CN105633368A - Negative electrode material of lithium ion battery and preparation method for negative electrode material - Google Patents
Negative electrode material of lithium ion battery and preparation method for negative electrode material Download PDFInfo
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- CN105633368A CN105633368A CN201511033265.2A CN201511033265A CN105633368A CN 105633368 A CN105633368 A CN 105633368A CN 201511033265 A CN201511033265 A CN 201511033265A CN 105633368 A CN105633368 A CN 105633368A
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- H01M4/02—Electrodes composed of, or comprising, active material
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- 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
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- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
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Abstract
The invention discloses a negative electrode material of a lithium ion battery and a preparation method for the negative electrode material. The preparation method of the negative electrode material of the lithium ion battery comprises the following steps of uniformly mixing a high-flexibility polymer and a SiOx based active substance to form a mixture; and processing the mixture to enable the high-flexibility polymer to form a uniform thin film on the surface of the SiOx based active substance to obtain the negative electrode material of the lithium ion battery. Through the above mode, the active substances can be effectively prevented from striping and dropping from each other, the volume expansion and shrinkage is reduced, the specific capacity of a SiOx (x is more than or equal to 0 and less than or equal to 2) based material is improved, and thus, the cycle stability performance of the SiOx (x is more than or equal to 0 and less than or equal to 2) based material is effectively improved.
Description
Technical field
The present invention relates to field of lithium ion battery, be specifically related to a kind of lithium ion battery cathode material and its preparation method.
Background technology
Running voltage height, service life cycle length, memory-less effect, self discharge be little, advantages of environment protection because having for lithium ion battery, extensive use in portable type electronic product and electric automobile field. At present, business-like lithium ion battery mainly adopts graphite negative electrodes material, although its capacity is close to theoretical specific capacity (372mAh/g), but still cannot meet the following lithium ion battery demand to high-energy-density. SiOx(0��x��2) material receives much concern with the theoretical specific capacity higher than graphite, becomes study hotspot and the developing direction of following lithium ion battery negative material.
At present, to SiOxThe research of (0��x��2) base negative material is concentrated mainly on the change in volume in reduction removal lithium embedded process, improves electric conductivity, improves circulation, improves efficiency aspect. Main method has SiOx(0��x��2) granule nanorize and various material with carbon element compound and metal and metal-oxide compound, and adopt different binding agents etc. But these methods are all without fundamentally solving SiOx(0��x��2) material efficiency is low, the deficiency of Cycle Difference.
Summary of the invention
What present invention mainly solves technical problem is how solution SiOx(0��x��2) material efficiency is low, the technical problem of Cycle Difference.
In view of this, the embodiment of the present invention provides a kind of lithium ion battery cathode material and its preparation method, it is possible to effectively stop mutually peeling off and coming off between active substance, reduces volumetric expansion and shrinks, improves SiOxThe specific capacity of (0��x��2) sill, thus being effectively improved SiOxThe stable circulation performance of (0��x��2) sill.
For solving above-mentioned technical problem, the technical scheme that the present invention adopts is: providing a kind of lithium ion battery negative material, described lithium ion battery negative material includes SiOxBase active substance and be coated on described SiOxThe strong flexible polymer of base active material surface, described 0 x 2.
Wherein, described SiOxBase active substance is SiOx��SiOx/C��SiOxAt least one in/M, wherein, described M is at least one in alkali metal, transition alkali metal, alkali metal oxide and transition alkali metal oxide; Described strong flexible polymer is the combination of the single polymers of elongation at break < 95% in 30 DEG C��vitrification point��300 DEG C, 1000��number equal relative molecular weight��800,000,0��degree of cross linking��80,0��swelling ratio��15 and electrolyte or multiple polymers.
Wherein, described SiOx/ C is SiOx/ organic carbon, SiOx/ DIC, SiOx/ graphite, SiOxAt least one in/Graphene, described M is Li, Li2O��B��B2O��Co��CoO��Fe��Fe2O3��Mg��MgO��Sn��SnO��Ti��TiO2, at least one in Ag, AgO and Cr; Described strong flexible polymer is at least one in naturally occurring or synthetic polyacrylate and derivant, polyimide and derivant, Kynoar class and derivant, polycyanate ester class and derivant, poly-butadiene-styrene rubber class and derivant, polyvinyl alcohol and derivant, carboxymethyl cellulose class and derivant, Sargassum acids and derivant thereof.
Wherein, described strong flexible polymer and described SiOxThe mass ratio of base active substance more than 0 less than 30%.
For solving above-mentioned technical problem, another technical solution used in the present invention is: the preparation method providing a kind of above-mentioned lithium ion battery negative material, said method comprising the steps of: by described strong flexible polymer and described SiOxBase active substance mix homogeneously forms mixture; Described mixture carries out process makes described strong flexible polymer at described SiOxBase active material surface forms homogeneous thin film, obtains described lithium ion battery negative material.
Wherein, described described mixture is carried out process make described strong flexible polymer at described SiOxBase active material surface forms homogeneous thin film; obtain described lithium ion battery negative material to include: be placed in by described mixture in the drying baker of 80-500 DEG C of vacuum or logical protective gas; insulation 0.5-5 was as a child cooled to room temperature; to obtain described lithium ion battery negative material, described protective gas is at least one in nitrogen, helium, neon, argon, Krypton and xenon.
Wherein, described method also includes: the material after described process is carried out screening process, to obtain the particle diameter material less than 50 microns as described lithium ion battery negative material.
Wherein, described strong flexible polymer and described SiOxAny of which mixing by solid phase mixing or solid liquid phase mixing of the base active substance, forms described mixture by least one mode mix homogeneously in centrifugal, ball milling and mechanical agitation.
Wherein, as described strong flexible polymer and described SiOxWhen base active substance is mixed by the mode that solid liquid phase mixes, described strong flexible polymer is dissolved in solvent and is configured to polymer solution, by described SiOxBase active substance adds mix homogeneously in described polymer solution and forms described mixture.
Wherein, described solvent is at least one in water, benzene, ethanol, polypyrrole alkanone, isopropanol, acetone, DMF, pentane, toluene and halogenated hydrocarbons.
The invention has the beneficial effects as follows: be different from the situation of prior art, the lithium ion battery negative material of the present invention, be coated on SiO by strong flexible polymerxBase active material surface. Such that it is able to utilize top layer polymer to be effectively isolated contacting between electrolyte with active substance, it is suppressed that the formation of SEI film; The high-flexibility utilizing polymer improves the contacted reliability between active particle material, stops mutually peeling off and coming off between active substance, reduces volumetric expansion and shrinks, improves SiOxThe specific capacity of (0��x��2) sill, improves its stable circulation performance.
Accompanying drawing explanation
Fig. 1 is the flow chart of the preparation method of a kind of lithium ion battery negative material that the embodiment of the present invention provides;
Fig. 2 is the embodiment of the present invention 1 gained lithium ion battery negative material head week electrochemistry cyclic curve schematic diagram;
Fig. 3 is 50 weeks circulation volume conservation rate schematic diagrams of the embodiment of the present invention 1 gained lithium ion battery negative material.
Detailed description of the invention
Below, in conjunction with specific embodiments and accompanying drawing the present invention is described in detail, it should be noted that, the concrete material being previously mentioned in present invention below embodiment, it is intended only as a kind of citing to illustrate, is not limited thereto, namely under the same terms, can also substituting with other materials that concrete material cited in the embodiment of the present invention is similar and realize technical scheme, the present invention does not illustrate one by one. Those skilled in the art, when paying creative work, adopt other materials that listed by the embodiment of the present invention, material is similar or structure is similar to realize the present invention, fall within the scope of protection of the invention.
The embodiment of the present invention provides a kind of lithium ion battery negative material, and this ion cathode material lithium includes SiOxBase active substance and be coated on SiOxThe strong flexible polymer of base active material surface, wherein, 0 x 2.
Wherein, SiOxBase active substance includes SiOx(0��x��2)��SiOx/C��SiOxOne or both and thing mixed above in/M or complex, M represents one or more the combination in alkali metal, transition alkali metal, alkali metal oxide and transition alkali metal oxide. For example, above-mentioned M can be Li, Li2O��B��B2O��Co��CoO��Fe��Fe2O3��Mg��MgO��Sn��SnO��Ti��TiO2, one of which in Ag, AgO and Cr or multiple combination. Above-mentioned SiOxCan be Si, SiO or SiO2, it is also possible to it is the combination of these three material. SiOx/C can be SiOx/ organic carbon, SiOx/ DIC, SiOx/ graphite, SiOxOne of which in/Graphene or multiple combination.
Wherein, used in embodiment of the present invention strong flexible polymer can be the material that physical characteristic meets the following conditions: the combination of the single polymers of elongation at break < 95% or multiple polymers in 30 DEG C��vitrification point��300 DEG C, 1000��number equal relative molecular weight��800,000,0��degree of cross linking��80,0��swelling ratio��15 and electrolyte. As long as it is to say, physical characteristic meets the strong flexible polymer as the embodiment of the present invention that is that the material of conditions above can be single or that be mutually combined simultaneously. For example, the strong flexible polymer of the embodiment of the present invention can be natural or synthesis following material: such as polyacrylate and derivant thereof, polyimide and derivant, Kynoar class and derivant, polycyanate ester class and derivant, the one of which gathered in butadiene-styrene rubber class and derivant, polyvinyl alcohol and derivant, carboxymethyl cellulose class and derivant, Sargassum acids and derivant thereof or multiple combination.
Wherein, as the preferred implementation of one, strong flexible polymer and SiO in the embodiment of the present inventionxThe mass ratio of base active substance more than 0 less than 30%. Preferred mass ratio is more than 0.001% less than 14%, and preferred mass ratio is less than 9% more than 0.005%. Such as strong flexible polymer and SiOxMass ratio 0.0001,0.0005,0.001,0.005 of base active substance etc.
The preparation method that the embodiment of the present invention also provides for a kind of lithium ion battery negative material, as it is shown in figure 1, the preparation method of the lithium ion battery negative material of the embodiment of the present invention comprises the following steps:
S11: strong flexible polymer is mixed homogeneously with SiOx base active substance and forms mixture.
Wherein, SiOxBase active substance includes SiOx(0��x��2)��SiOx/C��SiOxOne or both and thing mixed above in/M or complex, M represents one or more the combination in alkali metal, transition alkali metal, alkali metal oxide and transition alkali metal oxide. For example, above-mentioned M can be Li, Li2O��B��B2O��Co��CoO��Fe��Fe2O3��Mg��MgO��Sn��SnO��Ti��TiO2, one of which in Ag, AgO and Cr or multiple combination. Above-mentioned SiOxCan be Si, SiO or SiO2, it is also possible to it is the combination of these three material. SiOx/C can be SiOx/ organic carbon, SiOx/ DIC, SiOx/ graphite, SiOxOne of which in/Graphene or multiple combination.
Wherein, used in embodiment of the present invention strong flexible polymer can be the material that physical characteristic meets the following conditions: the combination of the single polymers of elongation at break < 95% or multiple polymers in 30 DEG C��vitrification point��300 DEG C, 1000��number equal relative molecular weight��800,000,0��degree of cross linking��80,0��swelling ratio��15 and electrolyte. As long as it is to say, physical characteristic meets the strong flexible polymer as the embodiment of the present invention that is that the material of conditions above can be single or that be mutually combined simultaneously. For example, the strong flexible polymer of the embodiment of the present invention can be natural or synthesis following material: such as polyacrylate and derivant thereof, polyimide and derivant, Kynoar class and derivant, polycyanate ester class and derivant, the one of which gathered in butadiene-styrene rubber class and derivant, polyvinyl alcohol and derivant, carboxymethyl cellulose class and derivant, Sargassum acids and derivant thereof or multiple combination.
Wherein, as the preferred implementation of one, strong flexible polymer and SiO in the embodiment of the present inventionxThe mass ratio of base active substance more than 0 less than 30%. Preferred mass ratio is more than 0.001% less than 14%, and preferred mass ratio is less than 9% more than 0.005%. Such as strong flexible polymer and SiOxMass ratio 0.0001,0.0005,0.001,0.005 of base active substance etc.
Wherein, any of which mixing that strong flexible polymer can be mixed by solid phase mixing or solid liquid phase with SiOx base active substance. When implementing, after both are mixed, combined strong flexible polymer and SiO by centrifugal, ball milling and churned mechanically a kind of mode or various ways furtherxBase active substance mix homogeneously so that strong flexible polymer is dispersed in SiOxThe surface of base active substance.
Wherein, as strong flexible polymer and SiOxWhen base active substance is mixed by the mode that solid liquid phase mixes, it is possible to realized by implementation in detail below: high-flexibility is and is dissolved in solvent and is configured to polymer solution, by SiOxBase active substance adds polymer solution mix homogeneously and forms mixture. Wherein, can be the one of which in water, benzene, ethanol, polypyrrole alkanone, isopropanol, acetone, DMF, pentane, toluene and halogenated hydrocarbons or multiple combination as the solvent of strong flexible polymer.
And as strong flexible polymer and SiOxWhen base active substance is with solid phase mixing, directly weighs two kinds of materials according to quality proportioning, then mix, it is possible to auxiliary adopts ball milling further, and the mode of stirring makes both be sufficiently mixed uniformly so that strong flexible polymer is dispersed in SiOxThe surface of base active substance.
S12: mixture is carried out process and makes strong flexible polymer at SiOxBase active material surface forms homogeneous thin film, obtains lithium ion battery negative material.
Mixture is carried out composite modified process, so that strong flexible polymer is at SiOxBase active material surface forms homogeneous thin film.
Wherein as a kind of preferred implementation; mixture is carried out composite modified process can implement in the following manner: be placed in by mixture in the drying baker of vacuum or logical protective gas; under 80-500 DEG C of temperature conditions, it is incubated 0.5-5 hour, is subsequently cooled to room temperature. For example, above-mentioned temperature conditions can be 100 DEG C, 120 DEG C, 150 DEG C, 200 DEG C, 250 DEG C, 350 DEG C, 400 DEG C etc., and above-mentioned temperature retention time can be 1 hour, 1.5 hours, 2 hours, 3 hours, 4 hours etc. Wherein, protective gas can be noble gas, and for example, protective gas can be the one of which in nitrogen, helium, neon, argon, Krypton and xenon or multiple combination.
Wherein, preferred as one, after above-mentioned process, process by screening further, product more than 50 microns or impurity in particle diameter in the product after removing process, to obtain the particle diameter polymer overmold SiO less than 50 micronsxThe negative material of base active substance, using as lithium ion battery negative material. Specifically can carry out screening process by corresponding molecular sieve.
The detailed description of the lithium ion battery cathode material and its preparation method of the embodiment of the present invention, it will be understood that the present invention passes through strong flexible polymer at SiOxSurface forms homogeneous protective layer thin film, utilizes contacting between strong flexible polymer isolation active substance and electrolyte on the one hand, it is suppressed that the formation of SEI film, thus reducing material generation of irreversible capacity in charge and discharge process. Utilize the high-flexibility of polymer, the surface texture of stabilizing actives on the other hand, increase the contacted reliability in charge and discharge process between active material particle, fundamentally improve SiOxThe structure of (0��x��2) active substance, thus reaching to improve the effect of cycle performance.
Additionally, said method processing procedure environmental protection of the present invention, generating without poisonous and harmful intermediate product, and raw material is easy to get, technique is simple and clear, and equipment requirements is not high, with low cost, it is easy to large-scale commercial applications uses.
In order to further illustrate technical scheme; it is illustrated below by way of specific embodiment; embodiment described below is limited the representative embodiment cited by the present invention; the concrete embodiment of above-mentioned material, formula proportion and the reaction condition being previously mentioned of concrete material, formula proportion and the reaction condition only present invention being previously mentioned, not in order to limit the scope of the invention.
Embodiment 1
By SiOx(x=1.8) weigh with polyvinyl alcohol vinyl polymer 92:8 in mass ratio, by solid phase mixing, polymer uniform is scattered in SiOxIn material, it is subsequently placed in atmosphere furnace 500 DEG C of heat treatment 4h, is cooled to room temperature and takes out to obtain polyvinyl alcohol coated Si OxNegative material. After tested, the ratio table 1.6m of this material2/ g, uses lithium ion battery prepared by this material, and the specific discharge capacity of this material reaches more than 1500mAh/g (referring to Fig. 2), and capability retention more than 92% (referring to Fig. 3) after circulation in 50 weeks, pole piece expansion rate is low to moderate less than 50%.
Embodiment 2
Taking 8g propylene glycol alginate, be dispersed in 2000g alcohol-water mixture, stirring adds the SiO of 92g after half an hourx(x=0.6) powder, then takes out to obtain propylene glycol alginate coated Si O after 500 DEG C of dry 4hxNegative material. After tested, the ratio table 1.5m of this material2/ g, uses lithium ion battery prepared by this material, and the specific discharge capacity of this material reaches more than 1500mAh/g, and capability retention more than 92% after circulation in 50 weeks, pole piece expansion rate is low to moderate less than 50%.
Embodiment 3
By SiOx(x=1.5)/organic carbon and hydroxymethyl cellulose base polymer 90:10 in mass ratio, be scattered in SiO by solid phase mixing by polymer uniformxIn/organic carbon material, it is subsequently placed in atmosphere furnace 500 DEG C of heat treatment 4h, is cooled to room temperature and takes out to obtain hydroxymethyl cellulose coated Si OxNegative material. After tested, the ratio table 1.3m of this material2/ g, uses lithium ion battery prepared by this material, and the specific discharge capacity of this material reaches more than 1500mAh/g, and capability retention more than 92% after circulation in 50 weeks, pole piece expansion rate is low to moderate less than 50%.
Embodiment 4
Taking 2g polyvinylidene fluoride vinyl polymer, be dispersed in 500g polypyrrole alkanone water mixed liquid, stirring adds the SiO of 98g after half an hourx/ Graphene (x=0.8) powder, then takes out to obtain polyvinylidene fluoride vinyl polymer coated Si O after 500 DEG C of dry 4hxNegative material. After tested, the ratio table 1.7m of this material2/ g, uses lithium ion battery prepared by this material, and the specific discharge capacity of this material reaches more than 1500mAh/g, and capability retention more than 92% after circulation in 50 weeks, pole piece expansion rate is low to moderate less than 50%.
The foregoing is only embodiments of the invention; not thereby the scope of the claims of the present invention is limited; every equivalent structure utilizing description of the present invention and accompanying drawing content to make or equivalence flow process conversion; or directly or indirectly it is used in other relevant technical fields, all in like manner include in the scope of patent protection of the present invention.
Claims (10)
1. a lithium ion battery negative material, it is characterised in that described lithium ion battery negative material includes SiOxBase active substance and be coated on described SiOxThe strong flexible polymer of base active material surface, described 0 x 2.
2. lithium ion battery negative material according to claim 1, it is characterised in that described SiOxBase active substance is SiOx��SiOx/C��SiOxAt least one in/M, wherein, described M is at least one in alkali metal, transition alkali metal, alkali metal oxide and transition alkali metal oxide; Described strong flexible polymer is the combination of the single polymers of elongation at break < 95% in 30 DEG C��vitrification point��300 DEG C, 1000��number equal relative molecular weight��800,000,0��degree of cross linking��80,0��swelling ratio��15 and electrolyte or multiple polymers.
3. lithium ion battery negative material according to claim 2, it is characterised in that described SiOx/ C is SiOx/ organic carbon, SiOx/ DIC, SiOx/ graphite, SiOxAt least one in/Graphene, described M is Li, Li2O��B��B2O��Co��CoO��Fe��Fe2O3��Mg��MgO��Sn��SnO��Ti��TiO2, at least one in Ag, AgO and Cr; Described strong flexible polymer is at least one in naturally occurring or synthetic polyacrylate and derivant, polyimide and derivant, Kynoar class and derivant, polycyanate ester class and derivant, poly-butadiene-styrene rubber class and derivant, polyvinyl alcohol and derivant, carboxymethyl cellulose class and derivant, Sargassum acids and derivant thereof.
4. lithium ion battery negative material according to claim 1, it is characterised in that described strong flexible polymer and described SiOxThe mass ratio of base active substance more than 0 less than 30%.
5. the preparation method of the lithium ion battery negative material described in an any one of claim 1-4, it is characterised in that said method comprising the steps of:
By described strong flexible polymer and described SiOxBase active substance mix homogeneously forms mixture;
Described mixture carries out process makes described strong flexible polymer at described SiOxBase active material surface forms homogeneous thin film, obtains described lithium ion battery negative material.
6. preparation method according to claim 5, it is characterised in that described described mixture is carried out process make described strong flexible polymer at described SiOxBase active material surface forms homogeneous thin film, obtains described lithium ion battery negative material and includes:
Described mixture is placed in the drying baker of 80-500 DEG C of vacuum or logical protective gas; insulation 0.5-5 was as a child cooled to room temperature; to obtain described lithium ion battery negative material, described protective gas is at least one in nitrogen, helium, neon, argon, Krypton and xenon.
7. the preparation method according to claim 5 or 6, it is characterised in that described method also includes:
Material after described process is carried out screening process, to obtain the particle diameter material less than 50 microns as described lithium ion battery negative material.
8. preparation method according to claim 5, it is characterised in that described strong flexible polymer and described SiOxAny of which mixing by solid phase mixing or solid liquid phase mixing of the base active substance, forms described mixture by least one mode mix homogeneously in centrifugal, ball milling and mechanical agitation.
9. preparation method according to claim 8, it is characterised in that as described strong flexible polymer and described SiOxWhen base active substance is mixed by the mode that solid liquid phase mixes, described strong flexible polymer is dissolved in solvent and is configured to polymer solution, by described SiOxBase active substance adds mix homogeneously in described polymer solution and forms described mixture.
10. preparation method according to claim 9, it is characterised in that described solvent is at least one in water, benzene, ethanol, polypyrrole alkanone, isopropanol, acetone, DMF, pentane, toluene and halogenated hydrocarbons.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201511033265.2A CN105633368A (en) | 2015-12-31 | 2015-12-31 | Negative electrode material of lithium ion battery and preparation method for negative electrode material |
| PCT/CN2016/099770 WO2017113898A1 (en) | 2015-12-31 | 2016-09-22 | Negative electrode material of lithium-ion battery, and preparation method thereof |
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| CN201511033265.2A CN105633368A (en) | 2015-12-31 | 2015-12-31 | Negative electrode material of lithium ion battery and preparation method for negative electrode material |
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| CN106848241A (en) * | 2017-02-27 | 2017-06-13 | 苏州大学 | A kind of preparation method of polymer overmold lithium ion battery electrode material |
| WO2017113898A1 (en) * | 2015-12-31 | 2017-07-06 | 深圳市贝特瑞新能源材料股份有限公司 | Negative electrode material of lithium-ion battery, and preparation method thereof |
| CN108063255A (en) * | 2017-11-17 | 2018-05-22 | 合肥国轩高科动力能源有限公司 | Modified polyacrylic acid type negative electrode binder |
| CN109103441A (en) * | 2018-09-10 | 2018-12-28 | 江苏塔菲尔新能源科技股份有限公司 | Modified composite material, preparation method and the purposes in lithium ion battery of siliceous substrates material |
| CN109301184A (en) * | 2018-09-10 | 2019-02-01 | 江苏塔菲尔新能源科技股份有限公司 | Modified composite material, preparation method and the purposes in lithium ion battery of siliceous substrates material |
| CN109411713A (en) * | 2018-09-10 | 2019-03-01 | 江苏塔菲尔新能源科技股份有限公司 | The machinery of the modified composite material of siliceous substrates material is total to method for coating, modified composite material and lithium ion battery |
| CN109473648A (en) * | 2018-11-02 | 2019-03-15 | 中国有色桂林矿产地质研究院有限公司 | A kind of Silicon-carbon composite material for lithium ion battery and preparation method thereof |
| CN109755496A (en) * | 2017-11-08 | 2019-05-14 | 三星Sdi株式会社 | Negative active material for rechargeable lithium battery and rechargeable lithium battery containing the same |
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