CN104916825A - Preparation method of lithium battery high-voltage modified cathode material - Google Patents
Preparation method of lithium battery high-voltage modified cathode material Download PDFInfo
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- CN104916825A CN104916825A CN201510356925.4A CN201510356925A CN104916825A CN 104916825 A CN104916825 A CN 104916825A CN 201510356925 A CN201510356925 A CN 201510356925A CN 104916825 A CN104916825 A CN 104916825A
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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
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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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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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
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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
- H01M4/13—Electrodes for accumulators with non-aqueous electrolyte, e.g. for lithium-accumulators; Processes of manufacture thereof
- H01M4/139—Processes of manufacture
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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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- 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
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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
- 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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Abstract
The invention provides a preparation method of a lithium battery high-voltage modified cathode material. A lithium battery made of the cathode material can be charged and discharged rapidly; the charging cut-off voltage is raised to 4.35V; and the energy density of the battery is greatly increased. In the cathode material prepared with the method, graphite is taken as a core, the surface of the graphite is uniformly coated with a layer of lithium titanate, and the surfaces of graphite particles coated with the lithium titanate are coated with a layer of conductive agent, thereby forming a graphite-lithium tianate-conductive agent three-layer composite structure. The obtained battery has high rapid charging-discharging performance, and the low-temperature performance is improved greatly. Meanwhile, the safety performance is improved greatly.
Description
Technical field
The present invention relates to lithium cell cathode material field, be specifically related to a kind of preparation method of high-voltage lithium ion batteries negative material of quickly-chargeable.
Background technology
Lithium ion battery has that specific capacity is high, self discharge is little, operating temperature range is wide, voltage platform is high, has extended cycle life, memory-less effect, the feature such as environmentally friendly, be widely used in the fields such as mobile phone, notebook computer, electric tool, and progressively promoted in electric automobile field.At present, the built charging station becoming hybrid vehicle and pure electric automobile charging in the important city such as China Beijing, Tianjin, Shenzhen, Shanghai.But according to the charging modes of current lithium battery, electric automobile once charges often needs 7-8 hour; And consumer electronics product is as general in the charging such as mobile phone, cells in notebook computer and electric bicycle at 0.5C, charging 50% is needs 1 hours just, and rapid charge characteristic is poor.With the quickening pace of modern life, people more wish that lithium ion battery has good quick charge capability, to shorten battery charge time.
In recent years, have research by arranging the aperture of some rules thus reach the object of quick charge on positive plate, but the method practice compares consume material and time; There is the material such as research submicron order lithium titanate, lithium metal oxide coated graphite, compound lithium metal oxide coated graphite, graphite coat lithium titanate as negative pole to reach quick charge effect, but it is low but to there is lithium titanate energy density, the problems such as lithium metal oxide conductivity is low, and the high rate performance of lithium titanate is poor, the easy aerogenesis of the battery core made, high-temperature behavior is poor.And at present about the research of quick charge, the charge cutoff voltage of battery core is only 4.2V, and energy density is low.Therefore in the urgent need to a kind of high-voltage lithium ion batteries negative material of quickly-chargeable.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of lithium battery high voltage modification negative material, adopt lithium battery obtained by the present invention can fast charging and discharging and charge cutoff voltage is promoted to 4.35V, greatly improve the energy density of battery.
The invention is characterized in that the high-voltage lithium ion batteries negative material of quickly-chargeable is made up of graphite and the coating layer that is wrapped in graphite surface, described coating layer is made up of lithium titanate and conductive agent, being formed with graphite is kernel, the even coated one deck lithium titanate of graphite surface, at the negative material of the surperficial three-layer composite structure of coated one deck conductive agent again of lithium titanate.Described conductive agent can be one or both the combination in carbon nano-tube, gas-phase growth of carbon fibre, and in described negative material, lithium titanate accounts for 1 ~ 10% of total weight; Conductive agent accounts for 1 ~ 5% of total weight.
Lithium titanate of the present invention has spinel structure, and in charging cycle process, the little and lithium ion diffusion coefficient of unit cell volume change greatly, can realize quick charge, and security performance is good, but poor electric conductivity; The interlamellar spacing of carbon nano-tube is slightly larger than the interlamellar spacing of spherical graphite, and the tubular structure of carbon nano-tube can not subside after the circulation of repeatedly charge-discharge, good cycle, carbon nano-tube has larger draw ratio and good axial one-dimensional electric ability simultaneously, is considered to desirable electric conducting material; Gas-phase growth of carbon fibre (VGCF) has large draw ratio and specific area and is conducive to Lithium-ion embeding and the meso-hole structure deviate from, and both can improve the conductivity of electrode, can also improve the cohesive force between active material and collector simultaneously.
The present invention will take graphite as kernel, the even coated one deck lithium titanate of graphite surface, at the three-layer composite structure material of lithium titanate surface coated one deck conductive agent again as cell negative electrode material, lithium titanate is coated on graphite surface on the one hand, the lithium ion diffusion coefficient of negative material increases, and makes battery lithium ion in high rate charge-discharge process to embed fast/to deviate from; Because the unit cell volume change of lithium titanate is little, the thickness swelling of battery is reduced; Lithium titanate is coated on the security performance that graphite granule surface energy obviously promotes battery simultaneously.On the other hand, in carbon nano-tube or VGCF coating layer, the interlamellar spacing of carbon nano-tube is slightly larger than the interlamellar spacing of spherical graphite, and the tubular structure of carbon nano-tube can not subside after repeatedly charge-discharge circulation; Gas-phase growth of carbon fibre (VGCF) has large draw ratio and specific area is conducive to Lithium-ion embeding and the meso-hole structure deviate from, both are all conducive to the quick embedding of lithium ion on negative material surface/deviate from, and the cycle performance of battery is also greatly improved.The conductive capability of carbon nano-tube/VGCF is strong, makes the battery core DC internal resistance made less, and the multiplying power of battery core and high temperature performance all have obvious lifting simultaneously; And the good capacity of heat transmission of carbon nano-tube/VGCF improves the security performance of battery greatly.
A preparation method for lithium battery high voltage modification negative material, its preparation process is as follows:
1) nanoscale lithium titanate material and graphite being carried out stirring makes it fully mix, and is uniformly mixed 3 ~ 5 hours time, makes lithium titanate material evenly be wrapped in graphite surface; Described lithium titanate material accounts for 1 ~ 10% of graphite and lithium titanate material total weight;
2) by the graphite being coated with lithium titanate material that mixes 1500 ~ 1800 DEG C of heat treatments 0.5 ~ 2 hour, make lithium titanate material melting be wrapped in graphite granule surface, thus form stable lithium titanate coating layer;
3) by conductive agent with through the coated graphite material of lithium titanate, by ball milling 8 ~ 24 hours, obtain graphite/lithium titanate/conductive agent three layers negative material; Wherein conductive agent accounts for 1 ~ 5% of negative material total weight.
Adopt lithium battery obtained by the present invention can fast charging and discharging and charge cutoff voltage is promoted to 4.35V, and energy density is high, with the current charges of 5C, 10min is chargeable to 85% of battery capacity, with the current discharge of 10C, can release more than 98.15% of battery capacity, capability retention more than 96.8% after circulating 1000 weeks, has good fast charging and discharging performance.Manufacture craft of the present invention is simple, and cost is low, is easy to suitability for industrialized production.
Embodiment
Reaching object to make technological means of the present invention, creation characteristic, workflow, using method and effect is easy to understand, below in conjunction with specific embodiment, setting forth the present invention further.
Embodiment 1
Lithium titanate material is accounted for graphite and lithium titanate material total weight 5% takes, and graphite carries out stirring and makes it fully mix, and is uniformly mixed 3 hours time, makes lithium titanate material evenly be wrapped in graphite surface; Then 1500 DEG C of heat treatments 1 hour, make lithium titanate material melting be wrapped in graphite granule surface, thus form stable lithium titanate coating layer; Finally in negative material total weight 2% ratio add carbon nano-tube, and through the coated graphite material of lithium titanate, by ball milling 8 hours, obtain graphite/lithium titanate/conductive agent three layers negative material.
Embodiment 2
Lithium titanate material is accounted for graphite and lithium titanate material total weight 1% takes, and graphite carries out stirring and makes it fully mix, and is uniformly mixed 5 hours time, makes lithium titanate material evenly be wrapped in graphite surface; Then 1800 DEG C of heat treatments 1 hour, make lithium titanate material melting be wrapped in graphite granule surface, thus form stable lithium titanate coating layer; Finally in negative material total weight 1% ratio add gas-phase growth of carbon fibre, and through the coated graphite material of lithium titanate, by ball milling 24 hours, obtain graphite/lithium titanate/conductive agent three layers negative material.
Embodiment 3
Lithium titanate material is accounted for graphite and lithium titanate material total weight 10% takes, and graphite carries out stirring and makes it fully mix, and is uniformly mixed 5 hours time, makes lithium titanate material evenly be wrapped in graphite surface; Then 1600 DEG C of heat treatments 1 hour, make lithium titanate material melting be wrapped in graphite granule surface, thus form stable lithium titanate coating layer; Finally in negative material total weight 5% ratio add carbon nano-tube, and through the coated graphite material of lithium titanate, by ball milling 20 hours, obtain graphite/lithium titanate/conductive agent three layers negative material.
Embodiment 4
Lithium titanate material is accounted for graphite and lithium titanate material total weight 8% takes, and graphite carries out stirring and makes it fully mix, and is uniformly mixed 4 hours time, makes lithium titanate material evenly be wrapped in graphite surface; Then 1700 DEG C of heat treatments 1 hour, make lithium titanate material melting be wrapped in graphite granule surface, thus form stable lithium titanate coating layer; Finally in negative material total weight 4% ratio add gas-phase growth of carbon fibre, and through the coated graphite material of lithium titanate, by ball milling 16 hours, obtain graphite/lithium titanate/conductive agent three layers negative material.
Comparative example 1
Undressed raw material nano lithium titanate.
Comparative example 2
Undressed raw graphite.
Half-cell detects
For the electrical property of negative material prepared by inspection the inventive method, test by half-cell method of testing, negative material with above embodiment and comparative example: acetylene black: PVDF(Kynoar)=93:3:4(weight ratio), add appropriate NMP(N-methyl pyrrolidone) furnishing pulpous state, coat on Copper Foil, within 8 hours, make negative plate through vacuum 110 DEG C of dryings; Be to electrode with metal lithium sheet, electrolyte is 1mol/L LiPF6/EC+DEC+DMC=1:1:1, and microporous polypropylene membrane is barrier film, is assembled into battery.Charging/discharging voltage is 1.0 ~ 2.5V, and charge-discharge velocity is 0.5C, and carry out testing to battery performance, test result is in table 1.
Full battery testing
Take positive active material cobalt acid lithium (96% mass ratio, as follows), super conductive black, binding agent Kynoar, make solvent with 1-METHYLPYRROLIDONE, make slurry, using aluminium foil as collector, slurry is coated on aluminium foil also dry; Pole piece is rolled, makes positive plate.
By negative material, super conductive black, sodium carboxymethylcellulose and butadiene-styrene rubber prepared in embodiment and comparative example, make solvent with 1-METHYLPYRROLIDONE, make slurry, using Copper Foil as collector, slurry is coated on Copper Foil also dry; Pole piece is rolled, makes negative plate.
Adopt lithium ion battery dedicated diaphragm as battery diaphragm, electrolyte is 1mol/L LiPF
6/ EC+DEC+DMC=1:1:1.
Put into battery case after positive/negative plate and barrier film being reeled together, inject electrolyte and seal, and carrying out changing into process.
Charging/discharging voltage is respectively 3.0 ~ 4.2V, 3.0 ~ 4.35V, and carry out testing to battery performance, test result is in table 1.
The electrical property testing result of table 1. comparative example and embodiment
As can be seen from above-mentioned data, charging/discharging voltage is the negative material of 3.0 ~ 4.35V, the battery of efficiency compared with normal voltage 3.0 ~ 4.2V is low first, because material surface prepared by the present invention is coated with conductive agent, conductive agent specific area is higher, cause irreversible capacity first to increase, therefore efficiency is on the low side first.In cycle performance, 1000 circulation conservation rate compared with normal voltages in high voltage discharge and recharge of material of the present invention low, and exceed a lot compared with the material specification of comparative example, its reason is, high voltage discharge and recharge causes the structure of material internal that larger change occurs, and causes cycle performance of battery sharply to decline.Therefore, the high voltage material prepared by the present invention, while having high power capacity performance, still keeps good cycle performance.
More than show and describe general principle of the present invention and principal character and advantage of the present invention; the technical staff of the industry should understand; the present invention is not restricted to the described embodiments; what describe in above-described embodiment and specification just illustrates principle of the present invention; without departing from the spirit and scope of the present invention; the present invention also has various changes and modifications; these changes and improvements all fall in the claimed scope of the invention, and application claims protection range is defined by appending claims and equivalent thereof.
Claims (6)
1. a preparation method for lithium battery high voltage modification negative material, its preparation process is as follows:
1) nanoscale lithium titanate material and graphite being carried out stirring makes it fully mix, and is uniformly mixed 3 ~ 5 hours time, makes lithium titanate material evenly be wrapped in graphite surface;
2) by the graphite being coated with lithium titanate material that mixes 1500 ~ 1800 DEG C of heat treatments 0.5 ~ 2 hour, make lithium titanate material melting be wrapped in graphite granule surface, thus form stable lithium titanate coating layer;
3) by conductive agent with through the coated graphite material of lithium titanate, by ball milling 8 ~ 24 hours, obtain graphite/lithium titanate/conductive agent three layers negative material.
2. the preparation method of a kind of lithium battery high voltage modification negative material according to claim 1, it is characterized in that, graphite described in step 1) comprises Delanium, native graphite, artificial and natural composite graphite, and average grain diameter D50 is at 1 ~ 30 μm.
3. the preparation method of a kind of lithium battery high voltage modification negative material according to claim 1, it is characterized in that, lithium titanate described in step 1) is nanoscale lithium titanate material.
4. the preparation method of a kind of lithium battery high voltage modification negative material according to claim 1, it is characterized in that, in step 1), lithium titanate material accounts for 1 ~ 10% of graphite and lithium titanate material total weight.
5. the preparation method of a kind of lithium battery high voltage modification negative material according to claim 1, it is characterized in that, conductive agent described in step 3) is one or both the combination in carbon nano-tube, gas-phase growth of carbon fibre.
6. the preparation method of a kind of lithium battery high voltage modification negative material according to claim 1, it is characterized in that, in step 3), conductive agent accounts for 1 ~ 5% of negative material total weight.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510356925.4A CN104916825A (en) | 2015-06-26 | 2015-06-26 | Preparation method of lithium battery high-voltage modified cathode material |
| PCT/CN2016/085617 WO2016206548A1 (en) | 2015-06-26 | 2016-06-13 | Preparation method for lithium battery high-voltage modified negative electrode material |
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| CN201510356925.4A CN104916825A (en) | 2015-06-26 | 2015-06-26 | Preparation method of lithium battery high-voltage modified cathode material |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016206548A1 (en) * | 2015-06-26 | 2016-12-29 | 田东 | Preparation method for lithium battery high-voltage modified negative electrode material |
| CN108232175A (en) * | 2018-02-06 | 2018-06-29 | 安徽科达铂锐能源科技有限公司 | A kind of lithium ion battery graphite/lithium titanate composite anode material and preparation method |
| CN110943208A (en) * | 2019-12-13 | 2020-03-31 | 成都爱敏特新能源技术有限公司 | Graphite negative electrode material of high-temperature lithium ion battery and preparation method of graphite negative electrode material |
| CN113745489A (en) * | 2021-09-15 | 2021-12-03 | 河北坤天新能源科技有限公司 | Low-expansion silicon-carbon composite negative electrode material and preparation method thereof |
| CN115000373A (en) * | 2022-06-08 | 2022-09-02 | 万向一二三股份公司 | Preparation method of lithium titanate/graphite composite negative electrode material |
| CN117810450A (en) * | 2024-02-29 | 2024-04-02 | 中国科学院山西煤炭化学研究所 | Modified graphite negative electrode material of lithium ion battery and preparation method thereof |
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| CA2981481C (en) | 2014-04-25 | 2023-09-12 | South Dakota Board Of Regents | High capacity electrodes |
| US10468674B2 (en) | 2018-01-09 | 2019-11-05 | South Dakota Board Of Regents | Layered high capacity electrodes |
| CN111599995A (en) * | 2020-04-28 | 2020-08-28 | 惠州锂威新能源科技有限公司 | Cathode material, preparation method thereof and high-voltage lithium ion battery |
| CN113363444B (en) * | 2021-06-15 | 2022-07-15 | 广东凯金新能源科技股份有限公司 | Nano lithium titanate-coated modified graphite negative electrode material, and preparation method and application thereof |
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| CN115395005B (en) * | 2022-07-25 | 2025-02-18 | 安庆超仁能源科技有限公司 | Modified sodium titanate negative electrode material, sodium ion battery negative electrode and sodium ion battery |
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| EP2282367A1 (en) * | 2008-04-29 | 2011-02-09 | Ls Mtron Ltd. | Negative electrode active material for lithium secondary battery, preparation method of the same, and lithium secondary battery containing the same |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2016206548A1 (en) * | 2015-06-26 | 2016-12-29 | 田东 | Preparation method for lithium battery high-voltage modified negative electrode material |
| CN108232175A (en) * | 2018-02-06 | 2018-06-29 | 安徽科达铂锐能源科技有限公司 | A kind of lithium ion battery graphite/lithium titanate composite anode material and preparation method |
| CN110943208A (en) * | 2019-12-13 | 2020-03-31 | 成都爱敏特新能源技术有限公司 | Graphite negative electrode material of high-temperature lithium ion battery and preparation method of graphite negative electrode material |
| CN113745489A (en) * | 2021-09-15 | 2021-12-03 | 河北坤天新能源科技有限公司 | Low-expansion silicon-carbon composite negative electrode material and preparation method thereof |
| CN115000373A (en) * | 2022-06-08 | 2022-09-02 | 万向一二三股份公司 | Preparation method of lithium titanate/graphite composite negative electrode material |
| CN117810450A (en) * | 2024-02-29 | 2024-04-02 | 中国科学院山西煤炭化学研究所 | Modified graphite negative electrode material of lithium ion battery and preparation method thereof |
| CN117810450B (en) * | 2024-02-29 | 2024-04-30 | 中国科学院山西煤炭化学研究所 | Modified graphite negative electrode material of lithium ion battery and preparation method thereof |
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| WO2016206548A1 (en) | 2016-12-29 |
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