CN107302081A - Negative material and preparation method thereof, battery and preparation method thereof - Google Patents
Negative material and preparation method thereof, battery and preparation method thereof Download PDFInfo
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- CN107302081A CN107302081A CN201610235279.0A CN201610235279A CN107302081A CN 107302081 A CN107302081 A CN 107302081A CN 201610235279 A CN201610235279 A CN 201610235279A CN 107302081 A CN107302081 A CN 107302081A
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- Prior art keywords
- nucleome
- carbon containing
- housing
- negative material
- carbon
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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
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—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
- H01M4/485—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of mixed oxides or hydroxides for inserting or intercalating light metals, e.g. LiTi2O4 or LiTi2OxFy
-
- 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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/583—Carbonaceous material, e.g. graphite-intercalation compounds or CFx
-
- 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
-
- 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 embodiment of the invention discloses a kind of negative material and preparation method thereof and a kind of battery and preparation method thereof, the negative material includes：Carbon containing nucleome and the housing for being wrapped in the carbon containing core surface, the housing only can allow electronics and ion to pass through, wherein, the carbon containing nucleome is more than theoretical capacity of the housing to lithium ion to the theoretical capacity of lithium ion, and under charging and discharging state, the deformation of the housing is less than the deformation of the carbon containing nucleome, so that the battery that the negative material provided using the embodiment of the present invention is made, both can have the high power capacity and high conductivity of the carbon containing nucleome, the carbon containing nucleome can be isolated using the housing again, avoid because the carbon containing nucleome and compatibility of electrolyte are bad, and cause the battery head made using the carbon containing nucleome to imitate the problem of low and cycle life is poor, improve the capacity of the battery.
Description
Technical field
The present invention relates to cell art, more particularly to a kind of negative material and preparation method thereof and one
Plant battery and preparation method thereof.
Background technology
Commercialization lithium battery graphite cathode material have have extended cycle life, first effect is high, cost is low, environment is friendly
A variety of advantages such as good and easy processing, are obtained extensively in mancarried electronic aid, electric car and energy storage field
Using.But the theoretical specific capacity of graphite relatively low (about 372mAh/g), with compatibility of electrolyte is poor, multiplying power
Characteristic is bad, although by carbon coating technology, and the compatibility of graphite and electrolyte is improved, but its
It is forthright again to be difficult to improve always, and capacity becomes the bottleneck for improving battery capacity close to the limit.
Therefore, developing new negative material turns into those skilled in the art's technical problem urgently to be resolved hurrily.
The content of the invention
In order to solve the above technical problems, the embodiments of the invention provide a kind of negative material and preparation method thereof
And a kind of battery and preparation method thereof, to improve the capacity of battery.
To solve the above problems, the embodiments of the invention provide following technical scheme：
In a first aspect, the embodiments of the invention provide a kind of negative material, including：Carbon containing nucleome and parcel
In the housing of the carbon containing core surface, the housing only can allow electronics and ion to pass through；Wherein, institute
State carbon containing nucleome and theoretical capacity of the housing to lithium ion is more than to the theoretical capacity of lithium ion, and filling
Under discharge condition, the deformation of the housing is less than the deformation of the carbon containing nucleome.
With reference in a first aspect, in the first possible implementation, it should be pointed out that the housing
Under charging and discharging state, it will not deform upon, wherein, the housing is titanium dioxide housing or lithium titanate
Housing.
With reference in a first aspect, in second of possible implementation, it should be pointed out that described carbon containing
The theoretical capacity of the material of nucleome is more than 372mAh/g, and optionally, the material of the carbon containing nucleome includes：
At least one of graphene, hard carbon, soft carbon, fullerene, CNT or carbon fiber, and it is described
Also include dopant material in carbon containing nucleome, the component of the dopant material include N, P, B, S,
At least one of O, F, Cl and H.
With reference in a first aspect, in the third possible implementation, it should be pointed out that described carbon containing
Nucleome and the housing are chondritic, and the diameter span of the housing is 200nm~10000nm,
Including endpoint value；The Thickness scope of the housing is 1nm-20nm, including endpoint value.
With reference in a first aspect, in the 4th kind of possible implementation, the housing and the carbon containing nucleome
Mass ratio be located at 1:10-1:Between 100, including endpoint value.
Second aspect, the embodiments of the invention provide a kind of preparation method of negative material, this method includes：
Emulsion polymerization is carried out using the carbon containing nucleome of nanoscale and organic monomer solution, carbon containing nucleome nanometer is obtained
Polymer microballoon, the surface of the carbon containing nucleome nanometer polymer microballoon has hydrophily；
Using the carbon containing nucleome nanometer polymer microballoon and the organic solution containing default material, wrapped
The carbon containing nucleome nanometer polymer particle of housing is wrapped with, the housing is used to isolate the carbon containing nucleome, only
Electronics and ion can be allowed to pass through；
The polymer in the carbon containing nucleome nanometer polymer particle of housing is enclosed with described in removing, is wrapped up
There is the carbon containing nucleome nano-particle of housing, cell negative electrode material is made；
Wherein, the carbon containing nucleome is more than theory of the housing to lithium ion to the theoretical capacity of lithium ion
Capacity, and under charging and discharging state, the deformation of the housing is less than the deformation of the carbon containing nucleome.
With reference to second aspect, in the first possible implementation, it should be pointed out that described to utilize
The carbon containing nucleome of nanoscale and organic monomer solution carry out emulsion polymerization, obtain carbon containing nucleome nanometer polymer micro-
Ball includes：
The carbon containing nucleome of nanoscale is dispersed in organic monomer solution, then mixed solution addition is gone
In ionized water, under surfactant, reaction is stirred, and in the presence of initiator, carries out breast
Liquid polymerize, and obtains carbon containing nucleome nanometer polymer microballoon.
Optionally, the quality span of the carbon containing nucleome of the nanoscale is：1g-5g, including endpoint value；
The span of the volume of the organic monomer solution is 20ml-50ml, including endpoint value.
With reference to second aspect, in second of possible implementation, it should be pointed out that described to utilize
Carbon containing nucleome nanometer polymer microballoon and the organic solution containing default material, obtain being enclosed with containing for housing
Carbon nucleome nanometer polymer particle includes：
Using carbon containing nucleome nanometer polymer microballoon and the ethanol solution of butyl titanate, obtain being enclosed with two
The carbon containing nucleome nanometer polymer particle of titanium oxide housing.
The third aspect, the embodiments of the invention provide a kind of preparation method of battery, this method includes：
Negative material, conductive black and the polyvinylidene fluoride that any of the above-described is provided are according to default matter
Ratio is measured with being applied in copper foil current collector, vacuum drying obtains cell piece；
Battery is constituted using the cell piece, to electrode, battery diaphragm and electrolyte.
Fourth aspect, the embodiments of the invention provide a kind of battery, the battery is carried including any of the above-described
The negative material of confession.
Compared with prior art, above-mentioned technical proposal has advantages below：
The negative material that the embodiment of the present invention is provided, including：Carbon containing nucleome and it is wrapped in the carbon containing core
The housing in body surface face, the housing only can allow electronics and ion to pass through, wherein, the carbon containing nucleome pair
The theoretical capacity of lithium ion is more than theoretical capacity of the housing to lithium ion, and under charging and discharging state,
The deformation of the housing is less than the deformation of the carbon containing nucleome, so that being carried using the embodiment of the present invention
The battery that the negative material of confession makes, the high power capacity and high conductivity both can with the carbon containing nucleome,
The carbon containing nucleome can be isolated using the housing again, it is to avoid due to the carbon containing nucleome and electrolyte
Compatibility is bad, and causes the battery head made using the carbon containing nucleome to imitate asking for low and cycle life difference
Topic, improves the capacity of the battery.
Brief description of the drawings
In order to illustrate more clearly about the embodiment of the present invention or technical scheme of the prior art, below will be to reality
The accompanying drawing used required for applying in example or description of the prior art is briefly described, it should be apparent that, below
Accompanying drawing in description is only some embodiments of the present invention, for those of ordinary skill in the art,
On the premise of not paying creative work, other accompanying drawings can also be obtained according to these accompanying drawings.
The structural representation for the negative material that Fig. 1 is provided by one embodiment of the invention；
The flow chart for the negative material preparation method that Fig. 2 is provided by one embodiment of the invention；
The flow chart for the battery production method that Fig. 3 is provided by one embodiment of the invention.
Embodiment
Just as described in the background section, new negative material is developed urgently to solve as those skilled in the art
Technical problem certainly.
Inventor's research finds that the research direction of novel anode material has two classes, and a class is brand-new negative pole
Material, including：Alloy, oxide, sulfide etc., this kind of material have higher theoretical capacity, good
Good intercalation/deintercalation ability, for example, the charge and discharge process Volume Changes very little of lithium titanate class material, has
Stable discharge platform, does not form SEI films (solid electrolyte interface, solid electrolyte interface
Film), the features such as coulombic efficiency is high, but the material reversible capacitance amount is low, electrical conductivity is low；Another kind of is new
The carbon material of form, including：Graphene, hard carbon, soft carbon, CNT, carbon fiber etc., with graphite
Exemplified by alkene, its electrical conductivity is high, but it is bad with compatibility of electrolyte, and head effects are low, and cycle life is poor.
In view of this, the embodiments of the invention provide a kind of negative material, including：Carbon containing nucleome and parcel
In the housing of the carbon containing core surface, the housing only can allow electronics and ion to pass through；
Wherein, the carbon containing nucleome is more than theory of the housing to lithium ion to the theoretical capacity of lithium ion
Capacity, and under charging and discharging state, the deformation of the housing is less than the deformation of the carbon containing nucleome.
Accordingly, the embodiment of the present invention additionally provides a kind of preparation method of negative material, including：
Emulsion polymerization is carried out using the carbon containing nucleome of nanoscale and organic monomer solution, carbon containing nucleome nanometer is obtained
Polymer microballoon, the carbon containing nucleome nanometer polymer microsphere surface has hydrophily；
Using the carbon containing nucleome nanometer polymer microballoon and the organic solution containing default material, wrapped
The carbon containing nucleome nanometer polymer particle of housing is wrapped with, the housing is used to isolate the carbon containing nucleome, only
Electronics and ion can be allowed to pass through；
The polymer in the carbon containing nucleome nanometer polymer particle of housing is enclosed with described in removing, is wrapped up
There is the carbon containing nucleome nano-particle of housing, cell negative electrode material is made；
Wherein, the carbon containing nucleome is more than theory of the housing to lithium ion to the theoretical capacity of lithium ion
Capacity, and under charging and discharging state, the deformation of the housing is less than the deformation of the carbon containing nucleome.
In addition, the embodiment of the present invention additionally provides a kind of preparation method of battery and utilizes the preparation method system
The battery of work, wherein, the preparation method includes：By above-mentioned negative material, conductive black and poly- inclined difluoro
Ethene is according to preset quality ratio with being applied in copper foil current collector, and vacuum drying obtains cell piece；
Battery is constituted using the cell piece, to electrode, battery diaphragm and electrolyte.
In negative material that the embodiment of the present invention is provided and preparation method thereof, the negative material includes containing
Carbon nucleome and the housing for being wrapped in the carbon containing core surface, the housing can only allow electronics and ion logical
Cross, wherein, the carbon containing nucleome is more than theory of the housing to lithium ion to the theoretical capacity of lithium ion
Capacity, and under charging and discharging state, the deformation of the housing is less than the deformation of the carbon containing nucleome, so that
So that the battery that the negative material provided using the embodiment of the present invention is made, can both have described carbon containing
The high power capacity and high conductivity of nucleome, can be isolated using the housing to the carbon containing nucleome again, it is to avoid
Because the carbon containing nucleome and compatibility of electrolyte are bad, and cause the electricity using the carbon containing nucleome making
The problem of Chi Shouxiao is low and cycle life is poor, improves the capacity of the battery.
Below in conjunction with the accompanying drawing in the embodiment of the present invention, the technical scheme in the embodiment of the present invention is carried out
Clearly and completely describe, it is clear that described embodiment is only a part of embodiment of the invention, and
The embodiment being not all of.Based on the embodiment in the present invention, those of ordinary skill in the art are not doing
Go out the every other embodiment obtained under the premise of creative work, belong to the scope of protection of the invention.
Many details are elaborated in the following description to facilitate a thorough understanding of the present invention, still this hair
Bright to be different from other manner described here using other and implement, those skilled in the art can be with
Similar popularization is done in the case of without prejudice to intension of the present invention, therefore the present invention is not by following public specific
The limitation of embodiment.
The embodiments of the invention provide a kind of negative material, as shown in figure 1, the negative material includes：Contain
Carbon nucleome 1 and the housing 2 for being wrapped in the surface of carbon containing nucleome 1, the housing 2 is used for will be described carbon containing
Nucleome 1 is isolated with external environment condition, only electronics and ion can be allowed to pass through；Wherein, the carbon containing core
Body 1 is more than theoretical capacity of the housing 2 to lithium ion to the theoretical capacity of lithium ion, and in discharge and recharge
Under state, the deformation of the housing 2 is less than the deformation of the carbon containing nucleome 1.
It should be noted that in embodiments of the present invention, due to the carbon containing nucleome 1 have capacity it is high,
The characteristics of good conductivity, thus the negative material provided using the embodiment of the present invention also have capacity it is high,
The characteristics of good conductivity.In addition, in embodiments of the present invention, the carbon containing surface of nucleome 1 is also enclosed with
Housing 2, the housing 2 is used to isolate the carbon containing nucleome 1, only electronics and ion can be allowed to pass through, from
And the battery that the negative material provided using the embodiment of the present invention is made, it can both avoid by institute
Capacity attenuation caused by the materials such as carbon containing nucleome 1 and electrolyte are in contact is stated, electronics can be ensured again
Transmission rate, it is ensured that the electric conductivity of the battery made using the negative material.
Moreover, in embodiments of the present invention, deformation of the housing 2 under charging and discharging state is less than described
Deformation of the carbon containing nucleome 1 under charging and discharging state, so as to alleviate because the carbon containing nucleome 1 is in charge and discharge
It is first caused by deformation is larger under electricity condition to imitate the problem of low and circular form is poor, improve and utilize the negative pole
The performance for the battery that material makes.
On the basis of above-described embodiment, in one embodiment of the invention, the housing 2 is in charge and discharge
Under electricity condition, deformation is smaller, will not even deform upon, to alleviate to greatest extent due to described carbon containing
First effect is low caused by deformation is larger under charging and discharging state and the problem of poor circular form for nucleome 1.
On the basis of any of the above-described embodiment, in one particular embodiment of the present invention, the housing 2
For titanium dioxide housing or lithium titanate housing, but the present invention is not limited this, is specifically depended on the circumstances.
On the basis of any of the above-described embodiment, in one embodiment of the invention, the carbon containing nucleome 1
Materials theory capacity be more than 372mAh/g, with described in utility negative material make battery theory
Capacity.Optionally, the material of the carbon containing nucleome 1 includes：Graphene, hard carbon, soft carbon, fullerene,
At least one of CNT or carbon fiber, the present invention are not limited this, are specifically depended on the circumstances.
It should be noted that on the basis of above-described embodiment, in one embodiment of the invention, institute
Dopant material can also be included by stating in carbon containing nucleome 1, specifically, the component of the dopant material
At least one of N, P, B, S, O, F, Cl and H can be included.
On the basis of any of the above-described embodiment, in one embodiment of the invention, the carbon containing nucleome 1
It is chondritic with the housing 2, the chondritic is nanostructured, optionally, the housing 2
Diameter span be 200nm~10000nm, including endpoint value, i.e., including 200nm and 10000nm,
When making battery using the negative material, to reduce adjacent chondritic when multiple chondritics are accumulated
Between space so that under same volume, increase stackable chondritic quantity, improve battery and hold
Amount.Optionally, the diameter span of the housing 2 be 200nm~1000nm, including 200nm and
1000nm, such as concretely 300nm, 500nm or 800nm, the present invention are not limited this,
Specifically depend on the circumstances.
On the basis of any of the above-described embodiment, in one embodiment of the invention, the housing 2
Thickness scope is 1nm-20nm, including endpoint value is described to ensure that is, including 1nm and 20nm
The electric conductivity of negative material.Optionally, the Thickness of the housing 2 can be 5nm, 10nm or 15nm
Deng, it is of the invention that this is not limited, specifically depend on the circumstances.
On the basis of any of the above-described embodiment, in one embodiment of the invention, the He of housing 2
The mass ratio of the carbon containing nucleome 1 is located at 1:10-1:Between 100, including endpoint value, to ensure the shell
On the premise of the buffer action of 2 pairs of the body carbon containing nucleome 1, improve the negative material electric conductivity and
Theoretical capacity.Optionally, the mass ratio of the housing 2 and the carbon containing nucleome 1 can be 1:10、1:30、
1:50、1:80 or 1:100 etc., the present invention is not limited this, is specifically depended on the circumstances.
In addition, the embodiment of the present invention additionally provides a kind of battery, the battery includes：Any of the above-described embodiment
The negative material provided.Optionally, GND electrode slice, anode electrode piece, battery diaphragm, non-
Water electrolysis liquid and shell, wherein, the negative electricity pole piece includes：Collector and it is coated in the collector
On negative material, the negative material that the negative material is provided by any of the above-described embodiment of the invention.
It should be noted that, although the battery in the embodiment of the present invention is described by taking lithium battery as an example,
But negative material that the embodiment of the present invention is provided and not only limit is applied to field of lithium, can also be applied
To other field of batteries, such as area of solar cell, the present invention is not limited this, specifically optionally
Depending on.
In the negative material that the embodiment of the present invention is provided and the battery including the negative material, including it is carbon containing
Nucleome 1 and the housing 2 for being wrapped in the surface of carbon containing nucleome 1, the housing 2 are used for the carbon containing core
Body 1 is isolated, and only electronics and lithium ion can be allowed to pass through, wherein, the carbon containing nucleome 1 to lithium from
The theoretical capacity of son is more than theoretical capacity of the housing 2 to lithium ion, and under charging and discharging state, institute
The deformation for stating housing 2 is less than the deformation of the carbon containing nucleome 1, so that utilizing institute of the embodiment of the present invention
The battery that the negative material of offer makes, can both have the high power capacity of the carbon containing nucleome 1 and highly conductive
Property, it can be isolated again using 2 pairs of the housing carbon containing nucleome 1, it is to avoid due to the carbon containing nucleome 1
It is in contact with electrolyte, and causes the battery head made using the carbon containing nucleome 1 to imitate low and cycle life
Poor the problem of, improve the capacity of the battery.
Accordingly, the embodiment of the present invention additionally provides a kind of preparation method of negative material, as shown in Fig. 2
This method includes：
S1：Emulsion polymerization is carried out using the carbon containing nucleome of nanoscale and organic monomer solution, carbon containing nucleome is obtained
Nanometer polymer microballoon, the carbon containing nucleome nanometer polymer microsphere surface has hydrophily.
It should be noted that the emulsion polymerization be monomer by emulsifying agent and mechanical agitation, make monomer point
It is dispersed in water and forms emulsion, adds initiator and trigger monomer polymerization.In one embodiment of the invention,
It is described to carry out emulsion polymerization using the carbon containing nucleome of nanoscale and organic monomer solution, obtain including carbon containing core
There is body nanometer polymer microballoon, the carbon containing nucleome nanometer polymer microsphere surface hydrophily to include：
The carbon containing nucleome of nanoscale is dispersed in organic monomer solution, then mixed solution addition is gone
In ionized water, in the presence of surfactant, reaction is stirred, and in the presence of initiator,
Emulsion polymerization is carried out, carbon containing nucleome nanometer polymer microballoon is obtained, the carbon containing nucleome nanometer polymer is micro-
Ball surface has hydrophily.
Specifically, in an embodiment of the invention, the carbon containing nucleome of nanoscale is dispersed in into organic list
In liquid solution, then by mixed solution addition deionized water, in the presence of surfactant, carry out
Stirring reaction, and in the presence of initiator, carry out emulsion polymerization, obtain carbon containing nucleome nanometer polymer
Microballoon includes：The carbon containing nucleome of nanoscale is dispersed in styrene liquid, then styrene is added into play
In the deionized water of strong stirring, then stirring and emulsifying adds potassium sulfate, and stirring reaction is included
The pipe/polyhenylethylene nano level microballoon emulsion of carbon containing nucleome, is eventually adding Klorvess Liquid demulsification filtering, wash,
It is dried to obtain the pipe/polyhenylethylene nano level microballoon for including carbon containing nucleome.It should be noted that in this implementation
In example, surfactant and alkaline solution have been previously added in the deionized water.
Optionally, the quality span of the carbon containing nucleome of the nanoscale is：1g-5g, including endpoint value 1g
And 5g；The span of the volume of the organic monomer solution is 20ml-50ml, including endpoint value 20ml
And 50ml；The surfactant is neopelex, and its quality span is 0.9g-2g；
The alkaline solution is sodium hydroxide or alundum (Al2O3), and its quality span is 3g-5g.But the present invention
This is not limited, specifically depended on the circumstances.
It should be noted that on the basis of any of the above-described embodiment, in one embodiment of the invention,
The carbon containing nucleome nanometer polymer microsphere surface that includes obtained after emulsion polymerization has hydrophily in itself；
In an alternative embodiment of the invention, obtained after emulsion polymerization to include carbon containing nucleome nanometer polymer micro-
Ball surface does not have hydrophily in itself, and in embodiments of the present invention, this method also includes：Utilize modifying agent
The carbon containing nucleome nanometer polymer microsphere surface is handled, hydrophily is made it have.Specifically,
In one embodiment of the present of invention, the utilization modifying agent is to the carbon containing nucleome nanometer polymer microballoon
Surface is handled, and making it have hydrophily includes：The carbon containing nucleome nanometer polymer microballoon is disperseed
In ethanol, add modifying agent and stir, make its surface that there is hydrophily.
Optionally, the modifying agent can be the concentrated sulfuric acid, vinylbenzenesulfonic acid sodium or the ethoxy of γ-aminopropyl three
Base silane (KH550), the present invention is not limited this, is specifically depended on the circumstances.
S2：Using the carbon containing nucleome nanometer polymer microballoon and the organic solution containing default material, obtain
To the carbon containing nucleome nanometer polymer particle for being enclosed with housing, the housing is used to isolate the carbon containing nucleome,
Only electronics and ion can be allowed to pass through.
It should be noted that in embodiments of the present invention, theoretical capacity of the carbon containing nucleome to lithium ion
More than theoretical capacity of the housing to lithium ion, and under charging and discharging state, the deformation of the housing is small
In the deformation of the carbon containing nucleome.
It is in one embodiment of the invention, described using described on the basis of any of the above-described embodiment
Carbon containing nucleome nanometer polymer microballoon and the organic solution containing default material, obtain being enclosed with containing for housing
Carbon nucleome nanometer polymer particle includes：By carbon containing the nucleome nanometer polymer microballoon and butyl titanate
Alcohols (such as methanol, ethanol) solution mixing, stirring, obtain being enclosed with containing for titanium dioxide housing
Carbon nucleome nanometer polymer particle.
Specifically, in an embodiment of the invention, using the carbon containing nucleome nanometer polymer microballoon and
Organic solution containing default material, the carbon containing nucleome nanometer polymer particle for obtaining being enclosed with housing is specific
Including：
The ethanol solution for being dispersed with butyl titanate is slowly added to the carbon containing nucleome nanometer polymer microballoon
Solution in, and be stirred vigorously, be then filtrated to get the carbon containing nucleome nanometer polymer grain for being enclosed with housing
Son.
S3：The polymer in the carbon containing nucleome nanometer polymer particle of housing is enclosed with described in removing, is obtained
The carbon containing nucleome nano-particle of housing is enclosed with, cell negative electrode material is made.
In one embodiment of the invention, polymer is gone in the carbon containing nucleome nanometer polymer particle
Except method is dissolving, in another embodiment of the present invention, the carbon containing nucleome nanometer polymer particle
The minimizing technology of middle polymer is sintering, in other embodiments of the invention, the carbon containing nucleome nanometer
Polymer can also be removed using other method in polymer particle, and the present invention is not limited this, be had
Body depends on the circumstances.
Specifically, in one embodiment of the invention, the carbon containing core of housing is enclosed with described in the removal
Polymer in body nanometer polymer particle, obtains being coated with the carbon containing nucleome nano-particle of housing,
Obtained cell negative electrode material includes：
The carbon containing nucleome nanometer polymer particle for being enclosed with housing is placed in tetrahydrofuran, magnetic force is stirred
Mix to dissolve the polymer being enclosed with described in removal in the carbon containing nucleome nanometer polymer particle of housing, obtain
The carbon containing nucleome nano-particle of housing is coated with, cell negative electrode material is made.
It should be noted that in order to further improve isolation performance of the housing to the carbon containing nucleome,
Obtain being coated with after the carbon containing nucleome nano-particle of housing, be made before lithium cell cathode material also
Including：The carbon containing nucleome structured particles for being coated with housing are sintered, obtain being enclosed with fine and close shell
The carbon containing nucleome nano-particle of body, the carbon containing nucleome structured particles for being enclosed with fine and close housing are used as negative pole
Material.
In addition, the embodiment of the present invention additionally provides a kind of preparation method of battery, as shown in figure 3, the party
Method includes：
S4：Negative material, conductive black and the poly- inclined difluoro that any of the above-described embodiment of the invention is provided
Ethene is according to preset quality ratio with being applied in copper foil current collector, and vacuum drying obtains cell piece.
Specifically, in an alternate embodiment of the present invention where, any of the above-described embodiment of the invention is carried
Negative material, conductive black and the polyvinylidene fluoride of confession are according to 85:10:5 mass ratio is with being applied to copper foil
On collector, 120 ° of vacuum dryings obtain cell piece.
S5：Battery is constituted using the cell piece, to electrode, battery diaphragm and electrolyte.Optionally,
Described is lithium metal to electrode, and the battery diaphragm is celgard C2400；The electrolyte is 1.3mol/L
LiPF6 EC and DEC solution.Wherein, EC (vinyl acetate) and DEC in EC and DEC solution
The volume ratio of (diethyl carbonate) is 3:7.Because the method that battery is made using negative material has been ability
Known to the personnel of domain, this is no longer described in detail the present invention.
In the preparation method for the negative material that the embodiment of the present invention is provided, the negative material includes carbon containing
Nucleome and the housing for being wrapped in the carbon containing core surface, the housing are used to isolate the carbon containing nucleome,
Only electronics and ion can be allowed to pass through, wherein, the carbon containing nucleome is more than institute to the theoretical capacity of lithium ion
Theoretical capacity of the housing to lithium ion is stated, and under charging and discharging state, the deformation of the housing is less than described
The deformation of carbon containing nucleome, so that the battery that the negative material provided using the embodiment of the present invention is made,
Both can have the high power capacity and high conductivity of the carbon containing nucleome, again can be using the housing to described
Carbon containing nucleome isolation, it is to avoid because the carbon containing nucleome is in contact with electrolyte, and cause to contain using described
The battery head that carbon nucleome makes imitates the problem of low and cycle life is poor, improves the capacity of the battery.
Below so that the battery is lithium battery as an example, in conjunction with specific embodiments, the embodiment of the present invention is carried
The negative material of confession and the preparation method of battery are illustrated.
In the first specific embodiment of the present invention, the preparation method of the negative material includes：
S101：1g nanoscale graphite alkene is scattered in 20ml styrene liquid, then styrene is added
In the 250ml deionized waters being stirred vigorously, then stirring and emulsifying adds potassium peroxydisulfate 0.5g, is warming up to
70 DEG C, stirring reaction stops reaction after 14 hours, the pipe/polyhenylethylene nano for obtaining including graphene is micro-
Ball emulsion, adds the demulsification filtering of a small amount of 50% Klorvess Liquid, and washs, is dried to obtain 6.5g and includes
There is the nano pipe/polyhenylethylene microballoon of graphene, wherein, 0.9g 12 has been previously added in the deionized water
Sodium alkyl benzene sulfonate and the dissolving of 3g sodium hydroxides；
S102：The nano pipe/polyhenylethylene microballoon for taking 3g to contain graphene is dispersed in 30ml ethanol, is added
0.6gKH550 stirs, and then slowly adds the 6ml ethanol solutions for being dispersed with 0.6ml butyl titanates
Enter above-mentioned solution, and be stirred vigorously filtering after 2h, obtain being coated with the graphene of compact titanium dioxide housing
- polystyrene spheres nucleocapsid shape particle；
S103：Take the graphene for the being coated with compact titanium dioxide housing-polyphenyl second prepared in 10mlS102
Alkene ball shelly particle is placed in 20mL tetrahydrofurans, and magnetic agitation 2h is removed in polystyrene with dissolving
Core, obtains being coated with the graphene nano particle of titanium dioxide housing, and obtain within 10 hours in 450 DEG C of sintering
It is described to be enclosed with anatase knot to the graphene nano particle for being enclosed with anatase structured titanium dioxide housing
The graphene nano particle of structure titanium dioxide housing can be used as lithium cell cathode material.
S104：By the negative material prepared in S103, conductive black and polyvinylidene fluoride according to mass ratio
85:10:5 are well mixed in 1-METHYLPYRROLIDONE and are applied in copper foil current collector, and are dried in 120 DEG C of vacuum
It is dry, electrode slice is obtained, button cell is then assembled into glove box is tested, wherein, the button
Lithium metal is used in formula battery to electrode, battery diaphragm is celgard 2400, and electrolyte is 1.3mol/L's
(volume ratio is 3 to LiPF6 EC and DEC:7) solution.
Understand after testing, prepared button cell 1C capacity reaches in the first specific embodiment of the invention
600mAh/g, 30C capability retention 60%, head effects can reach 80%.
In the second specific embodiment of the present invention, the preparation method of the negative material includes：
S201：1g nanoscale nitrogen-doped graphenes are scattered in 20ml styrene liquid, then by benzene second
Alkene is added in the 250ml deionized waters being stirred vigorously, stirring and emulsifying, then adds ammonium persulfate 0.5g,
80 DEG C are warming up to, stirring reaction stops reaction, obtains including containing nitrogen-doped graphene after 24 hours
Properties of Polystyrene Nano Particles emulsion, adds a small amount of 50% Klorvess Liquid demulsification filtering, and wash, do
The dry 6.8g that obtains includes the nano pipe/polyhenylethylene microballoon containing nitrogen-doped graphene, wherein, the deionization
0.9g neopelexes and the dissolving of 3g sodium hydroxides have been previously added in water；
S202：The nano pipe/polyhenylethylene microballoon for taking 3g to contain graphene is dispersed in 30ml ethanol, is added
0.6gKH550 stirs, and then slowly adds the 6ml ethanol solutions for being dispersed with 0.6ml butyl titanates
Enter above-mentioned solution, and be stirred vigorously after 2h and filter, obtain being coated with the nitrogenous of compact titanium dioxide housing and mix
Miscellaneous graphene-polystyrene spheres nucleocapsid shape particle；
S203：Take prepared in 10mlS202 be coated with compact titanium dioxide housing contain nitrogen-doped graphene
- polystyrene spheres nucleocapsid shape mix particles solution is placed in 20mL tetrahydrofurans, and magnetic agitation 2h is to dissolve
Polystyrene kernel is removed, obtains being coated with the nano-particle containing nitrogen-doped graphene of titanium dioxide housing,
And the nitrogenous doped graphite for obtaining being enclosed with anatase structured titanium dioxide housing for 10 hours is sintered at 450 DEG C
Alkene nano-particle, the nanoparticle containing nitrogen-doped graphene for being enclosed with anatase structured titanium dioxide housing
Son can be used as lithium cell cathode material.
S204：By the negative material prepared in S203, conductive black and polyvinylidene fluoride according to mass ratio
85:10:5 are well mixed in 1-METHYLPYRROLIDONE and are applied in copper foil current collector, and are dried in 120 DEG C of vacuum
It is dry, electrode slice is obtained, button cell is then assembled into glove box is tested, wherein, the button
Lithium metal is used in formula battery to electrode, battery diaphragm is celgard 2400, and electrolyte is 1.3mol/L's
(volume ratio is 3 to LiPF6 EC and DEC:7) solution.
Understand after testing, prepared button cell 1C capacity reaches in the second specific embodiment of the invention
650mAh/g, 30C capability retention 65%, head effects can reach 83%.
In the 3rd specific embodiment of the present invention, the preparation method of the negative material includes：
S301：1g nanoscale nitrogen-doped graphenes are scattered in 20ml styrene liquid, then by benzene second
Alkene is added in the 250ml deionized waters being stirred vigorously, stirring and emulsifying, then adds ammonium persulfate 0.5g,
80 DEG C are warming up to, stirring reaction stops reaction, obtains including containing nitrogen-doped graphene after 24 hours
Properties of Polystyrene Nano Particles emulsion, adds a small amount of 50% Klorvess Liquid demulsification filtering, and wash, do
The dry 6.8g that obtains includes the nano pipe/polyhenylethylene microballoon containing nitrogen-doped graphene, wherein, the deionization
0.9g neopelexes and the dissolving of 3g sodium hydroxides have been previously added in water；
S302：The nano pipe/polyhenylethylene microballoon for taking 3g to contain graphene is dispersed in 30ml ethanol, is added
0.6gKH550 stirs, and then slowly adds the 6ml ethanol solutions for being dispersed with 0.6ml butyl titanates
Enter above-mentioned solution, and be stirred vigorously after 2h and filter, obtain being coated with the nitrogenous of compact titanium dioxide housing and mix
Miscellaneous graphene-polystyrene spheres nucleocapsid shape particle；
S303：Take prepared in 10gS202 be coated with compact titanium dioxide housing containing nitrogen-doped graphene-
Polystyrene spheres nucleocapsid shape particle directly obtains being enclosed with anatase structured dioxy for 10 hours in 450 DEG C of sintering
Change the nano-particle containing nitrogen-doped graphene of titanium housing, it is described to be enclosed with anatase structured titanium dioxide housing
Nano-particle containing nitrogen-doped graphene can be used as lithium cell cathode material.
S304：By the negative material prepared in 303, conductive black and polyvinylidene fluoride according to mass ratio
85:10:5 are well mixed in 1-METHYLPYRROLIDONE and are applied in copper foil current collector, and are dried in 120 DEG C of vacuum
It is dry, electrode slice is obtained, button cell is then assembled into glove box is tested, wherein, the button
Lithium metal is used in formula battery to electrode, battery diaphragm is celgard 2400, and electrolyte is 1.3mol/L's
(volume ratio is 3 to LiPF6 EC and DEC:7) solution.
Understand after testing, prepared button cell 1C capacity reaches in the 3rd specific embodiment of the invention
550mAh/g, 30C capability retention 60%, head effects can reach 82%.
In the first comparative example of the present invention, the preparation method of battery and its negative material includes：
S401：20ml styrene liquid is added in the 250ml deionized waters being stirred vigorously, stirring and emulsifying,
Then ammonium persulfate 0.5g is added, 80 DEG C are warming up to, stirring reaction stops reaction, obtained after 24 hours
Properties of Polystyrene Nano Particles emulsion, adds a small amount of 50% Klorvess Liquid demulsification filtering, and wash, do
It is dry to obtain 7g nano pipe/polyhenylethylene microballoons, wherein, 0.9g dodecanes have been previously added in the deionized water
Base benzene sulfonic acid sodium salt and the dissolving of 3g sodium hydroxides；
S402：Take 3g nano pipe/polyhenylethylene microballoons to be dispersed in 30ml ethanol, add 0.6gKH550 and stir
Mix uniform, the 6ml ethanol solutions for being dispersed with 0.6ml butyl titanates be then slowly added to above-mentioned solution,
And filtering after 2h is stirred vigorously, obtain being coated with the polystyrene spheres nucleocapsid shape grain of compact titanium dioxide housing
Son；
S403：Take the polystyrene spheres nucleocapsid for being coated with compact titanium dioxide housing prepared in 10mlS402
Shape particle is placed in 20mL tetrahydrofurans, and magnetic agitation 2h removes polystyrene kernel to dissolve, and obtains
Hollow titanium dioxide housing nano-particle, and obtain anatase structured dioxy within 10 hours in 450 DEG C of sintering
Change titanium housing nano-particle, as lithium cell cathode material.
S404：By the negative material prepared in S403, conductive black and polyvinylidene fluoride according to mass ratio
85:10:5 are well mixed in 1-METHYLPYRROLIDONE and are applied in copper foil current collector, and are dried in 120 DEG C of vacuum
It is dry, electrode slice is obtained, button cell is then assembled into glove box is tested, wherein, the button
Lithium metal is used in formula battery to electrode, battery diaphragm is celgard 2400, and electrolyte is 1.3mol/L's
(volume ratio is 3 to LiPF6 EC and DEC:7) solution.
Understand after testing, prepared button cell 1C capacity reaches in the first comparative example of the invention
169mAh/g, 30C capability retention 70%, head effects can reach 95%.
In the second comparative example of the present invention, the preparation method of battery and its negative material includes：
S501：By grapheme material and conductive black, polyvinylidene fluoride according to mass ratio 85：10：5
It is well mixed and is applied in copper foil current collector in 1-METHYLPYRROLIDONE, and in 120 DEG C of vacuum dryings, obtains
To electrode slice, button cell is then assembled into glove box and is tested, wherein, lithium is used to electrode
Metal, battery diaphragm is celgard 2400, and electrolyte is 1.3mol/L LiPF6 EC and DEC (body
Product is than being 3:7) solution.
Understand after testing, prepared button cell 1C capacity reaches in the second comparative example of the invention
900mAh/g, 30C capability retention 40%, head effects can reach 45%.
From the contrast of above-mentioned specific embodiment and comparative example, it is negative that the embodiment of the present invention is provided
Pole material and preparation method thereof not simply mixes two kinds of materials, but uses core shell structure, both retains
The advantage of nucleome material and case material, avoids the defect of nucleome material and case material, obtains complementation again
Effect it is described to contain so that in negative material that the embodiment of the present invention is provided and preparation method thereof
Carbon nucleome material has the housing protection of densification, it is to avoid puzzlement of the SEI films to nucleome material, also has concurrently
The characteristics of carbon containing nucleome material high power capacity and high conductivity.
Moreover, in negative material that the embodiment of the present invention is provided and preparation method thereof, the case material
There is good transmission rate to electronics, so that the negative material provided using the embodiment of the present invention
The battery of making has fills function soon.
It should be noted that, although the negative material preparation method that the embodiment of the present invention is provided is with lithium electricity
Illustrated exemplified by pond, but the application of negative material provided by the present invention is not limited to that, may be used also
To be applied to other field of batteries such as solar cell, specifically depend on the circumstances.
In summary, negative material of the embodiment of the present invention and preparation method thereof and battery and preparation method thereof
In, the negative material includes carbon containing nucleome and is wrapped in the housing of the carbon containing core surface, the shell
Body is used to isolate the carbon containing nucleome, and electronics and ion can be allowed to pass through, wherein, the carbon containing nucleome pair
The theoretical capacity of lithium ion is more than theoretical capacity of the housing to lithium ion, and under charging and discharging state,
The deformation of the housing is less than the deformation of the carbon containing nucleome, so that being carried using the embodiment of the present invention
The battery that the negative material of confession makes, the high power capacity and high conductivity both can with the carbon containing nucleome,
The carbon containing nucleome can be isolated using the housing again, it is to avoid due to the carbon containing nucleome and electrolyte
Compatibility is good, and causes the battery head made using the carbon containing nucleome to imitate the problem of low and cycle life is poor,
Improve the capacity of the battery.
Various pieces are described by the way of progressive in this specification, what each some importance illustrated be with
Between the difference of other parts, various pieces identical similar portion mutually referring to.
It should be noted that herein, such as first and second or the like relational terms are used merely to
One entity or operation are made a distinction with another entity or operation, and not necessarily requires or implies
There is any this actual relation or order between these entities or operation.Moreover, term " comprising ",
"comprising" or any other variant thereof is intended to cover non-exclusive inclusion, so that being including one
Process, method, article or the equipment of row key element not only include those key elements, but also including not bright
Other key elements really listed, or also include for this process, method, article or equipment institute inherently
Key element.In the absence of more restrictions, the key element limited by sentence "including a ...",
It is not precluded from the process including the key element, method, article or equipment also the presence of in addition identical
Key element.
The foregoing description of the disclosed embodiments, enables professional and technical personnel in the field to realize or use
The present invention.A variety of modifications to these embodiments will be aobvious and easy for those skilled in the art
See, generic principles defined herein can without departing from the spirit or scope of the present invention,
Realize in other embodiments.Therefore, the present invention is not intended to be limited to embodiment illustrated herein, and
It is to fit to the most wide scope consistent with features of novelty with principles disclosed herein.
Claims (14)
1. a kind of negative material, it is characterised in that including：Carbon containing nucleome and it is wrapped in the carbon containing nucleome
The housing on surface, the housing only can allow electronics and ion to pass through；
Wherein, the carbon containing nucleome is more than theory of the housing to lithium ion to the theoretical capacity of lithium ion
Capacity, and under charging and discharging state, the deformation of the housing is less than the deformation of the carbon containing nucleome.
2. negative material according to claim 1, it is characterised in that the housing is in discharge and recharge shape
Under state, it will not deform upon.
3. negative material according to claim 1 or 2, it is characterised in that the housing is dioxy
Change titanium housing or lithium titanate housing.
4. the negative material according to claim any one of 1-3, the material of the carbon containing nucleome includes：
At least one of graphene, hard carbon, soft carbon, fullerene, CNT or carbon fiber.
5. negative pole according to claim 4 makes, it is characterised in that in the carbon containing nucleome also
Include dopant material, the component of the dopant material include N, P, B, S, O, F, Cl and
At least one of H.
6. the negative material according to claim any one of 1-5, it is characterised in that the carbon containing core
Body and the housing are chondritic, and the diameter span of the housing is 200nm~10000nm, bag
Include endpoint value.
7. negative material according to claim 6, it is characterised in that the Thickness of the housing
Scope is 1nm-20nm, including endpoint value.
8. the negative material according to claim any one of 1-7, it is characterised in that the housing and
The mass ratio of the carbon containing nucleome is located at 1:10-1:Between 100, including endpoint value.
9. a kind of preparation method of negative material, it is characterised in that this method includes：
Emulsion polymerization is carried out using the carbon containing nucleome of nanoscale and organic monomer solution, carbon containing nucleome nanometer is obtained
Polymer microballoon, the surface of the carbon containing nucleome nanometer polymer microballoon has hydrophily；
Using the carbon containing nucleome nanometer polymer microballoon and the organic solution containing default material, wrapped
The carbon containing nucleome nanometer polymer particle of housing is wrapped with, the housing is used to isolate the carbon containing nucleome, only
Electronics and ion can be allowed to pass through；
The polymer in the carbon containing nucleome nanometer polymer particle of housing is enclosed with described in removing, is wrapped up
There is the carbon containing nucleome nano-particle of housing, cell negative electrode material is made；
Wherein, the carbon containing nucleome is more than theory of the housing to lithium ion to the theoretical capacity of lithium ion
Capacity, and under charging and discharging state, the deformation of the housing is less than the deformation of the carbon containing nucleome.
10. preparation method according to claim 9, it is characterised in that the utilization nanoscale contains
Carbon nucleome and organic monomer solution carry out emulsion polymerization, and obtaining carbon containing nucleome nanometer polymer microballoon includes：
The carbon containing nucleome of nanoscale is dispersed in organic monomer solution, then mixed solution addition is gone
In ionized water, under surfactant, reaction is stirred, and in the presence of initiator, carries out breast
Liquid polymerize, and obtains carbon containing nucleome nanometer polymer microballoon.
11. preparation method according to claim 10, it is characterised in that the carbon containing core of nanoscale
The quality span of body is：1g-5g, including endpoint value；The value of the volume of the organic monomer solution
Scope is 20ml-50ml, including endpoint value.
12. the preparation method according to claim any one of 9-11, it is characterised in that the utilization
Carbon containing nucleome nanometer polymer microballoon and the organic solution containing default material, obtain being enclosed with containing for housing
Carbon nucleome nanometer polymer particle includes：
Using carbon containing nucleome nanometer polymer microballoon and the ethanol solution of butyl titanate, obtain being enclosed with two
The carbon containing nucleome nanometer polymer particle of titanium oxide housing.
13. a kind of preparation method of battery, it is characterised in that this method includes：
By the negative material described in claim 1-8, conductive black and polyvinylidene fluoride according to preset quality
Than with being applied in copper foil current collector, vacuum drying obtains cell piece；
Battery is constituted using the cell piece, to electrode, battery diaphragm and electrolyte.
14. a kind of battery, it is characterised in that including the negative material described in claim any one of 1-8.
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| CN108963229A (en) * | 2018-07-23 | 2018-12-07 | 中国科学院金属研究所 | A kind of high performance silicon negative electrode active material and preparation method thereof |
| CN114242966A (en) * | 2021-11-12 | 2022-03-25 | 惠州锂威新能源科技有限公司 | Negative electrode composite material, preparation method thereof, negative electrode plate and secondary battery |
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Application publication date: 20171027 |