CN108346820A - A kind of inhibition lithium dendrite growth cobalt acid lithium electrolyte preparation method - Google Patents
A kind of inhibition lithium dendrite growth cobalt acid lithium electrolyte preparation method Download PDFInfo
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- CN108346820A CN108346820A CN201810052577.5A CN201810052577A CN108346820A CN 108346820 A CN108346820 A CN 108346820A CN 201810052577 A CN201810052577 A CN 201810052577A CN 108346820 A CN108346820 A CN 108346820A
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- carbon nitrogen
- cobalt acid
- lightweight carbon
- lithium
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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
- H01M10/056—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes
- H01M10/0561—Accumulators with non-aqueous electrolyte characterised by the materials used as electrolytes, e.g. mixed inorganic/organic electrolytes the electrolyte being constituted of inorganic materials only
- H01M10/0562—Solid materials
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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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/42—Methods or arrangements for servicing or maintenance of secondary cells or secondary half-cells
- H01M10/4235—Safety or regulating additives or arrangements in electrodes, separators or electrolyte
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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
- H01M2300/00—Electrolytes
- H01M2300/0017—Non-aqueous electrolytes
- H01M2300/0065—Solid electrolytes
- H01M2300/0068—Solid electrolytes inorganic
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- 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 present invention relates to a kind of inhibition lithium dendrite growth cobalt acid lithium electrolyte preparing methods, the method is simple to operation, it is at low cost, it takes short, the method adulterates Nb ions in positive electrode, same order elements are carried out to the Co ionic sites in positive electrode lattice, changes lattice parameter, obtains the inorganic electrolyte of excellent electrochemical performance；It using lightweight carbon nitrogen polymer as filler in the present invention, is uniformly mixed with electrolyte, forms solid electrolyte, can be used for inhibiting the growth of dendrite in lithium metal battery.
Description
Technical field
The present invention relates to technical field of lithium batteries, and in particular to a kind of preparation inhibiting lithium dendrite growth cobalt acid lithium electrolyte
Method.
Background technology
LiCoO2The main positive electrode of current commercial Li-ion battery, but it there are it is expensive, be unfavorable for
Environmental protection, the disadvantages such as specific capacity is low.LiNbO2The positive electrode for adulterating Co elements is provided with LiNbO simultaneously2The higher electric discharge ratio of material
Capacity, and the layer structure of material is stabilized, the cyclical stability of material is enhanced, but there is also overcharging resisting energy for this material
The defects of force difference, thermal stability are poor, electric discharge irreversible capacity is higher for the first time.
In addition, the commercialized most important factor of safety problem lithium battery, main crux is sulphur lithium ion in cyclic process
Easily form Li dendrite.When the growth of dendrite is uncontrollable, diaphragm is easily pierced through, internal short-circuit of battery occurs, then causes quick-fried
It is fried.Organic electrolyte is substituted using solid electrolyte, the security risk of lithium battery can be solved.
To improve the security effectiveness of lithium ion battery, liquid electrolyte has been substituted using relatively reliable all solid state electrolyte
At important selection to solve this problem.Compared to the electrolyte that additive is reinforced, solid-state or quasi-solid electrolyte have
Better mechanical strength is expected to have better inhibiting effect to Li dendrite.However the usual conductivity of all solid state electrolyte is not
Enough, poor interfacial contact problem is also difficult to solve.Quasi-solid electrolyte has the conductivity similar with electrolyte and good
Interface wetting power, it is considered to be one of the optimal candidate of novel lithium metal cell electrolyte.Quasi-solid electrolyte often will
Polymer backbone (such as polyethylene glycol oxide) or inorganic nanoparticles (such as nanometer titanium dioxide is added in non-aqueous electrolyte or lithium salts
Silicon) filler cures.The quasi- solid state of electrolyte not but not leads to the significant decrease of conductivity, in some cases,
Due to space charge effect, its conductivity may be increased instead.However, the machine of traditional polymer film based on polyethylene glycol oxide
Tool intensity is weaker, cannot effectively inhibit Li dendrite, it is often necessary to which adding inorganic nano particle is improved.
Invention content
The present invention provides a kind of inhibition lithium dendrite growth cobalt acid lithium electrolyte preparation method, and the method is simply easily grasped
Make, at low cost, time-consuming short, the method adulterates Nb ions in positive electrode, to the Co ionic sites in positive electrode lattice
Same order elements are carried out, changes lattice parameter, obtains the inorganic electrolyte of excellent electrochemical performance；It is poly- with lightweight carbon nitrogen in the present invention
Object is closed as filler, is uniformly mixed with electrolyte, solid electrolyte is formed, can be used for inhibiting the life of dendrite in lithium metal battery
It is long.
To achieve the goals above, the present invention provides a kind of inhibition lithium dendrite growth cobalt acid lithium electrolyte preparation method,
This method comprises the following steps：
（1）It prepares niobium and is modified cobalt acid lithium
The chemical formula that the niobium is modified cobalt acid lithium is LiCo1-x-yFexNbyO2, wherein：X=0.12-0.15, y=0.02-0.03, according to
The mole of Li, Fe, Nb, Co in above-mentioned chemical formula weigh lithium carbonate, ferric acetate, niobium oxide and cobalt oxide, with suitable water
It is decentralized medium with ethyl alcohol, wet ball grinding batch mixing, the slurry mixed is carried out to the raw material weighed；The slurry that will be mixed
It is spray-dried, obtains cobalt acid lithium precursor；
Plasma-arc is imposed under reducing atmosphere to precursor, so that reaction powder is melted, plasma electric arc voltage 20-
40kV, plasma electric arc current 500-1000A；
Frit reaction powder is spurted into reducibility gas in cooling device, particle is crushed and screened after cooling, screening obtains
Granular size be 5-10 microns of niobium modified cobalt acid lithium material；The wherein nozzle diameter 2-5mm for injection；
（2）Prepare lightweight carbon nitrogen polymer filler
Melamine 2-2.5 parts by weight are weighed, are dissolved in the dimethyl sulfoxide (DMSO) of 100-125 parts by weight；It takes equal with melamine
The cyanuric acid of parts by weight is dissolved in the dimethyl sulfoxide (DMSO) of 45-50 parts by weight mL, is stirred at each 65-75 DEG C of leisure of two kinds of solution,
It after uniform dissolution, is mutually mixed, then is maintained at 65-75 DEG C and stirs 15-20 minutes, after being then allowed to stand, mixed liquor is centrifuged, is washed
It washs, it is dry, white powder is obtained, white powder is put into ceramic crucible, is placed in tube furnace, in the atmosphere of high-purity argon gas
In, sintering obtains lightweight carbon nitrogen polymer filler, and the grain size of the lightweight carbon nitrogen polymer filler is 1.5-2.5 μm；
（3）Network skeleton is prepared by electrostatic spinning technique
Lightweight carbon nitrogen polymer filler and polyvinylpyrrolidone are weighed, the mass ratio of the two is 1：(1-2), then by polyethylene
Pyrrolidones is added in ethylene glycol, in a water bath heating and magnetic agitation, and the polyvinylpyrrolidone that viscous consistency is made is molten
Liquid；Lightweight carbon nitrogen polymer filler is added in polyvinylpyrrolidonesolution solution again, ultrasonic disperse is uniform, and at 65-75 DEG C
Constant temperature is swollen 2-4h, the uniform lightweight carbon nitrogen polymer filler/polyvinylpyrrolidone/ethylene glycol spinning solution of forming component；It will
Lightweight carbon nitrogen polymer filler/polyvinylpyrrolidone/ethylene glycol spinning solution is fitted into device for spinning, by electrostatic spinning technique
It is prepared into lightweight carbon nitrogen polymer filler/high polymer nano fiber can be spun；By the nanofiber by 820-900 DEG C of sintering, obtain
To ceramic nano line network skeleton；
（4）The niobium modified cobalt acid lithium material is combined on ceramic nano line network skeleton by the method for magnetron sputtering, is obtained
To thin film solid state electrolyte.
Preferably, step（3）In, the actual conditions of magnetron sputtering are：Sputtering power is 75-90W, sputtering time 10-
15min；Operating pressure：0.5Pa, atmosphere are nitrogen, substrate temperature：100-200℃.
The invention has the advantages that and remarkable result：
（1）The plasma high-temperature fusion technology that the present invention uses, is a kind of new technique developed in recent years, and principle is：
After vacuum system preset vacuum, in melt chamber and cooling chamber introduce plasma working gas (generally inert gas, it is lazy
Property gas be one or more of helium, neon and argon gas, the inert gas in melt chamber and cooling chamber can be it is same,
Can also be mixed gas), voltage is added between the two poles of the earth, the inert gas plasma moment heating in melt chamber, temperature
Thousands of degree can be reached, the powder in addition feed appliance can be made to be rapidly reached molten condition, plasma high-speed motion, particle
Between can occur sharp impacts, the material under the required molten condition of in-time generatin, by be ejected come gas take out of
Melt chamber enters in cooling chamber, and required cobalt acid lithium material is obtained after cooling.This method can make cobalt acid lithium material in moment
It is formed, and continuous production can be formed.
（2）The method adulterates Nb ions in positive electrode, is carried out to the Co ionic sites in positive electrode lattice same
Crystalline substance substitution, changes lattice parameter, obtains the positive electrode of excellent electrochemical performance.
（3）It using lightweight carbon nitrogen polymer as filler in the present invention, is uniformly mixed with electrolyte, forms solid state electrolysis
Matter can be used for inhibiting the growth of dendrite in lithium metal battery.
Specific implementation mode
Embodiment one
The chemical formula that the present embodiment niobium is modified cobalt acid lithium is LiCo0.86Fe0.12Nb0.02O2, according in above-mentioned chemical formula Li, Fe,
The mole of Nb, Co weigh lithium carbonate, ferric acetate, niobium oxide and cobalt oxide, using suitable water and ethyl alcohol as decentralized medium, symmetrically
The raw material taken carries out wet ball grinding batch mixing, the slurry mixed；The slurry mixed is spray-dried, cobalt acid is obtained
Lithium precursor.
Plasma-arc is imposed under reducing atmosphere to precursor, so that reaction powder is melted, plasma electric arc voltage
20kV, plasma electric arc current 500A；Frit reaction powder is spurted into reducibility gas in cooling device, it is cooling after to
Grain crushes and screens, the niobium modified cobalt acid lithium material that the granular size sieved is 5 microns；The wherein nozzle for injection
Diameter 2mm.
Melamine 2-2.5 parts by weight are weighed, are dissolved in the dimethyl sulfoxide (DMSO) of 100-125 parts by weight；It takes and melamine
The cyanuric acid of equal weight part is dissolved in the dimethyl sulfoxide (DMSO) of 45-50 parts by weight mL, is stirred at each 65-75 DEG C of leisure of two kinds of solution
Mix, after uniform dissolution, be mutually mixed, then be maintained at 65-75 DEG C and stir 15-20 minutes, after being then allowed to stand, by mixed liquor from
The heart washs, dry, obtains white powder, white powder is put into ceramic crucible, be placed in tube furnace, in high-purity argon gas
In atmosphere, sintering obtains lightweight carbon nitrogen polymer filler, and the grain size of the lightweight carbon nitrogen polymer filler is 1.5-2.5 μm.
Lightweight carbon nitrogen polymer filler and polyvinylpyrrolidone are weighed, the mass ratio of the two is 1：1, then by polyethylene
Pyrrolidones is added in ethylene glycol, in a water bath heating and magnetic agitation, and the polyvinylpyrrolidone that viscous consistency is made is molten
Liquid；Lightweight carbon nitrogen polymer filler is added in polyvinylpyrrolidonesolution solution again, ultrasonic disperse is uniform, and in 65 DEG C of constant temperature
It is swollen 2h, the uniform lightweight carbon nitrogen polymer filler/polyvinylpyrrolidone/ethylene glycol spinning solution of forming component；By lightweight carbon
Nitrogen polymer filler/polyvinylpyrrolidone/ethylene glycol spinning solution is fitted into device for spinning, is prepared by electrostatic spinning technique
Lightweight carbon nitrogen polymer filler/high polymer nano fiber can be spun；By the nanofiber by 820 DEG C of sintering, ceramic nano is obtained
Line network skeleton；
The niobium modified cobalt acid lithium material is combined on ceramic nano line network skeleton by the method for magnetron sputtering, is obtained thin
Film solid electrolyte.The actual conditions of magnetron sputtering are：Sputtering power is 75W, sputtering time 10min；Operating pressure：
0.5Pa, atmosphere are nitrogen, substrate temperature：100℃.
Embodiment two
The chemical formula that the present embodiment niobium is modified cobalt acid lithium is LiCo0.82Fe0.15Nb0.03O2.According in above-mentioned chemical formula Li, Fe,
The mole of Nb, Co weigh lithium carbonate, ferric acetate, niobium oxide and cobalt oxide, using suitable water and ethyl alcohol as decentralized medium, symmetrically
The raw material taken carries out wet ball grinding batch mixing, the slurry mixed；The slurry mixed is spray-dried, cobalt acid is obtained
Lithium precursor.
Plasma-arc is imposed under reducing atmosphere to precursor, so that reaction powder is melted, plasma electric arc voltage
40kV, plasma electric arc current 1000A；Frit reaction powder is spurted into reducibility gas in cooling device, it is right after cooling
Particle crushes and screens, the niobium modified cobalt acid lithium material that the granular size sieved is 10 microns；For injection described in wherein
Nozzle diameter 5mm.
Melamine 2-2.5 parts by weight are weighed, are dissolved in the dimethyl sulfoxide (DMSO) of 100-125 parts by weight；It takes and melamine
The cyanuric acid of equal weight part is dissolved in the dimethyl sulfoxide (DMSO) of 45-50 parts by weight mL, is stirred at each 65-75 DEG C of leisure of two kinds of solution
Mix, after uniform dissolution, be mutually mixed, then be maintained at 65-75 DEG C and stir 15-20 minutes, after being then allowed to stand, by mixed liquor from
The heart washs, dry, obtains white powder, white powder is put into ceramic crucible, be placed in tube furnace, in high-purity argon gas
In atmosphere, sintering obtains lightweight carbon nitrogen polymer filler, and the grain size of the lightweight carbon nitrogen polymer filler is 1.5-2.5 μm.
Lightweight carbon nitrogen polymer filler and polyvinylpyrrolidone are weighed, the mass ratio of the two is 1：2, then by polyethylene
Pyrrolidones is added in ethylene glycol, in a water bath heating and magnetic agitation, and the polyvinylpyrrolidone that viscous consistency is made is molten
Liquid；Lightweight carbon nitrogen polymer filler is added in polyvinylpyrrolidonesolution solution again, ultrasonic disperse is uniform, and in 75 DEG C of constant temperature
It is swollen 4h, the uniform lightweight carbon nitrogen polymer filler/polyvinylpyrrolidone/ethylene glycol spinning solution of forming component；By lightweight carbon
Nitrogen polymer filler/polyvinylpyrrolidone/ethylene glycol spinning solution is fitted into device for spinning, is prepared by electrostatic spinning technique
Lightweight carbon nitrogen polymer filler/high polymer nano fiber can be spun；By the nanofiber by 900 DEG C of sintering, ceramic nano is obtained
Line network skeleton；
The niobium modified cobalt acid lithium material is combined on ceramic nano line network skeleton by the method for magnetron sputtering, is obtained thin
Film solid electrolyte.The actual conditions of magnetron sputtering are：Sputtering power is 90W, sputtering time 15min；Operating pressure：
0.5Pa, atmosphere are nitrogen, substrate temperature：200℃.
Claims (2)
1. a kind of inhibition lithium dendrite growth cobalt acid lithium electrolyte preparation method, this method comprises the following steps：
（1）It prepares niobium and is modified cobalt acid lithium
The chemical formula that the niobium is modified cobalt acid lithium is LiCo1-x-yFexNbyO2, wherein：X=0.12-0.15, y=0.02-0.03, according to
The mole of Li, Fe, Nb, Co in above-mentioned chemical formula weigh lithium carbonate, ferric acetate, niobium oxide and cobalt oxide, with suitable water
It is decentralized medium with ethyl alcohol, wet ball grinding batch mixing, the slurry mixed is carried out to the raw material weighed；The slurry that will be mixed
It is spray-dried, obtains cobalt acid lithium precursor；
Plasma-arc is imposed under reducing atmosphere to precursor, so that reaction powder is melted, plasma electric arc voltage 20-
40kV, plasma electric arc current 500-1000A；
Frit reaction powder is spurted into reducibility gas in cooling device, particle is crushed and screened after cooling, screening obtains
Granular size be 5-10 microns of niobium modified cobalt acid lithium material；The wherein nozzle diameter 2-5mm for injection；
（2）Prepare lightweight carbon nitrogen polymer filler
Melamine 2-2.5 parts by weight are weighed, are dissolved in the dimethyl sulfoxide (DMSO) of 100-125 parts by weight；It takes equal with melamine
The cyanuric acid of parts by weight is dissolved in the dimethyl sulfoxide (DMSO) of 45-50 parts by weight mL, is stirred at each 65-75 DEG C of leisure of two kinds of solution,
It after uniform dissolution, is mutually mixed, then is maintained at 65-75 DEG C and stirs 15-20 minutes, after being then allowed to stand, mixed liquor is centrifuged, is washed
It washs, it is dry, white powder is obtained, white powder is put into ceramic crucible, is placed in tube furnace, in the atmosphere of high-purity argon gas
In, sintering obtains lightweight carbon nitrogen polymer filler, and the grain size of the lightweight carbon nitrogen polymer filler is 1.5-2.5 μm；
（3）Network skeleton is prepared by electrostatic spinning technique
Lightweight carbon nitrogen polymer filler and polyvinylpyrrolidone are weighed, the mass ratio of the two is 1：(1-2), then by polyethylene
Pyrrolidones is added in ethylene glycol, in a water bath heating and magnetic agitation, and the polyvinylpyrrolidone that viscous consistency is made is molten
Liquid；Lightweight carbon nitrogen polymer filler is added in polyvinylpyrrolidonesolution solution again, ultrasonic disperse is uniform, and at 65-75 DEG C
Constant temperature is swollen 2-4h, the uniform lightweight carbon nitrogen polymer filler/polyvinylpyrrolidone/ethylene glycol spinning solution of forming component；It will
Lightweight carbon nitrogen polymer filler/polyvinylpyrrolidone/ethylene glycol spinning solution is fitted into device for spinning, by electrostatic spinning technique
It is prepared into lightweight carbon nitrogen polymer filler/high polymer nano fiber can be spun；By the nanofiber by 820-900 DEG C of sintering, obtain
To ceramic nano line network skeleton；
（4）The niobium modified cobalt acid lithium material is combined on ceramic nano line network skeleton by the method for magnetron sputtering, is obtained
To thin film solid state electrolyte.
2. the method as described in claim 1, which is characterized in that step（3）In, the actual conditions of magnetron sputtering are：Sputter work(
Rate is 75-90W, sputtering time 10-15min；Operating pressure：0.5Pa, atmosphere are nitrogen, substrate temperature：100-200℃.
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Cited By (2)
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| CN110592807A (en) * | 2019-09-18 | 2019-12-20 | 宁波大学 | Thin film material for inhibiting growth of lithium dendrite and preparation method thereof |
| CN114373984A (en) * | 2021-12-08 | 2022-04-19 | 湘潭大学 | Solid electrolyte, preparation method thereof and lithium ion battery |
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Application publication date: 20180731 |