CN105047891A - Preparation method of graphite tin-based composite anode material - Google Patents
Preparation method of graphite tin-based composite anode material Download PDFInfo
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- H01M4/36—Selection of substances as active materials, active masses, active liquids
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Abstract
The invention discloses a preparation method of a graphite tin-based composite anode material. According to the method, nanometer tin is coated with a resin carbon precursor; and a porous structure which is formed after carbonization of the resin carbon precursor is taken as a carrier for fixing the nanometer tin, so that the volume expansion effect of tin can be effectively relieved; the carrier is compounded with graphite, and is subjected to asphalt-coating modified treatment, so that the defect of over-large specific surface area of the resin material is overcome; the great irreversible capacity loss is avoided; the finally obtained material has the advantages of small specific surface area, good processability, high gram specific capacity, long periodic cycle and the like; and meanwhile, the method disclosed by the invention is simple to operate, easy to control, low in production cost and suitable for industrial production.
Description
Technical field
The present invention relates to lithium ion battery negative material field, be specifically related to a kind of preparation method of lithium ion battery graphite tinbase composite negative pole material.
Background technology
Since the beginning of the nineties in last century, Sony energy technology company took the lead in successfully developing the lithium ion battery using Carbon anode, lithium ion battery captures rapidly civil secondary Battery Market with the speed of average annual 15%, has become the first-selected power supply of current portable electronic equipment.The develop rapidly of lithium ion battery mainly has benefited from the contribution of electrode material, the particularly progress of negative material.Lithium ion battery negative material requires to possess following characteristics: 1. alap electrode potential; 2. ion has higher diffusivity in negative pole solid-state structure; 3. the deintercalation invertibity of height; 4. good conductivity and thermodynamic stability; 5. security performance is good; 6. good with electrolyte solvent compatibility; 7. aboundresources, cheap, environmentally safe.Negative material is one of large raw material (positive pole, negative pole, electrolyte, barrier film) of lithium ion battery four, what current commercial Li-ion battery negative material adopted is graphite-like material with carbon element, 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.
Inexpensive with it, the nontoxic and superior chemical property of material with carbon element is widely used in lithium ion battery, and state of interface and the fine structure of itself have a great impact electrode performance.At present, commercial carbon negative electrode material of lithium ion cell can be divided into graphite, hard carbon and soft carbon three class, and wherein graphite type material is still the main flow of lithium ion battery negative material.Graphite-like material with carbon element, 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.As lithium ion battery negative material, material with carbon element still exists that charge/discharge capacity is low, first cycle irreversible loss is large, solvent molecule intercalation and the shortcoming such as preparation cost is high altogether, and these are also the key issues solved needed in current Study on Li-ion batteries.
Carbon fiber is a kind of novel material with carbon element, divides mainly contain PAN base carbon fibre (on market, more than 90% is this kind of carbon fiber), viscose-based carbon fiber, asphalt base carbon fiber etc. three kinds by raw material.In general, the resistivity of asphalt base carbon fiber is less than PAN base carbon fibre, and PAN base carbon fibre resistivity is less than viscose-based carbon fiber.Electronics rate all can reduce along with the rising of heat treatment temperature.
Chinese patent CN102623704A, by adding carbon fiber, utilize its high conductivity and strong adsorptivity to prepare lithium carbonate-carbon fiber composite negative pole material to solve the problem of material high rate charge-discharge performance and raising conductivity, meet the requirement of modern society to lithium ion battery applications.Chinese patent CN102290582A, by adding nanometer overlength carbon fiber VGCF, improving battery conductive, reducing internal resistance.
A kind of tin/graphene/carbon fiber composite lithium cell cathode material preparation method that Chinese patent CN104037393A announces, the network configuration that Graphene and carbon fiber mixing are formed, for lithium ion turnover electrode provides a large amount of transfer passages smoothly, make it fully contact with negative material, improve the utilization ratio of negative material.Improve the transport velocity of lithium during active position and the discharge and recharge of negative material storage lithium.The high conduction performance of Graphene and carbon fiber can realize carrier mobility fast, effectively can reduce the internal resistance of battery itself while improving power output.
Metallic tin has the advantage such as high lithium storage content (994mAh/g) and low lithium ion deintercalation platform voltage, is the extremely potential non-carbon negative material of one.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.
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.Therefore, in order to improve the conductivity of tin carbon composite and alleviate metallic tin particle agglomeration under higher thermal treatment temperature, can have by introducing the thermal endurance that dystectic material improves tin carbon composite.Wherein, nickel is the metal with satisfactory electrical conductivity, and fusing point is 1453 DEG C, is incorporated in tin carbon composite and can improves composite material heat treatment temperature and obtain the negative material with good electrical chemical property.RenzongHu etc. adopt e-beam evaporation to prepare and have nucleocapsid and multiple dimensioned Sn-C-Ni negative material, and this electrode material shows excellent capability retention and high high rate performance.He Chunnian etc. adopt pyrolysismethod to prepare two-dimentional porous graphite carbon-coating nickel tin alloy material, and it has very high specific capacity and fabulous cycle performance (application number 201310715142.1) for lithium ion battery negative.
Summary of the invention
For prior art Problems existing, an object of the present invention is the preparation method providing a kind of graphite tinbase composite negative pole material, the method first adopts resinae carbon matrix precursor to carry out coated to nanometer tin, carbon matrix precursor forms loose structure after high temperature cabonization, effectively can alleviate the Volumetric expansion of tin, again by pulverizing, submicron powder is obtained to the material after coated carbonization, after mixing with graphite, pitch class carbon matrix precursor again, pass through high-temperature process, cooling is sieved, and obtains graphite tinbase composite negative pole material of the present invention.
A preparation method for graphite tinbase composite negative pole material, concrete preparation process is as follows:
(1) by the dispersion of resinae carbon matrix precursor in a solvent, add nanometer tin, then ultrasonic disperse, evaporate organic solvent, under inert gas shielding, high temperature cabonization, obtains materials A;
(2) by materials A by pulverizing, obtain particle diameter D50 between the submicron order powder B of 0.1 ~ 1 μm;
(3) powder B and graphite, pitch class carbon matrix precursor are carried out solid phase mixing, then under inert gas shielding, high temperature cabonization, cooling is sieved.
Further, resinae carbon matrix precursor refers to the combination of in furfural resin, epoxy resin, phenolic resins, polyethylene glycol, polyvinyl chloride, polyvinyl butyral resin, polyacrylonitrile, polyacrylic acid a kind or at least 2 kinds in step (1).
Further, in step (1), the ratio of resinae carbon matrix precursor and nanometer tin is 1:(0.05 ~ 0.15).
Further, in step (1), the temperature of high temperature cabonization is 650 ~ 850 DEG C, and heating rate is 1 ~ 5 DEG C/min, and temperature retention time is 0.5 ~ 3h.
Further, step (2) is pulverized and is referred to by the one or more kinds of combinations in ball milling, mechanical crushing or air-flow crushing mode.
Further, the weight ratio of step (3) powder B and graphite is (0.1 ~ 0.5): 1, and pitch class carbon matrix precursor accounts for 10 ~ 30% of powder B and graphite total weight.
Further, in step (3), the average grain diameter of graphite is 5 ~ 30 μm, tap density>=0.7g/cm
3.
Further, step (3) medium pitch class carbon forerunner refers to the combination of in coal tar pitch, petroleum asphalt, modified coal tar pitch, mesophase pitch, the condensation polycyclic polynuclear aromatic hydrocarbon that obtained by asphalt modifier a kind or at least 2 kinds.
Further, diameter of particle D50≤3 μm of step (3) medium pitch class carbon forerunner.
Further, in step (3), the temperature of high temperature cabonization is 850 ~ 1000 DEG C, and heating rate is 5 ~ 20 DEG C/min, and temperature retention time is 0.5 ~ 4h.
The loose structure carbon formed after the carbonization of resinae carbon matrix precursor is as the carrier of fixing nanometer tin, utilize the characteristic that organic molecule in resin is many, when high temperature, Small molecular therefrom overflows, form micropore, nanometer tin is evenly embedded in micropore, the method can improve the dispersiveness of nanometer tin particle in tinbase composite negative pole material, alleviate material take off/embedding lithium time volumetric expansion and contraction, enhance the structural stability of material, ensure that material has higher conductance, improve chemical property and the cyclical stability thereof of material.
Again by after carrying out compound with graphite, through pitch-coating modification, solve the shortcoming that resinous material specific area is excessive, avoid large irreversible capacity loss, the material of final gained has low specific area, good processing characteristics and the advantage such as Gao Ke specific capacity and long period circulation.
Meanwhile, method of the present invention is simple to operate, be easy to control, and production cost is low, be applicable to suitability for industrialized production.
Embodiment
In order to understand the present invention better, illustrate technical scheme of the present invention below by specific embodiment.
Embodiment 1
Epoxy resin is dispersed in acetone solvent, in epoxy resin: the ratio of nanometer tin=1:0.1 adds glass putty, then ultrasonic disperse, evaporate organic solvent, under inert gas shielding, 750 DEG C are risen to the heating rate of 2 DEG C/min, insulation 2h, utilize air-flow crushing that the powder of gained after carbonization is crushed to D50 between 0.1 ~ 1 μm, be the weight ratio of 0.3:1 by powder and graphite again, the petroleum asphalt (D50=2.15 μm) simultaneously adding 15% of powder and graphite total weight is mixed together, after each component mixes, under inert gas shielding, powder is risen to 850 DEG C with the heating rate of 10 DEG C/min, insulation 3h, after being cooled to room temperature, sieve and obtain the graphite tinbase composite negative pole material prepared by the present invention.
Embodiment 2
By phenolic resin dispersion in spirit solvent, in phenolic resins: the ratio of nanometer tin=1:0.15 adds glass putty, then ultrasonic disperse, evaporate organic solvent, under inert gas shielding, 800 DEG C are risen to the heating rate of 3 DEG C/min, insulation 3h, utilize ball mill grinding that the powder of gained after carbonization is crushed to D50 between 0.1 ~ 1 μm, be the weight ratio of 0.4:1 by powder and graphite again, the coal tar pitch (D50=2.15 μm) simultaneously adding 20% of powder and graphite total weight is mixed together, after each component mixes, under inert gas shielding, powder is risen to 1000 DEG C with the heating rate of 10 DEG C/min, insulation 0.5h, after being cooled to room temperature, sieve and obtain the graphite tinbase composite negative pole material prepared by the present invention.
Embodiment 3
Polyethylene glycol is dispersed in deionization, in polyethylene glycol: the ratio of nanometer tin=1:0.05 adds glass putty, then ultrasonic disperse, evaporate organic solvent, under inert gas shielding, 850 DEG C are risen to the heating rate of 5 DEG C/min, insulation 1h, utilize mechanical crushing that the powder of gained after carbonization is crushed to D50 between 0.1 ~ 1 μm, be the weight ratio of 0.5:1 by powder and graphite again, the mesophase pitch (D50=2.15 μm) simultaneously adding 30% of powder and graphite total weight is mixed together, after each component mixes, under inert gas shielding, powder is risen to 900 DEG C with the heating rate of 15 DEG C/min, insulation 1.5h, after being cooled to room temperature, sieve and obtain the graphite tinbase composite negative pole material prepared by the present invention.
Embodiment 4
By phenolic resin dispersion in spirit solvent, in resin: the ratio of nanometer tin=1:0.1 adds glass putty, then ultrasonic disperse, evaporate organic solvent, under inert gas shielding, 850 DEG C are risen to the heating rate of 2 DEG C/min, insulation 0.5h, utilize air-flow crushing that the powder of gained after carbonization is crushed to D50 between 0.1 ~ 1 μm, be the weight ratio of 0.25:1 by powder and graphite again, the modified coal tar pitch (D50=2.15 μm) simultaneously adding 20% of powder and graphite total weight is mixed together, after each component mixes, under inert gas shielding, powder is risen to 850 DEG C with the heating rate of 5 DEG C/min, insulation 2.5h, after being cooled to room temperature, sieve and obtain the graphite tinbase composite negative pole material prepared by the present invention.
Comparative example 1
One-component graphite in embodiment 1.
Comparative example 2
According to the preparation flow in embodiment 1, difference is not add the negative material that glass putty finally obtains.
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/LLiPF6/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
Negative material with embodiment and comparative example: SP:SBR(solid content 50%): CMC=94:2.5:1.5:2(weight ratio), add appropriate amount of deionized water and mix furnishing pulpous state, be applied on Copper Foil, at 90 DEG C, vacuumize drying; By LiCoO
2powder: SP:KS-6:PVDF=94:1.5:2:2.5(weight ratio), do after solvent evenly sizes mixing with NMP, be applied on aluminium foil, at 100 DEG C, vacuumize drying; By dried positive and negative electrode pole piece through roll-in, cut-parts, winding, fluid injection, sealing, formation process, make 18650 cylindrical batteries, barrier film is Celgard2400, electrolyte is 1MLiPF6 ∕ DMC:EC:DEC, use battery check device to carry out the detection of cycle performance, test result is in table 1.
The Performance comparision of negative material in the different embodiment of table 1 and comparative example
Above-described embodiment is the present invention's preferably execution mode; but embodiments of the present invention are not restricted to the described embodiments; change, the modification done under other any does not deviate from Spirit Essence of the present invention and principle, substitute, combine, simplify; all should be the substitute mode of equivalence, be included within protection scope of the present invention.
Claims (9)
1. a preparation method for graphite tinbase composite negative pole material, concrete preparation process is as follows:
(1) by the dispersion of resinae carbon matrix precursor in a solvent, add nanometer tin, then ultrasonic disperse, evaporate organic solvent, under inert gas shielding, high temperature cabonization, obtains materials A;
(2) by materials A by pulverizing, obtain particle diameter D50 between the submicron order powder B of 0.1 ~ 1 μm;
(3) powder B and graphite, pitch class carbon matrix precursor are carried out solid phase mixing, then under inert gas shielding, high temperature cabonization, cooling is sieved.
2. the preparation method of a kind of graphite tinbase composite negative pole material according to claim 1, is characterized in that resinae carbon matrix precursor in step (1) refers to the combination of in furfural resin, epoxy resin, phenolic resins, polyethylene glycol, polyvinyl chloride, polyvinyl butyral resin, polyacrylonitrile, polyacrylic acid a kind or at least 2 kinds.
3. the preparation method of a kind of graphite tinbase composite negative pole material according to claim 1, is characterized in that the ratio of resinae carbon matrix precursor and nanometer tin in step (1) is 1:(0.05 ~ 0.15).
4. the preparation method of a kind of graphite tinbase composite negative pole material according to claim 1, it is characterized in that the temperature of high temperature cabonization in step (1) is 650 ~ 850 DEG C, heating rate is 1 ~ 5 DEG C/min, and temperature retention time is 0.5 ~ 3h.
5. the preparation method of a kind of graphite tinbase composite negative pole material according to claim 1, is characterized in that step (2) is pulverized and refers to by the one or more kinds of combinations in ball milling, mechanical crushing or air-flow crushing mode.
6. the preparation method of a kind of graphite tinbase composite negative pole material according to claim 1, it is characterized in that the weight ratio of step (3) powder B and graphite is for (0.1 ~ 0.5): 1, pitch class carbon matrix precursor accounts for 10 ~ 30% of powder B and graphite total weight.
7. the preparation method of a kind of graphite tinbase composite negative pole material according to claim 1, is characterized in that the average grain diameter of graphite in step (3) is 5 ~ 30 μm, tap density>=0.7g/cm
3.
8. the preparation method of a kind of graphite tinbase composite negative pole material according to claim 1, it is characterized in that step (3) medium pitch class carbon forerunner refers to the combination of in coal tar pitch, petroleum asphalt, modified coal tar pitch, mesophase pitch, the condensation polycyclic polynuclear aromatic hydrocarbon that obtained by asphalt modifier a kind or at least 2 kinds, diameter of particle D50≤3 μm of pitch class carbon forerunner.
9. the preparation method of a kind of graphite tinbase composite negative pole material according to claim 1, it is characterized in that the temperature of high temperature cabonization in step (3) is 850 ~ 1000 DEG C, heating rate is 5 ~ 20 DEG C/min, and temperature retention time is 0.5 ~ 4h.
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| CN201510404737.4A CN105047891A (en) | 2015-07-10 | 2015-07-10 | Preparation method of graphite tin-based composite anode material |
| PCT/CN2016/085618 WO2017008606A1 (en) | 2015-07-10 | 2016-06-13 | Method for fabricating graphite tin-based composite negative-electrode material |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2017008606A1 (en) * | 2015-07-10 | 2017-01-19 | 田东 | Method for fabricating graphite tin-based composite negative-electrode material |
| CN108807873A (en) * | 2018-04-25 | 2018-11-13 | 福建翔丰华新能源材料有限公司 | A method of preparing the tin carbon lithium ion negative material of copper Sb doped |
| CN109004193A (en) * | 2018-07-18 | 2018-12-14 | 大同新成新材料股份有限公司 | A kind of negative electrode of lithium ion battery carbonizing plant and its carbonization method |
| CN109314225A (en) * | 2016-06-07 | 2019-02-05 | 纳米技术仪器公司 | With the alkali metal battery based on integral type 3D graphene-carbon-metal hybrid foam electrode |
| WO2020142585A1 (en) * | 2019-01-02 | 2020-07-09 | Global Graphene Group, Inc. | Graphite protected anode active material particles for rechargeable lithium batteries |
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| US11289697B2 (en) * | 2018-11-26 | 2022-03-29 | Global Graphene Group, Inc. | Graphite protected anode active material particles for lithium batteries |
| CN109603726A (en) * | 2019-01-25 | 2019-04-12 | 威海南海碳材料科技研究院有限公司 | A kind of negative electrode material integral preparation process and production equipment |
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| CN114520314B (en) * | 2020-11-19 | 2024-02-27 | 湖南中科星城石墨有限公司 | Negative electrode material with porous carbon coating layer, preparation method thereof and lithium ion battery |
| CN113880068A (en) * | 2021-09-29 | 2022-01-04 | 蜂巢能源科技有限公司 | Hard carbon composite material and preparation method and application thereof |
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| CN115692612A (en) * | 2022-11-03 | 2023-02-03 | 福州大学 | Tin-carbon negative electrode material and preparation method thereof |
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