CN105140483A - Preparation method of modified lithium battery anode material - Google Patents

Preparation method of modified lithium battery anode material Download PDF

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Publication number
CN105140483A
CN105140483A CN201510481031.8A CN201510481031A CN105140483A CN 105140483 A CN105140483 A CN 105140483A CN 201510481031 A CN201510481031 A CN 201510481031A CN 105140483 A CN105140483 A CN 105140483A
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powder
graphite
preparation
lithium battery
modified lithium
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CN201510481031.8A
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田东
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Priority to PCT/CN2016/086701 priority patent/WO2017024897A1/en
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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
    • 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
    • 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
    • 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
    • H01M4/621—Binders
    • 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

The invention discloses a preparation method of a modified lithium battery anode material. Raw materials are based on the ratio of parts by weight; and the method comprises the following steps: (1) adding graphite, phenolic resin and nanometer tin powder to hexamethylenetetramine with the resin content of 3%-5%, and mixing the raw materials into uniform slurry; (2) carrying out spray drying on the evenly mixed slurry to obtain graphite powder of which the surface is coated with a nanometer tin and phenolic resin mixture; (3) mixing the obtained powder with asphalt powder evenly; and (4) carrying out high-temperature treatment on the obtained powder. Through selecting the nanometer tin powder, the volume effect caused by relatively large particle sizes of the tin powder in charging and discharging processes is avoided; and the stability of the materials in the charging and discharging processes is ensured.

Description

A kind of preparation method of modified lithium battery negative material
Technical field
The present invention relates to a kind of preparation method of lithium ion battery negative material, be specially a kind of preparation method of modified lithium battery 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.
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.People have carried out this kind of material and have studied widely in recent years, and make some progress.But 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.
Research shows, the tin of small particle diameter or its alloy all improve a lot on capacity or on cycle performance, when the particle of alloy material reaches nanoscale, volumetric expansion in charge and discharge process can alleviate greatly, performance also can increase, but nano material has larger surface energy, easily reunites, efficiency for charge-discharge can be made on the contrary to reduce and accelerate the decay of capacity, thus counteract the advantage of nano particle.Another research tendency improving tin negative pole performance is exactly prepare composite material or the alloy of tin and other material, and wherein, the tin/carbon composite prepared in conjunction with the stability of material with carbon element and the height ratio capacity characteristic of tin shows huge application prospect.
Summary of the invention
Technical problem solved by the invention is the preparation method providing a kind of modified lithium battery negative material, to solve the shortcoming in above-mentioned background technology.
A kind of preparation method of modified lithium battery negative material, raw material is according to weight ratio, comprise the following steps: (1) by graphite, phenolic resins, nanometer glass putty according to 100:5 ~ 20:5 ~ 10, solid content is the ratio of 20% ~ 40%, first takes a certain amount of nanometer glass putty and puts into spirit solvent, and ultrasonic disperse, then phenolic resins and graphite is added respectively, the hexamethylenetetramine simultaneously adding amount of resin 3% ~ 5%, as resin curing agent, constantly stirs, and is mixed into even slurry; (2) by the slurry that mixes by spraying dry, obtain the graphite composite powder being coated with nanometer tin and phenolic resin blend; (3) again obtained powder is mixed with the ratio of pitch powder according to 100:5 ~ 20; (4) again by obtained powder under the protection of inert gas, be warming up to 800 ~ 1000 DEG C with the speed of 1 ~ 5 DEG C/min, then be incubated 1 ~ 5h, Temperature fall, sieve after cooling and namely obtain high power capacity modified graphite cathode material.
Further, graphite is native graphite or Delanium, and average grain diameter is 5 ~ 30 μm, tap density>=0.75g/cm 3, specific area≤6m 2/ g.
Further, the particle diameter of glass putty is not more than 100 nanometers.
Further, the inlet temperature of spray-dired hot-air is 150 DEG C ~ 200 DEG C, and outlet temperature is 40 DEG C ~ 70 DEG C.
Further, pitch powder comprises the powder prepared by one or more the mixture in coal tar pitch, petroleum asphalt, modified coal tar pitch, mesophase pitch, the condensation polycyclic polynuclear aromatic hydrocarbon that obtained by asphalt modifier, softening point is at 100--280 DEG C, and average grain diameter is 2 ~ 5 μm.
beneficial effect
(1) by selecting nanometer glass putty, avoid the bulk effect that glass putty produces when discharge and recharge because particle diameter is comparatively large, ensure that the stability in charge and discharge process of material, simultaneously and graphite carry out compound coating process, solve the shortcomings such as single graphite cathode material capacity is on the low side;
(2) resin is in heat treatment process, and the Small molecular in resin is too much, and the surface of coated rear material can be caused in overflow process to produce too much space, and the bulk effect of buffering glass putty can be played in these spaces, ensures the stable of material system;
(3) by last pitch, secondary carries out to material coated, reduce the specific area of material, improve the first charge-discharge efficiency of material;
(4) by adding resin curing agent---hexamethylenetetramine in preceding step, allow resin in spray drying step by hot curing, therefore can not melting because second time is heated, avoiding the later stage serious problem of luming after causing high temperature sintering because adding pitch again.
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
According to graphite, phenolic resins, nanometer glass putty according to 100:10:5, solid content is the ratio of 30%, the spirit solvent of 5366g put into by the nanometer glass putty taking 100g, and ultrasonic disperse, then phenolic resins and the 2000g native graphite of 200g is added respectively, add the hexamethylenetetramine 6g of amount of resin 3% simultaneously, constantly stir, be mixed into even slurry; Again slurry is carried out spraying dry; obtain the graphite composite powder being coated with nanometer tin and phenolic resin blend; after again powder being mixed according to the ratio of 100:5 with pitch powder; under the protection of inert gas; 1000 DEG C are warming up to the speed of 5 DEG C/min; be incubated 3h again, Temperature fall, sieve after cooling and namely obtain modification negative material of the present invention.
Embodiment 2
According to graphite, phenolic resins, nanometer glass putty according to 100:15:5, solid content is the ratio of 30%, the spirit solvent of 5600g put into by the nanometer glass putty taking 100g, and ultrasonic disperse, then phenolic resins and the 2000g native graphite of 300g is added respectively, add the hexamethylenetetramine 9g of amount of resin 3% simultaneously, constantly stir, be mixed into even slurry; Again slurry is carried out spraying dry; obtain the graphite composite powder being coated with nanometer tin and phenolic resin blend; after again powder being mixed according to the ratio of 100:5 with pitch powder; under the protection of inert gas; 900 DEG C are warming up to the speed of 3 DEG C/min; be incubated 4h again, Temperature fall, sieve after cooling and namely obtain modification negative material of the present invention.
Embodiment 3
According to graphite, phenolic resins, nanometer glass putty according to 100:15:10, solid content is the ratio of 30%, the spirit solvent of 5833g put into by the nanometer glass putty taking 200g, and ultrasonic disperse, then phenolic resins and the 2000g native graphite of 300g is added respectively, add the hexamethylenetetramine 9g of amount of resin 3% simultaneously, constantly stir, be mixed into even slurry; Again slurry is carried out spraying dry; obtain the graphite composite powder being coated with nanometer tin and phenolic resin blend; after again powder being mixed according to the ratio of 100:5 with pitch powder; under the protection of inert gas; 950 DEG C are warming up to the speed of 4 DEG C/min; be incubated 2.5h again, Temperature fall, sieve after cooling and namely obtain modification negative material of the present invention.
Comparative example 1
According to graphite, phenolic resins according to 100:10, solid content is the ratio of 30%, and the spirit solvent of 5113g put into by the phenolic resins of 200g and 2000g native graphite, adds the hexamethylenetetramine 6g of amount of resin 3% simultaneously, constantly stirs, be mixed into even slurry; Again slurry is carried out spraying dry; obtain the graphite composite powder being coated with phenolic resin blend; after again powder being mixed according to the ratio of 100:5 with pitch powder; under the protection of inert gas; 1000 DEG C are warming up to the speed of 5 DEG C/min; be incubated 3h again, Temperature fall, sieve after cooling and namely obtain high power capacity modified graphite cathode material.
Comparative example 2
Natural spherical plumbago without any process directly carries out electric performance test.
Electrochemical property test
For the performance of lithium ion modification 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/LLiPF6/EC+DEC+DMC=1:1:1, 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, test result is in table 1.
Table 1 is the Performance comparision of negative material in different embodiment and comparative example
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, and these changes and improvements all fall in the claimed scope of the invention.Application claims protection range is defined by appending claims and equivalent thereof.

Claims (5)

1. a preparation method for modified lithium battery negative material, raw material, according to weight ratio, is characterized in that, comprises the following steps:
(1) by graphite, phenolic resins, nanometer glass putty according to 100:5 ~ 20:5 ~ 10, solid content is the ratio of 20% ~ 40%, first take a certain amount of nanometer glass putty and put into spirit solvent, and ultrasonic disperse, then phenolic resins and graphite is added respectively, the hexamethylenetetramine simultaneously adding amount of resin 3% ~ 5%, as resin curing agent, constantly stirs, and is mixed into even slurry;
(2) by the slurry that mixes by spraying dry, obtain the graphite composite powder being coated with nanometer tin and phenolic resin blend;
(3) again obtained powder is mixed with the ratio of pitch powder according to 100:5 ~ 20;
(4) again by obtained powder under the protection of inert gas, be warming up to 800 ~ 1000 DEG C with the speed of 1 ~ 5 DEG C/min, then be incubated 1 ~ 5h, Temperature fall, sieve after cooling.
2. the preparation method of a kind of modified lithium battery negative material according to claim 1, is characterized in that, graphite is native graphite or Delanium, and average grain diameter is 5 ~ 30 μm, tap density>=0.75g/cm 3, specific area≤6.0m 2/ g.
3. the preparation method of a kind of modified lithium battery negative material according to claim 1, is characterized in that, the particle diameter of glass putty is not more than 100 nanometers.
4. the preparation method of a kind of modified lithium battery negative material according to claim 1, is characterized in that, the inlet temperature of spray-dired hot-air is 150 DEG C ~ 200 DEG C, and outlet temperature is 40 DEG C ~ 70 DEG C.
5. the preparation method of a kind of modified lithium battery negative material according to claim 1, it is characterized in that, pitch powder comprises the powder prepared by one or more the mixture in coal tar pitch, petroleum asphalt, modified coal tar pitch, mesophase pitch, the condensation polycyclic polynuclear aromatic hydrocarbon that obtained by asphalt modifier, softening point is at 100--280 DEG C, and average grain diameter is 2 ~ 5 μm.
CN201510481031.8A 2015-08-07 2015-08-07 Preparation method of modified lithium battery anode material Pending CN105140483A (en)

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PCT/CN2016/086701 WO2017024897A1 (en) 2015-08-07 2016-06-22 Preparation method for modified lithium-ion battery negative electrode material

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Cited By (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2017024897A1 (en) * 2015-08-07 2017-02-16 田东 Preparation method for modified lithium-ion battery negative electrode material
CN110679014A (en) * 2017-09-28 2020-01-10 株式会社Lg化学 Method for predicting manufacturability of electrode slurry and selecting electrode binder
CN112072124A (en) * 2020-08-17 2020-12-11 郭峰 Preparation method of cathode support body material of special-shaped direct ethanol fuel cell
CN112687874A (en) * 2020-12-28 2021-04-20 萝北奥星新材料有限公司 High-stability lithium battery negative electrode material and application thereof
CN113800510A (en) * 2021-09-07 2021-12-17 广东凯金新能源科技股份有限公司 Graphite negative electrode material and preparation method thereof

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CN111908462A (en) * 2020-07-21 2020-11-10 铜仁学院 Preparation method of long-cycle artificial graphite negative electrode precursor
CN114213126B (en) * 2021-12-22 2022-12-02 格龙新材料科技(常州)有限公司 Preparation method of high-capacity high-compaction-density graphite composite material
CN115579470B (en) * 2022-10-24 2023-09-12 赣州市瑞富特科技有限公司 Modified asphalt coated microcrystalline graphite negative electrode material and preparation method thereof

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Publication number Priority date Publication date Assignee Title
WO2017024897A1 (en) * 2015-08-07 2017-02-16 田东 Preparation method for modified lithium-ion battery negative electrode material
CN110679014A (en) * 2017-09-28 2020-01-10 株式会社Lg化学 Method for predicting manufacturability of electrode slurry and selecting electrode binder
CN110679014B (en) * 2017-09-28 2023-04-04 株式会社Lg新能源 Method for predicting manufacturability of electrode slurry and selecting electrode binder
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CN112072124A (en) * 2020-08-17 2020-12-11 郭峰 Preparation method of cathode support body material of special-shaped direct ethanol fuel cell
CN112687874A (en) * 2020-12-28 2021-04-20 萝北奥星新材料有限公司 High-stability lithium battery negative electrode material and application thereof
CN113800510A (en) * 2021-09-07 2021-12-17 广东凯金新能源科技股份有限公司 Graphite negative electrode material and preparation method thereof

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