in that: described lithium salts be one in lithium nitrate, Quilonorm (SKB), lithium carbonate or Lithium hydrate with On.
The preparation side of a kind of doping type micron order monocrystalline tertiary cathode material the most according to claim 3 Method, it is characterised in that: the described compound containing M be aluminum nitrate, aluminium acetate, aluminium oxide, aluminium hydroxide, In magnesium nitrate, magnesium acetate, magnesium oxide, magnesium hydroxide, titanium oxide, titanium hydroxide or butyl titanate one More than Zhong.
The preparation side of a kind of doping type micron order monocrystalline tertiary cathode material the most according to claim 3 Method, it is characterised in that: described fluoride is more than one in lithium fluoride, Afluon (Asta) or aluminium fluoride.
CN201610443127.XA 2016-06-20 2016-06-20 Doped micro-scale single-crystal ternary positive electrode material and preparation method thereof Pending CN105932321A (en)

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CN110265634A (en) * 2019-05-09 2019-09-20 浙江美都海创锂电科技有限公司 A kind of preparation method of the nickelic NCM anode material for lithium-ion batteries of monocrystalline
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CN113213553A (en) * 2021-04-28 2021-08-06 北京理工大学重庆创新中心 Concentration gradient doped lithium-rich manganese-based positive electrode material and preparation method thereof
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CN113422042A (en) * 2021-07-08 2021-09-21 贵州大学 Anion-cation co-doped NCM811 type high-nickel ternary material and preparation and application thereof
CN113437289A (en) * 2021-06-29 2021-09-24 中钢天源股份有限公司 High-capacity single crystal cathode material and preparation method thereof
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US10938030B2 (en) 2017-04-28 2021-03-02 Samsung Electronics Co., Ltd. Positive active material, positive electrode and lithium secondary battery containing the material, and method of preparing the material
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CN109796052A (en) * 2019-01-24 2019-05-24 桑顿新能源科技有限公司 Positive electrode and preparation method thereof and lithium ion battery
CN109796052B (en) * 2019-01-24 2023-03-14 湖南桑瑞新材料有限公司 Cathode material, preparation method thereof and lithium ion battery
CN110112385A (en) * 2019-04-24 2019-08-09 南昌大学 A method of improving tertiary cathode material stability and high rate performance
US20220052338A1 (en) * 2019-04-28 2022-02-17 Contemporary Amperex Technology Co., Limited Positive electrode active material, positive electrode plate, lithium-ion secondary battery, and apparatus
CN110265634A (en) * 2019-05-09 2019-09-20 浙江美都海创锂电科技有限公司 A kind of preparation method of the nickelic NCM anode material for lithium-ion batteries of monocrystalline
CN110808370A (en) * 2019-10-25 2020-02-18 合肥国轩高科动力能源有限公司 Ternary cathode material of lithium ion battery and preparation method and application thereof
US11121362B2 (en) * 2019-12-02 2021-09-14 Contemporary Amperex Technology Co., Limited Positive electrode sheet for secondary battery, secondary battery, battery module, battery pack, and apparatus
CN111416118A (en) * 2020-03-31 2020-07-14 江门市科恒实业股份有限公司 High-voltage ternary cathode material and preparation method thereof
WO2022138848A1 (en) * 2020-12-24 2022-06-30 パナソニックＩｐマネジメント株式会社 Positive electrode active material for nonaqueous electrolyte secondary batteries, and nonaqueous electrolyte secondary battery
CN113213553A (en) * 2021-04-28 2021-08-06 北京理工大学重庆创新中心 Concentration gradient doped lithium-rich manganese-based positive electrode material and preparation method thereof
CN113437289A (en) * 2021-06-29 2021-09-24 中钢天源股份有限公司 High-capacity single crystal cathode material and preparation method thereof
CN113422042A (en) * 2021-07-08 2021-09-21 贵州大学 Anion-cation co-doped NCM811 type high-nickel ternary material and preparation and application thereof
CN115000429A (en) * 2022-04-07 2022-09-02 湖北大学 LNCAF electrode material, fuel cell and preparation method thereof
CN115000429B (en) * 2022-04-07 2024-01-16 湖北大学 LNCAF electrode material, fuel cell and preparation method thereof

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Application publication date: 20160907