CN108493485A - A kind of preparation method of high power capacity high safety solid state lithium battery - Google Patents
A kind of preparation method of high power capacity high safety solid state lithium battery Download PDFInfo
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- CN108493485A CN108493485A CN201810272524.4A CN201810272524A CN108493485A CN 108493485 A CN108493485 A CN 108493485A CN 201810272524 A CN201810272524 A CN 201810272524A CN 108493485 A CN108493485 A CN 108493485A
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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
- H01M10/058—Construction or manufacture
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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
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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
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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
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P70/00—Climate change mitigation technologies in the production process for final industrial or consumer products
- Y02P70/50—Manufacturing or production processes characterised by the final manufactured product
Abstract
The present invention relates to a kind of preparation methods of high power capacity high safety solid state lithium battery, are prepared by electrolyte of solid electrolyte as negative electrode active material using liquid metal compound made of liquid metal nano particle, carbon nanotube and graphene.The negative electrode active material of the solid state lithium battery of the present invention uses liquid metal, carbon nanotube and graphene, and liquid metal tin and gallium possess high-energy density, can provide high power capacity for solid lithium ion battery, are the ideal materials of high-energy-density lithium battery;Construction three-dimensional framework makes lithium battery have higher ionic conductivity after carbon nanotube and graphene is added, and it is complicated, there is good mechanical performance, the Li dendrite that negative metal lithium surface can be inhibited to be formed, the security performance for improving battery, increases the cycle life and stability of battery;Using solid electrolyte, can high degree reduction interface resistance.
Description
Technical field
The invention belongs to green energy-storing technical fields, and in particular to a kind of preparation side of high power capacity high safety solid state lithium battery
Method.
Background technology
In in the past few decades, with the development of the times, on an electronic device increasingly for the requirement of energy density
It is high.Lithium ion battery becomes most perspective electric energy energy storage device because having high-conversion rate and environmental-friendly performance, separately exists
Electric vehicle, small-sized transmission facility and Portable movable energy storing devices lithium ion battery also have great development prospect.However,
The energy density of lithium ion battery still remains mismatch in volume and gravity;For the equipment for having battery requirements, most
What it is with challenge is the high-energy density of electrode material, e.g., the decaying of capacity, stability of circulating battery etc..
Invention content
Technical problem to be solved by the invention is to provide a kind of preparation method of high power capacity high safety solid state lithium battery, with
Overcome above-mentioned deficiency in the prior art.
The technical solution that the present invention solves above-mentioned technical problem is as follows:
A kind of preparation method of high power capacity high safety solid state lithium battery, with liquid metal nano particle, carbon nanotube and stone
Liquid metal compound made of black alkene is negative electrode active material, is prepared by electrolyte of solid electrolyte.
Further:The preparation method of the liquid metal compound is:
Step S1:It is 22 in mass ratio:3 weigh liquid metals tin and liquid metals gallium, and degassed ethanol is added thereto
Mercaptan solvent, ultrasonotomography, is made liquid metal nano particle later;
Step S2:The liquid metal nano particle and carbon nanotube are added to formation mixture I in absolute ethyl alcohol, then
The graphene being dissolved in ethyl alcohol is added to formation mixture II in the mixture I, the mixture II is placed in reaction kettle
Middle reaction 5-7h reacts 3-5h at a temperature of 900 DEG C later, is that synthesizing liquid metal is multiple after its cooled to room temperature
Close object.
Further:Ultrasonotomography is implemented as described in the step S1:The ultrasound 1h in 50 DEG C of environment.
Further:In the step S2 before adding graphene into the mixture I, to I ultrasound of the mixture
1h。
The advantageous effect of above-mentioned further scheme is:It can get more uniform suspension.
Further:Using before carbon nanotube in the step S2, using 2.6mol/L nitric acid to carbon nanotube into
Row reflow treatment.
The advantageous effect of above-mentioned further scheme is:Carbon nanotube can be purified.
Further:The negative plate of the solid state lithium battery is with mass ratio for 8:1:1 liquid metal compound, acetylene black and
PVDF is prepared.
The beneficial effects of the invention are as follows:1, negative electrode active material uses liquid metal, carbon nanotube and graphene, liquid gold
Belong to tin and gallium possesses high-energy density, high power capacity can be provided for solid lithium ion battery, be the ideal of high-energy-density lithium battery
Material;Three-dimensional framework is constructed after carbon nanotube and graphene is added, can effectively fix liquid metal nanoparticle, forms 3D
Spacial framework provides express passway for the migration of lithium ion, so that lithium battery is had higher ionic conductivity, and structure is multiple
It is miscellaneous, there is good mechanical performance, the migration of lithium ion in secondary lithium battery can be improved and inhibit negative metal lithium
The Li dendrite that surface is formed, improves the security performance of battery;The excellent self-healing ability of liquid metal tin and gallium makes electricity simultaneously
Pond is damaged smaller during high rate charge-discharge, increases the cycle life and stability of battery;2, using solid state electrolysis
Matter with replace diaphragm and liquid electrolyte, because the compatibility of solid electrolyte and cathode is good, can high degree reduction interface electricity
Resistance, reduces the in-fighting of battery;Another solid electrolyte can avoid the infiltration and loss of liquid electrolyte, thus have higher finished product
Rate reduces production cost;Make the battery prepared that there is higher energy density and cycle life using solid electrolyte simultaneously;
The electrochemical window mouth width of another solid electrolyte, up to 5V disclosure satisfy that the battery applications of some high voltage systems, can meet more
The requirement more applied.
Description of the drawings
Fig. 1 is the structural schematic diagram of liquid metal and solid electrolyte all-solid lithium-ion battery;
Fig. 2 is that the SEM of liquid metal nano particle schemes;
Fig. 3 a are SEM figure of the liquid metal cathode composite between charge-discharge test;
Fig. 3 b are that liquid metal cathode composite completes the SEM figures after charge-discharge test;
Fig. 3 c are the SEM figures after liquid metal compound completes charge-discharge test and stands a period of time;
Fig. 4 is the SEM figures for the 3d space structure that liquid metal nano particle, carbon nanotube and graphene are constituted;
Fig. 5 is cyclic voltammogram of the liquid metal compound before and after charge and discharge;
Fig. 6 a are a kind of specific volume spirogram of the liquid metal compound in high power capacity high safety solid state lithium battery;
Fig. 6 b are the high rate performance and cyclicity of the liquid metal compound in a kind of high power capacity high safety solid state lithium battery
It can figure;
Fig. 6 c are the high rate performance and cycle performance figure of the graphene in a kind of high power capacity high safety solid state lithium battery;
Fig. 6 d are the high rate performance and cycle performance figure of the carbon nanotube in a kind of high power capacity high safety solid state lithium battery;
Fig. 7 is the AC impedance figure after liquid metal compound and solid electrolyte assembled battery.
Specific implementation mode
The principle and features of the present invention will be described below with reference to the accompanying drawings, and the given examples are served only to explain the present invention, and
It is non-to be used to limit the scope of the present invention.
A kind of preparation method of high power capacity high safety solid state lithium battery, with liquid metal nano particle, carbon nanotube and stone
Liquid metal compound made of black alkene is negative electrode active material, is prepared by electrolyte of solid electrolyte.It is specific to prepare
Process and solid-state battery structure schematic diagram are as shown in Figure 1.
Further:The preparation method of the liquid metal compound is:
Step S1:It is 22 in mass ratio:3 weigh liquid metals tin and liquid metals gallium, and degassed ethanol is added thereto
Mercaptan solvent, ultrasonotomography, is made liquid metal nano particle later;Here degassed ethanol mercaptan refers to the second for removing oxygen
Alcohol mercaptan drives the oxygen wherein dissolved generally by inert gas such as argon gas, nitrogen etc. is passed through into solution;
Step S2:The liquid metal nano particle and carbon nanotube are added to formation mixture I in absolute ethyl alcohol, then
The graphene being dissolved in ethyl alcohol is added to formation mixture II in the mixture I, the mixture II is placed in reaction kettle
Middle reaction 5-7h reacts 3-5h at a temperature of 900 DEG C later, is that synthesizing liquid metal is multiple after its cooled to room temperature
Close object.Here graphene is prepared by reducing agent redox graphene, has good dispersibility.
Further:Ultrasonotomography is implemented as described in the step S1:The ultrasound 1h in 50 DEG C of environment.
Further:In the step S2 before adding graphene into the mixture I, to I ultrasound of the mixture
1h。
The advantageous effect of above-mentioned further scheme is:It can get more uniform suspension.
Further:Using before carbon nanotube in the step S2, using 2.6mol/L nitric acid to carbon nanotube into
Row reflow treatment.
The advantageous effect of above-mentioned further scheme is:Carbon nanotube can be purified.
Further:The negative plate of the solid state lithium battery is with mass ratio for 8:1:1 liquid metal compound, acetylene black and
PVDF is prepared.
The beneficial effects of the invention are as follows:1, negative electrode active material uses liquid metal, carbon nanotube and graphene, liquid gold
Belong to tin and gallium possesses high-energy density, high power capacity can be provided for solid lithium ion battery, be the ideal of high-energy-density lithium battery
Material;Three-dimensional framework is constructed after carbon nanotube and graphene is added, can effectively fix liquid metal nanoparticle, forms 3D
Spacial framework provides express passway for the migration of lithium ion, so that lithium battery is had higher ionic conductivity, and structure is multiple
It is miscellaneous, there is good mechanical performance, the migration of lithium ion in secondary lithium battery can be improved and inhibit negative metal lithium
The Li dendrite that surface is formed, improves the security performance of battery;The excellent self-healing ability of liquid metal tin and gallium makes electricity simultaneously
Pond is damaged smaller during high rate charge-discharge, increases the cycle life and stability of battery;2, using solid state electrolysis
Matter with replace diaphragm and liquid electrolyte, because the compatibility of solid electrolyte and cathode is good, can high degree reduction interface electricity
Resistance, reduces the in-fighting of battery;Another solid electrolyte can avoid the infiltration and loss of liquid electrolyte, thus have higher finished product
Rate reduces production cost;Make the battery prepared that there is higher energy density and cycle life using solid electrolyte simultaneously;
The electrochemical window mouth width of another solid electrolyte, up to 5V disclosure satisfy that the battery applications of some high voltage systems, can meet more
The requirement more applied.
Embodiment one, according to mass ratio 22:3 weigh liquid metal tin and liquid metal gallium in Ai Pengdao bottles, then add
Enter 1mmol/L degassed ethanols mercaptan as solvent, the ultrasound 1h at 50 DEG C, forms liquid metal nano particle, such as Fig. 2 institutes later
Show, prepared liquid metal particle is well dispersed, and particle size is uniform, can meet cell active materials requirement;
The carbon nanotube of the liquid metal nano particle of 60mg and 12mg is added to shape in the absolute ethyl alcohol of 0.5mL
Resulting mixture I;It is 1 hour ultrasonic to mixture I in order to obtain more uniform suspension;It is simultaneously the carbon for obtaining purer,
Before using carbon nanotube, the nitric acid of 2.6mol/L is first used to carry out reflow treatment to carbon nanotube;Mixture I is used later
Deionized water is cleaned repeatedly, and then the graphene of 4mg is dissolved in the ethyl alcohol of 2wt%, and 2wt% refers to mass percent and is
2%, and it is added to formation mixture II in mixture I;It is 10 minutes ultrasonic to mixture II, it is then sealed against in pyroreaction
6h is reacted in kettle at a temperature of 160 DEG C, reacts 4h at a temperature of 900 DEG C later, after its cooled to room temperature i.e.
Synthesizing liquid metal composite.Electronic scanner microscope observation is carried out to liquid metal compound, the results are shown in Figure 4, explanation
Product is dispersed in carbon material, and uniformity is fine.
Using liquid metal compound as negative electrode active material, with mass ratio for 8:1:1 liquid metal compound, acetylene black
It, using electrolytic salt and organic solvent as electrolyte, is negative with lithium piece to make negative plate using solid electrolyte as electrolyte with PVDF
Pole is assembled into the button cell of CR2032 formulas in the glove box full of argon gas;Wherein, the organic solvent is:Volume ratio is 1:
The mixed solution of 1 EC and DMC;The electrolytic salt is the LiPF of 1mol/L6;Solid electrolyte is oxide, solid state electrolysis
Matter can also be sulfide or ceramic-like;Here solid electrolyte is directly used, active matter is can avoid and is lost in the curing process.
Assembled battery is placed on electrochemical workstation and blue electric battery test system, fast progress is swept with 1mV/s
Ac impedance measurement and cyclic voltammetry.As shown in fig. 7, the boundary of liquid metal compound and the battery of solid electrolyte assembling
Face impedance is very small, and compatibility is good between active material and electrode.As shown in figure 5, liquid metal compound and solid state electrolysis
The stable electrochemical property of battery active material before and after cycle of matter assembling.
Simultaneously constant-current discharge test is carried out on blue electric battery test system;As shown in Figure 3a, liquid metal particle is filling
The electric smooth no groove crack of front surface;As shown in Figure 3b, its rough surface is covered with gully after charging;As shown in Figure 3c, after electric discharge
Its surface recovery is smooth;Test result shows that the active material has good embedding lithium performance, and repeatability is good.
As shown in Figure 6 a, the specific capacity of the liquid metal compound in the battery of preparation reaches 780mAh/g, voltage platform
Between 2.0-3.2V;As shown in Figure 6 b, the multiplying power of the liquid metal compound in the battery of preparation is in 0.2A/g to 2A/g electricity
Cycle performance is good under the conditions of current density;As fig. 6 c, the specific capacity of the graphene in the battery of preparation is in 0.2A/g to 2A/
It is 250mAh/g under g current density conditions, cycle performance is good;As shown in fig 6d, the ratio of the carbon nanotube in the battery of preparation
Capacity is 250mAh/g under 0.2A/g to 2A/g current density conditions, and cycle performance is good.
Embodiment two, according to mass ratio 22:3 weigh liquid metal tin and liquid metal gallium in Ai Pengdao bottles, then add
Enter 1mmol/L degassed ethanols mercaptan as solvent, the ultrasound 1h at 50 DEG C, forms liquid metal nano particle later;
The carbon nanotube of the liquid metal nano particle of 60mg and 12mg is added to shape in the absolute ethyl alcohol of 0.5mL
Resulting mixture I;It is 1 hour ultrasonic to mixture I in order to obtain more uniform suspension;It is simultaneously the carbon for obtaining purer,
Before using carbon nanotube, the nitric acid of 2.6mol/L is first used to carry out reflow treatment to carbon nanotube;Mixture I is used later
Deionized water is cleaned repeatedly, and then the graphene of 4mg is dissolved in the ethyl alcohol of 2wt%, and is added in mixture I and is formed
Mixture II;It is 10 minutes ultrasonic to mixture II, it is then sealed against in pyroreaction kettle reacting at a temperature of 160 DEG C
6h reacts 4h at a temperature of 900 DEG C later, is synthesizing liquid metal composite after its cooled to room temperature.To liquid
State metal composite carries out electronic scanner microscope observation, and the results are shown in Figure 4, illustrates that product is dispersed in carbon material, uniformly
Property is fine.
Using liquid metal compound as negative electrode active material, with mass ratio for 20:2:1:1 liquid metal compound, second
Acetylene black, CMC and SBR make negative plate, are cathode full of argon gas using lithium piece using electrolytic salt and organic solvent as electrolyte
The button cell of CR2032 formulas is assembled into glove box;Wherein, the organic solvent is:Volume ratio is 1:1 EC's and DMC is mixed
Close solution;The electrolytic salt is the LiPF of 1mol/L6;
Assembled battery is placed on electrochemical workstation and blue electric battery test system, fast progress is swept with 1mV/s
Ac impedance measurement and cyclic voltammetry.Simultaneously constant-current discharge test is carried out on blue electric battery test system.
Embodiment three, with carbon nanotube be anode, using electrolytic salt and organic solvent as electrolyte, exist by cathode of lithium piece
The button cell of CR2032 formulas is assembled into glove box full of argon gas;Wherein, the organic solvent is:Volume ratio is 1:1
The mixed solution of EC and DMC;The electrolytic salt is the LiPF of 1mol/L6;
Assembled battery is placed on electrochemical workstation and blue electric battery test system, fast progress is swept with 1mV/s
Ac impedance measurement, while carrying out constant-current discharge test on blue electric battery test system.
Example IV, with reduction-oxidation graphite be anode, be negative with lithium piece using electrolytic salt and organic solvent as electrolyte
Pole is assembled into the button cell of CR2032 formulas in the glove box full of argon gas;Wherein, the organic solvent is:Volume ratio is 1:
The mixed solution of 1 EC and DMC;The electrolytic salt is the LiPF of 1mol/L6;
Assembled battery is placed on electrochemical workstation and blue electric battery test system, fast progress is swept with 1mV/s
Ac impedance measurement and cyclic voltammetry while the progress constant-current discharge test on blue electric battery test system.
Embodiment one and embodiment two, embodiment three, example IV difference lies in:Embodiment one is successfully prepared liquid
Metal composite and solid electrolyte lithium battery possess high-energy density and good mechanical performance and ionic conductivity, and
It can apply to energy storage.It is used as the electrolyte of secondary lithium battery by the way that solid electrolyte is added, is assembled into battery and carries out constant current
Discharge test, the results showed that liquid metal compound and the battery of solid electrolyte its energy density highest is added.
The foregoing is merely a prefered embodiment of the invention, is not intended to limit the invention, all in the spirit and principles in the present invention
Within, any modification, equivalent replacement, improvement and so on should all be included in the protection scope of the present invention.
Claims (6)
1. a kind of preparation method of high power capacity high safety solid state lithium battery, it is characterised in that:It is received with liquid metal nano particle, carbon
Liquid metal compound made of mitron and graphene is negative electrode active material, is prepared by electrolyte of solid electrolyte.
2. a kind of preparation method of high power capacity high safety solid state lithium battery according to claim 1, it is characterised in that:The liquid
The preparation method of state metal composite is:
Step S1:It is 22 in mass ratio:3 weigh liquid metals tin and liquid metals gallium, and degassed ethanol mercaptan is added thereto
Solvent, ultrasonotomography, is made liquid metal nano particle later;
Step S2:The liquid metal nano particle and carbon nanotube are added to formation mixture I in absolute ethyl alcohol, then will be molten
Graphene in ethyl alcohol is added to formation mixture II in the mixture I, and the mixture II is placed in reaction kettle instead
5-7h is answered, reacts 3-5h at a temperature of 900 DEG C later, is synthesizing liquid metal composite after its cooled to room temperature
Object.
3. a kind of preparation method of high power capacity high safety solid state lithium battery according to claim 1, it is characterised in that:The step
Ultrasonotomography is implemented as described in rapid S1:The ultrasound 1h in 50 DEG C of environment.
4. a kind of preparation method of high power capacity high safety solid state lithium battery according to claim 2, it is characterised in that:The step
In rapid S2 before adding graphene into the mixture I, to I ultrasound 1h of the mixture.
5. a kind of preparation method of high power capacity high safety solid state lithium battery according to claim 2, it is characterised in that:The step
In rapid S2 before using carbon nanotube, reflow treatment is carried out to carbon nanotube using the nitric acid of 2.6mol/L.
6. a kind of preparation method of high power capacity high safety solid state lithium battery according to claim 1, it is characterised in that:It is described solid
The negative plate of state lithium battery is with mass ratio for 8:1:1 liquid metal compound, acetylene black and PVDF is prepared.
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Cited By (5)
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CN111430811A (en) * | 2020-03-31 | 2020-07-17 | 深圳供电局有限公司 | Polymer electrolyte coating, preparation method of material and battery |
CN112563448A (en) * | 2020-12-10 | 2021-03-26 | 国网内蒙古东部电力有限公司 | Method for treating SEI (solid electrolyte interphase) film on interface of low-temperature-resistant lithium ion battery |
CN112615013A (en) * | 2020-12-14 | 2021-04-06 | 桂林理工大学 | Liquid metal @ carbon nanotube lithium air battery anode and preparation method thereof |
CN113540587A (en) * | 2021-06-18 | 2021-10-22 | 江苏智蓝电源科技有限公司 | Method for improving compounding degree of gallium in polymer film |
US11404698B2 (en) | 2019-10-30 | 2022-08-02 | GM Global Technology Operations LLC | Liquid metal interfacial layers for solid electrolytes and methods thereof |
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Cited By (5)
Publication number | Priority date | Publication date | Assignee | Title |
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US11404698B2 (en) | 2019-10-30 | 2022-08-02 | GM Global Technology Operations LLC | Liquid metal interfacial layers for solid electrolytes and methods thereof |
CN111430811A (en) * | 2020-03-31 | 2020-07-17 | 深圳供电局有限公司 | Polymer electrolyte coating, preparation method of material and battery |
CN112563448A (en) * | 2020-12-10 | 2021-03-26 | 国网内蒙古东部电力有限公司 | Method for treating SEI (solid electrolyte interphase) film on interface of low-temperature-resistant lithium ion battery |
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Application publication date: 20180904 |