CN108376781A - A kind of lithium-ion-power cell silicon-carbon cathode material and preparation method thereof - Google Patents

A kind of lithium-ion-power cell silicon-carbon cathode material and preparation method thereof Download PDF

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CN108376781A
CN108376781A CN201810342770.2A CN201810342770A CN108376781A CN 108376781 A CN108376781 A CN 108376781A CN 201810342770 A CN201810342770 A CN 201810342770A CN 108376781 A CN108376781 A CN 108376781A
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silicon
lithium
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carbon cathode
preparation
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CN108376781B (en
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宋英杰
徐宁
伏萍萍
马倩倩
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Tianjin B&M Science and 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
    • H01M4/362—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
    • 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
    • H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
    • H01M4/386—Silicon or alloys based on silicon
    • 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
    • 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
    • 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
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • 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
    • H01M2004/021—Physical characteristics, e.g. porosity, surface area
    • 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
    • H01M2004/026—Electrodes composed of, or comprising, active material characterised by the polarity
    • H01M2004/027—Negative electrodes
    • 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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Abstract

The invention discloses a kind of lithium-ion-power cell silicon-carbon cathode materials and preparation method thereof, generate one layer of fine and close coated with silica layer in submicron order silicon powder surface by the method pre-oxidized in air first；Then the silicon particle of local sintering is opened by way of sand milling, obtains silicon/graphite composite material that carbon uniformly coats by means such as the uniform mixing and carbonization of silicon substrate and graphite matrix；Final products are waited until finally by the techniques such as uniformly mixing and post-processing with nano-oxide.The silicon materials of the present invention have three layers of clad, can not only completely cut off the contact with electrolyte, but also can further suppress the volume expansion of silicon.

Description

A kind of lithium-ion-power cell silicon-carbon cathode material and preparation method thereof
Technical field
The present invention relates to ion secondary battery cathode material lithium field more particularly to a kind of lithium-ion-power cell silicon-carbons Negative material and preparation method thereof.
Background technology
Power battery is the core of new-energy automobile, and wherein lithium ion battery has in terms of cost, energy density Clear superiority, the convenience that will significantly promote new-energy automobile economy and use, anode in lithium-ion battery system Material is deciding factor.New-energy automobile should completely or partially use electric drive that can subtract compared with conventional fuel oil automobile Few fuel consumption, but the expense that new-energy automobile is saved in Life cycle fuel consumption at present cannot still be offset and be increased Cost.If pure electric automobile course continuation mileage reaches 400 kilometers, in battery system cost reduction to 1.0 yuan/Wh conditions below Under, the economy in Life cycle can be close to conventional fuel oil automobile.The ease of use of new-energy automobile is promoted, is increased pure The course continuation mileage of electric drive traveling is crucial.To increase course continuation mileage, it is necessary to increase the energy for carrying electrokinetic cell system storage, Under the premise of not dramatically increasing new-energy automobile weight and volume, it is necessary to improve the ratio energy and energy density of power battery. If pure electric automobile course continuation mileage reaches 400 kilometers, electrokinetic cell system is promoted to 250Wh/kg or so, monomer than energy demand Battery specific energy need to promote 350Wh/kg.
In order to improve power battery specific energy density, most effective means are to improve the specific capacity of positive and negative pole material.Silicon material The theoretical specific capacity of material is 4200mAh/g, is 10 times of graphite negative electrodes or more, is 350Wh/kg and above lithium ion power electricity The cathode system of pond first choice.But silicon will produce huge volume expansion (＞ 300%) during inhaling lithium, cause material dusting de- It falls and persistently generates SEI films, cycle performance drastically declines, and affects its practical application.
Invention content
In order to solve the above technical problem, the present invention provides a kind of lithium-ion-power cell silicon-carbon cathode material and its systems Preparation Method.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：A kind of lithium-ion-power cell silicon-carbon The preparation method of negative material, includes the following steps：
1) by granularity D50The sub-micron silica flour of≤100nm is pre-oxidized in air atmosphere, Pre oxidation be 600~ 700 DEG C, preoxidation time is 4~8h, obtains material I；
2) material I and absolute ethyl alcohol are subjected to ball milling in sand mill, until granularity D after ball milling50≤ 100nm, obtains slurry II；
3) slurry II, graphite, binder and absolute ethyl alcohol are uniformly mixed in high speed dispersor, obtain slurry III；
4) slurry III is spray-dried in an inert atmosphere, obtains material IV, spray drying temperature is 110~120 ℃；
5) material IV is subjected to high-temperature roasting in an inert atmosphere, obtains material V, calcination temperature is 900~1000 DEG C, roasting The burning time is 2h~8h；
6) material V and nano-oxide are uniformly mixed in high-speed mixer, obtain material VI；
7) material VI is post-processed in an inert atmosphere, post-processing temperature is 450~550 DEG C, and finishing time is 4h~8h obtains material VII, and final silicon-carbon cathode material is obtained after crushing, being sieved.
Graphite is artificial graphite or natural graphite in the step 3), quality/graphite quality=5% of silicon in silicon slurry, Binder quality/graphite quality=5%~10%.
Binder is any one in phenolic resin and polyvinylpyrrolidone in the step 3).
The step 4), 5), 7) in inert atmosphere be nitrogen atmosphere, helium atmosphere and argon gas atmosphere in any one.
Nano-oxide is any one in magnesia and alundum (Al2O3), nano oxidized substance in the step 6) Amount/material V mass=0.5%~1%.
Above-mentioned lithium-ion-power cell lithium-ion-power cell silicon-carbon made from the preparation method of silicon-carbon cathode material Negative material.
The beneficial effects of the invention are as follows：Silicon materials have three layers of clad, innermost layer be nano silicon dioxide clad, two Silica is in process of intercalation since the presence of oxygen atom can generate Li2O and Li2SiO3Equal inert substances, volume expansion are much smaller than Silicon；Middle layer is carbon coating layer, and carbon can not only improve the electron conduction of composite material, but also the volume of silicon can be inhibited swollen It is swollen；Third layer is nano-oxide clad, and magnesia and titanium oxide are embedding lithium inert substance, can not only be completely cut off and electrolyte Contact, and the volume expansion of silicon can be further suppressed.
Description of the drawings
Fig. 1 is the process flow chart of the preparation method of lithium-ion-power cell silicon-carbon cathode material of the present invention.
Specific implementation mode
Technical scheme of the present invention is described in detail below in conjunction with drawings and examples.
As shown in Figure 1, the preparation method of the lithium-ion-power cell silicon-carbon cathode material of the present invention, including walk as follows Suddenly：
1) by granularity D50The sub-micron silica flour of≤100nm is pre-oxidized in air atmosphere, Pre oxidation be 600~ 700 DEG C, preoxidation time is 4~8h, obtains material I；
2) material I and absolute ethyl alcohol are subjected to ball milling in sand mill, until granularity D after ball milling50≤ 100nm, obtains slurry II；
3) slurry II, graphite, binder and absolute ethyl alcohol are uniformly mixed in high speed dispersor, obtain slurry III；
4) slurry III is spray-dried in an inert atmosphere, obtains material IV, spray drying temperature is 110~120 ℃；
5) material IV is subjected to high-temperature roasting in an inert atmosphere, obtains material V, calcination temperature is 900~1000 DEG C, roasting The burning time is 2h~8h；
6) material V and nano-oxide are uniformly mixed in high-speed mixer, obtain material VI；
7) material VI is post-processed in an inert atmosphere, post-processing temperature is 450~550 DEG C, and finishing time is 4h~8h obtains material VII, and final silicon-carbon cathode material is obtained after crushing, being sieved.
Graphite is artificial graphite or natural graphite in the step 3), quality/graphite quality=5% of silicon in silicon slurry, Binder quality/graphite quality=5%~10%.
Binder is any one in phenolic resin and polyvinylpyrrolidone in the step 3).
The step 4), 5), 7) in inert atmosphere be nitrogen atmosphere, helium atmosphere and argon gas atmosphere in any one.
Nano-oxide is any one in magnesia and alundum (Al2O3), nano oxidized substance in the step 6) Amount/material V mass=0.5%~1%.
Above-mentioned lithium-ion-power cell lithium-ion-power cell silicon-carbon made from the preparation method of silicon-carbon cathode material Negative material.
The present invention generates one layer fine and close two by the method pre-oxidized in air in submicron order silicon powder surface first Silica clad；Then the silicon particle of local sintering is opened by way of sand milling, by the equal of silicon substrate and graphite matrix The means such as even mixing and carbonization obtain silicon/graphite composite material that carbon uniformly coats；Finally by uniform with nano-oxide The techniques such as mixing and post-processing wait until final products.This method silicon materials have three layers of clad, and innermost layer is nano-silica SiClx clad, silica is in process of intercalation since the presence of oxygen atom can generate Li2O and Li2SiO3Equal inert substances, Volume expansion is much smaller than silicon；Middle layer is carbon coating layer, and carbon can not only improve the electron conduction of composite material, but also can be with Inhibit the volume expansion of silicon；Third layer is nano-oxide clad, and magnesia and titanium oxide are embedding lithium inert substance, not only may be used To completely cut off the contact with electrolyte, and the volume expansion of silicon can be further suppressed.
Embodiment 1
A kind of preparation method of silicon-carbon cathode material, includes the following steps：
1) by granularity D50The silica flour of=80nm is pre-oxidized in air atmosphere, and Pre oxidation is 600 DEG C, pre-oxidation Time is 8h, obtains material I；
2) the material I and absolute ethyl alcohol are subjected to ball milling in sand mill, until granularity D after ball milling50=80nm, is starched Expect II；
3) the slurry II, natural graphite, phenolic resin and absolute ethyl alcohol are uniformly mixed in high speed dispersor, are starched Expect III, quality/graphite quality=5% of silicon, phenolic resin quality/graphite quality=5% wherein in silicon slurry；
4) the slurry III is spray-dried in nitrogen atmosphere, obtains material IV, spray drying temperature 110 ℃；
5) the material IV in nitrogen atmosphere is subjected to high-temperature roasting, obtains material V, calcination temperature is 900 DEG C, roasting Time is 8h；
6) above-mentioned material V and nano magnesia are uniformly mixed in high-speed mixer, obtain material VI, wherein nano oxygen Change magnesia amount/material V mass=0.5%；
7) above-mentioned material VI is post-processed in nitrogen atmosphere, post-processing temperature is 450 DEG C, and finishing time is 8h obtains material VII, and final silicon-carbon cathode material is obtained after crushing, being sieved.
Comparative example 1
The omited steps 1 compared with embodiment 1), remaining step all same.
Embodiment 2
A kind of preparation method of silicon-carbon cathode material, includes the following steps：
1) by granularity D50The silica flour of=80nm is pre-oxidized in air atmosphere, and Pre oxidation is 700 DEG C, pre-oxidation Time is 6h, obtains material I；
2) the material I and absolute ethyl alcohol are subjected to ball milling in sand mill, until granularity D after ball milling50=80nm, is starched Expect II；
3) the slurry II, artificial graphite, polyvinylpyrrolidone and absolute ethyl alcohol are uniformly mixed in high speed dispersor, Slurry III is obtained, quality/graphite quality=5% of silicon wherein in silicon slurry, polyvinylpyrrolidone quality/graphite quality= 10%；
4) the slurry III is spray-dried in nitrogen atmosphere, obtains material IV, spray drying temperature 120 ℃；
5) the material IV in nitrogen atmosphere is subjected to high-temperature roasting, obtains material V, calcination temperature is 1000 DEG C, roasting The burning time is 4h；
6) above-mentioned material V and nano aluminium oxide are uniformly mixed in high-speed mixer, obtain material VI, wherein nano oxygen Change aluminum amount/material V mass=0.5%；
7) above-mentioned material VI is post-processed in nitrogen atmosphere, post-processing temperature is 450 DEG C, and finishing time is 8h obtains material VII, and final silicon-carbon cathode material is obtained after crushing, being sieved.Comparative example 2
The omited steps 6 compared with embodiment 1), remaining step all same.
Embodiment 3
A kind of preparation method of silicon-carbon cathode material, includes the following steps：
1) by granularity D50The silica flour of=80nm is pre-oxidized in air atmosphere, and Pre oxidation is 700 DEG C, pre-oxidation Time is 4h, obtains material I；
2) the material I and absolute ethyl alcohol are subjected to ball milling in sand mill, until granularity D after ball milling50=80nm, is starched Expect II；
3) the slurry II, natural graphite, phenolic resin and absolute ethyl alcohol are uniformly mixed in high speed dispersor, are starched Expect III, quality/graphite quality=5% of silicon, phenolic resin quality/graphite quality=8% wherein in silicon slurry；
4) the slurry III is spray-dried in nitrogen atmosphere, obtains material IV, spray drying temperature 120 ℃；
5) the material IV in nitrogen atmosphere is subjected to high-temperature roasting, obtains material V, calcination temperature is 1000 DEG C, roasting The burning time is 8h；
6) above-mentioned material V and nano magnesia are uniformly mixed in high-speed mixer, obtain material VI, wherein nano oxygen Change magnesia amount/material V mass=1%；
7) above-mentioned material VI is post-processed in helium atmosphere, post-processing temperature is 450 DEG C, and finishing time is 8h obtains material VII, and final silicon-carbon cathode material is obtained after crushing, being sieved.
Embodiment 4
A kind of preparation method of silicon-carbon cathode material, includes the following steps：
1) by granularity D50The silica flour of=80nm is pre-oxidized in air atmosphere, and Pre oxidation is 700 DEG C, pre-oxidation Time is 4h, obtains material I；
2) the material I and absolute ethyl alcohol are subjected to ball milling in sand mill, until granularity D after ball milling50=80nm, is starched Expect II；
3) the slurry II, natural graphite, polyvinylpyrrolidone and absolute ethyl alcohol are uniformly mixed in high speed dispersor, Slurry III is obtained, quality/graphite quality=5% of silicon, polyvinylpyrrolidone/graphite quality=10% wherein in silicon slurry；
4) the slurry III is spray-dried in nitrogen atmosphere, obtains material IV, spray drying temperature 110 ℃；
5) the material IV in nitrogen atmosphere is subjected to high-temperature roasting, obtains material V, calcination temperature is 950 DEG C, roasting Time is 8h；
6) above-mentioned material V and nano magnesia are uniformly mixed in high-speed mixer, obtain material VI, wherein nano oxygen Change magnesia amount/material V mass=1%；
7) above-mentioned material VI is post-processed in helium atmosphere, post-processing temperature is 550 DEG C, and finishing time is 4h obtains material VII, and final silicon-carbon cathode material is obtained after crushing, being sieved.Experimental conditions：
Table 1 lists the property that actual effect battery is made in silicon-carbon cathode material made from Examples 1 to 4 and comparative example 1~2 Energy.The test condition of actual effect battery is ICP053048,1C, 3.0~4.2V, and the charging/discharging apparatus used is blue electric charge and discharge Instrument.
1 actual effect battery performance test table of table
As can be seen from the data in the table, apparent bulging does not occur for silicon-carbon cathode material made from each embodiment, and recycle It has excellent performance；And apparent bulging then has occurred in comparative example, and cycle performance is poor.
In conclusion present disclosure is not limited in the above embodiments, the knowledgeable people in same area can Can propose other embodiments easily within the technological guidance's thought of the present invention, but this embodiment is included in this hair Within the scope of bright.

Claims (6)

1. a kind of preparation method of lithium-ion-power cell silicon-carbon cathode material, which is characterized in that include the following steps：
1) by granularity D50The sub-micron silica flour of≤100nm is pre-oxidized in air atmosphere, and Pre oxidation is 600~700 DEG C, preoxidation time is 4~8h, obtains material I；
2) material I and absolute ethyl alcohol are subjected to ball milling in sand mill, until granularity D after ball milling50≤ 100nm obtains slurry II；
3) slurry II, graphite, binder and absolute ethyl alcohol are uniformly mixed in high speed dispersor, obtain slurry III；
4) slurry III is spray-dried in an inert atmosphere, obtains material IV, spray drying temperature is 110~120 DEG C；
5) material IV is subjected to high-temperature roasting in an inert atmosphere, obtains material V, calcination temperature is 900~1000 DEG C, when roasting Between be 2h~8h；
6) material V and nano-oxide are uniformly mixed in high-speed mixer, obtain material VI；
7) material VI is post-processed in an inert atmosphere, post-processing temperature be 450~550 DEG C, finishing time be 4h~ 8h obtains material VII, and final silicon-carbon cathode material is obtained after crushing, being sieved.
2. the preparation method of lithium-ion-power cell silicon-carbon cathode material according to claim 1, which is characterized in that described Graphite is artificial graphite or natural graphite in step 3), quality/graphite quality=5% of silicon, binder quality/stone in silicon slurry Black quality=5%~10%.
3. the preparation method of lithium-ion-power cell silicon-carbon cathode material according to claim 1 or claim 2, which is characterized in that Binder is any one in phenolic resin and polyvinylpyrrolidone in the step 3).
4. the preparation method of lithium-ion-power cell silicon-carbon cathode material according to claim 1, which is characterized in that described Step 4), 5), 7) in inert atmosphere be nitrogen atmosphere, helium atmosphere and argon gas atmosphere in any one.
5. the preparation method of lithium-ion-power cell silicon-carbon cathode material according to claim 1, which is characterized in that described In step 6) nano-oxide be magnesia and alundum (Al2O3) in any one, nano oxidized amount of substance/material V mass= 0.5%~1%.
6. lithium made from the preparation method of lithium-ion-power cell silicon-carbon cathode material as described in any one of Claims 1 to 5 Ion battery silicon-carbon cathode material.
CN201810342770.2A 2018-04-17 2018-04-17 Silicon-carbon negative electrode material for lithium ion power battery and preparation method thereof Active CN108376781B (en)

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CN114784260A (en) * 2022-06-02 2022-07-22 内蒙古三信科技发展有限公司 Modified silicon material for lithium ion battery and preparation method and application thereof

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CN106941164A (en) * 2017-04-11 2017-07-11 东南大学 A kind of preparation method of lithium ion battery negative nucleocapsid clad structure material

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CN102122708A (en) * 2010-01-08 2011-07-13 中国科学院物理研究所 Negative pole material for lithium-ion secondary battery, negative pole containing negative pole material, preparation method of negative pole and battery containing negative pole
CN101986442A (en) * 2010-05-25 2011-03-16 耿世达 Lithium ion battery cathode material containing three-dimensional conductive structure and preparation method thereof
CN103236517A (en) * 2013-04-26 2013-08-07 中国东方电气集团有限公司 Lithium ion battery silicon-based negative material and preparation method thereof
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CN110504430A (en) * 2019-08-28 2019-11-26 陕西煤业化工技术研究院有限责任公司 A kind of lithium ion battery silicon-carbon cathode material and preparation method thereof
CN114784260A (en) * 2022-06-02 2022-07-22 内蒙古三信科技发展有限公司 Modified silicon material for lithium ion battery and preparation method and application thereof
CN114784260B (en) * 2022-06-02 2024-05-14 内蒙古三信科技发展有限公司 Modified silicon material for lithium ion battery and preparation method and application thereof

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