CN109360946B - Repeatedly mixing cladding high compacted density silicon-carbon cathode material and preparation method thereof - Google Patents

Repeatedly mixing cladding high compacted density silicon-carbon cathode material and preparation method thereof Download PDF

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CN109360946B
CN109360946B CN201810948489.3A CN201810948489A CN109360946B CN 109360946 B CN109360946 B CN 109360946B CN 201810948489 A CN201810948489 A CN 201810948489A CN 109360946 B CN109360946 B CN 109360946B
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silicon
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cathode material
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CN109360946A (en
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闫俊杰
曹泽正
侯佳宜
孟博
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Shandong Goldencell Electronics 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
    • H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
    • H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
    • 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 kind of repeatedly mixing cladding high compacted density silicon-carbon cathode materials and preparation method thereof, it overcomes current silicon carbon material material with carbon-coated surface unevenness and is difficult to complete defect, and solve the problems, such as that silicon-carbon cathode is difficult to improve compacted density by simple method.Silicon-carbon cathode material includes: primary particle and second particle, the primary particle is porous silicon carbon material, porous silicon is dispersed in active carbon, the pyrolysis carbon coating layer of a layer thickness 3-50nm is coated on the surface of porous silicon and active carbon, wherein porous silicon accounts for primary particle quality 5-50%, active carbon accounts for primary particle quality 20-30%, and pyrolytic carbon accounts for primary particle quality 20-75%；The second particle is primary particle and graphite is dispersed in the aggregate formed in pyrolytic carbon, aggregation size 5-100um, and the total carbon content of silicon-carbon cathode material is 80-90%, compacted density 1.1-1.7g/cm3。

Description

Repeatedly mixing cladding high compacted density silicon-carbon cathode material and preparation method thereof
Technical field
The present invention relates to field of lithium ion battery, specially a kind of repeatedly mixing cladding prepares high compacted density silicon-carbon cathode Material preparation method.
Background technique
With the fast development in electric car field, people are higher and higher to the quality capability density requirements of power battery. Commercial Li-ion secondary cell largely uses graphite as negative electrode material at present, since graphite cathode theoretical capacity is lower, Only 372mAh/g, commercialized its specific capacity of graphite negative electrodes material pass through the improvement of technique generally in 300-360mAh/g It has been difficult to be greatly improved to the energy force density of battery.Therefore, there is the negative electrode battery material of high specific energy power to become for development An urgent demand of lithium electricity industry.
In many negative electrode materials, silicon has high theoretical specific capacity (4200mAh/g), can increase substantially lithium The energy density of ion battery.But volume expansion, can be because residual during expansion-contraction up to 300% in charge and discharge process for silicon The effect of residue stress generates dusting, is crushed, also, silicon face cannot form stable SEI film.Therefore, it is necessary to carry out very to silicon Good cladding, contacts it directly with electrolyte.Furthermore, it is desirable to which the volume expansion for silicon reserves sufficient space or raising The ability of the anti-volume change of ambient enviroment.Therefore, silicon/carbon composite becomes being preferably selected for silicium cathode commercial applications.
Existing technology mostly uses the mode of cladding, forms amorphous carbon layer in silicon face.The cladding of silicon carbon material is adopted more With ball-milling method or liquid phase coating method.But the material silicon distribution of particles of this method preparation is uneven, and surface cladding is difficult completely；If By the way of electrostatic spray, although uniform and complete cladding can be formed to silicon particle, since production efficiency is not high, production Safety is lower and is difficult to be commercially produced on a large scale.
Summary of the invention
In order to provide one kind, repeatedly mixing cladding prepares high compacted density silicon-carbon cathode material preparation method, overcomes at present Silicon carbon material material with carbon-coated surface is uneven and is difficult to complete defect, and solves silicon-carbon cathode by simple method and be difficult to improve The problem of compacted density.The present invention provides a kind of low cost, high-pressure solid, the silicon-carbon cathode material preparation sides that can be prepared on a large scale Method.
A kind of repeatedly mixing cladding high compacted density silicon-carbon cathode material, silicon-carbon cathode material includes: primary particle and two Secondary particle, the primary particle are porous silicon carbon material, and porous silicon is dispersed in Carbon Materials, in porous silicon and Carbon Materials Surface coats the pyrolysis carbon coating layer of a layer thickness 3-50nm, and wherein porous silicon accounts for primary particle quality 5-50%, and Carbon Materials account for one Secondary granular mass 20-30%, pyrolytic carbon account for primary particle quality 20-75%；The second particle is that primary particle and graphite are uniform It is dispersed in the aggregate formed in pyrolytic carbon, aggregation size is 5-100 μm, the total carbon content quality of silicon-carbon cathode material Score is 80-90%, compacted density 1.1-1.7g/cm3 ；
The Carbon Materials are carbo lignius, coconut husk charcoal, graphene, carbon nanotube, acetylene black, Ketjen black, Super P, gas phase Deposit the combination of one or more of carbon fiber.
High compacted density silicon-carbon cathode material is coated according to the multiple mixing, the carbon source of pyrolytic carbon in the primary particle For sucrose, glucose, soluble starch, citric acid, phenolic resin, sodium cellulose glycolate, polyethylene pyrrole network alkanone, Vitamin C One or more of combinations of acid, chitosan, sodium alginate, polyaniline, polythiophene, polyacrylonitrile.
High compacted density silicon-carbon cathode material is coated according to the multiple mixing, the graphite is crystalline flake graphite or spherical stone Ink；Used pyrolytic carbon carbon source is wood pitch, selected from coal tar pitch and petroleum asphalt, phenolic resin, Portugal during preparing second particle Grape sugar, sodium cellulose glycolate, polyethylene pyrrole network alkanone one or more combination.
A kind of preparation method of silicon-carbon cathode material, is prepared in accordance with the following steps:
(1) by raw material silicon powder and metal powder, wet ball grinding, the drum's speed of rotation are 400-700r/ under high energy ball mill Min, the slurry being uniformly mixed, high-temperature calcination obtains the silicon powder of alloying under non-oxidizing atmosphere after solvent evaporated；
(2) silicon powder of step (1) resulting alloying is ground up, sieved, is added in pyrolytic carbon carbon source, speed of agitator is Carbon Materials are added under 300-1000r/min stirring condition, dry, calcining obtains solid powder under nonoxidizing atmosphere；
(3) solid powder that step (2) obtains is added in concentrated acid solution, stirring filters after a certain period of time, after drying Obtain primary particle；
(4) step (3) resulting primary particle is ground up, sieved；Then pyrolytic carbon carbon source is added in reaction kettle, reaction Revolving speed is 300-700r/min in kettle, after heating melting, primary particle is added, graphite obtains solid powder；Solid powder mixing The high-temperature calcination under non-oxidizing atmosphere after uniformly, is cooled to room temperature to obtain second particle；
Raw material silicon powder partial size is 20nm-2 μm in step (1), and concentrated acid solution is hydrochloric acid, sulfuric acid, phosphoric acid, nitre in step (3) One of acid, perchloric acid or a variety of combinations.
According to the preparation method of the silicon-carbon cathode material, the metal powder be magnesium powder, aluminium powder, calcium powder, zinc powder, copper powder, One of iron powder, nickel powder, cobalt powder, manganese powder.
According to the preparation method of the silicon-carbon cathode material, step (1), (2), the calcination temperature in (4) are 700-1000 DEG C, heating rate is 0.5-10 DEG C/min, soaking time 7-15h.
Technical solution of the present invention has the following characteristics that
1. compared with prior art, silicon-carbon cathode material provided by the invention has high compacted density, excellent circulation Performance, and preparation method is simple, is conducive to large-scale industrial production.
2. that present invention improves compacted densities existing for silicon based anode material is low, coulombic efficiency is low, cyclical stability is poor Problem.High compacted density silicon-carbon cathode material of the invention, in compacted density and the commercialization comparable condition of graphite cathode material Under, reversible capacity can reach 500-800mAh/g.
Detailed description of the invention
Fig. 1 is the SEM figure of silicon carbon material made from the embodiment of the present invention 1.
Fig. 2 is 0.2C charge/discharge capacity-cycle-index performance chart of negative electrode material made from the embodiment of the present invention 2.
Specific embodiment
A kind of repeatedly mixing cladding high compacted density silicon-carbon cathode material, it is characterized in that: silicon-carbon cathode material includes: primary Particle and second particle, the primary particle are porous silicon carbon material, and porous silicon is dispersed in active carbon, in porous silicon and The surface of active carbon coats the pyrolysis carbon coating layer of a layer thickness 3-50nm, and wherein porous silicon accounts for primary particle quality 5-50%, living Property charcoal accounts for primary particle quality 20-30%, and pyrolytic carbon accounts for primary particle quality 20-75%；The second particle be primary particle with Graphite is dispersed in the aggregate formed in pyrolytic carbon, and the total carbon of aggregation size 5-100um, silicon-carbon cathode material contain Amount is 80-90%, compacted density 1.1-1.7g/cm3 。
The carbon source of the pyrolytic carbon layer is sucrose, glucose, soluble starch, citric acid, phenolic resin, hydroxylmethyl cellulose One kind of plain sodium, polyethylene pyrrole network alkanone, ascorbic acid, chitosan, sodium alginate, polyaniline, polythiophene, polyacrylonitrile etc. or Several combinations.The active carbon be carbo lignius, coconut husk charcoal, shell carbon, graphene, carbon nanotube, acetylene black, Ketjen black, The combination of one or more of Super P, vapor deposition carbon fiber.The graphite is crystalline flake graphite or spherical graphite；It is described The cladding carbon source of pyrolytic carbon be wood pitch, selected from coal tar pitch and petroleum asphalt, plant asphalt, mid temperature pitch, soft pitch, phenolic resin, Glucose, sodium cellulose glycolate, polyethylene pyrrole network alkanone one or more combination.
A kind of silicon-carbon cathode material preparation method, it is characterized in that: being prepared in accordance with the following steps:
(1) by silicon powder and metal powder, the wet ball grinding under high energy ball mill, the drum's speed of rotation are 400-700r/ to Min, the slurry being uniformly mixed, high-temperature calcination obtains silicon powder under non-oxidizing atmosphere after solvent evaporated；
(2) step (1) resulting silicon powder is ground up, sieved by, is added in pyrolytic carbon carbon source, speed of agitator 300- Active carbon is added under 1000r/min stirring condition, dry, calcining obtains solid powder under nonoxidizing atmosphere；
(3) solid powder that step (2) obtains is added in concentrated acid solution by, and stirring filters after a certain period of time, after drying Obtain primary particle；
(4) step (3) resulting primary particle is ground up, sieved by；Then pyrolytic carbon carbon source is added in reaction kettle, reaction Revolving speed is 300-700r/min in kettle, after heating melting, primary particle is added, graphite obtains solid powder；Solid powder mixing The high-temperature calcination under non-oxidizing atmosphere after uniformly, is cooled to room temperature to obtain second particle；
Silicon powder partial size is 20nm-2um in step (1), and concentrated acid solution is hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid, height in step (3) One of chloric acid or a variety of combinations.
The metal powder is one of magnesium powder, aluminium powder, calcium powder, zinc powder, copper powder, iron powder, nickel powder, cobalt powder, manganese powder.Step (1), (2), the calcination temperature in (4) are 700-1000 DEG C, and heating rate is 0.5-10 DEG C/min, soaking time 7-15h.
The present invention is further described combined with specific embodiments below, and the present invention includes but is not limited to following implementation case Example.
Experimental method described in following embodiments is unless otherwise specified conventional method；The reagent and material, It can be obtained from commercialization approach.
Embodiment 1
It is with aluminium powder mass ratio by silicon powder and aluminium powder wet ball grinding, silicon powder under high energy ball mill that average grain diameter is 1um 4:1, drum's speed of rotation 700r/min, ball milling 5h, the slurry being uniformly mixed are forged for lower 900 DEG C of nitrogen atmosphere after solvent evaporated It burns, sintering time 10h.Resulting silica fume powder is ground up, sieved, and is added in the spirit solvent containing PVP, under stirring condition Ketjen black is added, silica fume powder, Ketjen black, PVP mass ratio are 80:5:64.Solvent evaporated, in a nitrogen atmosphere 800 DEG C of calcinings 3h obtains solid powder；Obtained solid powder is added in the HCl solution of 1M, is filtered after stirring 5h, one is obtained after drying Secondary particle；Primary particle is ground up, sieved.Medium temperature carbobitumen is added in reaction kettle, and liquid is formed after being warming up to 300 degree, is added Primary particle, 20um electrographite, phenolic resin；Primary particle, pitch, phenolic resin, electrographite mass ratio are 14:30: 10:60 stirs 2h, forms solid after cooling；By resulting solid 900 DEG C of high-temperature calcination 5h under nitrogen atmosphere, it is down to room temperature After obtain second particle.
Lithium ion cell electrode is prepared as follows in gained negative electrode material: using silicon-carbon cathode material obtained as active matter Matter, Super-P carbon black be conductive agent, chitosan is binder, after mixing by above-mentioned substance mass ratio 8:1:1, spend from Sub- water is sized mixing for solvent, and slurry is coated in the pole piece that 1.0cm × 1.5cm is made on copper foil, is depressed into institute in 60 DEG C of dry back rollers Thickness is needed, the dry 12h under 120 DEG C of vacuum.It is to electrode, using celgard2400 film as diaphragm, 1mlo/ with metal lithium sheet LiPF6/EC+DMC+DEC+VC(volume ratio 31:31:31:7) it is that electrolyte assembles experimental cell.With blue electric battery test system The charge-discharge performance of CT2001A tester test battery.Properties of product detection: Fig. 1 is to prepare silicon-carbon cathode material electron microscope, can To find out that silicon powder is wrapped by completely, surface is based on graphite-phase.
Embodiment 2
Silicon powder and the magnesium powder wet ball grinding under high energy ball mill for being 500nm by average grain diameter, silicon powder and magnesium powder mass ratio For 9:1, drum's speed of rotation 500r/min, ball milling 10h, the slurry being uniformly mixed, after solvent evaporated 1000 under nitrogen atmosphere DEG C calcining, sintering time 5h.Gained silica fume powder is ground up, sieved, and is added in the spirit solvent containing polyacrylic acid, stirring Under the conditions of be added acetylene black, silica fume powder, acetylene black, polyacrylic acid mass ratio are 70:5:55.Solvent evaporated, in nitrogen atmosphere Lower 1000 DEG C of calcinings 3h obtains solid powder；Obtained solid powder is added to the H of 5M2SO4In solution, taken out after stirring 10h Filter, obtains primary particle after drying；Primary particle is ground up, sieved.Medium temperature carbobitumen is added in reaction kettle, is warming up to 300 After form liquid, primary particle, 7um natural flake graphite, Ketjen black, primary particle, pitch, natural flake graphite, section is added The black mass ratio of qin is 15::40::50:5, stirs 2h, forms solid after cooling；By resulting solid under nitrogen atmosphere 900 DEG C high-temperature calcination 5h, is cooled to room temperature to obtain second particle.
Gained negative electrode material prepares electrode in the same manner as shown in Example 1, carries out electrochemical property test.Product Can detect: Fig. 2 is to prepare silicon-carbon cathode material 0.2C charge-discharge cycle performance chart, 100 weeks 86% or more capacity retention ratios.
Embodiment 3
Silicon powder and the iron powder wet ball grinding under high energy ball mill for being 100nm by average grain diameter, silicon powder and iron powder mass ratio It is passed through nitrogen protection for 4:1, drum's speed of rotation 700r/min, ball milling 5h, the slurry being uniformly mixed, nitrogen after solvent evaporated The lower 1000 DEG C of calcinings of gas atmosphere, sintering time 2h.Resulting solid powder is ground up, sieved, and is added to poly- containing glucose and shell In the aqueous solvent of sugar, single armed carbon nanotube, solid powder, single armed carbon nanotube, glucose, chitosan matter are added under stirring condition Amount is than being 75:3:30:30.Solvent evaporated, 1000 DEG C of calcining 3h obtain solid powder in a nitrogen atmosphere；The solid powder that will be obtained End is added to the H of 5M2SO4In solution, is filtered after stirring 5h, primary particle is obtained after drying；Primary particle is ground up, sieved.In Warm carbobitumen is added in reaction kettle, and liquid is formed after being warming up to 300 DEG C, and primary particle, 10um electrographite, phenolic aldehyde tree is added Rouge, primary particle, pitch, phenolic resin, electrographite mass ratio are 14:30:10:60, stir 2h, form solid after cooling； By resulting solid 900 DEG C of high-temperature calcination 5h under nitrogen atmosphere, it is cooled to room temperature to obtain second particle.
Gained negative electrode material prepares electrode in the same manner as shown in Example 1, carries out electrochemical property test.
The invention is not limited to above-mentioned specific embodiment modes, without departing from the spirit of the design of the present invention, this The technical staff of field that the present invention belongs to can also change and modify the above embodiment, to the specific embodiment of the invention Change and modification should all be fallen into the protection scope that claims of the present invention determines.In addition, some spies are employed herein Determine term, these terms are merely for convenience of description, does not limit the present invention in any way.

Claims (6)

1. a kind of repeatedly mixing cladding high compacted density silicon-carbon cathode material, it is characterized in that:
Silicon-carbon cathode material includes: primary particle and second particle, and the primary particle is porous silicon carbon material, and porous silicon is uniform It is dispersed in Carbon Materials, the pyrolysis carbon coating layer of a layer thickness 3-50nm is coated on the surface of porous silicon and Carbon Materials, wherein more Hole silicon accounts for primary particle quality 5-50%, and Carbon Materials account for primary particle quality 20-30%, and pyrolytic carbon accounts for primary particle quality 20- 75%；The second particle is that primary particle and graphite are dispersed in the aggregate formed in pyrolytic carbon, and aggregation size is 5-100 μm, the total carbon content mass fraction of silicon-carbon cathode material is 80-90%, compacted density 1.1-1.7g/cm3 ；
The Carbon Materials are carbo lignius, coconut husk charcoal, graphene, carbon nanotube, acetylene black, Ketjen black, Super P, vapor deposition The combination of one or more of carbon fiber.
2. repeatedly mixing coats high compacted density silicon-carbon cathode material according to claim 1, it is characterized in that: described primary The carbon source of pyrolytic carbon is sucrose, glucose, soluble starch, citric acid, phenolic resin, sodium cellulose glycolate, poly- second in grain One or more of combinations of alkene pyrrole network alkanone, ascorbic acid, chitosan, sodium alginate, polyaniline, polythiophene, polyacrylonitrile.
3. repeatedly mixing coats high compacted density silicon-carbon cathode material according to claim 1, it is characterized in that: the graphite is Crystalline flake graphite or spherical graphite；Used pyrolytic carbon carbon source is wood pitch, coal tar pitch, petroleum during preparing second particle Pitch, phenolic resin, glucose, sodium cellulose glycolate, polyethylene pyrrole network alkanone one or more combination.
4. the preparation method of any one of a kind of claim 1-3 silicon-carbon cathode material, it is characterized in that: making in accordance with the following steps It is standby to obtain:
(1) by raw material silicon powder and metal powder, wet ball grinding, the drum's speed of rotation are 400-700r/min under high energy ball mill, The slurry being uniformly mixed, high-temperature calcination obtains the silicon powder of alloying under non-oxidizing atmosphere after solvent evaporated；
(2) silicon powder of step (1) resulting alloying is ground up, sieved, is added in pyrolytic carbon carbon source, speed of agitator 300- Carbon Materials are added under 1000r/min stirring condition, dry, calcining obtains solid powder under nonoxidizing atmosphere；
(3) solid powder that step (2) obtains is added in concentrated acid solution, stirring filters after a certain period of time, obtains after drying Primary particle；
(4) step (3) resulting primary particle is ground up, sieved；Then pyrolytic carbon carbon source is added in reaction kettle, in reaction kettle Revolving speed is 300-700r/min, after heating melting, primary particle is added, graphite obtains solid powder；Solid powder is uniformly mixed The high-temperature calcination under non-oxidizing atmosphere afterwards is cooled to room temperature to obtain second particle；
Raw material silicon powder partial size is 20nm-2 μm in step (1), and concentrated acid solution is hydrochloric acid, sulfuric acid, phosphoric acid, nitric acid, height in step (3) One of chloric acid or a variety of combinations.
5. the preparation method of silicon-carbon cathode material according to claim 4, it is characterized in that: the metal powder be magnesium powder, aluminium powder, One of calcium powder, zinc powder, copper powder, iron powder, nickel powder, cobalt powder, manganese powder.
6. the preparation method of silicon-carbon cathode material according to claim 4, it is characterized in that: step (1), (2), forging in (4) Burning temperature is 700-1000 DEG C, and heating rate is 0.5-10 DEG C/min, soaking time 7-15h.
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CN112038603A (en) * 2020-09-03 2020-12-04 青海凯金新能源材料有限公司 Graphite negative electrode material and processing technology thereof
CN113193183B (en) * 2021-04-28 2023-07-25 四川大学 High-tap-density double-carbon-layer silicon-carbon composite material and preparation method thereof
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