CN105140496A - Preparation method for high-capacity and high-magnification negative electrode material - Google Patents
Preparation method for high-capacity and high-magnification negative electrode material Download PDFInfo
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- CN105140496A CN105140496A CN201510481576.9A CN201510481576A CN105140496A CN 105140496 A CN105140496 A CN 105140496A CN 201510481576 A CN201510481576 A CN 201510481576A CN 105140496 A CN105140496 A CN 105140496A
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/387—Tin or alloys based on tin
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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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- 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
Abstract
A preparation method for a high-capacity and high-magnification negative electrode material is disclosed. The preparation method comprises the following steps: (1) preparing an ultra-fine tin powder colloidal solution; (2) preparing a precursor sizing agent; (3) atomizing, drying, pelleting and classifying; and (4) thermal treatment; and cooling to obtain a lithium ion battery negative electrode material. According to the preparation method, the problems of charge-discharge efficiency drop and capacity degradation acceleration caused by agglomeration of nanometer tins due to higher surface energy are avoided, and the production cost is lowered; environmental pollution easily caused by using organic solvents and potential safety hazards of high possibility of explosion in atomizing and pelleting are avoided; and the problem of insufficient conductivity of amorphous carbon is overcome, and the conductivity of the negative electrode material is further enhanced.
Description
Technical field
The present invention relates to field of lithium ion battery, be specially a kind of preparation method of high power capacity high magnification negative material.
Background technology
Since nineteen ninety Sony corporation of Japan take the lead in succeeding in developing lithium ion battery and by its commercialization since, lithium ion battery obtains fast development.Nowadays lithium ion battery has been widely used in civilian and military every field.Along with the continuous progress of science and technology, the performance of people to battery proposes more higher requirements: the miniaturization of electronic equipment and individualized development, and the specific energy needing battery to have less volume and Geng Gao exports; Aero-Space energy requirements battery has cycle life, the security performance of better low temperature charge-discharge performance and Geng Gao; Electric automobile needs the battery of Large Copacity, low cost, high stability and security performance.
What current commercial Li-ion battery negative material adopted is graphite-like material with carbon element, and having lower lithium embedding/deintercalation current potential, suitable reversible capacity and aboundresources, the advantage such as cheap, is more satisfactory lithium ion battery negative material.But its theoretical specific capacity only has 372mAh/g, thus limit the further raising of lithium ion battery specific energy, the demand of growing high-energy Portable power source can not be met.Meanwhile, when graphite is as negative material, in first charge-discharge process, form one deck solid electrolyte film (SEI) on its surface.Solid electrolyte film is the formation that react to each other such as electrolyte, negative material and lithium ion, irreversibly consumes lithium ion, is to form the main factor of of irreversible capacity; It two is in the process of Lithium-ion embeding, electrolyte easily and its be embedded in the process of moving out altogether, electrolyte is reduced, the gaseous product generated causes graphite flake layer to peel off, especially containing in the electrolyte of PC, graphite flake layer comes off new for formation interface, causes further SEI to be formed, irreversible capacity increases, and cyclical stability declines simultaneously.And the degree of order of the amorphous carbon formed after resin polymers pyrolysis is low, structure comparison is loose, and lithium ion can embed relatively freely wherein and deviate from and can not produce large impact to its structure.
In addition, tin is a kind of negative material being hopeful to replace material with carbon element most, this is because tin has the height gram specific capacity up to 994mAh/g; And there is the stable discharge platform being similar to graphite.But with other high power capacity Metal Phase seemingly, the non-constant of cycle performance of tin, can not carry out normal charge and discharge cycles.In reversible lithium storage process, metallic tin volumetric expansion is remarkable, and cause cycle performance to be deteriorated, capacity is decayed rapidly, is therefore difficult to the requirement meeting large-scale production.For this reason, by introducing the nonmetalloids such as carbon, carrying out stable metal tin in the mode of alloying or compound, slowing down the volumetric expansion of tin.Carbon can stop the direct contact between tin particles, suppresses the reunion of tin particles and grows up, playing the effect of resilient coating.
Although the research of tin material with carbon element obtains larger progress, the fusing point of metallic tin only has 232 DEG C, and it inevitably volumetric expansion occurs when carrying out high-temperature heat treatment.Current, when tin material with carbon element is heat-treated, be mainly faced with following problems.Tin carbon composite is when higher temperatures heat treatment, and tin particles is easier to merge and is agglomerated into bulky grain, electrode material powder of detached in cyclic process, causes the rapid reduction of battery capacity and cycle performance to be deteriorated; When Low Temperature Heat Treatment, the resistance of tin carbon composite is large, and conductivity is bad.
Summary of the invention
Technical problem solved by the invention is the preparation method providing a kind of high power capacity high magnification negative material, to solve the problem proposed in above-mentioned background technology.
Technical problem solved by the invention realizes by the following technical solutions:
A preparation method for high power capacity high magnification negative material, its preparation process is as follows:
(1) ultra-fine glass putty colloidal solution is prepared: join in the deionized water containing dispersant by the glass putty of Large stone according to solid content 15% ~ 30%, then mill ball is added, agitation grinding, until the average grain diameter D50 of glass putty reaches 0.1 ~ 1 μm, obtains containing ultra-fine glass putty colloidal solution;
(2) precursor pulp is prepared: according to water-soluble resin: glass putty: the ratio of conductive black is 1:0.05 ~ 0.15:0.02 ~ 0.05, take water-soluble resin and conductive black to join in step (1) containing in ultra-fine glass putty colloidal solution, and add a certain amount of deionized water, regulate solid content to 25% ~ 45%, then constantly stir, obtain precursor pulp;
(3) be atomized, dry, granulation and classification: by the precursor pulp of preparation in step (2) by atomization, dry and granulation, then obtain the powder of average grain diameter between 5 ~ 35 μm through particle classifying;
(4) heat treatment: by the powder that obtains in step (3) under the protection of inert gas, be warming up to 500 ~ 700 DEG C with the speed of 1 ~ 5 DEG C/min, then be incubated 1 ~ 5h, Temperature fall, namely obtain lithium ion battery negative material after cooling.
Further, the particle diameter of the glass putty of described Large stone is 1 μm ~ 3mm.
Further, the glass putty of the middle Large stone of step (1): dispersant: deionized water: the mass ratio of mill ball is 1:0.02 ~ 0.05:5 ~ 10:2 ~ 5.
Further, described dispersant is one or more in polyvinyl alcohol, neopelex, lauryl sodium sulfate, alcohol and sodium cellulose glycolate.
Further, described mill ball is zirconia ball, choose sphere diameter be in 2mm ~ 40mm one or more collocation use; The rotating speed of agitating ball mill used is that 60 ~ 350 turns of ∕ divide.
Further, described water-soluble resin is thermosetting resin, comprises one or more the mixture in water soluble phenol resin, water-soluble epoxy resin, water soluble alkyd resin, water-soluble polyester resin, water soluble acrylic resin, water-soluble poly butadiene resin, water-soluble cationic resins.
Further, in step (3), the inlet temperature of spray-dired hot-air is 150 DEG C ~ 250 DEG C, and outlet temperature is 40 DEG C ~ 90 DEG C.
Compared with prior art, beneficial effect of the present invention is as follows:
1, prepare the method for particle diameter at the ultra-fine glass putty of 0.1 ~ 1 μm by Large stone glass putty, avoid the bulk effect that glass putty produces when discharge and recharge greatly because of particle diameter; Also avoid nanometer tin because larger surface energy simultaneously, occur reunite and cause efficiency for charge-discharge to reduce and accelerate the problem of capacity attenuation, save production cost;
2, select water-soluble resin, avoid with an organic solvent easily pollution on the environment, also avoid in the potential safety hazard by danger of easily blasting during mist projection granulating simultaneously;
3, the amorphous carbon that formed after high temperature cabonization of water-soluble resin, to electrolyte, there is stronger corrosion resistance ability, simultaneously, the interlamellar spacing of amorphous carbon is larger, lithium ion can pass in and out fast, meet the requirement of lithium ion battery high power charging-discharging, the bulk effect that glass putty produces when discharge and recharge can be cushioned in the hole secondly formed after water-soluble resin carbonization and space, ensures the overall stability of material;
4, add conductive black, in material system, define a conductive network, compensate for the deficiency of amorphous carbon electric conductivity, further enhancing the performance of conduction.
Embodiment
Reaching object to make technological means of the present invention, creation characteristic, workflow, using method and effect is easy to understand, setting forth the present invention further below.
Embodiment 1
Take the glass putty 1Kg that a certain amount of particle diameter is 2mm, join in 8Kg deionized water, then the sodium cellulose glycolate of 25g is added as dispersant, then the zirconium oxide abrasive ball 4Kg (1Kg of diameter 2mm is added, the 2Kg of diameter 5mm, the 1Kg of diameter 10mm) after, start stirring ball-milling, through detecting after 6h, diameter of particle D50 is 0.76 μm; According to water-soluble resin: glass putty: the ratio of conductive black is 1:0.1:0.03; add 10Kg water-soluble epoxy resin and 30g conductive black; add 25Kg deionized water simultaneously, regulate solid content to 25%, start to be uniformly mixed until evenly; then spray drying granulation; collect the powder of average grain diameter between 5 ~ 35 μm, be then heated to 650 DEG C under nitrogen protection, be incubated 3 hours; then be cooled to room temperature, finally obtain lithium ion battery negative material.
The performance of inspection embodiment 1 lithium ion battery negative material, test by half-cell method of testing, lithium ion battery negative material with prepared by embodiment 1: acetylene black: PVDF(Kynoar) weight ratio is 93:3:4, 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 the LiPF6/EC+DEC+DMC=1:1:1 of 1mol/L, and microporous polypropylene membrane is barrier film, is assembled into battery.Charging/discharging voltage is 0 ~ 2.0V, and charge-discharge velocity is 0.2C, and carry out testing to battery performance, the discharge capacity first of this electrode material reaches 445mAh/g, and the capacity after 100 circulations still has 392mAh/g, and conservation rate is 88.1%.
Embodiment 2
Take the glass putty 1Kg that a certain amount of particle diameter is 5mm, join in 10Kg deionized water, then the sodium cellulose glycolate of 30g is added as dispersant, then the zirconium oxide abrasive ball 5Kg (2Kg of diameter 2mm is added, the 2Kg of diameter 5mm, the 1Kg of diameter 10mm) after, start stirring ball-milling, through detecting after 10h, diameter of particle D50 is 0.54 μm.According to water-soluble resin: glass putty: conductive black=1:0.09:0.04; add 11Kg water-soluble epoxy resin and 40g conductive black; add 20Kg deionized water simultaneously, regulate solid content to 30%, start to be uniformly mixed until evenly; then spray drying granulation; collect the powder of average grain diameter between 10 ~ 35 μm, be then heated to 700 DEG C under nitrogen protection, be incubated 4 hours; then be cooled to room temperature, finally obtain lithium ion battery negative material.
The performance of inspection embodiment 2 lithium ion battery negative material, adopt the identical detection method of embodiment 1 to detect, the discharge capacity first of this motor material reaches 469mAh/g, and the capacity after 100 circulations still has 405mAh/g, and conservation rate is 86.3%.
More than show and describe general principle of the present invention, 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, and these changes and improvements all fall in the claimed scope of the invention.Claimed scope of the present invention is defined by appending claims and equivalent thereof.
Claims (7)
1. a preparation method for high power capacity high magnification negative material, is characterized in that: its preparation process is as follows:
(1) ultra-fine glass putty colloidal solution is prepared: join in the deionized water containing dispersant by the glass putty of Large stone according to solid content 15% ~ 30%, then mill ball is added, agitation grinding, until the average grain diameter D50 of glass putty reaches 0.1 ~ 1 μm, obtains containing ultra-fine glass putty colloidal solution;
(2) precursor pulp is prepared: according to water-soluble resin: glass putty: the ratio of conductive black is 1:0.05 ~ 0.15:0.02 ~ 0.05, take water-soluble resin and conductive black to join in step (1) containing in ultra-fine glass putty colloidal solution, and add a certain amount of deionized water, regulate solid content to 25% ~ 45%, then constantly stir, obtain precursor pulp;
(3) be atomized, dry, granulation and classification: by the precursor pulp of preparation in step (2) by atomization, dry and granulation, then obtain the powder of average grain diameter between 5 ~ 35 μm through particle classifying;
(4) heat treatment: by the powder that obtains in step (3) under the protection of inert gas, be warming up to 500 ~ 700 DEG C with the speed of 1 ~ 5 DEG C/min, then be incubated 1 ~ 5h, Temperature fall, namely obtain lithium ion battery negative material after cooling.
2. the preparation method of a kind of high power capacity high magnification negative material according to claim 1, it is characterized in that: described in step (1), the particle diameter of the glass putty of Large stone is 1 μm ~ 3mm, and the glass putty of Large stone: dispersant: deionized water: the mass ratio of mill ball is 1:0.02 ~ 0.05:5 ~ 10:2 ~ 5.
3. the preparation method of a kind of high power capacity high magnification negative material according to claim 1 and 2, is characterized in that: dispersant described in step (1) is one or more in polyvinyl alcohol, neopelex, lauryl sodium sulfate, alcohol and sodium cellulose glycolate.
4. the preparation method of a kind of high power capacity high magnification negative material according to claim 1, is characterized in that: described in step (1), mill ball is zirconia ball, choose sphere diameter be in 2mm ~ 40mm one or more collocation use.
5. the preparation method of a kind of high power capacity high magnification negative material according to claim 4, is characterized in that: select the rotating speed of agitating ball mill to be that 60 ~ 350 turns of ∕ divide.
6. the preparation method of a kind of high power capacity high magnification negative material according to claim 1, it is characterized in that: described in step (2), water-soluble resin is thermosetting resin, comprise one or more the mixture in water soluble phenol resin, water-soluble epoxy resin, water soluble alkyd resin, water-soluble polyester resin, water soluble acrylic resin, water-soluble poly butadiene resin, water-soluble cationic resins.
7. the preparation method of a kind of high power capacity high magnification negative material according to claim 1, is characterized in that: in step (3), during spraying dry, the inlet temperature of hot-air is 150 DEG C ~ 250 DEG C, and outlet temperature is 40 DEG C ~ 90 DEG C.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201510481576.9A CN105140496A (en) | 2015-08-07 | 2015-08-07 | Preparation method for high-capacity and high-magnification negative electrode material |
| PCT/CN2016/071956 WO2017024774A1 (en) | 2015-08-07 | 2016-01-25 | Preparation method for high capacity, high magnification negative electrode material |
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| CN201510481576.9A CN105140496A (en) | 2015-08-07 | 2015-08-07 | Preparation method for high-capacity and high-magnification negative electrode material |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017024774A1 (en) * | 2015-08-07 | 2017-02-16 | 田东 | Preparation method for high capacity, high magnification negative electrode material |
| CN106876678A (en) * | 2017-03-30 | 2017-06-20 | 苏州载物强劲新材料科技有限公司 | A kind of metal and its oxide and carbon composite production technology |
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| CN101017893A (en) * | 2006-02-08 | 2007-08-15 | 深圳市比克电池有限公司 | A tin carbon compound electrode material for lithium ion battery cathode and preparing method |
| CN101202340A (en) * | 2007-12-07 | 2008-06-18 | 广西师范大学 | Tin carbon nanometer compound material for lithium ion battery and method for making same |
| CN101997110A (en) * | 2009-08-19 | 2011-03-30 | 深圳市贝特瑞新能源材料股份有限公司 | Method for preparing stannum-carbon composite cathode material for lithium ion battery by utilizing thermal carbon reduction method |
| CN103259005A (en) * | 2013-05-08 | 2013-08-21 | 深圳市斯诺实业发展有限公司永丰县分公司 | Method for preparing high-capacity high-magnification lithium ion battery cathode material |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN103346304B (en) * | 2013-06-25 | 2015-04-22 | 南开大学 | Tin-carbon composite material for lithium secondary battery negative electrode and preparation method thereof |
| CN103346305B (en) * | 2013-07-01 | 2016-05-11 | 华南师范大学 | Delanium is preparation and the application of the lithium battery silicon-carbon composite cathode material of carrier |
| CN104009218B (en) * | 2014-05-07 | 2016-02-03 | 上海应用技术学院 | The preparation method of lithium ion battery negative material tin/lithium titanate composite electrode material |
| CN105140496A (en) * | 2015-08-07 | 2015-12-09 | 田东 | Preparation method for high-capacity and high-magnification negative electrode material |
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- 2015-08-07 CN CN201510481576.9A patent/CN105140496A/en active Pending
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- 2016-01-25 WO PCT/CN2016/071956 patent/WO2017024774A1/en active Application Filing
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101017893A (en) * | 2006-02-08 | 2007-08-15 | 深圳市比克电池有限公司 | A tin carbon compound electrode material for lithium ion battery cathode and preparing method |
| CN101202340A (en) * | 2007-12-07 | 2008-06-18 | 广西师范大学 | Tin carbon nanometer compound material for lithium ion battery and method for making same |
| CN101997110A (en) * | 2009-08-19 | 2011-03-30 | 深圳市贝特瑞新能源材料股份有限公司 | Method for preparing stannum-carbon composite cathode material for lithium ion battery by utilizing thermal carbon reduction method |
| CN103259005A (en) * | 2013-05-08 | 2013-08-21 | 深圳市斯诺实业发展有限公司永丰县分公司 | Method for preparing high-capacity high-magnification lithium ion battery cathode material |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017024774A1 (en) * | 2015-08-07 | 2017-02-16 | 田东 | Preparation method for high capacity, high magnification negative electrode material |
| CN106876678A (en) * | 2017-03-30 | 2017-06-20 | 苏州载物强劲新材料科技有限公司 | A kind of metal and its oxide and carbon composite production technology |
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| WO2017024774A1 (en) | 2017-02-16 |
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