CN109755645A - Boron nitride/polyethylene glycol oxide composite solid electrolyte preparation method and application - Google Patents
Boron nitride/polyethylene glycol oxide composite solid electrolyte preparation method and application Download PDFInfo
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- CN109755645A CN109755645A CN201811652751.6A CN201811652751A CN109755645A CN 109755645 A CN109755645 A CN 109755645A CN 201811652751 A CN201811652751 A CN 201811652751A CN 109755645 A CN109755645 A CN 109755645A
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- boron nitride
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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
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- 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
Acetonitrile is added in a kind of preparation method and application of boron nitride/polyethylene glycol oxide solid electrolyte, (1) in nm-class boron nitride, and ultrasonic cleaning obtains boron nitride-acetonitrile dispersion liquid, and polyethylene glycol oxide PEO is added, and stirring becomes uniform lotion；(2) bis-trifluoromethylsulfoandimide lithium LiTFSI is added into lotion, stirs to get uniform mixed liquor；(3) mixed liquor is poured into Teflon mould, being cut into disk to apply the binder used in solid-state lithium metal battery, solid-state lithium metal battery by the solid polyelectrolyte prepared after evaporation drying box of divulging information is polyethylene glycol oxide PEO；The present invention improves the mechanical performance of solid polyelectrolyte, improve lithium ion transference number, assembling solid-state lithium metal battery in, effectively avoid existing for organic liquid battery dry up, leakage the problem of, keep good electrochemical cycle stability and safety.
Description
Technical field
The invention belongs to solid electrolyte preparation technical field, in particular to a kind of boron nitride/polyethylene glycol oxide composite solid
State electrolyte preparation method and application.
Background technique
Requirement of the electronic equipment now for high-energy density power supply system is very big, however existing lithium ion battery
Energy density do not still meet these application demand.Lithium metal battery is the energy storage system base with larger potential
In height ratio capacity (the 3860mAh g of itself-1) and lower reduction potential (- 3.04V is relative to reversible hydrogen electrode potential).But
Lithium ion battery is still common electrolyte in lithium ion battery using traditional esters organic liquid electrolytes at present, still
When working at high temperature, leakage, it is dry and it is inflammable and explosive be still serious safety problem.Due to above, people are positive
Develop the all-solid-state battery that can be worked at high temperature.Wherein, solid electrolyte is the critical component of all-solid-state battery, therefore is prepared
Electrochemically stable out, conductivity is high and the solid electrolyte of good mechanical property becomes significant challenge.Polymer itself has good
Type, flexibility and encapsulation can be processed in good machinery, it is considered to be the ideal material of preparation flexible solid electrolyte.Based on polyoxy
Change ethylene (referred to as: PEO) machinability, film forming and with the preferable compatibility of lithium salts, become excellent electrolysis material
Material.However, polymer dielectric (including PEO) there is also some problems, such as crystallization degree are higher, causes its conductivity lower
It is low with electrochemical stability.Therefore, how reducing the crystallinity of polymer and then increasing ionic conductivity becomes preparation with excellent
The research hotspot of the polymer dielectric of benign matter.People adulterate organic and inorganic (active material), other polymerizations in the polymer
The methods of fillers such as object are modified polymer dielectric.And the microstructure and size of filler itself and with polymer
Compatibility and dispersibility are to influence the key factor of polymer dielectric property.Compared to the nanoparticle of zero dimension and one-dimensional receive
Rice noodles filler is reported less since two-dimensional material is mostly semiconductor or insulator.Graphene oxide, vermiculite and nitridation
Boron nanometer sheet etc. is all modified polymer dielectric as two-dimentional filler.But graphene oxide electrochemistry is unstable,
Vermiculite is hygroscopic, is affected to lithium an- ode.Due to the biggish specific surface area of two-dimensional nano boron nitride lamella, and
It is the excellent material modified for polymer dielectric with strong-hydrophobicity.2017, Jong-Chan Lee was in Energy&
It publishes an article to report on Environmental Science magazine and mixes boron nitride progress the pyrene functionalized of perfluoro-polyether chain
It is miscellaneous to enter in Kynoar-hexafluoropropylene copolymer, gel electrolyte is prepared.2017, Bingqing Wei existed
Publishing thesis on Electrochimica Acta magazine, report will be in hexagonal boron nitride nanosheet polyvinyl alcohol-sulfuric acid
It prepares gel electrolyte and is applied to supercapacitor, be not applied in lithium metal battery.
Summary of the invention
In order to overcome the defects of the prior art described above, the purpose of the present invention is to provide a kind of boron nitride/polyethylene glycol oxides
Boron nitride nanosheet is mixed into polyoxyethylene by the preparation method and application of composite solid electrolyte under stirring conditions
Alkene prolongs stream method using solution and prepares modified solid electrolyte, and is applied to solid-state lithium metal battery, boron nitride
The lithium ion transference number and mechanical performance for improving solid polyelectrolyte is added, is applied to solid-state lithium metal battery
In, show preferable electrochemical cycle stability.
In order to achieve the above object, the technical solution of the present invention is as follows:
A kind of preparation method of boron nitride/polyethylene glycol oxide composite solid electrolyte, comprising the following steps:
(1) nm-class boron nitride of 0.3-0.9g is put into round-bottomed flask, 200-300mL acetonitrile is added thereto, is put into super
Sound cleaning device obtains boron nitride-acetonitrile dispersion liquid, and 10g polyethylene glycol oxide PEO is added, and magnetic agitation becomes uniformly mixed cream
Liquid；
(2) 0.7-1.5g bis-trifluoromethylsulfoandimide lithium LiTFSI is added into the lotion of step 1, uses magnetic stirring apparatus
It is stirred, obtains uniform mixed liquor；
(3) mixed liquor made from step 2 is poured into Teflon mould, is placed in ventilating kitchen, acetonitrile is waited to steam
Hair forms solid polyelectrolyte film, and after being placed in vacuum oven, it is spare less than the disk of 1.9cm to be cut into diameter.
It is cleaned by ultrasonic instrument in the step one, power 40W carries out ultrasound, and the time is 1-6 hours.
The acetonitrile for dispersing boron nitride in the step one can be replaced with methanol.
It places in the step three in a vacuum drying oven, is dried in vacuo 6 hours at 80 DEG C.
The nm-class boron nitride is that diameter is 50-1000nm and nanometer sheet or diameter with a thickness of 10-100nm
Range is 10-30 μm, with a thickness of the m array form boron nitride of 0.1-1 μ.
A kind of application of boron nitride/polyethylene glycol oxide composite solid electrolyte, the solid polyelectrolyte that will be prepared
It is cut into disk or arbitrary shape, it is suitable according to anode cover+anode pole piece+solid electrolyte+lithium piece+gasket+spring leaf+negative electrode casing
Sequence is assembled into solid-state lithium metal battery, and binder used in solid-state lithium metal battery is polyethylene glycol oxide PEO.
Advantages of the present invention:
(1) solid polyelectrolyte prepared is cut into disk, can direct-assembling solid-state lithium metal battery, have preparation
Method is simple and quick, mild condition, reproducible feature.
(2) preparation condition is simply mild, it is only necessary to can uniformly be nitrogenized by mixing, stirring and drying and other steps
Boron/polyethylene glycol oxide composite solid electrolyte does not need stringent anhydrous and oxygen-free, the reaction such as inert gas shielding item in glove box
Part, and reagent price used is cheap, reduces costs, obtained solid electrolyte membrane is uniform, can carry out under high temperature environment
The charge and discharge cycles of battery, and show preferable electrochemical stability.
(3) since boron nitride, PEO and LiTFSI are mixed in acetonitrile, belong to liquid phase mixing, mixing is more uniform, obtains
Dielectric film also more uniformly, simultaneously as the doping of boron nitride, improves the springform of solid polyelectrolyte entirety
Amount, increases its mechanical performance and improves lithium ion transference number.
(4) solid electrolyte is applied to LiFePO4-boron nitride/polyethylene glycol oxide composite solid electrolyte-metal
In the solid state battery system of lithium, due to boron nitride and PEO is solid-state and chemical stability is strong, and encapsulation is good, effectively keeps away
Exempted from existing for organic liquid battery dry up, leakage the problem of, provide guarantee for the stability of battery system.
(5) at a high temperature of 60 DEG C, LiFePO4-boron nitride/polyethylene glycol oxide composite solid electrolyte-lithium metal battery
Circulating ring number reach 50 circles, illustrate that the solid electrolyte can work at relatively high temperatures, and have good electrochemistry
Cyclical stability and safety.
Detailed description of the invention
Fig. 1 is the obtained boron nitride of the embodiment of the present invention one/polyethylene glycol oxide composite solid electrolyte optical photograph,
Embedded figure illustrates the flexibility of electrolyte.
Fig. 2 is the preparation-obtained boron nitride of the embodiment of the present invention one/polyethylene glycol oxide composite solid electrolyte in difference
At a temperature of impedance curve.
Fig. 3 is the preparation-obtained boron nitride of the embodiment of the present invention one/polyethylene glycol oxide composite solid electrolyte at 60 DEG C
Lower time current curve and impedance curve (b), wherein Fig. 3 (a) is time current curve, and wherein Fig. 3 (b) is impedance curve.
Fig. 4 is the preparation-obtained boron nitride of the embodiment of the present invention 1/polyethylene glycol oxide composite solid electrolyte stress-
Strain curve.
Fig. 5 is the preparation-obtained boron nitride of the embodiment of the present invention one/polyethylene glycol oxide composite solid electrolyte in lithium-phosphorus
Charging and discharging curve and coulombic efficiency curve in sour iron lithium solid state battery.
Fig. 6 is the optical photograph of the obtained solid electrolyte of the embodiment of the present invention two, and embedded figure illustrates electrolyte
It is flexible.
Fig. 7 is the optical photograph of the obtained solid electrolyte of the embodiment of the present invention three, and embedded figure illustrates electrolyte
It is flexible.
Specific embodiment
Below with reference to embodiment, the present invention is described in further detail.It will be understood to those of skill in the art that following
Embodiment is merely to illustrate the present invention, and should not be taken as limiting the scope of the invention.Particular technique or item are not specified in embodiment
Part person described technology or conditions or carries out according to the literature in the art according to product description.Raw materials used and change
Learning reagent is that analysis is pure.
Embodiment one
The preparation method of the present embodiment the following steps are included:
(1) nm-class boron nitride of 0.6g is put into 500mL round-bottomed flask, 200mL acetonitrile is added thereto, be put into ultrasonic clear
Instrument is washed, power 40W carries out ultrasound, and the time is 6 hours, obtains boron nitride-acetonitrile dispersion liquid, 10g polyethylene glycol oxide is added
(referred to as: PEO) becomes uniformly mixed lotion in magnetic agitation 1 hour in dispersion liquid；Nm-class boron nitride is that diameter is 50-
1000nm and nanometer sheet with a thickness of 10-100nm；
(2) 1g bis-trifluoromethylsulfoandimide lithium (referred to as: LiTFSI) is added into the mixed emulsion of step 1, is stirred with magnetic force
It mixes device to be stirred 1 hour, obtains mixed liquor；
(3) mixed liquor made from step 2 is slowly poured into Teflon mould, is placed in ventilating kitchen, wait second
Nitrile evaporation, forms solid polyelectrolyte film.It places in a vacuum drying oven, is dried in vacuo 6 hours at 80 DEG C, uses tablet press machine
Being cut into diameter is 1.9cm disk.
The exterior appearance optical photograph of electrolyte and flexible displaying photo are as shown in Figure 1, electrolyte appearance is translucent
Film, and have flexible well.Solid electrolyte is measured at 30-80 DEG C using Shanghai Chen Hua board electrochemical workstation
Impedance (Fig. 2), the conductivity being calculated are respectively 7.8 × 10-6S cm-1、1.9×10-5S cm-1、4.7×10-5S cm-1、
8.9×10-5S cm-1、1.1×10-4S cm-1、1.4×10-4S cm-1The solid electrolyte measured also with the work station
Lithium ion transference number is 0.33 (Fig. 3).Measured time current curve under the polarizing voltage that a figure is 10mV, b figure is to survey
Impedance curve before and after polarization curve.The lithium ion mobility of polymer dielectric prepared by case one is calculated using formula
Number is 0.33.As shown in figure 4, being 0.98MPa using the tensile strength that universal testing machine measures solid electrolyte.
A kind of application of boron nitride/polyethylene glycol oxide composite solid electrolyte, is applied in solid-state lithium metal battery, specifically
Steps are as follows:
(1) preparation of anode pole piece: will be 70% iron phosphate powder, 10% carbon black and 20% containing mass fraction
Polyethylene glycol oxide (referred to as: PEO) be added in N-Methyl pyrrolidone as binder, formed within magnetic agitation 48 hours sticky
Slurry is coated on aluminium foil.It places in a vacuum drying oven, is dried in vacuo 12 hours at 100 DEG C.
(2) assembling of button cell, in the glove box full of argon gas, (moisture content < 0.1ppm, oxygen content <
0.1ppm), it is assembled according to anode cover+anode pole piece+solid electrolyte+lithium piece+gasket+spring leaf+negative electrode casing sequence.
Assembled battery is carried out to the charge and discharge cycles test and coulomb effect of battery in the voltage range of 2.8-4.0V
Rate test.Incubator temperature setting is 60 DEG C.The solid-state lithium metal battery that Fig. 5 is participated in for this poly ion liquid solid electrolyte
Charging and discharging capacity curve and coulombic efficiency curve under 0.5C current density, specific capacity reach 145.4mAh g-1, circulation
Circle number reaches 50 circles, and coulombic efficiency is maintained at 97% or more, illustrates that coulombic efficiency height, electrochemical cycle stability are good.
Embodiment two
The preparation method of the present embodiment the following steps are included:
(1) nm-class boron nitride of 0.3g is put into 500mL round-bottomed flask, 300mL acetonitrile is added thereto, be put into ultrasonic clear
Instrument is washed, power 40W carries out ultrasound, and the time is 1 hour, obtains boron nitride-acetonitrile dispersion liquid, 10g polyethylene glycol oxide is added
(referred to as: PEO) becomes uniformly mixed lotion in magnetic agitation 1 hour in dispersion liquid；Nm-class boron nitride is that diameter is 50-
1000nm and nanometer sheet with a thickness of 10-100nm；
(2) 0.7g bis-trifluoromethylsulfoandimide lithium (referred to as: LiTFSI) is added into the mixed emulsion of step 1, uses magnetic force
Blender is stirred 1 hour, obtains mixed liquor；
(3) mixed liquor made from step 2 is poured slowly into Teflon mould, is placed in ventilating kitchen, wait second
Nitrile evaporation, forms solid polyelectrolyte film；It places in a vacuum drying oven, is dried in vacuo 6 hours at 80 DEG C；Use tablet press machine
Being cut into diameter is 1.9cm disk.
The exterior appearance optical photograph for the electrolyte that this embodiment is prepared and flexible displaying photo are as shown in fig. 6, electricity
Solution matter appearance is the film of white, and has flexible well.The stretching for measuring solid electrolyte using universal testing machine is strong
Degree is 0.4MPa.
Product made from the present embodiment is applied in solid-state lithium metal battery in the way of embodiment one, will be assembled
Battery carried out in the voltage range of 2.8-4.0V battery charge and discharge cycles test and coulombic efficiency test.Incubator temperature
It is set as 60 DEG C.Charging and discharging capacity curve and coulombic efficiency curve under 0.1C current density show that specific capacity reaches
134.3mAh g-1, circulating ring number reach 50 circles, and coulombic efficiency is maintained at 98% or more, illustrate coulombic efficiency height, and electrochemistry is followed
Ring stability is good.
Embodiment three
The preparation method of the present embodiment the following steps are included:
(1) nm-class boron nitride of 0.9g is put into 500mL round-bottomed flask, 250mL methanol is added thereto, be put into ultrasonic clear
Instrument is washed, power 40W carries out ultrasound, and the time is 3 hours, obtains boron nitride-acetonitrile dispersion liquid, 10g polyethylene glycol oxide is added
(referred to as: PEO) becomes uniformly mixed lotion in magnetic agitation 1 hour in dispersion liquid；Nm-class boron nitride is that diameter range is
10-30 μm, with a thickness of 0.1-1 μm of array form boron nitride；
(2) 1.5g bis-trifluoromethylsulfoandimide lithium (referred to as: LiTFSI) is added into the mixed emulsion of step 1, uses magnetic force
Blender is stirred 1 hour, obtains mixed liquor；
(3) mixed liquor made from step 2 is poured slowly into Teflon mould, is placed in ventilating kitchen, wait first
Alcohol evaporation, forms solid polyelectrolyte film；It places in a vacuum drying oven, is dried in vacuo 6 hours at 80 DEG C.Use tablet press machine
It is cut into arbitrary shape.
The exterior appearance optical photograph for the electrolyte that the present embodiment is prepared and flexible displaying photo are as shown in fig. 7, electricity
Solution matter appearance is the film of white, and has flexible well.The stretching for measuring solid electrolyte using universal testing machine is strong
Degree is 0.69MPa.
Product made from the present embodiment is cut into arbitrary shape, according to aluminum plastic film+anode pole piece+solid electrolyte+lithium piece+
The sequence of aluminum plastic film is assembled into Soft Roll lithium metal battery, and binder used in battery is polyethylene glycol oxide PEO.It will assemble
Battery carried out in the voltage range of 2.8-4.0V battery charge and discharge cycles test and coulombic efficiency test.Incubator temperature
It is set as 60 DEG C.Charging and discharging capacity curve and coulombic efficiency curve under 0.1C current density show that specific capacity reaches
60mAh g-1, circulating ring number reach 20 circles, and coulombic efficiency is maintained at 97% or more, illustrate coulombic efficiency height, and electrochemistry circulation is steady
It is qualitative good.
Claims (7)
1. a kind of boron nitride/polyethylene glycol oxide solid electrolyte preparation method, which comprises the following steps:
(1) nm-class boron nitride of 0.3-0.9g is put into round-bottomed flask, 200-300mL acetonitrile is added thereto, be put into ultrasonic clear
Instrument is washed, boron nitride-acetonitrile dispersion liquid is obtained, 10g polyethylene glycol oxide PEO is added, magnetic agitation becomes uniformly mixed lotion；
(2) 0.7-1.5g bis-trifluoromethylsulfoandimide lithium LiTFSI is added into the lotion of step 1, is carried out with magnetic stirring apparatus
Stirring, obtains uniform mixed liquor；
(3) mixed liquor made from step 2 is poured into Teflon mould, is placed in ventilating kitchen, wait acetonitrile evaporation,
Solid polyelectrolyte film is formed, after being placed in vacuum oven, it is spare less than the disk of 1.9cm to be cut into diameter.
2. a kind of preparation method of boron nitride/polyethylene glycol oxide solid electrolyte according to claim 1, feature exist
In being cleaned by ultrasonic instrument in the step one, power 40W carries out ultrasound, and the time is 1-6 hours.
3. a kind of preparation method of boron nitride/polyethylene glycol oxide solid electrolyte according to claim 1, feature exist
In the acetonitrile for dispersing boron nitride in the step one can be replaced with methanol.
4. a kind of preparation method of boron nitride/polyethylene glycol oxide solid electrolyte according to claim 1, feature exist
In placing in the step three in a vacuum drying oven, be dried in vacuo 6 hours at 80 DEG C.
5. a kind of preparation method of boron nitride/polyethylene glycol oxide solid electrolyte according to claim 1, feature exist
In the nm-class boron nitride is that diameter is 50-1000nm and the nanometer sheet with a thickness of 10-100nm；Or diameter range is
10-30 μm, with a thickness of 0.1-1 μm of array form boron nitride.
6. based on a kind of application of boron nitride/polyethylene glycol oxide solid electrolyte described in claim 1, which is characterized in that will
The solid polyelectrolyte prepared is cut into disk, according to anode cover+anode pole piece+solid electrolyte+lithium piece+gasket+bullet
Reed+negative electrode casing sequence is assembled into solid-state lithium metal battery, and binder used in solid-state lithium metal battery is polyoxygenated
Ethylene PEO.
7. based on a kind of application of boron nitride/polyethylene glycol oxide solid electrolyte as claimed in claim 6, which is characterized in that will
The solid polyelectrolyte prepared is cut into arbitrary shape, according to aluminum plastic film+anode pole piece+solid electrolyte+lithium piece+plastic-aluminum
The sequence of film is assembled into Soft Roll lithium metal battery, and binder used in battery is polyethylene glycol oxide PEO.
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|---|---|---|---|---|
| CN110600798A (en) * | 2019-09-30 | 2019-12-20 | 西安交通大学 | Preparation method and application of manganese dioxide/polyoxyethylene composite solid electrolyte |
| CN110994017A (en) * | 2020-01-03 | 2020-04-10 | 南京工业大学 | Nitride-enhanced polymer electrolyte, preparation method and long-life solid lithium ion battery |
| CN111193064A (en) * | 2020-01-09 | 2020-05-22 | 北京理工大学 | Solid polymer ionic gel electrolyte membrane and preparation method and application thereof |
| CN111370760A (en) * | 2020-03-19 | 2020-07-03 | 香港科技大学 | Wide electrochemical window composite solid electrolyte and preparation method thereof |
| CN111969246A (en) * | 2020-06-01 | 2020-11-20 | 西安交通大学 | Preparation method and application of nano bacterial cellulose/polyoxyethylene composite solid electrolyte |
| CN112436188A (en) * | 2020-12-26 | 2021-03-02 | 哈尔滨工业大学 | Polymer-based solid electrolyte with high room temperature ionic conductivity and preparation method and application thereof |
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| CN114512715A (en) * | 2022-01-20 | 2022-05-17 | 贵阳学院 | Polyoxyethylene-based solid electrolyte, preparation method thereof and lithium ion battery |
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| CN110600798A (en) * | 2019-09-30 | 2019-12-20 | 西安交通大学 | Preparation method and application of manganese dioxide/polyoxyethylene composite solid electrolyte |
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| CN111193064A (en) * | 2020-01-09 | 2020-05-22 | 北京理工大学 | Solid polymer ionic gel electrolyte membrane and preparation method and application thereof |
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| CN111969246A (en) * | 2020-06-01 | 2020-11-20 | 西安交通大学 | Preparation method and application of nano bacterial cellulose/polyoxyethylene composite solid electrolyte |
| CN112436188A (en) * | 2020-12-26 | 2021-03-02 | 哈尔滨工业大学 | Polymer-based solid electrolyte with high room temperature ionic conductivity and preparation method and application thereof |
| CN112436188B (en) * | 2020-12-26 | 2021-11-09 | 哈尔滨工业大学 | Polymer-based solid electrolyte with high room temperature ionic conductivity and preparation method and application thereof |
| CN114373995A (en) * | 2021-12-20 | 2022-04-19 | 河北金力新能源科技股份有限公司 | Composite solid polymer electrolyte and preparation method thereof |
| CN114512715A (en) * | 2022-01-20 | 2022-05-17 | 贵阳学院 | Polyoxyethylene-based solid electrolyte, preparation method thereof and lithium ion battery |
| CN114824459A (en) * | 2022-05-18 | 2022-07-29 | 电子科技大学 | Metallic lithium and solid electrolyte interface layer and preparation method |
| CN115425283A (en) * | 2022-09-20 | 2022-12-02 | 浙江理工大学 | Boron nitride nanofiber composite solid electrolyte, preparation method and application |
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Application publication date: 20190514 |