CN109411725A - A method of improving solid state lithium battery silicon based anode material performance - Google Patents
A method of improving solid state lithium battery silicon based anode material performance Download PDFInfo
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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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
- H01M4/38—Selection of substances as active materials, active masses, active liquids of elements or alloys
- H01M4/386—Silicon or alloys based on silicon
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/626—Metals
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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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- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The invention discloses a kind of methods for improving solid state lithium battery silicon based anode material performance.The step of negative electrode material performance boost are as follows: a, by aliphatic polyester mixture, trihydroxy first propane, dimethylbenzene, butyl acetate, isophorone diisocyanate, fluorinated graphene into hybrid reaction, fluoride glass state polyurethane is made;B, aluminium chloride, metal simple-substance, silica-rich zeolite stick and sealing thermal insulation stirring are added in fluoride glass state polyurethane, washing removes remaining miscellaneous phase silicon after taking-up, and the negative electrode material of fluorinated polyurethane load nano-silicon is made.The method has the advantages that the present invention by the fluorinated polyurethane supporting silicon nanoparticles with high toughness as cathode, make the volume expansion of silicon in battery charge and discharge process be fluorinated polyurethane to be absorbed, inhibit the volume expansion of negative electrode material, remaining metallic particles is dispersed in inside fluorinated polyurethane simultaneously, improves the conductivity of negative electrode material.
Description
Technical field
The present invention relates to field of lithium, and in particular to the preparation of negative electrode material, more particularly, to a kind of raising solid-state lithium
The method of battery silicon based anode material performance.
Background technique
With the continuous breakthrough of lithium ion battery technology, the positive and negative pole material capacity of battery is gradually increased, and is expected to 2020
Reach the national standard of 300Wh/kg before year.Lithium ion battery because have specific energy height, charge discharge life length, memory-less effect,
Self-discharge rate is low, quick charge, it is pollution-free, operating temperature range is wide and safe and reliable the advantages that, it has also become modern communication, just
Take the desirable chemical power supply of formula electronic product and hybrid vehicle etc..
Current commercialized negative electrode material is mainly graphite-like carbon negative pole material, and actual capacity has been approached theoretical value, because
This is not able to satisfy the requirement of high energy density lithium ion micro cell, the big multi-steering silica-base material of current negative electrode material research or silicon
Carbon composite.Silicon has the theoretical specific capacity (4200mAh/g) and lower de- lithium current potential (< 0.5V) of superelevation, and the electricity of silicon
Flattening bench is slightly above graphite, and in charging, difficulty causes surface to analyse lithium, and security performance is more preferable.Silica-base material becomes carbon in lithium ion battery
One of potential selection of the richness of base cathode upgrading.
Silica-base material is huge volume change adjoint while lithium ion is compounded to form silicon lithium alloy, causes cathode
Material and bonding agent are detached from, structural breakdown, have very detrimental effect for the service life of lithium ion battery.Current solution
Certainly scheme passes through the space that poromerics or core-shell type material make silicon particle have volume change, but this synthesis mostly
Mode can reduce the density of negative electrode material, and the bulk density of integral battery is had adverse effect.Therefore, for lithium battery
The control of silicon based anode material volume expansion has highly important practical significance.
Number of patent application 201810026308.1 discloses a kind of silicon substrate composite negative pole material and preparation method thereof, the silicon substrate
Composite negative pole material includes conductive base and based particles, is coupled between based particles by conductive base and forms three-dimensional conductive
Network structure;Conductive base is at least one of carbon nanotube, carbon nano-fiber, Ketjen black and graphene;Based particles are
SiOxParticle and SixFeyAt least one of particle.
Number of patent application 201610022471.1 discloses a kind of Silicon Based Anode Materials for Lithium-Ion Batteries and preparation method thereof,
Silicon Based Anode Materials for Lithium-Ion Batteries is the silicon-metal alloy 3-layer composite material of nucleocapsid structure, and stratum nucleare is silicon, and middle layer is
Silicon and the alloy cpd of metal X and the mixture of X, pyrolytic carbon is outermost layer, wherein X is to close with silication in charge and discharge process
In with rock-steady structure metallic element.
Number of patent application 201711457110.0 discloses a kind of carbon coating micro-nano hierarchical structure silicium cathode material and its system
Preparation Method and application, carbon coating micro-nano hierarchical structure silicium cathode material include micro-nano hierarchical structure silicon particle and are wrapped in described micro-
Receive the amorphous carbon layer of hierarchical structure silicon particle outer layer;Wherein micro-nano hierarchical structure silicon particle includes a silicon core and radially
It is distributed in the porous silicon nanowire array on silicon core surface.
Number of patent application 201711183576.6 discloses a kind of modified silicon based anode material of lithium ion battery comprising nothing
Sizing silica substrate, multiple nano-silicon cores, conductive black and carbon coating layer;Multiple nano-silicon cores are embedded in unformed titanium dioxide
In silicon substrate, conductive black is distributed in around nano-silicon core, and carbon coating layer is coated on outside amorphous silica matrix.The invention
It also proposed a kind of preparation method of modified silicon based anode material of the lithium ion battery, comprising: alkali soluble is added in nano silica fume
In liquid, conductive black is added and is uniformly dispersed to obtain intermediate material;Carbon source is added in intermediate material, is spray-dried after stirring,
Then it is sintered under the protection of inert gas.
It can be seen that being used for the silicon based anode material of lithium ion battery, in electrochemistry cyclic process, lithium in the prior art
The insertion and abjection of ion can make the expansion and contraction of 300% or more material volume generation, and the mechanicals efforts of generation can make material
Gradually dusting causes structure collapses, eventually leads to electrode active material and collector is detached from, lose electrical contact, battery is caused to follow
The problems such as ring performance substantially reduces.
Summary of the invention
Effectively to solve above-mentioned technical problem, the invention proposes a kind of raising solid state lithium battery silicon based anode material performances
Method, can be effectively suppressed volume expansion of the negative electrode material in charging and discharging lithium battery cyclic process, and conductivity is high.
The specific technical solution of the present invention is as follows:
A method of improving solid state lithium battery silicon based anode material performance, comprising the following steps:
A, aliphatic polyester mixture is mixed with trihydroxy first propane, dimethylbenzene, butyl acetate, then one side heating stirring is returned
Isophorone diisocyanate is added on one side in stream dehydration, fluorinated graphene is reacted, then is heated under inert gas protection
200 ~ 250 DEG C until solvent evaporating completely, is made fluoride glass state polyurethane;
B, aluminium chloride, metal simple-substance, silica-rich zeolite stick are added in the fluoride glass state polyurethane made from step a, then by body
System's sealing is stirred simultaneously held for some time, is washed after taking-up using hydrofluoric acid and deionized water repeatedly and remove remaining miscellaneous phase silicon,
The negative electrode material of fluorinated polyurethane load nano-silicon is made.
Preferably, in the step a, aliphatic polyester mixture is poly butylene succinate, polyglycolide, gathers in oneself
Two or more in ester, polytrimethylene carbonate.
Preferably, in the step a, 30 ~ 40 parts by weight of aliphatic polyester mixture, 5 ~ 8 parts by weight of trihydroxy first propane,
5 ~ 10 parts by weight of dimethylbenzene, 3 ~ 5 parts by weight of butyl acetate, 37 ~ 57 parts by weight of isophorone diisocyanate, fluorinated graphene 1-
3 parts by weight.
Preferably, in the step a, the temperature of reaction is 60 ~ 80 DEG C, and the time is 1 ~ 3h.
Preferably, in the step a, inert gas is one of argon gas, xenon, helium.
Preferably, in the step b, metal simple-substance is at least one of aluminium, magnesium.
Preferably, in the step b, 10 ~ 15 parts by weight of fluoride glass state polyurethane, 4 ~ 8 parts by weight of aluminium chloride, metal list
5 ~ 10 parts by weight of matter, 30 ~ 50 parts by weight of silica-rich zeolite stick.
Preferably, in the step b, the temperature of heat preservation is 80 ~ 90 DEG C, and the time is 10 ~ 15h.
Preferably, in the step b, the number of hydrofluoric acid wash is 2 ~ 3 times, and the number of deionized water washing is 3 ~ 5 times.
Pass through aliphatic polyester mixture and trihydroxy first propane, dimethylbenzene, butyl acetate, isophorone diisocyanate
Ester, fluorographite alkene reaction form the higher fluorinated polyurethane of decomposition temperature, with the nano crystal silicon particle synthesized in aluminium chloride
It is compound, form the negative electrode material of fluorinated polyurethane load nano single crystal silicon and metallic particles.Wherein, with the fluorination of high toughness
Polyurethane supporting silicon nanoparticles can inhibit the volume expansion of negative electrode material;And negative electrode material can be improved in the metallic particles on surface
Conductivity.
The method for a kind of raising solid state lithium battery silicon based anode material performance that above content of the present invention proposes, by aliphatic
Polyester mixture is stirred at reflux dehydration after mixing with trihydroxy first propane, dimethylbenzene, butyl acetate, two isocyanide of isophorone is added
After acid esters, fluorographite alkene reaction, heating is until solvent evaporating completely, obtains the poly- ammonia of fluoride glass state under inert gas protection
Ester, backward system in aluminium chloride, aluminium and silica-rich zeolite stick is added, be stirred and keep the temperature after system is sealed, will obtain later
The sample obtained takes out, and is washed repeatedly using hydrofluoric acid and deionized water and removes remaining miscellaneous phase silicon, obtains fluorinated polyurethane load
The negative electrode material of nano-silicon, obtains required negative electrode material, realizes and the performance of solid state lithium battery silicon based anode material is mentioned
It is high.
The invention has the benefit that
Nano single crystal silicon and metallic particles raising solid state lithium battery silicon based anode material are loaded using fluorinated polyurethane 1. proposing
The method of performance.
2. the present invention, as cathode, makes battery charge and discharge by the fluorinated polyurethane supporting silicon nanoparticles with high toughness
The volume expansion of silicon is fluorinated polyurethane and is absorbed in electric process, it is suppressed that the volume expansion of negative electrode material.
3. the present invention prepares silicon nanoparticle, remaining metallic particles is dispersed in inside fluorinated polyurethane,
Improve the conductivity of negative electrode material.
Specific embodiment
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
A, aliphatic polyester mixture is mixed with trihydroxy first propane, dimethylbenzene, butyl acetate, then one side heating stirring is returned
Isophorone diisocyanate, fluorinated graphene are added on one side and is reacted for stream dehydration, and the temperature of reaction is 70 DEG C, and the time is
2h, then it is heated to 225 DEG C under inert gas protection until solvent evaporating completely, is made fluoride glass state polyurethane;Wherein, rouge
35 parts by weight of fat adoption ester mixture, 6 parts by weight of trihydroxy first propane, 8 parts by weight of dimethylbenzene, 4 parts by weight of butyl acetate, different Buddhist
47 parts by weight of that ketone diisocyanate, 1 parts by weight of fluorinated graphene;Aliphatic polyester mixture be poly butylene succinate,
Polyglycolide, inert gas are argon gas;
B, aluminium chloride, metal simple-substance aluminium, silica-rich zeolite stick are added in the fluoride glass state polyurethane made from step a, then will
System sealing, is stirred and held for some time, the temperature of heat preservation are 85 DEG C, time 12h, after taking-up using hydrofluoric acid and go from
Sub- water washs repeatedly removes remaining miscellaneous phase silicon wherein, and the number of hydrofluoric acid wash is 3 times, and the number of deionized water washing is 4
It is secondary, the negative electrode material of fluorinated polyurethane load nano-silicon is made;Wherein, 10 parts by weight of fluoride glass state polyurethane, 6 weight of aluminium chloride
Measure part, 8 parts by weight of metal simple-substance, 50 parts by weight of silica-rich zeolite stick.
Embodiment 2
A, aliphatic polyester mixture is mixed with trihydroxy first propane, dimethylbenzene, butyl acetate, then one side heating stirring is returned
Isophorone diisocyanate, fluorinated graphene are added on one side and is reacted for stream dehydration, and the temperature of reaction is 65 DEG C, and the time is
2.5h, then it is heated to 210 DEG C under inert gas protection until solvent evaporating completely, is made fluoride glass state polyurethane;Wherein,
It is 32 parts by weight of aliphatic polyester mixture, 6 parts by weight of trihydroxy first propane, 6 parts by weight of dimethylbenzene, 3 parts by weight of butyl acetate, different
53 parts by weight of isophorone diisocyanate, 3 parts by weight of fluorinated graphene;Aliphatic polyester mixture is polycaprolactone, poly- carbonic acid
Propylidene ester, inert gas are xenon;
B, aluminium chloride, metal simple-substance magnesium, silica-rich zeolite stick are added in the fluoride glass state polyurethane made from step a, then will
System sealing, is stirred and held for some time, the temperature of heat preservation are 83 DEG C, time 14h, after taking-up using hydrofluoric acid and go from
Sub- water washs repeatedly removes remaining miscellaneous phase silicon, wherein the number of hydrofluoric acid wash is 2 times, and the number of deionized water washing is 4
It is secondary, the negative electrode material of fluorinated polyurethane load nano-silicon is made;Wherein, 15 parts by weight of fluoride glass state polyurethane, 5 weight of aluminium chloride
Measure part, 7 parts by weight of metal simple-substance, 45 parts by weight of silica-rich zeolite stick.
Embodiment 3
A, aliphatic polyester mixture is mixed with trihydroxy first propane, dimethylbenzene, butyl acetate, then one side heating stirring is returned
Isophorone diisocyanate, fluorinated graphene are added on one side and is reacted for stream dehydration, and the temperature of reaction is 60 DEG C, and the time is
3h, then it is heated to 200 DEG C under inert gas protection until solvent evaporating completely, is made fluoride glass state polyurethane;Wherein, rouge
30 parts by weight of fat adoption ester mixture, 5 parts by weight of trihydroxy first propane, 5 parts by weight of dimethylbenzene, 3 parts by weight of butyl acetate, different Buddhist
57 parts by weight of that ketone diisocyanate, 3 parts by weight of fluorinated graphene;Aliphatic polyester mixture be polyglycolide, polycaprolactone,
Inert gas is helium;
B, aluminium chloride, metal simple-substance aluminium, silica-rich zeolite stick are added in the fluoride glass state polyurethane made from step a, then will
System sealing, is stirred and held for some time, the temperature of heat preservation are 80 DEG C, time 15h, after taking-up using hydrofluoric acid and go from
Sub- water washs repeatedly removes remaining miscellaneous phase silicon, wherein the number of hydrofluoric acid wash is 2 times, and the number of deionized water washing is 3
It is secondary, the negative electrode material of fluorinated polyurethane load nano-silicon is made;Wherein, 12 parts by weight of fluoride glass state polyurethane, 4 weight of aluminium chloride
Measure part, 5 parts by weight of metal simple-substance, 45 parts by weight of silica-rich zeolite stick.
Embodiment 4
A, aliphatic polyester mixture is mixed with trihydroxy first propane, dimethylbenzene, butyl acetate, then one side heating stirring is returned
Isophorone diisocyanate, fluorinated graphene are added on one side and is reacted for stream dehydration, and the temperature of reaction is 75 DEG C, and the time is
1.5h, then it is heated to 240 DEG C under inert gas protection until solvent evaporating completely, is made fluoride glass state polyurethane;Wherein,
It is 37 parts by weight of aliphatic polyester mixture, 7 parts by weight of trihydroxy first propane, 9 parts by weight of dimethylbenzene, 5 parts by weight of butyl acetate, different
42 parts by weight of isophorone diisocyanate, 3 parts by weight of fluorinated graphene;Aliphatic polyester mixture is poly-succinic acid-butanediol
Ester, polytrimethylene carbonate, inert gas are argon gas;
B, aluminium chloride, metal simple-substance magnesium, silica-rich zeolite stick are added in the fluoride glass state polyurethane made from step a, then will
System sealing, is stirred and held for some time, the temperature of heat preservation are 88 DEG C, time 11h, after taking-up using hydrofluoric acid and go from
Sub- water washs repeatedly removes remaining miscellaneous phase silicon, wherein the number of hydrofluoric acid wash is 3 times, and the number of deionized water washing is 4
It is secondary, the negative electrode material of fluorinated polyurethane load nano-silicon is made;Wherein, 10 parts by weight of fluoride glass state polyurethane, 7 weight of aluminium chloride
Measure part, 9 parts by weight of metal simple-substance, 44 parts by weight of silica-rich zeolite stick.
Embodiment 5
A, aliphatic polyester mixture is mixed with trihydroxy first propane, dimethylbenzene, butyl acetate, then one side heating stirring is returned
Isophorone diisocyanate, fluorinated graphene are added on one side and is reacted for stream dehydration, and the temperature of reaction is 80 DEG C, and the time is
1h, then it is heated to 250 DEG C under inert gas protection until solvent evaporating completely, is made fluoride glass state polyurethane;Wherein, rouge
It is 40 parts by weight of fat adoption ester mixture, 8 parts by weight of trihydroxy first propane, 10 parts by weight of dimethylbenzene, 5 parts by weight of butyl acetate, different
37 parts by weight of isophorone diisocyanate, 3 parts by weight of fluorinated graphene;Aliphatic polyester mixture is poly-succinic acid-butanediol
Ester, polyglycolide, polycaprolactone, inert gas are xenon;
B, aluminium chloride, metal simple-substance aluminium, silica-rich zeolite stick are added in the fluoride glass state polyurethane made from step a, then will
System sealing, is stirred and held for some time, the temperature of heat preservation are 90 DEG C, time 10h, after taking-up using hydrofluoric acid and go from
Sub- water washs repeatedly removes remaining miscellaneous phase silicon.Wherein, the number of hydrofluoric acid wash is 3 times, and the number of deionized water washing is 5
It is secondary, the negative electrode material of fluorinated polyurethane load nano-silicon is made;Wherein, 12 parts by weight of fluoride glass state polyurethane, 8 weight of aluminium chloride
Measure part, 10 parts by weight of metal simple-substance, 50 parts by weight of silica-rich zeolite stick.
Comparative example 1
A, aliphatic polyester mixture is mixed with trihydroxy first propane, dimethylbenzene, butyl acetate, then one side heating stirring is returned
Isophorone diisocyanate is added on one side and is reacted for stream dehydration, and the temperature of reaction is 80 DEG C, time 1h, then in inertia
250 DEG C are heated under gas shield until solvent evaporating completely, is made fluoride glass state polyurethane;Wherein, aliphatic polyester is mixed
Fit 40 parts by weight, 8 parts by weight of trihydroxy first propane, 10 parts by weight of dimethylbenzene, 5 parts by weight of butyl acetate, isophorone two are different
37 parts by weight of cyanate;Aliphatic polyester mixture is poly butylene succinate, polyglycolide, polycaprolactone, inert gas
For xenon;
B, aluminium chloride, metal simple-substance aluminium, silica-rich zeolite stick are added in the fluoride glass state polyurethane made from step a, then will
System sealing, is stirred and held for some time, the temperature of heat preservation are 90 DEG C, time 10h, after taking-up using hydrofluoric acid and go from
Sub- water washs repeatedly removes remaining miscellaneous phase silicon.Wherein, the number of hydrofluoric acid wash is 3 times, and the number of deionized water washing is 5
It is secondary, the negative electrode material of fluorinated polyurethane load nano-silicon is made;Wherein, 12 parts by weight of fluoride glass state polyurethane, 8 weight of aluminium chloride
Measure part, 10 parts by weight of metal simple-substance, 50 parts by weight of silica-rich zeolite stick.
Fluorinated graphene is not added for comparative example, fails to be fluorinated polyurethane, and toughness and inhibition dilatancy, electrical conductance drop
It is low.
Negative electrode material made from the method for above-described embodiment 1 ~ 5 and comparative example 1 tests its cubical expansivity, conductivity, surveys
The method or condition for sign of taking temperature are as follows:
Cubical expansivity: electrode slice is made in the negative electrode material that method of the invention obtains, initial volume is measured, is transferred to gloves
It is that button cell is made to electrode with lithium metal, it is anti-that electrolyte, which is the LiPF6/EC:DMC (1:1, V/V) of 1mol/L, in case
Clamping formula inside battery poor contact is added foaming nickel sheet in negative pole end and makees filler, carries out charge and discharge cycles test, charge and discharge
System are as follows: charging and discharging currents density 0.25mA/cm2, 0.02 ~ 1.5V of charging/discharging voltage, respectively at 500 times, 1000 times and 2000
The volume that test negative electrode material is taken out when secondary calculates cubical expansivity according to volume ratio.
Conductivity: the conductivity that conductivity measurement measures negative electrode material produced by the present invention is directlyed adopt.
The results are shown in Table 1.
Table 1:
Claims (9)
1. a kind of method for improving solid state lithium battery silicon based anode material performance, it is characterised in that: the following steps are included:
A, aliphatic polyester mixture is mixed with trihydroxy first propane, dimethylbenzene, butyl acetate, then one side heating stirring is returned
Isophorone diisocyanate is added on one side in stream dehydration, fluorinated graphene is reacted, then is heated under inert gas protection
200 ~ 250 DEG C, until solvent evaporating completely, is made fluoride glass state polyurethane;
B, aluminium chloride, metal simple-substance, silica-rich zeolite stick are added in the fluoride glass state polyurethane made from step a, then by body
System's sealing is stirred simultaneously held for some time, is washed after taking-up using hydrofluoric acid and deionized water repeatedly and remove remaining miscellaneous phase silicon,
The negative electrode material of fluorinated polyurethane load nano-silicon is made.
2. a kind of method for improving solid state lithium battery silicon based anode material performance according to claim 1, it is characterised in that: institute
It states in step a, aliphatic polyester mixture is poly butylene succinate, polyglycolide, polycaprolactone, polytrimethylene carbonate
In two or more.
3. a kind of method for improving solid state lithium battery silicon based anode material performance according to claim 1, it is characterised in that: institute
State in step a, 30 ~ 40 parts by weight of aliphatic polyester mixture, 5 ~ 8 parts by weight of trihydroxy first propane, 5 ~ 10 parts by weight of dimethylbenzene,
3 ~ 5 parts by weight of butyl acetate, 37 ~ 57 parts by weight of isophorone diisocyanate, fluorinated graphene 1-3 parts by weight.
4. a kind of method for improving solid state lithium battery silicon based anode material performance according to claim 1, it is characterised in that: institute
It states in step a, the temperature of reaction is 60 ~ 80 DEG C, and the time is 1 ~ 3h.
5. a kind of method for improving solid state lithium battery silicon based anode material performance according to claim 1, it is characterised in that: institute
It states in step a, inert gas is one of argon gas, xenon, helium.
6. a kind of method for improving solid state lithium battery silicon based anode material performance according to claim 1, it is characterised in that: institute
It states in step b, metal simple-substance is at least one of aluminium, magnesium.
7. a kind of method for improving solid state lithium battery silicon based anode material performance according to claim 1, it is characterised in that: institute
It states in step b, 10 ~ 15 parts by weight of fluoride glass state polyurethane, 4 ~ 8 parts by weight of aluminium chloride, 5 ~ 10 parts by weight of metal simple-substance, high silicon
30 ~ 50 parts by weight of zeolite stick.
8. a kind of method for improving solid state lithium battery silicon based anode material performance according to claim 1, it is characterised in that: institute
It states in step b, the temperature of heat preservation is 80 ~ 90 DEG C, and the time is 10 ~ 15h.
9. a kind of method for improving solid state lithium battery silicon based anode material performance according to claim 1, it is characterised in that: institute
It states in step b, the number of hydrofluoric acid wash is 2 ~ 3 times, and the number of deionized water washing is 3 ~ 5 times.
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CN112397718A (en) * | 2020-11-06 | 2021-02-23 | 开封大学 | Self-healing silicon-based negative electrode material of lithium ion battery and preparation method thereof |
CN112397718B (en) * | 2020-11-06 | 2022-08-09 | 开封大学 | Self-healing silicon-based negative electrode material of lithium ion battery and preparation method thereof |
CN112881922A (en) * | 2020-12-30 | 2021-06-01 | 天津国安盟固利新材料科技股份有限公司 | Button lithium battery and method for detecting assembling quality of button lithium battery |
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