CN1697212A - Method for processing positive pole material of lithium cobalt acid in lithium ion battery - Google Patents

Method for processing positive pole material of lithium cobalt acid in lithium ion battery Download PDF

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CN1697212A
CN1697212A CNA2005100348932A CN200510034893A CN1697212A CN 1697212 A CN1697212 A CN 1697212A CN A2005100348932 A CNA2005100348932 A CN A2005100348932A CN 200510034893 A CN200510034893 A CN 200510034893A CN 1697212 A CN1697212 A CN 1697212A
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esters
cobalt acid
lithium
licoo
positive electrode
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CN1319192C (en
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陈鸣才
王洪
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Guangzhou Institute of Chemistry of CAS
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Guangzhou Institute of Chemistry of CAS
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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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    • Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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    • Y02E60/10—Energy storage using batteries

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Abstract

Usage ratio of cobalt ion in material of positive pole is only 50% currently. The treating method disclosed in the invention includes following steps: coating a layer of metallic oxide film on surface of LiCoO2 granules; carrying out drying and sintering treatment. Features of the product produced from the method are: improving high temperature property, cyclical stability, stability of anti overcharge; postponing ascend of internal resistance in charging procedure. The battery is posible to be charged at higher voltage. The method raises weight of material and volume energy density more than 20%.

Description

The processing method of lithium ion cell anode material lithium cobaltate
Technical field
The present invention relates to the used positive electrode LiCoO of a kind of secondary lithium battery 2Surface modifying method.
Background technology
Lithium ion battery contains electrolyte, mainly the negative pole that is made of carbon and by lithium-contained composite oxide such as LiCoO 2, LiNiO 2, LiMn 2O 4The positive pole of forming.Than other aqueous electrolysis solution battery high voltage and energy density are arranged based on lithium ion battery, lithium ion battery becomes the main energy sources of mobile appliance equipment and related facility rapidly.
Because the function and the performance of movable electrical appliances constantly promote, and the energy density of lithium ion battery have been proposed the demand of continuous improvement.Yet, present available lithium ion battery, just, the utilance of negative pole has roughly reached its limit 100%, improve energy density again, just requires 1. to replace original active matter with the active matter of new higher energy density; 2. increase the obturator density of active material in the pole plate; 3. increase the thickness of pole plate.
If replace new material, then use the circuit of the equipment of lithium ion battery to redesign, because of the discharge proterties of battery changes.Therefore, the battery that adopts the material of new high-energy-density to make can not be used for common electrical equipment, so have only by increasing the thickness of both positive and negative polarity active matter obturator density or increase electrode, reduce the ratio of inert matter such as collector or barrier film in other words, reach the high-energy-density of battery.
Yet, the filling volume density of excessive increase pole piece thickness or excessive increase active material, meeting influence the charge-discharge performance of battery greatly.High-rate charge-discharge capability particularly.Reason is as follows: electrode is loaded volume density to be increased, and then its hole descends.Thickness increases, and electrolyte just can not transmit lithium ion fast.And the viscosity of electrolyte when low temperature increases, the decline that the charge-discharge performance of electrode can be bigger, and the utilance of positive and negative electrode active material may drop to the 20-30% level like this, and final actual energy density reduces.
At LiCoO 2, LiNiO 2, LiMn 2O 4In three kinds of positive electrodes, LiCoO 2It is the positive electrode that is still commercial main use at present.Its reason is other two kinds of positive electrode LiNiO 2, LiMn 2O 4Till current, also have a lot of technical difficulty to overcome after, just can be used for commercially producing.
LiCoO in the present lithium ion battery 2, the lithium ion that in fact really uses has only 1/2nd of its lithium ion content.People will expect that naturally if remaining 1/2nd lithium is used, then capacity can promote nearly one times.But LiCoO 2LiCoO in the attitude of discharging fully 2LiCo with half Charging state 0.5O 2Circulation time between (4.2V vs.Li), performance is only stable.
If continue to deviate from wherein other lithium ion, then its capacity decay rapidly.LiCoO 2When charging, lose electronics and lithium ion, in taking off the lithium process, Co 3+Be oxidized to very unsettled Co 4+Thereby, be dissolved in the electrolyte.Co 4+Concentration increases and can brokenly encircle the positive electrode structure cell, makes LiCoO along the axial contraction of structure cell c 2The broken ring of the mechanical performance of particle, thus capacity reduces rapidly.
In order to overcome the problems referred to above, SnO such as Cho 2LiCoO is handled in cladding 2, Ho-Jin Kweon etc. have handled LiNi with the MgO cladding 1-xCo xO 2.Japhil Cho is with sol-gal process Al 2O 3LiCoO has been handled in cladding 2. the Z.X.Wang of physics institute of the Chinese Academy of Sciences has handled LiCoO with the MgO cladding 2.Seungsuk usefulness gaseous suspension method Al such as Oh 2O 3LiCoO has been handled in cladding 2.Zhaohui Chen and J.R.Dahn etc. has handled LiCoO with the ZrO2 cladding 2. but the positive electrode cycle performance after handling does not still reach commercial requirement of using.
Summary of the invention
At the deficiencies in the prior art, the processing method that the purpose of this invention is to provide a kind of lithium ion cell anode material lithium cobaltate, make positive electrode after this method is handled, cycle performance instability when solving it and being used for lithium ion battery, high-temperature behavior difference and the excessive capacity problem of decay rapidly of taking off behind the lithium.Product can be between high voltage 3.0 ~ 4.7V stable circulation.
Method of the present invention is to adopt sol-gel process, uses MgO/TiO 2/ SiO 2To LiCoO 2Carry out surface treatment, at anodal material LiCoO 2The surface forms one deck LiCo 1-x-y-zMg xTi ySi zO 2The solid solution film, this skim has improved former LiCoO 2High-temperature behavior, cyclical stability, the anti-over-charging electrical stability delays the rising of battery internal resistance in charging process.And battery can carry out charge and discharge cycles under higher voltage, and the weight and volume energy density that has improved material is more than 20%.
Designed the anodal modification technology with cobalt acid lithium material of a kind of secondary lithium battery according to above-mentioned purpose, this technology is at cobalt acid lithium LiCoO 2The surface of particle coats the layer of metal oxidation film, promptly earlier at cobalt acid lithium LiCoO 2The surface of particle is coated with the precursor film of one deck even compact, is by titanate esters before this precursor film, magnesium salts, and the presoma that esters of silicon acis (with 0.05 ~ 3: 0.05 ~ 3: 0.01 ~ 1.0 ratio) reaction generates is applied to LiCoO 2Particle surface and forming.The cobalt acid lithium/titanate esters/alcohol of magnesium salts/esters of silicon acis/1 ~ 8 carbon or the ratio of ketones solvent are 100/0.05 ~ 3: 0.05 ~ 3: 0.01 ~ 1.0: 20 ~ 50.
For titanate esters and magnesium salts consumption preferably at 0.1 ~ 1.0g (per 100 gram cobalts acid lithiums); During less than 0.1g (titanate esters and magnesium salts total amount are less than 0.2g), the oxide cladding can not be with positive electrode particle parcel fully, and cladding just can not effectively be protected the whole surface of positive electrode, thereby the performance after the modification is not very good.When greater than 0.5g (or titanate esters and magnesium salts total amount greater than 1.0g), cladding thickness is too big, and because cladding there is no electro-chemical activity, so its proportion in whole system then can reduce the specific capacity of positive electrode too greatly.
Preferably at 0.05 ~ 0.5g (per 100 gram cobalt acid lithiums), if content is measured greater than this, because the poorly conductive of Si oxide, ending that then the positive electrode sheet resistance can be bigger rises the consumption of esters of silicon acis, just can influence the cycle performance of battery like this.If content is measured less than this; then influence the uniformity of surperficial coated very little owing to content; make oxide bigger particle agglomeration occur on the surface, cladding also can reduce the surface protection effect of body positive electrode particle like this, thus the reduction that the cycle performance of material also can be bigger.
Main points of the present invention are: hydrolysis partly takes place by absorbing airborne moisture in esters of silicon acis in air, generate a kind of polymer-organic siliconresin, and this polymer is evenly distributed to positive electrode material cobalt acid lithium LiCoO as a kind of carrier with presoma 2The surface of particle forms one deck precursor film.After through heat treated, precursor film is converted into one deck LiCo again 1-x-y-zMg xTi ySi zO 2The solid solution film, this one deck solid solution film has been protected LiCoO as the SEI film 2LiCoO has been avoided on the surface of particle 2Particle directly contacts with electrolyte and chemical reaction takes place, and has improved former LiCoO from face 2High-temperature behavior, cyclical stability, anti-over-charging electrical stability, and delay the rising of battery internal resistance in charging process.
The method of the invention detailed process comprises as follows:
1, esters of silicon acis is dissolved in anhydrous alcohols or the acetone solvent, titanate esters is dissolved in anhydrous alcohols or the acetone solvent, magnesium nitrate is dissolved in alcohols or the acetone solvent.Again above-mentioned three kinds of solution are mixed, make titanate esters, magnesium salts, the esters of silicon acis proportioning is 0.05 ~ 3: 0.05 ~ 3: 0.01 ~ 1.0 ratio.
2, pending cobalt acid lithium is added blender, stir the slow down above-mentioned processing mixed liquor that adds, making cobalt acid lithium/titanate esters/esters of silicon acis/magnesium nitrate/ethanol is 100/0.05 ~ 3: 0.05 ~ 3 with the cobalt acid lithium/titanate esters/alcohol of magnesium salts/esters of silicon acis/1 ~ 8 carbon or the ratio of ketones solvent: 0.01 ~ 1.0: 20 ~ 50.High-speed stirred, high-speed mixing is 0.1～24 hour under 30～150 ℃ of temperature.
3, take out mixture, in baking oven 50 ~ 150 ℃ of dryings 0.5～24 hour; Then dried positive electrode is placed 200～1, sintering is 0.5～12 hour under 000 ℃ of high temperature.
4, be as cold as the positive electrode of normal temperature, with 150 ~ 300 order stainless steel sift net filtrations, the positive electrode that obtains handling.
Method of the present invention is in order to handle positive electrode LiCoO 2Make it can normal circulation under high voltage, reach promote specific energy in, do not influence circulation and other performance of battery, even promote other performance.Improved former LiCoO 2High-temperature behavior, cyclical stability, the anti-over-charging electrical stability delays the rising of battery internal resistance in charging process.And battery can carry out charge and discharge cycles under higher voltage, and the weight and volume energy density that has improved material is more than 20%.
Embodiment
Embodiment 1
Tetraethoxysilane is dissolved in absolute ethyl alcohol, positive butyl titanate independently is dissolved in absolute ethyl alcohol, magnesium nitrate is dissolved in ethanol, more above-mentioned three kinds of solution are mixed.
Pending cobalt acid lithium is added blender, stir the slow down above-mentioned processing mixed liquor that adds, cobalt acid lithium/tetrabutyl titanate/tetraethoxysilane/magnesium nitrate/ethanol is mixed with certain proportion.High-speed stirred was 50～60 ℃ of following high-speed mixing of temperature 10 hours.Take out mixture, 100 ℃ of dryings are 5 hours in baking oven; Then dried positive electrode is placed high-temperature cabinet 800 ℃ of sintering 12 hours.With 300 order stainless steel sift net filtrations, the positive electrode that obtains handling.
Above-mentioned processing positive electrode is made battery, be shaped on other batteries with quadrat method, the positive electrode that these batteries use and the difference of other battery only are not pass through surface treatment, and these battery mark are test of " C (being used for the comparison battery) " Performance Evaluation as table-1.
Table-1
Numbering C: T: S: M weight ratio 20% cycle-index falls in appearance, discharges and recharges between 3.0 ~ 4.5V 1C * 10V overcharges ??LiCoO 2Initial capacity (mAh/g), 3.0 ~ 4.2V charges and discharge 3.0 ~ 4.2V; 300 circulation back capacity declines (%)
??1 ??100/0.1/0.05/0.1 ??85 Blast ??142 ??18
??2 ??100/0.2/0.05/0.2 ??312 By ??140 ??10
??3 ??100/0.4/0.05/0.4 ??386 By ??138 ??8
??4 ??100/0.6/0.05/0.6 ??388 By ??135 ??9
??5 ??100/0.8/0.05/0.8 ??420 By ??130 ??12
??6 ??100/1/0.5/1 ??410 By ??128 ??13
??7 ??100/2/0.5/2 ??450 By ??125 ??11
??C-1 ??100/0/00/0 ??28 Blast ??145 ??20
C: expression cobalt acid lithium, T: expression tetrabutyl titanate, S: expression tetraethoxysilane, M: expression magnesium nitrate.
Embodiment 2
Other is with example 1, and just making the ratio of cobalt acid lithium/tetrabutyl titanate/tetraethoxysilane/magnesium nitrate/ethanol is 100/0.2/0.05/0.1 ~ 1/30.
Above-mentioned processing positive electrode is made battery, be shaped on other batteries with quadrat method, the positive electrode that these batteries use and the difference of other battery only are not pass through surface treatment, and these battery mark are test of " C (being used for the comparison battery) " Performance Evaluation as table--2.
Table-2
Numbering C: T: S: M weight ratio 20% cycle-index falls in appearance, discharges and recharges between 3.0 ~ 4.5V 1C * 10V overcharges ??LiCoO 2Initial capacity (mAh/g) 3.0 ~ 4.5V charges and discharge 3.0 ~ 4.2V; 300 circulation back capacity declines (%)
??1 ??100/0.2/0.05/0.0 ??5 ??115 Blast ??181 ??16
??2 ??100/0.2/0.05/0.2 ??300 Blast ??180 ??9
??3 ??100/0.2/0.05/0.4 ??332 By ??175 ??9
??4 ??100/0.2/0.05/0.6 ??376 By ??165 ??9
??5 ??100/0.2/0.05/0.8 ??320 By ??160 ??11
??6 ??100/0.2/0.5/1 ??310 By ??155 ??12
??7 ??100/0.2/0.5/2 ??400 By ??150 ??11
??C-2 ??100/0/00/0 ??25 Blast ??185 ??19
C: expression cobalt acid lithium, T: expression tetrabutyl titanate, S: expression tetraethoxysilane, M: expression magnesium nitrate.
Embodiment 3
Other is with example 1, and making the ratio of cobalt acid lithium/tetrabutyl titanate/tetraethoxysilane/magnesium nitrate/ethanol is 100/0/0.05/0.1 ~ 1/30.
Above-mentioned processing positive electrode is made battery, be shaped on other batteries with quadrat method, the positive electrode that these batteries use and the difference of other battery only are not pass through surface treatment, and these battery mark are test of " C (being used for the comparison battery) " Performance Evaluation as table-3.
Table-3
Numbering C: T: S: M weight ratio 20% cycle-index falls in appearance, discharges and recharges between 3.0～4.5V 1C * 10V overcharges ?LiCoO 2Initial capacity (mAh/g) discharges and recharges mensuration between 3.0～4.5V 3.0～4.2V; 300 circulation back capacity declines (%)
??1 ??100/0.05/0.05/0.1 ??35 Blast ??183 ??18
??2 ??100/0.2/0.05/0.4 ??330 By ??180 ??10
??3 ??100/0.4/005/0.4 ??416 By ??172 ??9
??4 ??100/0.6/0.05/0.4 ??300 By ??166 ??10
??5 ??100/0.8/0.05/0.4 ??312 By ??161 ??12
??6 ??100/1.0/0.5/0.4 ??450 By ??156 ??11
??7 ??100/3.0/0.5/0.4 ??447 By ??152 ??10
??C-3 ??100/0/00/0 ??30 Blast ??185 ??20
C: expression cobalt acid lithium, T: expression tetrabutyl titanate, S: expression tetraethoxysilane, M: expression magnesium nitrate.Embodiment 4
Embodiment 4
Other is with example 1, and making the ratio of cobalt acid lithium/tetrabutyl titanate/tetraethoxysilane/magnesium nitrate/ethanol is 100/0.1 ~ 1/0.05/0/30.
Above-mentioned processing positive electrode is made battery, be shaped on other batteries with quadrat method, the positive electrode that these batteries use and the difference of other battery only are not pass through surface treatment, and these battery mark are test of " C (being used for the comparison battery) " Performance Evaluation as table-4.
Table-4
Numbering C: T: S: M weight ratio 20% cycle-index falls in appearance, discharges and recharges between 3.0～4.5V 1C * 10V overcharges ??LiCoO 2Discharge and recharge mensuration between initial capacity (mAh/g) 3.0～4.2V 3.0～4.2V; 300 circulation back capacity declines (%)
??1 ??100/0.4/0.01/0.4 ??305 By ??140 ??18
??2 ??100/0.4/0.05/0.4 ??410 By ??138 ??11
??3 ??100/0.4/0.2//0.4 ??276 By ??136 ??10
??4 ??100/0.4/0.4/0.4 ??165 By ??135 ??10
??5 ??100/0.4/0.68/0.4 ??150 By ??132 ??13
??6 ??100/0.4/0.8/0.4 ??110 By ??130 ??16
??7 ??100/0.4/1.0/0.4 ??78 By ??130 ??19
??C-4 ??100/0/00/0 ??30 Blast ??145 ??20
C: expression cobalt acid lithium, T: expression tetrabutyl titanate, S: expression tetraethoxysilane, M: expression magnesium nitrate.
Embodiment 5
Other is with example 1, and making the ratio of cobalt acid lithium/tetrabutyl titanate/tetraethoxysilane/magnesium nitrate/ethanol is 100/0.1 ~ 1/0/0/30.
Above-mentioned processing positive electrode is made battery, be shaped on other batteries with quadrat method, the positive electrode that these batteries use and the difference of other battery only are not pass through surface treatment, and these battery mark are test of " C (being used for the comparison battery) " Performance Evaluation as table-5.
Table-5
Numbering C: T: S: M weight ratio 20% cycle-index falls in appearance, discharges and recharges between 3.0～4.5V 1C * 10V overcharges ??LiCoO 2Discharge and recharge between initial capacity (mAh/g) 3.0～4.2V 3.0～4.2V; 300 circulation back capacity declines (%)
??1 ??100/0/0/0.1 ??31 Blast ??145 ??20
??2 ??100/0/0/0.2 ??45 Blast ??142 ??17
??3 ??100/00/0.4 ??67 Blast ??140 ??17
??4 ??100/0/0/0.6 ??68 Blast ??135 ??15
??5 ??100/0/0/0.8 ??90 Blast ??135 ??13
??6 ??100/0/0/1 ??91 By ??130 ??11
??7 ??100/0/0/2 ??94 By ??130 ??11
??C-5 ??100/0/0/0 ??32 Blast ??145 ??20
C: expression cobalt acid lithium, T: expression tetrabutyl titanate, S: expression tetraethoxysilane, M: expression magnesium nitrate.
Embodiment 6
Other is with example 1, and making the ratio of cobalt acid lithium/tetrabutyl titanate/tetraethoxysilane/magnesium nitrate/ethanol is 100/0/0/0.1 ~ 1/30.
Above-mentioned processing positive electrode is made battery, be shaped on other batteries with quadrat method, the positive electrode that these batteries use and the difference of other battery only are not pass through surface treatment, and these battery mark are test of " C (being used for the comparison battery) " Performance Evaluation as table-6.
Table-6
Numbering C: T: S: M weight ratio 20% cycle-index falls in appearance, fills between 3.0～4.5V 1C * 10V overcharges ??LiCoO 2Fill between initial capacity (mAh/g) 3.0～4.2V 3.0～4.2V; 300 circulation back capacity declines (%)
Discharge Discharge
??1 ??100/0.1/0/0 ??27 Blast ??145 ??19
??2 ??100/0.2/0/0 ??33 Blast ??140 ??16
??3 ??100/0.4/0/0 ??45 Blast ??138 ??17
??4 ??100/0.6/0//0 ??38 Blast ??135 ??14
??5 ??100/0.8/0/0 ??42 Blast ??135 ??15
??6 ??100/1/0/0 ??50 Blast ??130 ??13
??7 ??100/2/0/0 ??37 By ??130 ??13
??C ??100/0/0/0 ??28 Blast ??145 ??20
C: expression cobalt acid lithium, T: expression tetrabutyl titanate, S: expression tetraethoxysilane, M: expression magnesium nitrate.

Claims (3)

1, a kind of processing method of lithium ion cell anode material lithium cobaltate, this method are at cobalt acid lithium LiCoO 2The surface of particle coats the layer of metal oxidation film, promptly earlier at cobalt acid lithium LiCoO 2The surface of particle is coated with the precursor film of one deck even compact, is by titanate esters before this precursor film, magnesium salts, and the presoma that the esters of silicon acis reaction generates is applied to LiCoO 2Particle surface and forming specifically comprises following process:
1), esters of silicon acis is dissolved in anhydrous alcohols or the acetone solvent, titanate esters is dissolved in anhydrous alcohols or the acetone solvent, magnesium nitrate is dissolved in alcohols or the acetone solvent, again above-mentioned three kinds of solution are mixed, make titanate esters, magnesium salts, esters of silicon acis is with 0.05 ~ 3: 0.05 ~ 3: 0.01 ~ 1.0 mixed;
2), pending cobalt acid lithium is added blender, stir and slowly add above-mentioned processing mixed liquor down, making cobalt acid lithium/titanate esters/esters of silicon acis/magnesium nitrate/ethanol is 100/0.05 ~ 3: 0.05 ~ 3 with the cobalt acid lithium/titanate esters/alcohol of magnesium salts/esters of silicon acis/1 ~ 8 carbon or the ratio of ketones solvent: 0.01 ~ 1.0: 20 ~ 50, high-speed stirred, high-speed mixing is 0.1～24 hour under 30～150 ℃ of temperature;
3), take out mixture, in baking oven 50 ~ 150 ℃ of dryings 0.5～24 hour; Then dried positive electrode is placed 200～1, sintering is 0.5～12 hour under 000 ℃ of high temperature;
4), be as cold as the positive electrode of normal temperature, with 150 ~ 300 order stainless steel sift net filtrations, the positive electrode that obtains handling.
2,, it is characterized in that described is 0.1-1.0g with the titanate esters of per 100 gram cobalt acid lithiums calculating or the consumption of magnesium salts according to the processing method of the lithium ion cell anode material lithium cobaltate described in the claim 1.
3,, it is characterized in that described is 0.05-0.5g with per 100 consumptions that restrain the esters of silicon acis of cobalts acid lithiums calculating according to the processing method of the lithium ion cell anode material lithium cobaltate described in the claim 1.
CNB2005100348932A 2005-05-31 2005-05-31 Method for processing positive pole material of lithium cobalt acid in lithium ion battery Expired - Fee Related CN1319192C (en)

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CN104752685A (en) * 2013-12-30 2015-07-01 北京当升材料科技股份有限公司 Lithium ion batteries cathode material and preparation method thereof
CN105633356A (en) * 2014-11-06 2016-06-01 中国电子科技集团公司第十八研究所 Preparation method for safe and high-specific energy positive electrode material of lithium ion battery
CN105633356B (en) * 2014-11-06 2020-07-28 中国电子科技集团公司第十八研究所 Preparation method of safe high-specific energy lithium ion battery anode material
CN106340637A (en) * 2015-07-07 2017-01-18 中国科学院成都有机化学有限公司 Polysilicate/NCM three-component composite positive electrode material for lithium ion battery and preparation method thereof
CN109755530A (en) * 2019-01-07 2019-05-14 华东师范大学 A kind of titanium barium bimetallic oxide surface coating method of high pressure lithium cobaltate cathode material
CN109755530B (en) * 2019-01-07 2022-04-05 华东师范大学 Surface coating method for titanium barium bimetallic oxide of high-pressure lithium cobalt oxide positive electrode material

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