CN104681816A - Lithium-manganese-oxide-based positive electrode active material and preparation method thereof - Google Patents
Lithium-manganese-oxide-based positive electrode active material and preparation method thereof Download PDFInfo
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- 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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- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/131—Electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
- H01M4/1391—Processes of manufacture of electrodes based on mixed oxides or hydroxides, or on mixtures of oxides or hydroxides, e.g. LiCoOx
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- 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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- H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
- H01M2004/028—Positive electrodes
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Abstract
The invention relates to a lithium-manganese-oxide-based positive electrode active material and a preparation method thereof. According to the lithium-manganese-oxide-based positive electrode active material, the surfaces of spinel lithium manganese oxide particles are coated with phosphate, and the mole ratio of chemical elements in the material is 0<P/Mn<0.03. The preparation method comprises the following steps: firstly, dissolving raw material phosphate into pure water so as to form a solution; then adding with spinel lithium manganese oxide, stirring to form a turbid liquid, then carrying out spray drying, carrying out thermal treatment on the dry powder formed by spray driving, cooling, crushing, and screening so as to obtain the spinel lithium manganese oxide coated with phosphate. According to the invention, phosphate coating the lithium manganese oxide particles has relatively good chemical stability, and is difficult to damage, and the coating layer is relatively uniform and complete, so that the lithium-manganese-oxide-based positive electrode active material has relatively good cyclic performance in a lithium ion battery; the preparation method provided by the invention has a good effect, and is convenient to implement, and the production process is environmentally friendly.
Description
Technical field
The present invention relates to a kind of preparation method of cell positive material, particularly a kind of lithium manganese oxide base positive electrode active materials and preparation method thereof.
Background technology
Li-ion batteries piles is made up of one or more lithium-ion battery monomer.The lithium ion battery of each monomer is made up of positive plate, negative plate, the electrical insulating film being clipped in porous between the two and electrolyte.Common electrolyte is liquid, is as LiPF by specific lithium salts
6be dissolved in and obtain in specific organic solvent.Electrolyte is filled between positive plate and negative plate, realizes the conduction of lithium ion in charging and discharging process.Lithium ion battery is in charge and discharge process, and lithium ion comes and goes migration at positive plate and negative plate, and on pole piece, the chemical constitution of active material significant change does not occur, and therefore lithium ion battery has good discharge and recharge invertibity.
There is cubic spinel crystal structure, chemical formula is LiMn
2o
4material be the positive electrode active materials for lithium ion battery comparatively early found.But well-known, the cycle performance of this material is poor, particularly under higher temperature (45 ~ 60 DEG C).This shortcoming major reason is caused to be, when lithium manganese oxide particles is soaked in the electrolytic solution, due to H
2the erosion of the microscale harmful substances such as O, HF, some manganese ion dissolution of particle surface in the electrolytic solution, thus cause the loss of active material.Therefore, if at the spacer of lithium manganese oxide particles Surface coating one deck inertia, it can be avoided to contact with the direct of electrolyte, just can reduce the dissolving of manganese ion, thus realize slowing down of capacity attenuation in lithium ion battery.
Application number be 00807771.1 Chinese invention patent provide and a kind of modification carried out with the method preventing electricity from declining to spinel lithium-manganese oxide, that lithium manganese oxide is mixed with a certain amount of lithium carbonate, then heat-treat, obtain the spinel lithium-manganese oxide being rich in lithium.Application number be 201010602136.1 Chinese invention patent be the Surface coating oxide of aluminium in lithium manganese oxide particles, thus obtain high-temperature lithium manganate material.Application number be 201010142538.8 Chinese invention patent be mixed with the elements such as Nb, Al when synthetic spinel lithium manganate material, and at the coated oxide of particle surface.The invention provides a kind of new lithium manganese oxide base positive electrode active materials, and spinel lithium-manganese oxide is carried out to the method for modification, its lithium manganese mol ratio of lithium manganese oxide used is different from above patent, and the present invention is Li
1+xmn
2-yo
4, 0 < y < x≤0.1 in formula, and the coating used is different.
Summary of the invention
A kind of lithium manganese oxide base positive electrode active materials of the present invention and preparation method thereof, the method is easy, environmental protection, low cost, be therefore beneficial to industrial applications.
A kind of lithium manganese oxide base positive electrode active materials of the present invention, phosphate is coated with at spinel lithium-manganese oxide particle surface, in lithium manganese oxide base positive electrode active materials, chemical element mol ratio is 0 < P/Mn < 0.03, and described spinel lithium-manganese oxide can by general formula Li
1+xmn
2-yo
4represent, 0 < y < x≤0.1 in formula, described phosphate is one or more in manganese phosphate, lithium phosphate, lithium manganese phosphate.
The preparation method of a kind of lithium manganese oxide base positive electrode active materials of the present invention, comprises the following steps:
1), first raw material phosphor hydrochlorate is dissolved in pure water and forms solution, add spinel lithium-manganese oxide again and stir formation suspension-turbid liquid, the solid content of suspension-turbid liquid is 20 ~ 50%, then spraying dry, the inlet temperature of drying machine is 250 ~ 300 DEG C, and leaving air temp is 100 ~ 130 DEG C;
2) dry powder, by spraying dry obtained at 500 ~ 800 DEG C in air atmosphere heat treatment 1 ~ 6h, cooling;
3), by cooled product pulverize, sieve, thus obtain being coated with phosphatic spinel lithium-manganese oxide.
Described raw material phosphor hydrochlorate is one or more in ammonium dihydrogen phosphate, diammonium hydrogen phosphate, lithium dihydrogen phosphate.
The building-up process of described spinel lithium-manganese oxide is for weigh lithium carbonate or lithium hydroxide, to mix with manganese dioxide according to chemical element mol ratio 0.53≤Li/Mn≤0.57, then in air atmosphere with 800 DEG C at heat treatment 12h, slowly cool to room temperature again, cross 250 mesh sieves.
Preparation method provided by the present invention can make raw material phosphor hydrochlorate be evenly distributed on the surface of lithium manganese oxide particles, and in heat treatment process, react the phosphate of generation, no matter be the phosphate of lithium, the phosphate of manganese, or the composite phosphate of lithium and manganese, all has good chemical stability in lithium ion battery.Therefore, this Phosphate coating layer can effectively avoid the surface of lithium manganese oxide particles to be directly exposed in electrolyte, thus in the charge and discharge process of lithium ion battery, reduce or avoid the generation of side reaction and the dissolving of manganese ion on positive plate, the capacity being beneficial to lithium ion battery keeps.
Phosphate coated in lithium manganese oxide particles in the present invention (in manganese phosphate, lithium phosphate, lithium manganese phosphate one or more), compared with the metal oxides such as aluminium oxide, there is better chemical stability, be not easy to be destroyed, and coating layer is more all even complete.This just makes positive electrode active materials provided by the present invention in lithium ion battery, have better cycle performance.Preparation method provided by the present invention is not only effective, and implements convenient, and the raw material used is less expensive, production process environmental protection, does not make the chemical element increasing other in material, be therefore adapted at applying in suitability for industrialized production except introducing P elements.
Accompanying drawing explanation
Fig. 1 is X-ray diffraction (XRD) figure of lithium manganese oxide base positive electrode active materials (i.e. modification lithium manganese oxide) obtained in embodiment 1.
Fig. 2 is modification lithium manganese oxide obtained in embodiment 1 and the cycle performance comparison diagram of lithium manganese oxide before modified.
Fig. 3 is X-ray diffraction (XRD) figure of lithium manganese oxide base positive electrode active materials (i.e. modification lithium manganese oxide) obtained in embodiment 2.
Fig. 4 is modification lithium manganese oxide obtained in embodiment 2 and the cycle performance comparison diagram of lithium manganese oxide before modified.
Fig. 5 is X-ray diffraction (XRD) figure of lithium manganese oxide base positive electrode active materials (i.e. modification lithium manganese oxide) obtained in embodiment 3.
Fig. 6 is modification lithium manganese oxide obtained in embodiment 3 and the cycle performance comparison diagram of lithium manganese oxide before modified.
Embodiment
For obtained lithium manganese oxide base positive electrode active materials (i.e. modification lithium manganese oxide) of the present invention, first synthetic spinel lithium manganese oxide.Its building-up process is: take lithium carbonate 248.27g, manganese dioxide 1043.28g (i.e. chemical element mol ratio Li/Mn=0.56), 10h is mixed in the tumbling ball mill that agate ball is housed, then in air atmosphere, heat treatment 12h at 800 DEG C, slowly cool to room temperature again, cross 250 mesh sieves.
Embodiment 1:
Take lithium dihydrogen phosphate 11.50g, be dissolved in 1.5L pure water, then add 1000g spinel lithium-manganese oxide and stir 10 ~ 30min.By this suspension-turbid liquid spraying dry, the inlet temperature of drying machine is 250 ~ 300 DEG C, and leaving air temp is 100 ~ 130 DEG C.By the dry powder that obtains in Muffle furnace with 600 DEG C of heat treatment 4h, keep air atmosphere in heat treatment process, after naturally cooling to room temperature, cross 250 mesh sieves.
Carry out XRD analysis to resulting materials, as shown in Figure 1, products therefrom remains the original cubic spinel crystal structure of lithium manganese oxide, does not see the diffraction maximum of other thing phases.Not seeing that the reason of the diffraction maximum of surface cover may be that the amount of surface cover is little, also may be that surface cover presents glassy state.
Embodiment 2:
Take ammonium dihydrogen phosphate 12.72g, be dissolved in 1.8L pure water, then add 1000g spinel lithium-manganese oxide and stir 10 ~ 30min.By this suspension-turbid liquid spraying dry, the inlet temperature of drying machine is 250 ~ 300 DEG C, and leaving air temp is 100 ~ 130 DEG C.By the dry powder that obtains in Muffle furnace with 700 DEG C of heat treatment 3h, keep air atmosphere in heat treatment process, after naturally cooling to room temperature, cross 250 mesh sieves.
XRD analysis (see figure 3) is carried out to product, does not find impurity phase diffraction maximum, illustrate and do not destroy original cubic spinel crystal structure.
Embodiment 3:
Take diammonium hydrogen phosphate 14.60g, be dissolved in 1.8L pure water, then add 1000g spinel lithium-manganese oxide and stir 10 ~ 30min.By this suspension-turbid liquid spraying dry, the inlet temperature of drying machine is 250 ~ 300 DEG C, and leaving air temp is 100 ~ 130 DEG C.By the dry powder that obtains in Muffle furnace with 700 DEG C of heat treatment 3h, keep air atmosphere in heat treatment process, after naturally cooling to room temperature, cross 250 mesh sieves.
XRD analysis (see figure 5) is carried out to product, does not find impurity phase diffraction maximum, illustrate and do not destroy original cubic spinel crystal structure.
Test example:
The material obtained with embodiment 1 ~ embodiment 3 is for positive active material, and being equipped with conductive agent and bonding agent, being coated on aluminium foil and making positive plate, is negative pole with metal lithium sheet, is assembled into CR2025 button cell and carries out charge-discharge test, voltage range 3.30 ~ 4.35V.As can be seen from Fig. 2, Fig. 4, Fig. 6, the material after coated phosphate, compared with lithium manganese oxide before modified, cycle performance has clear improvement.
With the performance comparison of lithium manganese oxide before modified after table 1 is coated
Claims (4)
1. a lithium manganese oxide base positive electrode active materials, it is characterized in that: be coated with phosphate at spinel lithium-manganese oxide particle surface, in lithium manganese oxide base positive electrode active materials, chemical element mol ratio is 0 < P/Mn < 0.03, and described spinel lithium-manganese oxide can by general formula Li
1+xmn
2-yo
4represent, 0 < y < x≤0.1 in formula, described phosphate is one or more in manganese phosphate, lithium phosphate, lithium manganese phosphate.
2. a preparation method for lithium manganese oxide base positive electrode active materials, is characterized in that comprising the following steps:
1), first raw material phosphor hydrochlorate is dissolved in pure water and forms solution, add spinel lithium-manganese oxide again and stir formation suspension-turbid liquid, the solid content of suspension-turbid liquid is 20 ~ 50%, then spraying dry, the inlet temperature of drying machine is 250 ~ 300 DEG C, and leaving air temp is 100 ~ 130 DEG C;
2) dry powder, by spraying dry obtained at 500 ~ 800 DEG C in air atmosphere heat treatment 1 ~ 6h, cooling;
3), by cooled product pulverize, sieve, thus obtain being coated with phosphatic spinel lithium-manganese oxide.
3. the preparation method of a kind of lithium manganese oxide base positive electrode active materials according to claim 2, is characterized in that: described raw material phosphor hydrochlorate is one or more in ammonium dihydrogen phosphate, diammonium hydrogen phosphate, lithium dihydrogen phosphate.
4. the preparation method of a kind of lithium manganese oxide base positive electrode active materials according to claim 2, it is characterized in that: the building-up process of described spinel lithium-manganese oxide is for weigh lithium carbonate or lithium hydroxide, to mix with manganese dioxide according to chemical element mol ratio 0.53≤Li/Mn≤0.57, then in air atmosphere with 800 DEG C at heat treatment 12h, slowly cool to room temperature again, cross 250 mesh sieves.
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105261740A (en) * | 2015-11-24 | 2016-01-20 | 宁德新能源科技有限公司 | Lithium battery cathode material, preparation method thereof and lithium battery including same |
| US20160293951A1 (en) * | 2014-02-28 | 2016-10-06 | Lg Chem, Ltd. | Lithium-nickel based positive electrode active material, method of preparing the same, and lithium secondary battery including the same |
| CN106328933A (en) * | 2015-06-30 | 2017-01-11 | 中国科学院苏州纳米技术与纳米仿生研究所 | Phosphate-coated lithium-rich layered positive electrode material and preparation method and application thereof |
| CN108110252A (en) * | 2018-01-10 | 2018-06-01 | 香河昆仑化学制品有限公司 | A kind of heat safe lithium manganate composite anode material and its synthetic method |
| CN108807913A (en) * | 2018-06-13 | 2018-11-13 | 中科廊坊过程工程研究院 | One kind anode material for lithium-ion batteries containing zirconium and preparation method thereof and lithium ion battery |
| CN109411804A (en) * | 2017-08-17 | 2019-03-01 | 江苏津谊新能源科技有限公司 | A kind of manufacturing method of mine anti-explosion lithium ion battery |
| CN111180702A (en) * | 2020-01-06 | 2020-05-19 | 天能帅福得能源股份有限公司 | Preparation method of coated lithium manganate positive electrode material and positive electrode material thereof |
| CN112216815A (en) * | 2019-07-11 | 2021-01-12 | 深圳市比亚迪锂电池有限公司 | Lithium manganese battery positive electrode and lithium manganese battery |
| CN114506830A (en) * | 2020-11-17 | 2022-05-17 | 松山湖材料实验室 | Preparation method of phosphate-coated positive electrode active material |
| CN114744188A (en) * | 2022-06-13 | 2022-07-12 | 河南科隆新能源股份有限公司 | Lithium ion battery anode material with non-hollow porous structure and preparation method and application thereof |
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Cited By (15)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20160293951A1 (en) * | 2014-02-28 | 2016-10-06 | Lg Chem, Ltd. | Lithium-nickel based positive electrode active material, method of preparing the same, and lithium secondary battery including the same |
| US10608251B2 (en) * | 2014-02-28 | 2020-03-31 | Lg Chem, Ltd. | Lithium-nickel based positive electrode active material, method of preparing the same, and lithium secondary battery including the same |
| CN106328933A (en) * | 2015-06-30 | 2017-01-11 | 中国科学院苏州纳米技术与纳米仿生研究所 | Phosphate-coated lithium-rich layered positive electrode material and preparation method and application thereof |
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| CN108807913A (en) * | 2018-06-13 | 2018-11-13 | 中科廊坊过程工程研究院 | One kind anode material for lithium-ion batteries containing zirconium and preparation method thereof and lithium ion battery |
| CN112216815A (en) * | 2019-07-11 | 2021-01-12 | 深圳市比亚迪锂电池有限公司 | Lithium manganese battery positive electrode and lithium manganese battery |
| CN112216815B (en) * | 2019-07-11 | 2021-12-07 | 深圳市比亚迪锂电池有限公司 | Lithium manganese battery positive electrode and lithium manganese battery |
| CN111180702A (en) * | 2020-01-06 | 2020-05-19 | 天能帅福得能源股份有限公司 | Preparation method of coated lithium manganate positive electrode material and positive electrode material thereof |
| CN111180702B (en) * | 2020-01-06 | 2021-08-20 | 天能帅福得能源股份有限公司 | Preparation method of coated lithium manganate positive electrode material and positive electrode material thereof |
| CN114506830A (en) * | 2020-11-17 | 2022-05-17 | 松山湖材料实验室 | Preparation method of phosphate-coated positive electrode active material |
| CN114506830B (en) * | 2020-11-17 | 2023-07-14 | 松山湖材料实验室 | Preparation method of phosphate-coated cathode active material |
| CN114744188A (en) * | 2022-06-13 | 2022-07-12 | 河南科隆新能源股份有限公司 | Lithium ion battery anode material with non-hollow porous structure and preparation method and application thereof |
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Application publication date: 20150603 |