CN110391406A - A kind of lithium ion battery silicon oxygen negative electrode material and preparation method thereof, lithium ion battery - Google Patents
A kind of lithium ion battery silicon oxygen negative electrode material and preparation method thereof, lithium ion battery Download PDFInfo
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- CN110391406A CN110391406A CN201910585030.6A CN201910585030A CN110391406A CN 110391406 A CN110391406 A CN 110391406A CN 201910585030 A CN201910585030 A CN 201910585030A CN 110391406 A CN110391406 A CN 110391406A
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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
- 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
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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
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- H—ELECTRICITY
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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
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
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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
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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
- H01M4/628—Inhibitors, e.g. gassing inhibitors, corrosion inhibitors
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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 silicon oxygen negative electrode materials and preparation method thereof, lithium ion battery, the lithium ion battery silicon oxygen negative electrode material is core-shell structure, the core-shell structure is made of kernel and clad, the kernel is the mixture of Si oxide and element doping graphite, and the clad is organic matter pyrolysis carbon；Wherein, the element is at least one of H, S, P, Cu, Fe, Ni.Negative electrode material initial coulomb efficiency of the invention is high, and long service life has high rate capability.
Description
Technical field
The present invention relates to technical field of lithium ion, more particularly to a kind of lithium ion battery silicon oxygen negative electrode material
And preparation method thereof, lithium ion battery.
Background technique
Lithium ion battery is because of high-energy density, excellent cycle life, high working voltage, lower self-discharge rate, environment
The outstanding advantages such as close friend, in portable electronic device field of power supplies instantly in occupation of leading position and electric car and energy storage
The ideal source in field.2015, global lithium ion battery industry scale reached 52,300,000,000 dollars, presented great market valence
It is worth, the market share shared by China has also reached 49.2 %.In automobile industry, many countries are using electric car as automobile at present
The future thrust of industry obtains the policy support of many countries.
It is main that graphite negative electrodes material (theoretical capacity only 372 mAh g-1) is that current commercial Li-ion battery uses
Negative electrode material has been unable to meet the demand of next-generation energy-density lithium ion battery.Therefore, the cathode of superelevation storage lithium ability is found
Material is to substitute the research hotspot that graphite type material is always field of lithium ion battery.In non-carbon negative material, silica-base material
With the capacity advantage of its superelevation and the de-/intercalation potential for being suitable for become most promising next-generation lithium ion battery negative material it
One, however silica-base material is because causing the rapid decay of capacity with bulk effect huge when lithium alloyage, in addition, silicon itself
Conductivity is lower also to constrain its chemical property especially high rate performance.Silica-base material and the compound of carbon material can effectively be delayed
It rushes the bulk effect of silicon and improves the electric conductivity of material, silica-base material can be accelerated by obtaining the silico-carbo composite material haveing excellent performance
Application process.
In silica-base material, the lithium capacity embedding for the first time of Si oxide is 2615mAh/g, although lithium more embedding than the theory of elemental silicon
Capacity 4200mAh/g is much lower, but still is much higher than conventional graphite cathode, embedding lithium/de- lithium volume expansion phase with elemental silicon 300%
Than the expansion of Si oxide only has 160%.In addition, Si oxide will form irreversible oxidation in lithium ion telescopiny
Lithium (Li2O) and lithium metasilicate (LixSiyOz) by-product can be used as natural buffered layer and alleviate silicon lithium alloy LixSi in lithium ion
Volume expansion when insertion, Particle Breakage caused by avoiding silicon materials expansion excessive, material surface SEI film is unstable, persistently disappears
It consumes activity Li ion and final cycle life in electrolyte to decay the problems such as too fast, therefore using Si oxide as the electricity of cathode
Pond cycle life and capacity retention ratio are often higher than common silicon carbon material.
However, Si oxide absorbed during battery initial charge embedding lithium lithium ion will form by-product lithia and
Lithium metasilicate, the by-product during discharge cannot the completely out lithium ions that it is absorbed in charging process.It is this can not be converse
The loss of a large amount of active lithium-ions in battery should be will cause, form irreversible capacity.Therefore, traditional silicon oxide cathode is for the first time
Coulombic efficiency is low, limits the development of this kind of material.
In addition, inventor has found during realizing the embodiment of the present application, the composite negative pole material of Si oxide and graphite
The high rate performance of material was general, it is hard to meet the requirement of high power charging-discharging.
Therefore, it is necessary to develop more new lithium ion battery silicon oxygen negative electrode materials with outstanding high rate capability.
Summary of the invention
In order to make up the defect of prior art, the present invention provides a kind of lithium ion battery silicon oxygen negative electrode material and its preparation side
Method, lithium ion battery.
The technical problems to be solved by the invention are achieved by the following technical programs:
A kind of lithium ion battery silicon oxygen negative electrode material, the lithium ion battery silicon oxygen negative electrode material are core-shell structure, the nucleocapsid
Structure is made of kernel and clad, and the kernel is the mixture of Si oxide and element doping graphite, and the clad is
Organic matter pyrolysis carbon；Wherein, the element is at least one of H, S, P, Cu, Fe, Ni.
A kind of preparation method of lithium ion battery silicon oxygen negative electrode material, includes the following steps:
(1) graphite and elemental dopant are subjected to high speed ball milling under an inert atmosphere, obtain mixture；Wherein, the graphite and
The mass ratio of elemental dopant is (10-100): 1；
(2) Si oxide is added in above-mentioned mixture and continues ball milling, obtain the mixing of Si oxide and element doping graphite
Object；
(3) mixture of the Si oxide and element doping graphite, organic carbon and organic solvent are mixed, in inertia
Granulation is dried under atmosphere, obtains negative electrode material presoma；
(4) negative electrode material presoma will be obtained under an inert atmosphere in step (3), is warming up to 500-1200 DEG C of roasting, kept the temperature, it is cold
But the lithium ion battery negative material is obtained afterwards.
Further, the elemental dopant is in simple substance or compound powder containing H, S, P, Cu, Fe, Ni element
One or more of combinations.
Further, the partial size of the mixture obtained in step (1) is 0.2-2 μm.
Further, the partial size of the mixture of the Si oxide and element doping graphite that obtain after the step (2) exists
7000nm or less.
Further, the mass ratio of the Si oxide and element doping graphite is (1-4): 1；
Further, the mixture of the Si oxide and element doping graphite, organic carbon mass ratio be (3-50): 100.
Further, the inert atmosphere is at least one of nitrogen, helium, neon, argon gas, Krypton, xenon.
Further, the time of the heat preservation at least 0.5 hour.
Further, the method for the drying-granulating is spray drying, vacuum drying or freeze-drying.
A kind of lithium ion battery using above-mentioned lithium ion battery negative material.
The invention has the following beneficial effects:
Lithium ion battery silicon oxygen negative electrode material of the invention is core-shell structure, and the core-shell structure is made of kernel and clad,
The kernel is the mixture of Si oxide and element doping graphite, and the clad is organic matter pyrolysis carbon；Wherein, the member
Element is at least one of H, S, P, Cu, Fe, Ni, and negative electrode material initial coulomb efficiency of the invention is high, and long service life has
High rate capability.
Using lithium ion battery silicon oxygen negative electrode material of the invention, so that lithium ion battery holds with high first charge-discharge
Amount, low volume bulking effect, high rate capability and excellent cycling performance.
Preparation process of the present invention is simple and unique, and entire material preparation process carries out in a protected environment, easy to operate, packet
It covers uniformly, raw material economics pollutes small.
Detailed description of the invention
Fig. 1 is the X x ray diffraction map of the silicon oxygen negative electrode material of the embodiment of the present invention 1；
Fig. 2 is the scanning electron microscope (SEM) photograph of the silicon oxygen negative electrode material of the embodiment of the present invention 1；
Fig. 3 is the first charge-discharge curve of the silicon oxygen negative electrode material of the embodiment of the present invention 1；
Fig. 4 is the cycle performance curve of the silicon oxygen negative electrode material of the embodiment of the present invention 1.
Specific embodiment
In a first aspect, the present invention provides a kind of lithium ion battery silicon oxygen negative electrode material, the lithium ion battery silicon oxygen cathode
Material is core-shell structure, and the core-shell structure is made of kernel and clad, and the kernel is Si oxide and element doping stone
The mixture of ink, the clad are organic matter pyrolysis carbon；Wherein, the element is at least one in H, S, P, Cu, Fe, Ni
Kind.
The chemical formula of the Si oxide is SiOx, wherein 0 x≤2 <.
Second aspect, the present invention provide a kind of preparation method of lithium ion battery silicon oxygen negative electrode material, include the following steps:
(1) graphite and elemental dopant are subjected to high speed ball milling under an inert atmosphere, obtain mixture；
(2) Si oxide is added in above-mentioned mixture and continues ball milling, obtain the mixing of Si oxide and element doping graphite
Object；
(3) mixture of the Si oxide and element doping graphite, organic carbon and organic solvent are mixed, in inertia
Granulation is dried under atmosphere, obtains negative electrode material presoma；
(4) negative electrode material presoma will be obtained under an inert atmosphere in step (3), is warming up to 500-1200 DEG C of roasting, kept the temperature, it is cold
But the lithium ion battery negative material is obtained afterwards.
Wherein, the graphite and the mass ratio of elemental dopant are (10-100): 1, such as can be 10:1,20:1,30:
Isosorbide-5-Nitrae 0:1,50:1,60:1,70:1,90:1,90:1,100:1.
Wherein, the elemental dopant is one of the simple substance containing H, S, P, Cu, Fe, Ni element or compound powder
Or several combination.Particular kind of element is adulterated in the present invention, in graphite, can effectively improve the high rate performance of negative electrode material.
Preferably, the elemental dopant is simple substance or compound powder containing P and S element, by adulterating P and S in graphite
Element is conducive to buffer the volume change of silicon in the circulating cycle in kernel.
As an example, the elemental dopant can be H2、CS2, dicyanodiamine, 1- butyl -3- methylimidazole hexafluorophosphoric acid
Salt, copper nitrate, iron chloride, nickel nitrate etc., but not limited to this, be also possible to other it is unlisted in the present embodiment but by this
Material known to the technical staff of field.
In the present invention, the partial size of the mixture obtained in step (1) is 0.2-2 μm.By mixture in the present invention
Size controlling is conducive to the dispersion of silicon within the above range and buffers the volume expansion of silicon.Inventor is in practice, it has been found that when mixed
When closing the partial size of material beyond the range, the dispersion of silicon can be seriously affected.
In the present invention, the partial size of the mixture of the Si oxide and element doping graphite that obtain after the step (2) exists
7000nm or less.In the present invention, within the above range by the size controlling of mixture, be conducive to the diffusion and material vibration of lithium ion
The raising of real density.
In the present invention, the mass ratio of the Si oxide and element doping graphite is (1-4): 1；It is highly preferred that the silicon
The mass ratio of oxide and element doping graphite is 3:1.
In the present invention, the mass ratio of the mixture of the Si oxide and element doping graphite, organic carbon are as follows: 100:(3-
50) if the mixture of the Si oxide and element doping graphite, the mass ratio of organic carbon are 100:3,100:10,100:30,
100:40,100:50.
In the present invention, the inert atmosphere is at least one of nitrogen, helium, neon, argon gas, Krypton, xenon.
In the present invention, the time of the heat preservation at least 0.5 hour.
In the present invention, the method for the drying-granulating is spray drying, vacuum drying or freeze-drying, it will be understood that this
The method of the drying-granulating of invention include but is not limited to it is enumerated supra several, it is unlisted in the present embodiment to be also possible to other
In but by other methods well-known to those skilled in the art.Preferably, the method for the drying-granulating is spray drying.
The organic carbon be selected from resin, one of pitch and coal tar, it will be understood that organic carbon of the invention include but
Be not limited to different materials enumerated supra, be also possible to other it is unlisted in the present embodiment but by those skilled in the art
Known other materials.Preferably, the organic carbon is selected from pitch.
In the present invention, the type of organic solvent is not limited specifically, those skilled in the art, which can according to need, to be selected
It selects.Preferably, the organic solvent is tetrahydrofuran.
The third aspect, the present invention provide a kind of lithium ion battery using above-mentioned lithium ion battery negative material.
The present invention will now be described in detail with reference to examples, and the examples are only preferred embodiments of the present invention,
It is not limitation of the invention.
Embodiment 1
A kind of lithium ion battery silicon oxygen negative electrode material, preparation method include the following steps:
(1) 100 parts of graphite and 10 parts of carbon disulfide are subjected to high speed ball milling 5h under an inert atmosphere, revolving speed 600r/min is obtained
To mixture；
(2) Si oxide (SiOx, x=1) is added to continuation 10 h of ball milling, revolving speed in mixture obtained in step (1) is
500r/min obtains the mixture of Si oxide and element doping graphite；
(3) mixture of the Si oxide and element doping graphite, pitch and tetrahydrofuran are mixed, in indifferent gas
It is spray-dried under atmosphere, obtains negative electrode material presoma；
(4) negative electrode material presoma will be obtained in step (3) is warming up to 800 DEG C of roasting 3h, heat preservation at least 0.5 under an inert atmosphere
Hour, it is cooled to room temperature, smashes sieving and obtain lithium ion battery silicon oxygen negative electrode material.
Wherein, the partial size of the mixture obtained in step (1) is 0.2-2 μm；The silicon oxidation that the step (2) obtains
The partial size of the mixture of object and element doping graphite is in 7000nm or less；The inert atmosphere is helium.
The mass ratio of the Si oxide and mixture is 3:1；, the mixture of the Si oxide and element doping graphite
Mass ratio with pitch is 100:25.
Embodiment 2
A kind of lithium ion battery silicon oxygen negative electrode material, preparation method include the following steps:
(1) graphite is carried out to high speed ball milling 5h in a hydrogen atmosphere, internal pressure 1bar-5bar, revolving speed 600r/min are obtained
To mixture；
(2) Si oxide (SiOx, x=1) is added to continuation 10 h of ball milling, revolving speed in mixture obtained in step (1) is
500r/min obtains the mixture of Si oxide and element doping graphite；
(3) mixture of the Si oxide and element doping graphite, pitch and tetrahydrofuran are mixed, in indifferent gas
It is spray-dried under atmosphere, obtains negative electrode material presoma；
(4) negative electrode material presoma will be obtained in step (3) and is warming up to 1200 DEG C of roasting 1h under an inert atmosphere, and heat preservation is at least
It 0.5 hour, is cooled to room temperature, smashes sieving and obtain lithium ion battery silicon oxygen negative electrode material.
Wherein, the partial size of the mixture obtained in step (1) is 0.2-2 μm；The silicon oxidation that the step (2) obtains
The partial size of the mixture of object and element doping graphite is in 7000nm or less；The inert atmosphere is nitrogen.
The mass ratio of the Si oxide and mixture is 4:1；, the mixture of the Si oxide and element doping graphite
Mass ratio with pitch is 100:50.
Embodiment 3
A kind of lithium ion battery silicon oxygen negative electrode material, preparation method include the following steps:
(1) 500 parts of graphite and 10 parts of copper nitrates are subjected to high speed ball milling 5h under an inert atmosphere, revolving speed 600r/min is obtained
Mixture；
(2) Si oxide (SiOx, x=1) is added to continuation 10 h of ball milling, revolving speed in mixture obtained in step (1) is
500r/min obtains the mixture of Si oxide and element doping graphite；
(3) mixture of the Si oxide and element doping graphite, pitch and tetrahydrofuran are mixed, in indifferent gas
It is spray-dried under atmosphere, obtains negative electrode material presoma；
(4) negative electrode material presoma will be obtained in step (3) is warming up to 500 DEG C of roasting 4h, heat preservation at least 0.5 under an inert atmosphere
Hour, it is cooled to room temperature, smashes sieving and obtain lithium ion battery silicon oxygen negative electrode material.
Wherein, the partial size of the mixture obtained in step (1) is 0.2-2 μm；The silicon oxidation that the step (2) obtains
The partial size of the mixture of object and element doping graphite is in 7000nm or less；The inert atmosphere is at least one of neon.
The mass ratio of the Si oxide and mixture is 2:1；, the mixture of the Si oxide and element doping graphite
Mass ratio with pitch is 100:3.
Embodiment 4
A kind of lithium ion battery silicon oxygen negative electrode material, preparation method include the following steps:
(1) by 1000 parts of graphite, 4 parts of 1- butyl -3- methylimidazole hexafluorophosphates and 6 parts of carbon disulfide, under an inert atmosphere
High speed ball milling 5h is carried out, revolving speed 600r/min obtains mixture；
(2) Si oxide (SiOx, x=1) is added to continuation 10 h of ball milling, revolving speed in mixture obtained in step (1) is
500r/min obtains the mixture of Si oxide and element doping graphite；
(3) mixture of the Si oxide and element doping graphite, pitch and tetrahydrofuran are mixed, in indifferent gas
It is spray-dried under atmosphere, obtains negative electrode material presoma；
(4) negative electrode material presoma will be obtained in step (3) is warming up to 500 DEG C of roasting 4h, heat preservation at least 0.5 under an inert atmosphere
Hour, it is cooled to room temperature, smashes sieving and obtain lithium ion battery silicon oxygen negative electrode material.
Wherein, the partial size of the mixture obtained in step (1) is 0.2-2 μm；The silicon oxidation that the step (2) obtains
The partial size of the mixture of object and element doping graphite is in 7000nm or less；The inert atmosphere is at least one of neon.
The mass ratio of the Si oxide and mixture is 1:1；, the mixture of the Si oxide and element doping graphite
Mass ratio with pitch is 100:30.
Embodiments of the present invention above described embodiment only expresses, the description thereof is more specific and detailed, but can not
Therefore limitations on the scope of the patent of the present invention are interpreted as, as long as skill obtained in the form of equivalent substitutions or equivalent transformations
Art scheme should all be fallen within the scope and spirit of the invention.
Claims (10)
1. a kind of lithium ion battery silicon oxygen negative electrode material, which is characterized in that the lithium ion battery silicon oxygen negative electrode material is nucleocapsid
Structure, the core-shell structure are made of kernel and clad, and the kernel is the mixture of Si oxide and element doping graphite,
The clad is organic matter pyrolysis carbon；Wherein, the element is at least one of H, S, P, Cu, Fe, Ni.
2. the preparation method of lithium ion battery silicon oxygen negative electrode material as described in claim 1, which is characterized in that it includes as follows
Step:
(1) graphite and elemental dopant are mixed, high speed ball milling is carried out under inert atmosphere, obtains mixture；Wherein, the graphite
Mass ratio with elemental dopant is (10-100): 1；
(2) Si oxide is added in above-mentioned mixture and continues ball milling, obtain the mixing of Si oxide and element doping graphite
Object；
(3) mixture of the Si oxide and element doping graphite, organic carbon and organic solvent are mixed, in inertia
Granulation is dried under atmosphere, obtains negative electrode material presoma；
(4) negative electrode material presoma will be obtained under an inert atmosphere in step (3), is warming up to 500-1200 DEG C of roasting, kept the temperature, it is cold
But the lithium ion battery negative material is obtained afterwards.
3. the preparation method of lithium ion battery silicon oxygen negative electrode material as claimed in claim 2, which is characterized in that the element is mixed
The miscellaneous dose of combination for the simple substance containing H, S, P, Cu, Fe, Ni element or one or more of compound powder.
4. the preparation method of lithium ion battery silicon oxygen negative electrode material as claimed in claim 2, which is characterized in that the step
(1) partial size of mixture obtained in is 0.2-2 μm；The Si oxide that is obtained after the step (2) and element doping graphite
The partial size of mixture is in 7000nm or less.
5. the preparation method of lithium ion battery silicon oxygen negative electrode material as claimed in claim 2, which is characterized in that the silicon oxidation
The mass ratio of object and element doping graphite is (1-4): 1.
6. the preparation method of lithium ion battery silicon oxygen negative electrode material as claimed in claim 2, which is characterized in that the silicon oxidation
The mixture of object and element doping graphite, organic carbon mass ratio be (3-50): 100.
7. the preparation method of lithium ion battery silicon oxygen negative electrode material as claimed in claim 2, which is characterized in that the indifferent gas
Atmosphere is at least one of nitrogen, helium, neon, argon gas, Krypton, xenon.
8. the preparation method of lithium ion battery silicon oxygen negative electrode material as claimed in claim 2, which is characterized in that the heat preservation
Time at least 0.5 hour.
9. the preparation method of lithium ion battery silicon oxygen negative electrode material as claimed in claim 2, which is characterized in that the drying is made
The method of grain is spray drying, vacuum drying or freeze-drying.
10. a kind of lithium ion battery, which is characterized in that it uses lithium ion battery silicon oxygen cathode material described in claim 1
Material.
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| CN110890531A (en) * | 2019-11-14 | 2020-03-17 | 宁德新能源科技有限公司 | Negative electrode material, and electrochemical device and electronic device comprising same |
| CN111710848A (en) * | 2020-06-30 | 2020-09-25 | 贝特瑞新材料集团股份有限公司 | Silica composite negative electrode material, preparation method thereof and lithium ion battery |
| CN112357916A (en) * | 2020-12-11 | 2021-02-12 | 安徽工业大学 | Method for improving capacity of graphite electrode material |
| CN113725415A (en) * | 2021-08-31 | 2021-11-30 | 常州高态信息科技有限公司 | Power type graphite-silicon oxide composite material and preparation method and application thereof |
| CN113839014A (en) * | 2020-06-08 | 2021-12-24 | 中国石油化工股份有限公司 | Silicon-carbon negative electrode material, preparation method and application thereof, and lithium ion battery |
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