CN107785561A - A kind of preparation method of high voltage monocrystalline lithium ion tertiary cathode material - Google Patents
A kind of preparation method of high voltage monocrystalline lithium ion tertiary cathode material Download PDFInfo
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- CN107785561A CN107785561A CN201711173950.4A CN201711173950A CN107785561A CN 107785561 A CN107785561 A CN 107785561A CN 201711173950 A CN201711173950 A CN 201711173950A CN 107785561 A CN107785561 A CN 107785561A
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- H—ELECTRICITY
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- 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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- 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
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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
- H01M4/50—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
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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
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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
- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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- 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
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Abstract
The present invention relates to a kind of preparation method of high voltage monocrystalline lithium ion tertiary cathode material, its step includes：After small grain size ternary anode material precursor, lithium source mixing, the tertiary cathode material of monocrystalline pattern is obtained through oversintering, crushing, by the tertiary cathode material and Al of the monocrystalline pattern of above-mentioned acquisition2O3、TiO2, after mixing, by the tertiary cathode material of once sintered monocrystalline pattern, obtain doping Ti and coat Al high voltage monocrystalline lithium ion tertiary cathode material；The preparation method of the present invention can reduce processing step, reduce production cost, and can improve crystal structural stability, suppress the side reaction of plane of crystal, so as to improve the chemical property of material.
Description
Technical field
The invention belongs to anode material for lithium-ion batteries technical field, more particularly to a kind of high voltage monocrystalline lithium ion ternary
The preparation method of positive electrode.
Background technology
In recent years, the demand of tertiary cathode material increases substantially, and the demand of particularly 2017 new-energy automobiles is pre-
Meter increases by 120%.2017, the yield of first quarter country's positive electrode is about 3.8 ten thousand tons, and wherein tertiary cathode material accounts for
Than maximum, the shipment amount of the positive electrodes such as LiFePO4, LiMn2O4, cobalt acid lithium is exceeded.Monocrystalline ternary is because of its high voltage, high pressure
Real characteristic, it is the regeneration product of traditional secondary spheric granules ternary material.
At present, the ternary material of traditional secondary spheric granules has that structural integrity is poor, primary particle size is small and fault of construction
More, inside be difficult to cladding cause the median surface side reaction of high voltage charge and discharge process to be difficult to suppress, easy inflatable the problems such as.Study table
It is bright, the ternary material of secondary spherical particle is transformed into the tertiary cathode material of monocrystalline pattern, effectively improves the machine of structure
Tool intensity has increased compacted density, has reduced specific surface area so as to reduce side reaction, can uniformly coat, make surface is smooth to be advantageous to lithium
The advantages such as ion transport.
Research shows, Ti4+Ratio of ionic radii Ni3+、Co3+、Mn4+Radius it is bigger, adulterate Ti4+Positive electrode can be made
The increase of crystal structure radius, reduces lithium ion diffusional resistance, makes structure more stable.And Al3+Surface coating tertiary cathode material,
Corrosion of the electrolyte to active material can be effectively prevented, maintains the structural stability of active material, so as to improve following for material
Ring stability.Application No. CN 201610739897 patent application stresses using multiple element, using specific high temperature sintering
Technique synthetic single crystal pattern and the tertiary cathode material and its preparation technology under high voltages with excellent electrochemical performance, still
Sintering process is relatively complicated, and application value in production has much room for improvement.
The content of the invention
The problem of existing for prior art, it is an object of the invention to provide a kind of high voltage monocrystalline lithium ion tertiary cathode
The preparation method of material.The present invention coats, adulterates and regulated and controled the sintering process of multistage temperature curve by element, is adulterated
Ti and cladding Al high voltage monocrystalline ternary material.
In order to achieve the above object, technical scheme is as follows：
A kind of preparation method of high voltage monocrystalline lithium ion tertiary cathode material, comprises the following steps：
(1) by ternary anode material precursor and lithium source in molar ratio 1:0.5-2 is well mixed；
(2) in air ambient, the mixture that step (1) obtains is sintered；
(3) crushed after the completion of sintering, obtain the tertiary cathode material of monocrystalline pattern；
(4) tertiary cathode material for the monocrystalline pattern for obtaining step (3) is 1 in molar ratio with Al2O3, TiO2：a：B enters
Row mixing, wherein 0≤a≤0.15,0≤b≤0.04；
(5) in air ambient, the mixture that step (4) obtains is sintered；
(6) crushed after the completion of sintering, obtain adulterating Ti and coat Al high voltage monocrystalline lithium ion tertiary cathode material
Material.
Preferably, the chemical formula of the ternary anode material precursor is Ni1-x-yCoxMnyO2, wherein 0 ＜ x≤0.2,0 ＜
y≤0.3。
Preferably, the chemical formula of the tertiary cathode material of the monocrystalline pattern is LiNi1-x-yCoxMnyO2, wherein 0 ＜ x≤
0.2,0 ＜ y≤0.3
Preferably, the particle diameter of the ternary anode material precursor is 3-6 μm.
Preferably, the lithium source is selected from Li2CO3At least one of with LiOH.
Preferably, in step (2), to be incubated 5 hours after being raised to 700-750 DEG C with 4 hours the step of the sintering, 2
Hour is incubated 10 hours after being raised to 860-960 DEG C
Preferably, in step (5), to be incubated 4 hours after being raised to 600-650 DEG C with 3 hours the step of the sintering, 2
Hour is incubated 4 hours after being raised to 700-730 DEG C, is incubated 8 hours after being raised to 800-850 DEG C within 1 hour, is raised to 890-930 DEG C within 1 hour
It is incubated 10 hours afterwards.
Preferably, in step (3) and step (6), the crushing is air-flow crushing or mechanical crushing.
A kind of high voltage monocrystalline lithium ion tertiary cathode material, it is prepared by above-mentioned preparation method.
Beneficial effects of the present invention
After the present invention is using small grain size ternary anode material precursor, lithium source mixing, is sintered by multistage temperature, crush and obtain
The tertiary cathode material of monocrystalline pattern is obtained, then by the tertiary cathode material and Al of the monocrystalline pattern2O3、TiO2After mixing, lead to
Cross that multistage temperature is once sintered, obtain doping Ti and coat Al high voltage monocrystalline lithium ion tertiary cathode material.The present invention's
Method can reduce technological process, reduce production cost, and can improve crystal structural stability, and the pair for suppressing plane of crystal is anti-
Should, so as to improve the chemical property of material.
Brief description of the drawings
Fig. 1 is the SEM figures of the tertiary cathode material of the monocrystalline pattern prepared by embodiment 1；
Fig. 2 is the high-resolution SEM figures of the tertiary cathode material of the monocrystalline pattern prepared by embodiment 1；
Fig. 3 is the SEM figures of the high voltage monocrystalline lithium ion tertiary cathode material prepared by embodiment 1；
Fig. 4 is the high-resolution SEM figures of the high voltage monocrystalline lithium ion tertiary cathode material prepared by embodiment 1；
Fig. 5 is the tertiary cathode of the high voltage monocrystalline lithium ion tertiary cathode material and monocrystalline pattern prepared by embodiment 1
The comparison diagram of the electrochemistry cycle performance discharge capacity of material.
Embodiment
The present invention is expanded on further below by way of specific embodiment, but this is not limitation of the present invention, this area phase
Various modifications and improvements of the technical staff according to made by the basic thought of the present invention are closed, without departing from the basic think of of the present invention
Think, within the scope of the present invention.
Embodiment 1
A kind of preparation method of high voltage monocrystalline lithium ion tertiary cathode material, comprises the following steps：
(1) by D50For 3-4 μm of Ni5Co2Mn3(OH)2Presoma, Li2CO3According to mol ratio 1：1.08 ratio is mixed
Close；
(2) after being well mixed, in air ambient, after being raised to 720 DEG C with 4 hours, 5 hours is incubated, is raised to 950 within 2 hours
The condition for being incubated 10 hours after DEG C is sintered；
(3) air-flow crushing is carried out after sintering, obtains the tertiary cathode material of monocrystalline pattern；
(4) by tertiary cathode material, the Al of above-mentioned monocrystalline pattern2O3、TiO2According to mol ratio 1：0.1：0.02 ratio
Mixed；
(5) after being well mixed, in air ambient, 4 hours is incubated after being raised to 750 DEG C with 4 hours, is raised to 800 DEG C within 2 hours
8 hours are incubated afterwards, the condition for being incubated 10 hours after 910 DEG C is raised within 1 hour and is sintered；
(6) air-flow crushing is carried out after sintering, obtains adulterating Ti and coats Al high voltage monocrystalline lithium ion tertiary cathode material
Material.
It is the SEM figures of the tertiary cathode material of the monocrystalline pattern prepared by embodiment 1 shown in Fig. 1, is embodiment shown in Fig. 2
The tertiary cathode material of monocrystalline pattern prepared by 1 high-resolution SEM figure, it is seen that its be monocrystalline pattern particle, D50For 5.2 μ
m.It is the SEM figures of the high voltage monocrystalline lithium ion tertiary cathode material prepared by embodiment 1 shown in Fig. 3, is embodiment shown in Fig. 4
The high-resolution SEM figures of high voltage monocrystalline lithium ion tertiary cathode material prepared by 1, it is seen that the crystal shape after overdoping, cladding
Looks are more mellow and full.It is the three of high voltage monocrystalline lithium ion tertiary cathode material prepared by embodiment 1 and monocrystalline pattern shown in Fig. 5
The electrochemistry cycle performance discharge capacity comparison diagram of first positive electrode, it is seen that the cycle performance of material has after overdoping, cladding
Preferably improve.
Embodiment 2
A kind of preparation method of high voltage monocrystalline lithium ion tertiary cathode material, comprises the following steps：
(1) by D50For 3-4 μm of Ni5Co2Mn3(OH)2Presoma, Li2CO3According to mol ratio 1：1.08 ratio is mixed
Close；
(2) after being well mixed, in air ambient, after being raised to 720 DEG C with 4 hours, 5 hours is incubated, is raised to 950 within 2 hours
The condition for being incubated 10 hours after DEG C is sintered；
(3) air-flow crushing is carried out after sintering, obtains the tertiary cathode material of monocrystalline pattern；
(4) by tertiary cathode material, the Al of above-mentioned monocrystalline pattern2O3、TiO2According to mol ratio 1：0.15：0.01 ratio
Example is mixed；
(5) after being well mixed, in air ambient, 4 hours is incubated after being raised to 750 DEG C with 4 hours, is raised to 800 DEG C within 2 hours
8 hours are incubated afterwards, the condition for being incubated 10 hours after 910 DEG C is raised within 1 hour and is sintered；
(6) air-flow crushing is carried out after sintering, obtains adulterating Ti and coats Al high voltage monocrystalline lithium ion tertiary cathode material
Material.
Embodiment 3
A kind of preparation method of high voltage monocrystalline lithium ion tertiary cathode material, comprises the following steps：
(1) by D50For 3-4 μm of Ni5Co2Mn3(OH)2Presoma, Li2CO3According to mol ratio 1：1.08 ratio is mixed
Close；
(2) after being well mixed, in air ambient, after being raised to 720 DEG C with 4 hours, 5 hours is incubated, is raised to 950 within 2 hours
The condition for being incubated 10 hours after DEG C is sintered；
(3) air-flow crushing is carried out after sintering, obtains the tertiary cathode material of monocrystalline pattern；
(4) by tertiary cathode material, the Al of above-mentioned monocrystalline pattern2O3、TiO2According to mol ratio 1：0.05：0.04 ratio
Example is mixed；
(5) after being well mixed, in air ambient, 4 hours is incubated after being raised to 750 DEG C with 4 hours, is raised to 800 DEG C within 2 hours
8 hours are incubated afterwards, the condition for being incubated 10 hours after 910 DEG C is raised within 1 hour and is sintered；
(6) air-flow crushing is carried out after sintering, obtains adulterating Ti and coats Al high voltage monocrystalline lithium ion tertiary cathode material
Material.
Claims (9)
1. a kind of preparation method of high voltage monocrystalline lithium ion tertiary cathode material, it is characterised in that comprise the following steps：
(1) by ternary anode material precursor and lithium source in molar ratio 1:0.5-2 is well mixed；
(2) in air ambient, the mixture that step (1) obtains is sintered；
(3) crushed after the completion of sintering, obtain the tertiary cathode material of monocrystalline pattern；
(4) tertiary cathode material and Al for the monocrystalline pattern for obtaining step (3)2O3、TiO2In molar ratio 1：a：B is mixed,
Wherein 0≤a≤0.15,0≤b≤0.04；
(5) in air ambient, the mixture that step (4) obtains is sintered；
(6) crushed after the completion of sintering, obtain adulterating Ti and coat Al high voltage monocrystalline lithium ion tertiary cathode material.
2. the preparation method of high voltage monocrystalline lithium ion tertiary cathode material according to claim 1, it is characterised in that institute
The chemical formula for stating ternary anode material precursor is Ni1-x-yCoxMnyO2, wherein 0 ＜ x≤0.2,0 ＜ y≤0.3.
3. the preparation method of high voltage monocrystalline lithium ion tertiary cathode material according to claim 1, it is characterised in that institute
The chemical formula for stating the tertiary cathode material of monocrystalline pattern is LiNi1-x-yCoxMnyO2, wherein 0 ＜ x≤0.2,0 ＜ y≤0.3.
4. the preparation method of high voltage monocrystalline lithium ion tertiary cathode material according to claim 1 or 2, its feature exist
In the particle diameter of the ternary anode material precursor is 3-6 μm.
5. the preparation method of high voltage monocrystalline lithium ion tertiary cathode material according to claim 1, it is characterised in that institute
State lithium source and be selected from Li2CO3At least one of with LiOH.
6. the preparation method of high voltage monocrystalline lithium ion tertiary cathode material according to claim 1, it is characterised in that
In step (2), to be incubated 5 hours after being raised to 700-750 DEG C with 4 hours the step of the sintering, 860-960 DEG C is raised within 2 hours
It is incubated 10 hours afterwards.
7. the preparation method of high voltage monocrystalline lithium ion tertiary cathode material according to claim 1, it is characterised in that
In step (5), to be incubated 4 hours after being raised to 600-650 DEG C with 3 hours the step of the sintering, 700-730 DEG C is raised within 2 hours
4 hours are incubated afterwards, 8 hours is incubated after being raised to 800-850 DEG C within 1 hour, 10 hours is incubated after being raised to 890-930 DEG C within 1 hour.
8. the preparation method of high voltage monocrystalline lithium ion tertiary cathode material according to claim 1, it is characterised in that
In step (3) and step (6), the crushing is air-flow crushing or mechanical crushing.
9. a kind of high voltage monocrystalline lithium ion tertiary cathode material, it is characterised in that it is as any one of claim 1-7
Preparation method be prepared.
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Cited By (7)
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| CN109037614A (en) * | 2018-07-05 | 2018-12-18 | 佛山市德方纳米科技有限公司 | A kind of high-pressure solid monocrystalline nickel-cobalt-manganese ternary material and preparation method thereof |
| CN110459760A (en) * | 2019-08-20 | 2019-11-15 | 湖北融通高科先进材料有限公司 | A method of preparing nickle cobalt lithium manganate monocrystalline ternary material |
| CN111276691A (en) * | 2020-03-24 | 2020-06-12 | 江门市科恒实业股份有限公司 | High-voltage single-crystal low-cobalt ternary cathode material and preparation method thereof |
| CN111370685A (en) * | 2020-02-28 | 2020-07-03 | 江门市科恒实业股份有限公司 | High-compaction-density single crystal ternary cathode material and preparation method thereof |
| CN111682170A (en) * | 2020-05-20 | 2020-09-18 | 广东邦普循环科技有限公司 | Single crystal ternary cathode material and preparation method and application thereof |
| CN112117451A (en) * | 2020-09-29 | 2020-12-22 | 山东省科学院能源研究所 | Mixed-phase titanium dioxide modified high-nickel ternary cathode material and preparation method and application thereof |
| CN113292111A (en) * | 2021-04-23 | 2021-08-24 | 陕西彩虹新材料有限公司 | Cobalt-free single crystal cathode material and preparation method thereof |
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| CN109037614B (en) * | 2018-07-05 | 2021-06-11 | 佛山市德方纳米科技有限公司 | High-compaction single crystal nickel-cobalt-manganese ternary material and preparation method thereof |
| CN110459760A (en) * | 2019-08-20 | 2019-11-15 | 湖北融通高科先进材料有限公司 | A method of preparing nickle cobalt lithium manganate monocrystalline ternary material |
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| CN111370685A (en) * | 2020-02-28 | 2020-07-03 | 江门市科恒实业股份有限公司 | High-compaction-density single crystal ternary cathode material and preparation method thereof |
| CN111276691A (en) * | 2020-03-24 | 2020-06-12 | 江门市科恒实业股份有限公司 | High-voltage single-crystal low-cobalt ternary cathode material and preparation method thereof |
| CN111682170A (en) * | 2020-05-20 | 2020-09-18 | 广东邦普循环科技有限公司 | Single crystal ternary cathode material and preparation method and application thereof |
| CN112117451A (en) * | 2020-09-29 | 2020-12-22 | 山东省科学院能源研究所 | Mixed-phase titanium dioxide modified high-nickel ternary cathode material and preparation method and application thereof |
| CN113292111A (en) * | 2021-04-23 | 2021-08-24 | 陕西彩虹新材料有限公司 | Cobalt-free single crystal cathode material and preparation method thereof |
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Application publication date: 20180309 |