CN108899512A - A kind of preparation method of multi-element metal compound codope trielement composite material - Google Patents
A kind of preparation method of multi-element metal compound codope trielement composite material Download PDFInfo
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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
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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
- 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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
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- 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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- H01M4/02—Electrodes composed of, or comprising, active material
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- 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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- H01M4/02—Electrodes composed of, or comprising, active material
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Abstract
The invention belongs to field of lithium ion battery material preparation, specifically a kind of preparation method of multi-element metal compound codope trielement composite material, preparation process is：First by LiNixCoyMn1‑x‑yO2It is dissolved in organic solvent, metallic compound A is added later, metallic compound B and its oxidant, after mixing evenly, it is transferred in autoclave and carries out hydro-thermal reaction, filter, it is freeze-dried, it is transferred in tube furnace, and is passed through oxidizing gas progress material surface and changes surname, finally prepare multi-element metal doping Li（NixCoyMn1‑x‑yAaBb）O2Trielement composite material, the material prepared improves the specific capacity and cycle performance of material by the synergistic effect between two kinds of doped metallic elements, while improving its imbibition ability using the porous structure that material is formed and improving its cycle performance.
Description
Technical field
The invention belongs to field of lithium ion battery material preparation, specifically a kind of multi-element metal compound codope three
First composite material and preparation method.
Background technique
Lithium-ion-power cell is because its energy density is high, self discharge is low, memory-less effect, the series of advantages such as at low cost are made
For a kind of important secondary cell.Positive electrode is the performances such as energy density and the service life of battery in lithium-ion-power cell
Key influence factor.How to make lithium-ion-power cell best in quality and is heavily dependent on how to prepare performance
Excellent positive electrode.Nickel-cobalt-manganternary ternary anode material with stratiform packed structures relies on height ratio capacity, excellent cyclicity
The advantages that energy, reasonable cost, is rapidly of interest by people, is one kind particularly suitable for electric vehicle and hybrid power
High-energy positive electrode.But nickel-cobalt-manganternary ternary anode material is with the increase of nickel content, the stability of material in the electrolytic solution
Poorer, the cycle performance of prepared battery is poorer.Meanwhile higher residual alkali is unfavorable for the control of cell manufacturing process, hinders
The process of material commercialized development.In order to improve these problems, carrying out material surface modifying and be doped to improve its property at present
The main method of energy, the modified lattice structure for mainly improving its material by solid phase method doped metal ion of current ternary are steady
It is qualitative and improve its cycle performance.Such as patent（CN106395920A）Disclose a kind of codoping modified ternary lithium ion of element
Cell positive material and preparation method mainly pass through solid phase method for the doped transition metal ions of different ions radius in nickel cobalt
It is sintered in manganese ternary material precursor, and plays the synergistic effect between its two kinds of metals, improve its cycle performance.It is above-mentioned
The cycle performance of material although can be improved for material but amplitude is unobvious, consistency is poor, while by solid phase method in its material
Although the aluminium layer of cladding can reduce its side reaction, binding force between kernel and clad and its cladding consistency compared with
Difference.And its surface is modified by oxidizing gas, have homogeneity good and its consistency height, and reduce its material surface
With the side reaction Probability of electrolyte, the ratio of its material is improved in combination with the high density persursor material that hydro-thermal method is prepared
Capacity and cycle performance.
Summary of the invention
For the imbibition liquid-keeping property and its cycle performance for improving its ternary material, the present invention is prepared polynary by hydro-thermal method
Metallic compound adulterates ternary material precursor, then is modified by oxidizing gas to its surface and prepares specific capacity
Height, the excellent trielement composite material of cycle performance.
The technical scheme is that be accomplished by the following way：A kind of multi-element metal compound codope tri compound
The preparation method of material, it is characterised in that：Include the following steps：
1）Hydro-thermal reaction：By LiNixCoyMn1-x-yO2It is dissolved in organic solvent, adds metallic compound A, metallic compound B
After ultrasonic disperse is uniform, then add additive, be transferred in autoclave, and temperature be 100~200 DEG C reaction 12~
72h, by filtering, freeze-drying obtains porous LiNixCoyMn1-x-yO2Composite A；Wherein mass ratio,
LiNixCoyMn1-x-yO2：Organic solvent：Metallic compound A：Metallic compound B：Additive=100:（500~1000）:（1~
5）:（1~5）:（0.1~0.5）；
2）It is modified：Composite A is transferred in tube furnace, and is warming up under inert gas protection（200~400）DEG C, change
It is passed through chlorine trifluoride oxidizing gas, flow is（1~10）Ml/min, time（10~120）Min, then it is passed through inert gas drop
Temperature arrives room temperature, obtains LiNixCoyMn1-x-yO2Composite material B, as multi-element metal compound codope trielement composite material.
The step（1）Middle metallic compound A is：Acetic acid zirconium, zirconium sulfate, zirconium nitrate, zirconium chloride, any in basic zirconium phosphate
Kind；
The step（1）Middle metallic compound B is：Vanadium hydroxide, vanadium oxide, vanadic sulfate, acetic acid vanadium, any in nitric acid vanadium
Kind；
The step（1）Middle oxidant is：Any one of fatty acid/amino acid, fat amido polyacid, polyacrylic acid；
The step（1）Middle organic solvent is：N-Methyl pyrrolidone, carbon tetrachloride, aniline, toluene, any in ethylene glycol
Kind.
Beneficial effect of the present invention：1, pass through hydro-thermal method for two kinds of doped metallic oxides in LiNixCoyMn1-x-yO2Between,
On the one hand play synergistic effect between its metallic compound A and metallic compound B, i.e., zirconium compounds structural stability it is strong and its
The high feature of vfanadium compound voltage platform improves the capacity and its cycle performance of its material；Had simultaneously using hydro-thermal reaction equal
The advantages that evenness height, uniform doping.2, its surface is modified by oxidizing gas, is formed on its surface fluorine/chlorination and closes
Object has with the preferable compatibility of electrolyte, and the Probability for reducing its side reaction improves its cycle performance.
Detailed description of the invention
Fig. 1 is the SEM figure for the trielement composite material that embodiment 1 is prepared.
Specific embodiment
Embodiment 1：
A kind of preparation method of multi-element metal compound codope trielement composite material, includes the following steps：
1, hydro-thermal reaction：By 100g LiNi0.6Co0.2Mn0.2O2It is dissolved in the N-Methyl pyrrolidone of 800ml, adds 3g vinegar
Sour zirconium after 3g vanadium hydroxide ultrasonic disperse is uniform, then adds 0.3g fatty acid/amino acid, is transferred in autoclave, and in temperature
For 24 hours for 150 DEG C of reactions, by filtering, freeze-drying is obtained containing zirconium/vfanadium compound porous Li degree（Ni0.6Co0.2Mn0.2）
O2Composite A；
2, modified：Composite A is transferred in tube furnace, and is warming up to 300 DEG C under argon inert gas protection, Zhi Hougai
It is passed through chlorine trifluoride oxidizing gas, flow 5ml/min, time 60min stop being passed through chlorine trifluoride oxidisability gas later
Body changes logical argon gas and cools to room temperature, obtains containing the porous Li of zirconium/vfanadium compound（Ni0.6Co0.2Mn0.2）O2Composite wood
Expect B；As multi-element metal compound codope trielement composite material.
Embodiment 2：
1, hydro-thermal reaction：By 100g LiNi0.6Co0.2Mn0.2O2It is dissolved in 500ml carbon tetrachloride organic solvent, adds later
1g zirconium nitrate after 1g vanadic sulfate ultrasonic disperse is uniform, then adds 0.1g fat amido polyacid, is transferred to autoclave later
In, and be 100 DEG C of reaction 72h in temperature, later by filtering, freeze-drying is obtained containing the porous Li of zirconium/vfanadium compound
（Ni0.6Co0.2Mn0.2）O2Composite A；
2, modified：Composite A is transferred in tube furnace, and is warming up to 200 DEG C under argon inert gas protection, Zhi Hougai
It is passed through chlorine trifluoride oxidizing gas, flow 1ml/min, time 120min stop being passed through chlorine trifluoride gas later, change logical
Argon inert gas cools to room temperature, obtains containing the porous Li of zirconium/vfanadium compound（Ni0.6Co0.2Mn0.2）O2Composite material B,
As multi-element metal compound codope trielement composite material.
Embodiment 3：
1, hydro-thermal reaction：By 100g LiNi0.6Co0.2Mn0.2O2It is dissolved in 1000ml toluene organic solvent, adds 5g chlorination
Zirconium after 5g nitric acid vanadium ultrasonic disperse is uniform, then adds 0.5g polyacrylic acid, is transferred in autoclave later, and in temperature
For 200 DEG C of reaction 12h, by filtering, freeze-drying is obtained containing the porous Li of zirconium/vfanadium compound（Ni0.6Co0.2Mn0.2）O2
Composite A；
2, modified：Composite A is transferred in tube furnace later, and is warming up to 400 DEG C under argon inert gas protection, it
After change and be passed through chlorine trifluoride oxidizing gas, flow 10ml/min, time 10min stop being passed through chlorine trifluoride gas later,
Change logical argon inert gas and cool to room temperature, obtains containing the porous Li of zirconium/vfanadium compound（Ni0.6Co0.2Mn0.2）O2Composite wood
Expect B.
Comparative example：
Comparative example is the modified ternary material in undoped and its surface.Model：RS622；Producer：The auspicious Xiang new material share in Hunan has
Limit company.
1）SEM test
Fig. 1 is that embodiment 1 is prepared containing the porous Li of zirconium/vfanadium compound（Ni0.6Co0.2Mn0.2）O2The SEM of composite material B
Figure, as can be seen from Figure, material present it is spherical, partial size between（1~10）Between μm.
2）Button cell test：
It takes 95g embodiment 1-3 and comparative example positive electrode, 1g Kynoar, add 220mLN- methyl in 4g conductive agent SP
It in pyrrolidones, stirs evenly and prepares anode sizing agent, be coated on aluminium foil, drying, roll pressing obtains anode pole piece.Electrolyte uses
LiPF6For electrolyte, concentration 1.3mol/L, volume ratio 1:1 EC and DEC is solvent, and metal lithium sheet is used as to electrode, every
Film uses polyethylene (PE), polypropylene (PP) or poly- second propylene (PEP) composite membrane, according to existing side in the glove box of applying argon gas
Method assembles button cell A1, A2, A3 and B1.Above-mentioned button cell is tested on new prestige 5V/10mA type cell tester, charge and discharge
Piezoelectric voltage range 3.0-4.35V, charge-discharge magnification 0.1C, test result are as shown in table 1.
1 button cell test result of table
As can be seen from Table 1, the gram volume and its first charge discharge efficiency that embodiment prepares trielement composite material are former better than comparative example
Because blended metal oxide improves the voltage platform of material, to improve its specific capacity inside ternary material, while relying on three
Chlorine fluoride oxidizing gas is modified the active site for reducing its surface to its surface, to improve its first charge discharge efficiency.
3）Electrochemical property test
Tertiary cathode material in Example 1-3 and comparative example, and according to formula：900g ternary material, 50g Kynoar,
50g conductive agent SP, which is added to stir evenly in the N-Methyl pyrrolidone of 1500ml, prepares anode pole piece, is with artificial graphite
Negative electrode material, electrolyte LiPF6/ EC+DEC (volume ratio 1:1) solution, concentration 1.3mol/L, diaphragm are Celgard 2400
Film prepares 5Ah soft-package battery C1, C2, C3, D1.Test the imbibition ability of positive plate and the cycle performance of lithium battery（1.0C/
1.0C）, multiplying power charging performance（Multiplying power charging standard be：0.5C,1.0C,2.0C,3.0C）, discharge-rate 0.3C）
3.1 cycle performance：
2 cycle performance of table compares
As can be seen from Table 2, the soft-package battery cycle performance that embodiment is prepared is better than comparative example, the reason for this is that by three
Blended metal oxide improves the structural stability of material to improve its cycle performance, simultaneous oxidation gas pair in first material
Its surface carries out changing surname, is formed on its surface fluorine/chlorine compound, have with the preferable compatibility of electrolyte, reduce its side reaction
Probability improve its cycle performance.
3.2 high rate performance：
Testing standard：Charging/discharging voltage 3.0~4.35V of range, 25 ± 3.0 DEG C of temperature, with 0.5C, 1.0C, 5.0C, 10.0C,
20.C charges, and is discharged with 0.5C.
Table 3, embodiment are compared with the multiplying power of comparative example
As shown in Table 3, the multiplying power charging performance of soft-package battery is substantially better than comparative example in Examples 1 to 3, i.e., the charging time compared with
Short, analysis reason is：The migration of lithium ion is needed in battery charging process, and by material surface modifying, the pair of material is anti-
It should reduce, improve the consumption of its lithium ion, so that it is forthright again to improve it to provide sufficient lithium ion in charge and discharge process
Energy.
Claims (5)
1. a kind of preparation method of multi-element metal compound codope trielement composite material, which is characterized in that include the following steps：
Hydro-thermal reaction：By LiNixCoyMn1-x-yO2It is dissolved in organic solvent, adds metallic compound A, metallic compound B ultrasound sound
After being uniformly dispersed, then additive is added, is transferred in autoclave, and reacts 12~72h at being 100~200 DEG C in temperature,
By filtering, freeze-drying obtains porous Li（NixCoyMn1-x-yAaBb）O2(x >=0.3, y≤0.3) composite A；
Wherein, mass ratio, LiNixCoyMn1-x-yO2：Organic solvent：Metallic compound A：Metallic compound B：Additive=100:
500~1000:1~5:1~5:0.1~0.5；
It is modified：Composite A is transferred in tube furnace, and is warming up to 200~400 DEG C under inert gas protection, changes and is passed through
Chlorine trifluoride oxidizing gas, flow are 1~10ml/min, 10~120min of time, after change logical inert gas and cool to
Room temperature obtains Li（NixCoyMn1-x-yAaBb）O2Composite material B；As multi-element metal compound codope trielement composite material.
2. a kind of preparation method of multi-element metal compound codope trielement composite material according to claim 1, special
Sign is：The step（1）Middle metallic compound A is：Acetic acid zirconium, zirconium sulfate, zirconium nitrate, zirconium chloride, any in basic zirconium phosphate
Kind.
3. a kind of preparation method of multi-element metal compound codope trielement composite material according to claim 1, special
Sign is：The step（1）Middle metallic compound B is：Vanadium hydroxide, vanadium oxide, vanadic sulfate, acetic acid vanadium, appointing in nitric acid vanadium
It is a kind of.
4. a kind of preparation method of multi-element metal compound codope trielement composite material according to claim 1, special
Sign is：The step（1）Middle oxidant is：Any one of fatty acid/amino acid, fat amido polyacid, polyacrylic acid.
5. a kind of preparation method of multi-element metal compound codope trielement composite material according to claim 1, special
Sign is：The step（1）Middle organic solvent is：N-Methyl pyrrolidone, carbon tetrachloride, aniline, toluene, appointing in ethylene glycol
It is a kind of.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111326814A (en) * | 2018-12-14 | 2020-06-23 | 中国科学院深圳先进技术研究院 | Method for repairing anode material of waste ternary battery by ultrasonic hydrothermal method |
| CN114628663A (en) * | 2022-04-21 | 2022-06-14 | 华鼎国联四川电池材料有限公司 | Cerium-doped ternary cathode material and preparation method thereof |
| CN114759172A (en) * | 2021-05-07 | 2022-07-15 | 广州倬粤电能科技有限公司 | Preparation method of graphene/zinc oxide negative electrode material for zinc-based battery |
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| CN101630735A (en) * | 2009-06-09 | 2010-01-20 | 北京交通大学 | Method for modifying spinel lithium titanate Li4Ti5O12, anode material for lithium-ion batteries |
| CN103490051A (en) * | 2013-09-18 | 2014-01-01 | 成都晶元新材料技术有限公司 | Multi-element anode lithium battery material suitable for high voltage and preparation method for material |
| CN105655554A (en) * | 2016-01-11 | 2016-06-08 | 山东玉皇新能源科技有限公司 | Hydrothermal modification method of lithium-rich manganese-based positive material |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN101630735A (en) * | 2009-06-09 | 2010-01-20 | 北京交通大学 | Method for modifying spinel lithium titanate Li4Ti5O12, anode material for lithium-ion batteries |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111326814A (en) * | 2018-12-14 | 2020-06-23 | 中国科学院深圳先进技术研究院 | Method for repairing anode material of waste ternary battery by ultrasonic hydrothermal method |
| CN114759172A (en) * | 2021-05-07 | 2022-07-15 | 广州倬粤电能科技有限公司 | Preparation method of graphene/zinc oxide negative electrode material for zinc-based battery |
| CN114628663A (en) * | 2022-04-21 | 2022-06-14 | 华鼎国联四川电池材料有限公司 | Cerium-doped ternary cathode material and preparation method thereof |
| CN114628663B (en) * | 2022-04-21 | 2024-04-09 | 华鼎国联四川电池材料有限公司 | Cerium doped ternary cathode material and preparation method thereof |
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