CN105958026A - Preparation method of graphite tin composite material for negative electrode of lithium-ion battery - Google Patents

Preparation method of graphite tin composite material for negative electrode of lithium-ion battery Download PDF

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Publication number
CN105958026A
CN105958026A CN201610434280.6A CN201610434280A CN105958026A CN 105958026 A CN105958026 A CN 105958026A CN 201610434280 A CN201610434280 A CN 201610434280A CN 105958026 A CN105958026 A CN 105958026A
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graphite
composite material
preparation
negative electrode
ion battery
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CN105958026B (en
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石磊
邵浩明
蒋文昶
皮涛
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Hunan Shinzoom Technology Co Ltd
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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
    • H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
    • 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
    • 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
    • H01M4/364—Composites as mixtures
    • 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
    • H01M4/624—Electric conductive fillers
    • H01M4/625—Carbon or graphite
    • 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

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Electrochemistry (AREA)
  • General Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Composite Materials (AREA)
  • Inorganic Chemistry (AREA)
  • Materials Engineering (AREA)
  • Manufacturing & Machinery (AREA)
  • Carbon And Carbon Compounds (AREA)
  • Battery Electrode And Active Subsutance (AREA)

Abstract

The invention provides a preparation method of a graphite tin composite material for a negative electrode of a lithium-ion battery. The graphite tin composite material is prepared by fusing, coating, carbonizing and screening natural flake graphite, tin oxide and asphalt as raw materials. According to the negative electrode material powder of the graphite tin composite material prepared by the method, the resistivity is smaller than 20mohm.cm, the compaction density can reach 1.6g/cc, the reversible capacity is 400-500mAh/g, the first efficiency is about 93%, the full-charge expansion rate of an electrode plate is lower than 25% and the capacity retention ratio after 800 cycles at 0.5C rate is still over 80%. The preparation method has the advantages that the efficiency is high, the operation is simple and full automation is easy to achieve.

Description

A kind of preparation method of used as negative electrode of Li-ion battery graphite tin composite material
Technical field
The present invention relates to the preparation method of the negative material of a kind of lithium ion battery, particularly to a kind of lithium ion battery The preparation method of the graphite tin composite material of negative pole.
Background technology
Improving the main development direction that energy density is lithium ion battery, traditional graphite cathode material theoretical capacity is only 372mAh/g, therefore, exploitation novel high-capacity negative material just becomes the task of top priority to replace conventional graphite negative material.
The research of high power capacity Li-like ions battery focuses primarily upon: silica-base material, metal and alloy materials, metal-oxide Material etc..Electric conductivity and the embedding de-lithium bulk effect of silica-base material constrain its application in lithium ion battery negative； The circulation of metal-oxide electrochemistry first there is obvious side reaction so that the lithium ion in positive pole cannot reversible return, greatly Have impact on the performance of battery integral energy density；Metal and alloy materials electric conductivity is good, and bulk effect is weaker than silicon substrate Material, coulombic efficiency is high first, and therefore, this type of material is easiest to substituted for silicon sill.
Tin-based material is a model in metal and alloy materials, and it is to study metals most for ＆ the earliest and alloy to bear Pole material, but, by the end of at present, there is no a tin-based material in the world and accomplish scale production, on the one hand this be due to lithium Electricity negative pole enterprise thinks directly to develop the higher silicon based anode material of capacity, is on the other hand that tin-based material fine powder preparation process is numerous Trivial, product reactivity is high, be difficult to storage.
This patent puts forth effort on the preparation method developing a kind of graphite tin composite material negative material, and the method is simple, Products obtained therefrom capacity is high, easily store, and electric conductivity, cycle performance also meet and use requirement.
Summary of the invention
It is desirable to provide the preparation method of the graphite tin composite material material of a kind of used as negative electrode of Li-ion battery, specifically Scheme is as follows:
The preparation method of a kind of used as negative electrode of Li-ion battery graphite tin composite material, comprises the following steps:
A1, natural flake graphite and stannum oxide are joined in fusion machine, heat fusion under protective atmosphere, obtain natural scale The fusion material that graphite and stannum oxide merge into each other；
A2, by the A1 fusion material that obtains of step, directly from fusion machine, vacuum handling in mixer, and adds Colophonium and mixes Close cladding；
A3, cladding material A2 step obtained are by, in mechanical hand loading crucible, being then placed on the crucible roller-way of roller kilns Carry out carbonization treatment；
A4, A3 is walked in the carbonized material that obtains directly poured out from crucible by mechanical arm, and entered by vacuum conveying system Entering double-spiral conical mixer, after stirring, blanking is sieved, and obtains this patent product.
Further, in described A1 step, first with oxidizing agent solution, natural flake graphite is sprayed so that it is surface shape Become rough oxidation pitting, then the natural flake graphite after oxidation processes is laid in fusion machine bottom surface, described fusion Machine uses compartment heating, is first heated to 200 ~ 300 DEG C, is cooled to 0 ~ 10 DEG C, heats with cooling alternately, interval time Cycle is 5-10 min, and when natural flake graphite produces Texturized, spraying into temperature with shot-blasting machine is 1600 DEG C-1630 DEG C Granules of stannic oxide, starts blender simultaneously, carries out high-speed stirred and carries out, every closing heating, obtaining natural flake graphite and stannum oxide The fusion material merged into each other.
Further, in described A1 step the purity of natural flake graphite be 99.95%, granularity be 200 mesh, shot-blasting machine sprays The granularity of the granules of stannic oxide entered is 3 ~ 7 μm, and the weight ratio that described natural flake graphite and described granules of stannic oxide are added is 100:5 ~ 20, are filled with N inside described fusion machine2Protective gas, described every close computer heating control at 250 ~ 400 DEG C, constant temperature 2 ~ 5h, institute The rotating speed stating high-speed stirred controls 3000 ~ 5000rpm, obtains the fusion material that natural flake graphite merges into each other with stannum oxide；
Further, described A2 step in add Colophonium total amount be A1 step in natural flake graphite quality 4 ~ 10%, mixing Cladding speed is 200 ~ 300rpm, mixes cladding time 10 ~ 30min；
Further, in described A3 step, the carbonization maximum temperature of carbonization treatment is 900 ~ 1300 DEG C, temperature retention time 0.5 ~ 2h, roller Road kiln entirety uses N2Protection, stove tail condensed water cools down, it is ensured that the crucible surface temperature come out of the stove is less than 100 DEG C；
Further, the carbonized material in described A4 step stirs 10 ~ 40min in double-spiral conical mixer, and then blanking is extremely Sieving in screening machine, screen cloth is double-deck, and upper strata 270 mesh, lower floor 200 mesh, siftage is this patent product.
Further, in described A1 step, stannum oxide is commercial analytical pure, and natural flake graphite is without spheroidising.
Further, described A2 step medium pitch is ultra-temperature pitch, and softening point is 150 ~ 280 DEG C, and ash is less than 0.1%.
Compared with prior art, the present invention is had the advantage that
1., in the method for the present invention, first make the surface of natural flake graphite form rough oxidation with oxidizing agent solution little Hole, then uses compartment heating, heats with cooling alternately, makes natural flake graphite produce Texturized, then use grit blast Machine sprays into granules of stannic oxide, and granules of stannic oxide is wound onto in the gap of spherical natural graphite granule, occurs at a certain temperature Redox reaction generates tin liquor and is partly filled in the gap being wound on spherical natural graphite granule；Through pitch-coating, carbonizer Skill, then the gap that spherical graphite and winding thereof are formed is wrapped up.The stannum in this material volume effect during embedding de-lithium Should, first being buffered a part by graphite gap, the package action then adding bitumencarb inhibits again a part, and material is whole The full electricity bounce-back that body shows does not has difference with the carbon coated natural graphite of volume production, and the full electric expansion of pole piece is less than 25%, but capacity But increasing to 400 ~ 500mAh/g, the effect of carbon cladding can also ensure that the coulombic efficiency first of material is higher than 93%.
2. only it is filled in graphite gap due to tin material, therefore, the pole piece of graphite tin composite material negative material Compacted density is even above traditional carbon coated graphite negative material, reaches 1.6g/cc, and the effect being coated with also makes this material Under 0.5C multiplying power, circulate 800 weeks capability retentions maintain more than 80%.
3. tin material is by graphite and bitumencarb double-coating, will not impact material storage.
4. the inventive method can be completely achieved automatic production line production.
Detailed description of the invention
Embodiment 1
A kind of preparation method of used as negative electrode of Li-ion battery graphite tin composite material, step is as follows:
A1. by purity be 99.95%, granularity be natural flake graphite and the granularity of 200 mesh be that the stannum oxide of 3 μm is according to 100:5 Ratio join in fusion machine, in N2250 DEG C it are heated under protective atmosphere, constant temperature 2h, merges machine equal during heating and constant temperature Keeping high-speed stirred, rotating speed is at 3000rpm；
A2. by the A1 fusion material that obtains of step directly from fusion machine vacuum handling in VC mixer, and add appropriate softening Point is that the Colophonium of 180 DEG C carries out mixing cladding, and Colophonium total amount is in A1 step the 10% of natural flake graphite quality, mixing cladding Speed is 200rpm, mixes cladding time 30min；
A3. the cladding material that A2 step obtains is loaded in crucible by mechanical hand, be then placed on the crucible roller-way of roller kilns Carrying out carbonization treatment, carbonization maximum temperature is 1150 DEG C, temperature retention time 2h, and roller kilns entirety uses N2Protection, stove tail has condensation Water cooling, it is ensured that the crucible surface temperature come out of the stove is less than 100 DEG C；
A4. the carbonized material obtained in being walked by A3 is directly poured out from crucible by mechanical arm, and is entered by vacuum conveying system Entering double-spiral conical mixer, after stirring 20min, blanking is in screening machine, and screen cloth be bilayer, upper strata 270 mesh, lower floor 200 mesh, Siftage is this patent and relates to product.
Embodiment 2
A kind of preparation method of used as negative electrode of Li-ion battery graphite tin composite material, step is as follows:
Be the most first 99.95% with oxidizing agent solution to purity, granularity be that the natural flake graphite of 200 mesh sprays so that it is table Face forms rough oxidation pitting, wherein, oxidizing agent solution can use peroxide, permanganic acid, chlorate, hydrochloric acid, Sulphuric acid etc..Then natural flake graphite after oxidation processes is laid in fusion machine bottom surface, and described fusion machine uses compartment to add Heat, is first heated to 200 ~ 300 DEG C, is cooled to 0 ~ 10 DEG C, heats with cooling alternately, and interval time period is 5-10 Min, when natural flake graphite produces Texturized, sprays into, with shot-blasting machine, the granules of stannic oxide that temperature is 1600 DEG C-1630 DEG C, The granularity of granules of stannic oxide is 7 μm, and sprays into according to the ratio that mass ratio is 100:20 of natural flake graphite with stannum oxide, N2400 DEG C it are heated under protective atmosphere, constant temperature 5h, merge machine during heating and constant temperature and all keep high-speed stirred, rotating speed exists 5000rpm, obtains the fusion material that natural flake graphite merges into each other with stannum oxide.
A2. by the A1 fusion material that obtains of step directly from fusion machine vacuum handling in VC mixer, and add appropriate Softening point is that the Colophonium of 250 DEG C carries out mixing cladding, and Colophonium total amount is in A1 step the 4% of natural flake graphite quality, mixing bag Covering speed is 300rpm, mixes cladding time 30min；
A3. the cladding material that A2 step obtains is loaded in crucible, be then placed within the crucible roller-way of roller kilns carrying out at carbonization Reason, carbonization maximum temperature is 1150 DEG C, temperature retention time 2h, and roller kilns entirety uses N2Protection, stove tail has condensed water to cool down, permissible Ensure that the crucible surface temperature come out of the stove is less than 100 DEG C；
A4. the carbonized material obtained in being walked by A3 is directly poured out from crucible by mechanical arm, and is entered by vacuum conveying system Entering double-spiral conical mixer, after stirring 30min, blanking is in screening machine, and screen cloth be bilayer, upper strata 270 mesh, lower floor 200 mesh, Siftage is this patent and relates to product.
Comparative example: use commercial glass putty (analytical pure) to be milled to D50=4.529 μm, as a comparison case:
From table, contrast understands, and uses product prepared by the inventive method, and coulombic efficiency and cycle performance are the most obvious first for they It is better than comparative example.

Claims (5)

1. the preparation method of a used as negative electrode of Li-ion battery graphite tin composite material, it is characterised in that: comprise the following steps:
A1, natural flake graphite and stannum oxide are joined in fusion machine, heat fusion under protective atmosphere, obtain natural scale The fusion material that graphite and stannum oxide merge into each other；
A2, by the A1 fusion material that obtains of step, directly from fusion machine, vacuum handling in mixer, and adds Colophonium and mixes Close cladding；
A3, cladding material A2 step obtained are by, in mechanical hand loading crucible, being then placed on the crucible roller-way of roller kilns Carry out carbonization treatment；
A4, A3 is walked in the carbonized material that obtains directly poured out from crucible by mechanical arm, and entered by vacuum conveying system Entering double-spiral conical mixer, after stirring, blanking is sieved, and obtains this patent product.
The preparation method of used as negative electrode of Li-ion battery graphite tin composite material the most according to claim 1, it is characterised in that:
In described A1 step, first with oxidizing agent solution, natural flake graphite is sprayed so that it is surface is formed rough Oxidation pitting, is then laid in fusion machine bottom surface by the natural flake graphite after oxidation processes, and described fusion machine uses compartment Heating, is first heated to 200 ~ 300 DEG C, is cooled to 0 ~ 10 DEG C, heats with cooling alternately, and interval time period is 5-10 Min, when natural flake graphite produces Texturized, sprays into, with shot-blasting machine, the granules of stannic oxide that temperature is 1600 DEG C-1630 DEG C, Start blender simultaneously, carry out high-speed stirred and carry out, every closing heating, obtaining what natural flake graphite and stannum oxide merged into each other Merge material.
The preparation method of used as negative electrode of Li-ion battery graphite tin composite material the most according to claim 2, it is characterised in that:
In described A1 step the purity of natural flake graphite be 99.95%, granularity be 200 mesh, the granules of stannic oxide that shot-blasting machine sprays into Granularity be 3 ~ 7 μm, the weight ratio that described natural flake graphite and described granules of stannic oxide are added is 100:5 ~ 20, described in melt It is filled with N inside conjunction machine2Protective gas, described every close computer heating control at 250 ~ 400 DEG C, constant temperature 2 ~ 5h, described high-speed stirred turn Speed controls 3000 ~ 5000rpm, obtains the fusion material that natural flake graphite merges into each other with stannum oxide；
The preparation method of used as negative electrode of Li-ion battery graphite tin composite material according to claim 1, it is characterised in that:
Described A2 step in add Colophonium total amount be A1 step in natural flake graphite quality 4 ~ 10%, mixing cladding speed It is 200 ~ 300rpm, mixes cladding time 10 ~ 30min；
The preparation method of used as negative electrode of Li-ion battery graphite tin composite material according to claim 1, it is characterised in that:
In described A3 step, the carbonization maximum temperature of carbonization treatment is 900 ~ 1300 DEG C, temperature retention time 0.5 ~ 2h, and roller kilns are overall Use N2Protection, stove tail condensed water cools down, it is ensured that the crucible surface temperature come out of the stove is less than 100 DEG C；
The preparation method of used as negative electrode of Li-ion battery graphite tin composite material according to claim 1, it is characterised in that:
Carbonized material in described A4 step stirs 10 ~ 40min in double-spiral conical mixer, and then blanking is entered to screening machine Row screening, screen cloth is double-deck, and upper strata 270 mesh, lower floor 200 mesh, siftage is this patent product.
4. according to the preparation method of the used as negative electrode of Li-ion battery graphite tin composite material described in any one of claim 1-3, its It is characterised by: in described A1 step, stannum oxide is commercial analytical pure, and natural flake graphite is without spheroidising.
The preparation method of used as negative electrode of Li-ion battery graphite tin composite material the most according to claim 4, it is characterised in that: Described A2 step medium pitch is ultra-temperature pitch, and softening point is 150 ~ 280 DEG C, and ash is less than 0.1%.
CN201610434280.6A 2016-06-18 2016-06-18 A kind of preparation method of negative electrode of lithium ion battery graphite tin composite material Active CN105958026B (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN110564299A (en) * 2019-08-07 2019-12-13 湖北安达精密工业有限公司 Lubricating wear-resistant paint for coating bearing bush, bearing bush and bearing bush spraying method
CN111463416A (en) * 2020-04-14 2020-07-28 广东东岛新能源股份有限公司 Low-cost low-expansion-rate long-circulation natural graphite-based composite material and preparation method and application thereof
CN111785935A (en) * 2019-04-03 2020-10-16 江苏载驰科技股份有限公司 Preparation method of lithium ion battery cathode composite material

Citations (3)

* Cited by examiner, † Cited by third party
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
US20110039157A1 (en) * 2008-04-30 2011-02-17 Sumitomo Bakelite Co., Ltd. Anodic carbon material for lithium secondary battery, method for manufacturing the same, lithium secondary battery anode, and lithium secondary battery
CN105523544A (en) * 2016-01-19 2016-04-27 内蒙古三信新材料科技有限公司 Preparation method of negative electrode material of lithium ion battery and prepared negative electrode material

Patent Citations (3)

* Cited by examiner, † Cited by third party
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
US20110039157A1 (en) * 2008-04-30 2011-02-17 Sumitomo Bakelite Co., Ltd. Anodic carbon material for lithium secondary battery, method for manufacturing the same, lithium secondary battery anode, and lithium secondary battery
CN105523544A (en) * 2016-01-19 2016-04-27 内蒙古三信新材料科技有限公司 Preparation method of negative electrode material of lithium ion battery and prepared negative electrode material

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN111785935A (en) * 2019-04-03 2020-10-16 江苏载驰科技股份有限公司 Preparation method of lithium ion battery cathode composite material
CN110564299A (en) * 2019-08-07 2019-12-13 湖北安达精密工业有限公司 Lubricating wear-resistant paint for coating bearing bush, bearing bush and bearing bush spraying method
CN111463416A (en) * 2020-04-14 2020-07-28 广东东岛新能源股份有限公司 Low-cost low-expansion-rate long-circulation natural graphite-based composite material and preparation method and application thereof
CN111463416B (en) * 2020-04-14 2021-09-07 广东东岛新能源股份有限公司 Low-cost low-expansion-rate long-circulation natural graphite-based composite material and preparation method and application thereof

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