CN108493438A - A kind of lithium ion battery SiOxBase composite negative pole material and preparation method thereof - Google Patents
A kind of lithium ion battery SiOxBase composite negative pole material and preparation method thereof Download PDFInfo
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- 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
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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- 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 lithium ion battery SiOxBase composite negative pole material and preparation method thereof, the sub- silicon raw material of oxidation is subjected to ball-milling treatment first and is spray-dried after mixing with metallic salt, high temperature disproportionation occurs and in particle surface one layer silicate of cladding by roasting under an inert atmosphere, then one layer of unformed conductive carbon layer is coated in particle surface again and increase electric conductivity, finally obtain SiOxBase composite negative pole material finished product.The synthesis technology of the present invention is simple, and process conditions are easily controllable and are easily industrialized；Obtained SiOxBase composite negative pole material head effects are high, recycle, can be used as cathode material of lithium-ion power battery of new generation.
Description
Technical field
The present invention relates to lithium ion battery negative material field, especially a kind of lithium ion battery SiOxBase composite negative pole
Material and preparation method thereof.
Background technology
The theoretical capacity of graphite cathode material is 372mAh/g, cannot be satisfied new type lithium ion battery to high-energy density
Requirement.Therefore it is most important to develop new cathode material for high capacity lithium ion battery.
Currently, the Major Technology for promoting battery energy density both at home and abroad is to use nickelic system's positive electrode and Fabrication of High Specific Capacitance
The silicon-carbon cathode material of amount coordinates.Silicon has highest theoretical specific capacity (4200mAh/g) in lithium ion battery negative material, is
The optimal selection of lithium ion battery with high energy density negative material at present.But it is expanded big that there are volumes in silicon materials process of intercalation
The problem of (>=300%).The oxide of silicon equally has higher theoretical specific capacity, but relative to pure silicon, the oxide of silicon is embedding
There is smaller bulk effect, and due to, there are the higher Si-O keys of bond energy, can effectively inhibit silicon in material during lithium
Volume expansion, therefore cycle performance has more advantage.And Li can be generated in process of intercalation by aoxidizing sub- silicon2O and Li4SiO4It is non-live
Property mutually can be good at the volume expansion of padded coaming, but these the nonactive phases generated also consume part lithium, therefore oxygen
Change sub- silicon materials and equally exists the low problem of first effect.
The current main method for improving the sub- silicon chemical property of oxidation be by particle nanosizing, with various carbon materials it is compound,
With metal and metal oxide be compound and prelithiation etc..
CN102306759A discloses a kind of lithium ion battery silicon monoxide composite cathode material and preparation method thereof, the material
The preparation method of material includes the following steps：1) sub- silicon high temperature sintering under an inert atmosphere will be aoxidized, silicon nanoparticle and nothing are generated
Sizing silica；2) a certain amount of oxidation Asia silicon and conductive agent after sintering is accurately weighed, is added in planetary ball mill,
Mixing and ball milling is to get to silicon monoxide composite cathode material.The silicon monoxide composite cathode material first circle capacity is higher
(1100mAh/g), but very fast decay to 500mAh/g or so, cycle performance is very poor.After the material only will be simply sintered
Oxidation Asia silicon and conductive carbon carry out mechanical mixture, the electric conductivity for aoxidizing sub- silicon particle surface itself is poor, and does not also solve
The certainly volume expansion problem of itself.
Therefore, a kind of first effect height of exploitation, good cycle, Volumetric expansion small oxidation silicon based anode material and its system
Preparation Method is the technical barrier of fields.
Invention content
The technical problem to be solved by the invention is to provide a kind of lithium ion battery SiOxBase composite negative pole material and its
Preparation method, head effects are high, recycle, can be used as cathode material of lithium-ion power battery of new generation.
In order to solve the above-mentioned technical problem, the technical solution adopted by the present invention is：A kind of lithium ion battery SiOxBase is multiple
Close negative material, SiOxBase composite negative pole material includes the sub- silicon substrate of oxidation, silicate clad and agraphitic carbon clad, oxygen
Change sub- silicon substrate surface and be coated with silicate, agraphitic carbon clad is outermost clad, the median particle diameter of composite negative pole material
For 1~10um.
The median particle diameter of the composite negative pole material is 2~5um.
The SiOxIt is the sub- silicon particle of oxidation that sub- silicon substrate is aoxidized in base composite negative pole material, wherein 0.5≤x≤1.5.
The SiOxSilicate mass content is below 10% in base composite negative pole material.Particularly preferably 5% or less.
The SiOxThe carbon mass content of agraphitic carbon clad is below 15% in base composite negative pole material.Particularly preferably
It is 10% or less.
The agraphitic carbon clad is that organic carbon source cracks carbon, and organic carbon source is can be in the carbonaceous organic material of Pintsch process
Any one or a few.
Above-mentioned lithium ion battery SiOxThe preparation method of base composite negative pole material, includes the following steps successively：
1) the sub- silicon materials of oxidation are uniformly mixed with absolute ethyl alcohol and are carried out ball-milling treatment, it is 0.1 to be milled to median particle diameter
~1um, obtains slurry；Wherein, the quality of absolute ethyl alcohol is aoxidize sub- siliceous amount 1~4 times；
2) metallic salt is added into a small amount of absolute ethyl alcohol or deionized water dissolving, and be added in above-mentioned slurry, is uniformly mixed；
3) slurry is spray-dried, inlet temperature is 100 DEG C~300 DEG C, obtains powder；
4) 700 DEG C~1100 DEG C under an inert atmosphere by powder, are risen to the heating rate of 1 DEG C~10 DEG C/min, constant temperature
Heat treatment 1~for 24 hours, obtain a roasting material；
5) roasting material is subjected to air-flow break process；
6) broken material, organic carbon source are uniformly mixed to obtain slurry with absolute ethyl alcohol and stirring, and to slurry
Material is stirred drying；
7) 600 DEG C~900 DEG C under an inert atmosphere by material drying, are risen to the heating rate of 1 DEG C~10 DEG C/min, perseverance
Warm 1~12h of processing, obtains the SiOxBase composite negative pole material.
Step 2) the metallic salt is aluminium isopropoxide, aluminum acetate, magnesium carbonate, magnesium acetate, magnesium citrate, calcium acetate, carbon
Sour calcium is one such or several.
Step 6) the organic carbon source is pitch, glucose, starch, sucrose, polyethylene glycol, polyvinyl alcohol, polyethylene pyrrole
One or more of pyrrolidone, phenolic resin.
The step 4) and step 7) inert atmosphere are nitrogen or argon gas.
The beneficial effects of the invention are as follows：Compared with prior art, the present invention passing through the ball-milling technology of industrialization easy to implement
And drying process with atomizing, a kind of SiO being coated with silicate and agraphitic carbon has been madexBased composites：The material is first
Sub- silicon raw material ball milling will be aoxidized into nano-scale particle, substantially reduce lithium ion in SiOxTransmission range inside particle；Using
High temperature disproportionated reaction makes annealing treatment the sub- silicon of oxidation at high temperature and under inert atmosphere, and preparation is dispersed in silica
Nano-silicon (＜ 20nm), while so that partial oxidation silicon is transformed into using metallic salt and not consuming the silicate of lithium, reduce silica
Irreversible capacity loss caused by compound improves the coulombic efficiency for the first time of material；Finally in SiOxExtra-granular, which coats one layer, to be had
Machine object cracks carbon-coating, the electric conductivity of particle can be improved, and can effectively buffer the volume change of material in charge and discharge process, except this it
Outside, SiO is reducedxParticle and electrolyte are in direct contact, and can generate stable SEI films, improve coulombic efficiency for the first time.The present invention
Synthesis technology it is simple, process conditions are easily controllable, be suitble to industrialized production.
Description of the drawings
Fig. 1 is SiO made from embodiment 1xThe stereoscan photograph of base composite negative pole material；
Fig. 2 is SiO made from embodiment 1xThe cycle performance figure of base composite negative pole material.
Specific implementation mode
Technical scheme of the present invention is described in detail below in conjunction with drawings and examples.
Embodiment 1
A kind of SiOxThe preparation method of base composite negative pole material, includes the following steps：
1) the oxidation Asia silicon raw material 200g that median particle diameter is 5um is uniformly mixed with 400g absolute ethyl alcohols, then uses nanometer
Ball mill carries out ball milling, and it is 500nm to be milled to median particle diameter, obtains slurry；
2) it takes 6g aluminium isopropoxide 30g absolute ethyl alcohols to dissolve, and is added in the slurry, be uniformly mixed；
3) slurry is spray-dried, inlet temperature is 120 DEG C, obtains powder；
4) powder is roasted, 5 DEG C/min of heating rate in nitrogen atmosphere, rises to 1000 DEG C of heat preservation 6h, obtains one
Secondary roasting material；
5) roasting material is carried out air-flow to be crushed, broken median particle diameter is 2um；
6) 150g absolute ethyl alcohol and stirrings are added to mix with 10g pitches, 5g polyvinylpyrrolidones the broken material 100g
Uniformly, the then stirring and drying at 60 DEG C；
7) material drying is roasted, 2 DEG C/min of heating rate in nitrogen atmosphere, rises to 850 DEG C of heat preservations
8h obtains the SiOxBase composite negative pole material.Performance is shown in Fig. 1,2.
Comparative example 1
A kind of SiOxThe preparation method of base composite negative pole material, includes the following steps：
1) the oxidation Asia silicon raw material 200g that median particle diameter is 5um is uniformly mixed with 400g absolute ethyl alcohols, then uses nanometer
Ball mill carries out ball milling, and it is 500nm to be milled to median particle diameter, obtains slurry；
2) slurry is spray-dried, inlet temperature is 120 DEG C, obtains powder；
3) powder is roasted, 5 DEG C/min of heating rate in nitrogen atmosphere, rises to 1000 DEG C of heat preservation 6h, obtains one
Secondary roasting material；
4) roasting material is carried out air-flow to be crushed, broken median particle diameter is 2um；
5) 150g absolute ethyl alcohol and stirrings are added to be uniformly mixed with 10g pitches the broken material 100g, then at 60 DEG C
Stirring and drying；
6) material drying is roasted, 2 DEG C/min of heating rate in nitrogen atmosphere, rises to 850 DEG C of heat preservations
8h obtains the SiOxBase composite negative pole material.
Embodiment 2
A kind of SiOxThe preparation method of base composite negative pole material, includes the following steps：
1) the oxidation Asia silicon raw material 200g that median particle diameter is 5um is uniformly mixed with 400g absolute ethyl alcohols, then uses nanometer
Ball mill carries out ball milling, and it is 800nm to be milled to median particle diameter, obtains slurry；
2) 8.5g magnesium acetate 30g deionized water dissolvings are taken, and are added in the slurry, are uniformly mixed；
3) slurry is spray-dried, inlet temperature is 120 DEG C, obtains powder；
4) powder is roasted, 5 DEG C/min of heating rate in nitrogen atmosphere, rises to 1000 DEG C of heat preservation 6h, obtains one
Secondary roasting material；
5) roasting material is carried out air-flow to be crushed, broken median particle diameter is 2.5um；
6) 150g absolute ethyl alcohol and stirrings are added to be uniformly mixed with 10g pitches, 20g polyethylene glycol the broken material 100g,
Then the stirring and drying at 60 DEG C；
7) material drying is roasted, 2 DEG C/min of heating rate in nitrogen atmosphere, rises to 900 DEG C of heat preservations
4h obtains the SiOxBase composite negative pole material.
Embodiment 3
A kind of SiOxThe preparation method of base composite negative pole material, includes the following steps：
1) the oxidation Asia silicon raw material 200g that median particle diameter is 3um is uniformly mixed with 300g absolute ethyl alcohols, then uses nanometer
Ball mill carries out ball milling, and it is 500nm to be milled to median particle diameter, obtains slurry；
2) 5.5g calcium acetate 30g deionized water dissolvings are taken, and are added in the slurry, are uniformly mixed；
3) slurry is spray-dried, inlet temperature is 150 DEG C, obtains powder；
4) powder is roasted, 5 DEG C/min of heating rate in nitrogen atmosphere, rises to 1000 DEG C of heat preservation 2h, obtains one
Secondary roasting material；
5) roasting material is carried out air-flow to be crushed, broken median particle diameter is 1um；
6) 150g absolute ethyl alcohol and stirrings are added to be uniformly mixed with 10g sucrose, 8g polyvinyl alcohol the broken material 100g, so
The stirring and drying at 60 DEG C afterwards；
7) material drying is roasted, 2 DEG C/min of heating rate in nitrogen atmosphere, rises to 900 DEG C of heat preservations
6h obtains the SiOxBase composite negative pole material.
Embodiment 4
A kind of SiOxThe preparation method of base composite negative pole material, includes the following steps：
1) the oxidation Asia silicon raw material 200g that median particle diameter is 3um is uniformly mixed with 300g absolute ethyl alcohols, then uses nanometer
Ball mill carries out ball milling, and it is 500nm to be milled to median particle diameter, obtains slurry；
2) 6g aluminum acetate 30g deionized water dissolvings are taken, and are added in the slurry, are uniformly mixed；
3) slurry is spray-dried, inlet temperature is 180 DEG C, obtains powder；
4) powder is roasted, 10 DEG C/min of heating rate in nitrogen atmosphere, rises to 1000 DEG C of heat preservation 2h, obtains one
Secondary roasting material；
5) roasting material is carried out air-flow to be crushed, broken median particle diameter is 1um；
6) 150g absolute ethyl alcohol and stirrings are added to be uniformly mixed with 8g pitches, 4g phenolic resin the broken material 100g, so
The stirring and drying at 60 DEG C afterwards；
7) material drying is roasted, 2 DEG C/min of heating rate in nitrogen atmosphere, rises to 900 DEG C of heat preservations
6h obtains the SiOxBase composite negative pole material.
Experimental conditions：
Table 1, which lists, utilizes SiO made from above-described embodiment and comparative examplexBase composite negative pole material, is made button cell
Charging and discharging capacity.The test condition of button cell is：23 DEG C ± 2 DEG C, LR 2032, I=0.1C, 0.005~2.0V
vs.Li/Li+。
Table 1
The SiO prepared according to the method for the invention it can be seen from the above correction dataxThe head of base composite negative pole material
The chemical properties such as secondary coulombic efficiency and cyclical stability are superior to the negative material in comparative example.
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 (10)
1. a kind of lithium ion battery SiOxBase composite negative pole material, which is characterized in that SiOxBase composite negative pole material includes oxidation
Sub- silicon substrate, silicate clad and agraphitic carbon clad aoxidize sub- silicon substrate surface and are coated with silicate, agraphitic carbon packet
Coating is outermost clad, and the median particle diameter of composite negative pole material is 1~10um.
2. lithium ion battery SiO according to claim 1xBase composite negative pole material, which is characterized in that the composite negative pole
The median particle diameter of material is 2~5um.
3. lithium ion battery SiO according to claim 1xBase composite negative pole material, which is characterized in that the SiOxBase is multiple
It is the sub- silicon particle of oxidation to close and aoxidize sub- silicon substrate in negative material, wherein 0.5≤x≤1.5.
4. lithium ion battery SiO according to claim 1xBase composite negative pole material, which is characterized in that the SiOxBase is multiple
Silicate mass content is below 10% in conjunction negative material.
5. lithium ion battery SiO according to claim 1xBase composite negative pole material, which is characterized in that the SiOxBase is multiple
The carbon mass content of agraphitic carbon clad in negative material is closed below 15%.
6. lithium ion battery SiO according to claim 1xBase composite negative pole material, which is characterized in that the agraphitic carbon
Clad is that organic carbon source cracks carbon, and organic carbon source is any one or a few that can be in the carbonaceous organic material of Pintsch process.
7. the ion battery SiO as described in any one of claim 1~6xThe preparation method of base composite negative pole material, feature exist
In including the following steps successively：
1) the sub- silicon materials of oxidation are uniformly mixed with absolute ethyl alcohol and are carried out ball-milling treatment, be milled to median particle diameter for 0.1~
1um obtains slurry；Wherein, the quality of absolute ethyl alcohol is aoxidize sub- siliceous amount 1~4 times；
2) metallic salt is added into a small amount of absolute ethyl alcohol or deionized water dissolving, and be added in above-mentioned slurry, is uniformly mixed；
3) slurry is spray-dried, inlet temperature is 100 DEG C~300 DEG C, obtains powder；
4) 700 DEG C~1100 DEG C, at constant temperature heating under an inert atmosphere by powder, are risen to the heating rate of 1 DEG C~10 DEG C/min
Reason 1~for 24 hours, obtain a roasting material；
5) roasting material is subjected to air-flow break process；
6) broken material, organic carbon source are uniformly mixed to obtain slurry with absolute ethyl alcohol and stirring, and drying is stirred to slurry；
7) 600 DEG C~900 DEG C under an inert atmosphere by material drying, are risen to the heating rate of 1 DEG C~10 DEG C/min, constant temperature heating
1~12h is handled, the SiO is obtainedxBase composite negative pole material.
8. ion battery SiO according to claim 7xThe preparation method of base composite negative pole material, which is characterized in that described
Step 2) metallic salt is aluminium isopropoxide, aluminum acetate, magnesium carbonate, magnesium acetate, magnesium citrate, calcium acetate, calcium carbonate therein one
Kind is several.
9. ion battery SiO according to claim 7xThe preparation method of base composite negative pole material, which is characterized in that described
Step 6) organic carbon source is pitch, glucose, starch, sucrose, polyethylene glycol, polyvinyl alcohol, polyvinylpyrrolidone, phenolic aldehyde tree
One or more of fat.
10. ion battery SiO according to claim 7xThe preparation method of base composite negative pole material, which is characterized in that described
Step 4) and step 7) inert atmosphere are nitrogen or argon gas.
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| CN109713286A (en) * | 2018-12-29 | 2019-05-03 | 安普瑞斯（南京）有限公司 | A kind of silicon based composite material and preparation method thereof for lithium ion secondary battery |
| CN109728276A (en) * | 2018-12-28 | 2019-05-07 | 安普瑞斯（南京）有限公司 | A kind of lithium ion battery siloxy solid solution negative electrode material and preparation method thereof |
| CN110021741A (en) * | 2019-03-30 | 2019-07-16 | 苏州宇量电池有限公司 | A kind of preparation method and material of Gao Shouxiao lithium ion battery negative material |
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