CN101325253A - Method for preparing cathode material for high capacity lithium ion battery - Google Patents
Method for preparing cathode material for high capacity lithium ion battery Download PDFInfo
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- CN101325253A CN101325253A CNA2007100116830A CN200710011683A CN101325253A CN 101325253 A CN101325253 A CN 101325253A CN A2007100116830 A CNA2007100116830 A CN A2007100116830A CN 200710011683 A CN200710011683 A CN 200710011683A CN 101325253 A CN101325253 A CN 101325253A
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention relates to the preparation technology of cathode materials for rechargeable secondary lithium-ion batteries and provides a method of preparing the cathode materials for high-capacity lithium-ion batteries. The lithium-ion battery utilizes the techniques of the in-situ carbothermic reduction reaction and the in-situ chemical reaction ball milling to prepare the uniformly-dispersed metal oxide/carbon composite cathode materials. The prepared composite cathode materials can remarkably increase the capacity of the lithium-ion batteries and have excellent cycle performance. The composite cathode materials prepared by the method make full use of high-capacity metal oxides, additionally, the metal oxides, in the form of small granules, are uniformly dispersed on the surface of the carbon-based matrix with high interface bonding strength, so that the volume change caused by the insertion and the extraction of lithium ions during the recharging process is well attenuated by the carbon-based matrix and the cycle performance is also kept excellent.
Description
Technical field:
The present invention relates to chargeable secondary lithium battery negative material technology of preparing, a kind of method for preparing cathode material for high capacity lithium ion battery is provided, the capacity that the present invention can improve lithium ion battery has good cycle performance simultaneously.
Background technology:
Lithium rechargeable battery is big because of monomer whose voltage height, energy and power density, long-life, light weight are little, memory-less effect, advantage such as pollution-free, become current widely used power supply product, its application mainly comprises all kinds of portable electronic consumer goods (as mobile phone, notebook computer, digital camera etc.); Electric motor car (EV) and hybrid electric vehicle (HEV); Military weaponry; Space industry etc.Especially in recent years along with the application in electric motor car, people have proposed higher performance requirement to lithium ion battery.And the raising of lithium ion battery performance is decided by the performance improvement of electrode material to a great extent, particularly the raising of negative material performance.
The negative pole of current commercialization lithium ion battery mainly adopts carbonaceous materials such as MCMB, modified natural graphite, Delanium.But these graphitized carbon material theoretical capacities have only 372mAh/g, have limited the further lifting of cell integrated capacity greatly.Tinbase, alloy type negative material such as silica-based are owing to have the focus that high theoretical capacity (being respectively 991mAh/g and 4200mAh/g) becomes research in recent years always.But they and lithium alloyage process are accompanied by significant change in volume (about amplification 300%), cause electrode material efflorescence and inactivation, so capacity attenuation is very fast, and are never applied in the commercial prod.
How to prepare a kind ofly can provide high power capacity, and the negative material that has excellent cycle performance again becomes current lithium ion battery field and is badly in need of dealing with problems.
Summary of the invention:
The object of the present invention is to provide a kind of method that high power capacity has the lithium ion battery negative material of excellent cycle performance simultaneously for preparing.
Technical scheme of the present invention is:
Utilize two mechanism of original position carbothermic reduction reaction and original position " chemical reaction ball milling " to realize preparing metal oxide and be dispersed in composite negative pole material in the carbonaceous material.
The specific implementation process:
Ball milling: with raw material (different kinds of metals oxide and carbonaceous material) weighing according to a certain ratio, wherein the weight percentage ranges of metal oxide is 10%-50% (being preferably 20-30%), all the other are carbonaceous material, carry out 10-300 minute mechanical ball milling;
The carbon thermal response: ball milling is obtained mixture put into heat-treatment furnace, heating and temperature control applies reaction atmosphere simultaneously at 500-1500 ℃, is specially the mist of oxygen and inert gas; Control the feeding amount of oxygen according to the quality of processing sample, through the cooling of 10-300 minute reaction natural cooling.
In a kind of method for preparing cathode material for high capacity lithium ion battery provided by the invention, carbonaceous material can be selected from native graphite, modified natural graphite, MCMB, amorphous carbon, hard charcoal, pyrolytic carbon, petroleum coke etc.; For metal oxide, select those to have the theoretical capacity that is higher than carbonaceous material and can carry out carbothermic reduction reaction, as SnO, SnO
2, NiO, CoO, Co
3O
4, PbO, In
2O
3, ZnO, Sb
2O
3, RuO
2, FeO, Fe
2O
3, CuO, Cu
2O, MnO
2, MnO, Mn
2O
3, Ga
2O
3, SrO, SrO
2Deng.
Inert dilution gas among the present invention can be: nitrogen, argon gas, helium etc.
The feeding amount of oxygen is a key parameter among the present invention, need be controlled at 2-5 times of oxide oxygen content in the initiation material.Among the present invention the addition of inert dilution gas be oxygen feeding amount 4-15 doubly.
Reaction temperature should need guarantee that the metal that carbon thermal reduction goes out is in molten melt drop state (being the fusion temperature of a little higher than metal) according to selecting metal oxide to determine among the present invention.
The composite negative pole material that obtains through method provided by the invention also can carry out surface modification and modification once more, as by being dipped in the suitable functional group of introducings in the electrolyte, with the better chemical property of acquisition.
Characteristics of the present invention:
1, the present invention utilizes the original position carbothermic reduction reaction, will be dispersed in that metal oxide is reduced into metal at the carbonaceous material surface in situ in the material with carbon element, and is in the drop state.
2, the present invention not only makes to restore molten drop generation oxidation by control carbon thermal process reactor oxygen feeding amount, makes the carbonaceous material surface that slight oxidation takes place simultaneously again.
3, slight oxidation also can take place in carbonaceous material in the processing procedure of the present invention, and surface roughness increases, and also occurs some nanometers, micron order hole simultaneously, has increased the molten condition molten drop that restores at the carbonaceous material surface wettability.Meanwhile, the molten drop surface also carrying out oxidation reaction, generates the high-melting point metal oxide skin(coating) gradually.
4, metal oxide generation carbon thermal response of the present invention and the molten drop that restores increase and the oxidation reaction acting in conjunction of drop surface is divided molten melt drop in the carbonaceous material surface wettability, form a plurality of more droplets.Because there is the existence of refractory oxide layer on the drop surface, has stoped melting mutually also, growing up of droplet.
5, the present invention is after the metal droplet is completely oxidized to metal oxide, and carbothermic reduction reaction carries out once more, and is reduced into molten drop, subsequently this drop experience transition process identical with top description.These a series of processes (being referred to as original position " chemical reaction ball milling ") repeat, and finish up to the reaction time, obtain a kind of metal oxide is dispersed in the carbonaceous material surface with granule (diameter is generally at 10-100nm) original position composite negative pole material.
6, to obtain obtaining even dispersing metal oxides by the in-situ chemical reaction ball milling in the composite material be that other conventional method (as the simple mechanical ball milling) is difficult to realize in the present invention.Pass through original position " chemical reaction ball milling " simultaneously, metal oxide combines with the interface of carbonaceous material and becomes more firmly closely.
In a word, the original position composite negative pole material that utilizes method provided by the invention to prepare not only can be given full play to the contribution of high power capacity metal oxide.In addition, because metal oxide is dispersed in the carbonaceous material surface with granule, the interface is in conjunction with firm, and lithium ion embeds the change in volume of deviating to cause and can well be cushioned absorption by the carbonaceous matrix like this.Therefore, You Yi cycle performance also can be kept.
Description of drawings:
Fig. 1 (a)-(b) is SnO
2With carbonaceous mesophase spherules through secondary electron image (a) after the invention provides method and handling and backscattered electron image (b) accordingly.
Fig. 2 (a)-(b) is SnO
2With secondary electron image (a) and the corresponding backscattered electron image (b) of carbonaceous mesophase spherules process mechanical ball milling after 50 minutes.
Fig. 3 is the chemical property contrast.
Embodiment:
Embodiment 1
Weighing carbonaceous mesophase spherules (76wt.%) and SnO
2Mixture (24wt.%) is 0.5g altogether,, is put in the heating furnace after 50 minutes through mechanical ball milling, reacts under 800 ℃ 40 minutes.Oxygen feeding amount is initial SnO in the course of reaction
23 times of oxygen content, inert gas is N
2, the addition of inert gas is 5 times of oxygen.Reaction finishes the electron scanning micrograph of back sample and sees (Fig. 1 (a)-(b)), can see SnO
2Granule is dispersed on the carbosphere surface.Conventional lithium ion battery negative evaluation method testing result shows, sample have high specific capacity (＞500mAh/g) and excellent cycle performance, (Fig. 3) seen in the detailed data contrast.
Comparative Examples 1
Weighing carbonaceous mesophase spherules (76wt.%) and SnO
2Mixture (24wt.%) is 0.5g altogether, and mechanical ball milling was handled 50 minutes.(Fig. 2 (a)-(b)) can see SnO from electron scanning micrograph
2With big particle agglomeration, disperse very inhomogeneous.(Fig. 3) seen in the chemical property contrast, and capacity is decayed very below 300mAh/g from initial 500mAh/g.
Embodiment 2
Weighing carbonaceous mesophase spherules (56wt.%) and SnO
2Mixture (44wt.%) is 0.5g altogether,, is put in the heating furnace after 90 minutes through mechanical ball milling, reacts under 950 ℃ 40 minutes.Oxygen feeding amount is initial SnO in the course of reaction
23 times of oxygen content, inert gas is N
2, the addition of inert gas is 7 times of oxygen.Reaction finishes the back sample and carries out conventional lithium ion battery negative evaluation method detection, and the result shows that 30 circulation back capacity are still more than 450mAh/g.
Comparative Examples 2
Weighing carbonaceous mesophase spherules (56wt.%) and SnO
2Mixture (44wt.%) is 0.5g altogether.After mechanical ball milling was handled in 90 minutes, carry out conventional lithium ion battery negative evaluation method and detect, the result shows that 30 circulation back capacity decay to below the 250mAh/g.
Embodiment 3
Weighing natural graphite nodule (75wt.%) and Fe
2O
3Mixture (25wt.%) is 0.5g altogether,, is put in the heating furnace after 90 minutes through mechanical ball milling, reacts under 1500 ℃ 20 minutes.Oxygen feeding amount is initial Fe in the course of reaction
2O
32 times of oxygen content, inert gas is Ar, the addition of inert gas is 15 times of oxygen.Reaction finishes the back sample and carries out conventional lithium ion battery negative evaluation method detection, and the result shows that 30 circulation back capacity are still more than 500mAh/g.
Embodiment 4
The mixture of hard charcoal ball of weighing (70wt.%) and PbO (30wt.%) is 0.5g altogether,, is put in the heating furnace after 60 minutes through mechanical ball milling, reacts under 700 ℃ 40 minutes.Oxygen feeding amount is 5 times of initial PbO oxygen content in the course of reaction, and inert gas is N
2, the addition of inert gas is 4 times of oxygen.Reaction finishes the back sample and carries out conventional lithium ion battery negative evaluation method detection, and the result shows that 30 circulation back capacity are still more than 470mAh/g.
Embodiment 5
The mixture of weighing natural graphite nodule (60wt.%) and ZnO (40wt.%) is 0.5g altogether,, is put in the heating furnace after 90 minutes through mechanical ball milling, reacts under 1300 ℃ 25 minutes.Oxygen feeding amount is 2 times of initial ZnO oxygen content in the course of reaction, and inert gas is N
2, the addition of inert gas is 11 times of oxygen.Reaction finishes the back sample and carries out conventional lithium ion battery negative evaluation method detection, and the result shows that 30 circulation back capacity are still more than 450mAh/g.
Embodiment 6
The mixture of hard charcoal ball of weighing (60wt.%) and CuO (40wt.%) is 0.5g altogether,, is put in the heating furnace after 40 minutes through mechanical ball milling, reacts under 1100 ℃ 30 minutes.Oxygen feeding amount is 2.5 times of initial CuO oxygen content in the course of reaction, and inert gas is N
2, the addition of inert gas is 9 times of oxygen.Reaction finishes the back sample and carries out conventional lithium ion battery negative evaluation method detection, and the result shows that 30 circulation back capacity are still more than 500mAh/g.
Embodiment 7
The mixture of weighing carbonaceous mesophase spherules (75wt.%) and CoO (25wt.%) is 0.5g altogether,, is put in the heating furnace after 90 minutes through mechanical ball milling, reacts under 1450 ℃ 25 minutes.Oxygen feeding amount is 2 times of initial CoO oxygen content in the course of reaction, and inert gas is N
2, the addition of inert gas is 13 times of oxygen.Reaction finishes the back sample and carries out conventional lithium ion battery negative evaluation method detection, and the result shows that 50 circulation back capacity are still more than 450mAh/g.
Embodiment 8
Weighing natural graphite nodule (50wt.%) and Sb
2O
3Mixture (50wt.%) is 0.5g altogether,, is put in the heating furnace after 30 minutes through mechanical ball milling, reacts under 750 ℃ 45 minutes.Oxygen feeding amount is initial Sb in the course of reaction
2O
34 times of oxygen content, inert gas is N
2, the addition of inert gas is 5 times of oxygen.Reaction finishes the back sample and carries out conventional lithium ion battery negative evaluation method detection, and the result shows that 50 circulation back capacity are still more than 440mAh/g.
Claims (5)
1, a kind of method for preparing cathode material for high capacity lithium ion battery is characterized in that: utilize original position carbothermic reduction reaction and in-situ chemical reaction ball milling to realize the homodisperse metal oxide/carbon compound cathode materials of preparation, concrete steps are as follows:
A evenly disperses: metal oxide and carbonaceous material are put into ball mill, carry out 10-300 minute mechanical ball milling, realize that metal oxide and carbonaceous material evenly disperse;
B carbon thermal response: ball milling obtains mixture and puts into heat-treatment furnace, utilize the carbon thermal response that oxide is reduced into metal and forms the molten melt drop state, heating and temperature control is at 500-1500 ℃, apply reaction atmosphere simultaneously, be specially oxygen and inert gas mist, the feeding amount of oxygen is 2-5 a times of oxide oxygen content in the initiation material, after reaction in 10-300 minute, and the natural cooling cooling.
2, according to the described method for preparing cathode material for high capacity lithium ion battery of claim 1, it is characterized in that: the weight percentage ranges of metal oxide is 10%-50%, and all the other are carbonaceous material.
3, according to the described method for preparing cathode material for high capacity lithium ion battery of claim 1, it is characterized in that: inert gas is nitrogen, argon gas or helium, and its feeding amount is 4-15 a times of oxygen feeding amount.
4, according to the described method for preparing cathode material for high capacity lithium ion battery of claim 1, it is characterized in that: described carbonaceous material is native graphite, MCMB, amorphous carbon, hard charcoal, pyrolytic carbon or petroleum coke.
5, according to the described method for preparing cathode material for high capacity lithium ion battery of claim 1, it is characterized in that: described metal oxide is SnO, SnO
2, NiO, CoO, Co
3O
4, PbO, In
2O
3, ZnO, Sb
2O
3, RuO
2, FeO, Fe
2O
3, CuO, Cu
2O, MnO
2, MnO, Mn
2O
3, Ga
2O
3, SrO or SrO
2
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|---|---|---|---|
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| CN100583503C CN100583503C (en) | 2010-01-20 |
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| CN102280640A (en) * | 2011-07-12 | 2011-12-14 | 南开大学 | Novel anode material for lithium-ion secondary battery |
| CN102318107A (en) * | 2009-02-16 | 2012-01-11 | 丰田自动车株式会社 | Lithium secondary battery |
| CN102983308A (en) * | 2012-12-17 | 2013-03-20 | 中国科学院上海硅酸盐研究所 | Carbon nanotube array/nickel oxide nanoparticle coaxial composite cathode material and preparation method thereof |
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- 2007-06-13 CN CN200710011683A patent/CN100583503C/en not_active Expired - Fee Related
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| CN102280640B (en) * | 2011-07-12 | 2013-11-06 | 南开大学 | Novel anode material for lithium-ion secondary battery |
| CN102983308A (en) * | 2012-12-17 | 2013-03-20 | 中国科学院上海硅酸盐研究所 | Carbon nanotube array/nickel oxide nanoparticle coaxial composite cathode material and preparation method thereof |
| CN103050679A (en) * | 2012-12-26 | 2013-04-17 | 浙江工业大学 | Spherical hollow porous MnO/C composite material and application thereof |
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