CN104269509A - Ceramic coating diaphragm for lithium battery and preparation method of ceramic coating diaphragm - Google Patents
Ceramic coating diaphragm for lithium battery and preparation method of ceramic coating diaphragm Download PDFInfo
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- CN104269509A CN104269509A CN201410542516.9A CN201410542516A CN104269509A CN 104269509 A CN104269509 A CN 104269509A CN 201410542516 A CN201410542516 A CN 201410542516A CN 104269509 A CN104269509 A CN 104269509A
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/403—Manufacturing processes of separators, membranes or diaphragms
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/411—Organic material
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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
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/40—Separators; Membranes; Diaphragms; Spacing elements inside cells
- H01M50/409—Separators, membranes or diaphragms characterised by the material
- H01M50/44—Fibrous material
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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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Abstract
The invention discloses a ceramic coating diaphragm for a lithium battery and a preparation method of the ceramic coating diaphragm, and belongs to the technical field of batteries. The ceramic coating diaphragm comprises a ceramic coating and a substrate diaphragm, wherein the ceramic coating is prepared by uniformly coating the substrate diaphragm with water-based ceramic coating slurry; the ceramic coating slurry comprises components in percentage by weight as follows: 10%-30% of aluminum oxide, 0.5%-3% of a bonding agent, 0.2%-1.0% of an additive and 0.01%-0.1% of an auxiliary; and the aluminum oxide is nanometer aluminum oxide powder with the grain diameter ratio D1/D2 of 0.10-0.20. According to the technical scheme, the safety of the ceramic coating diaphragm is improved, the wetting ability of electrolyte is improved, and the cycle life of the battery can be prolonged when the ceramic coating diaphragm is applied to the lithium battery.
Description
Technical field
The invention belongs to technical field of lithium batteries, relate to a kind of lithium battery diaphragm, particularly relate to a kind of energy-storage lithium battery ceramic coating membrane and preparation method thereof.
Background technology
Lithium ion battery is because of the characteristic such as its high voltage, high-energy-density, long-life, memory-less effect, automatic discharging be little, not only be widely used and development prospect on mobile battery and electrokinetic cell, its developmental research in electrical network energy storage is also coming into one's own gradually.Because electrical network energy storage requires that energy storage technology meets the requirements such as extensive, high cycle life, high efficiency, mass production and cost are low, and the properties of binding analysis lithium ion battery, therefore lithium ion battery becomes a very promising electrical network energy storage mode.
Lithium ion battery separator is the key component of lithium ion battery, must possess good chemical stability, electrochemical stability, and possesses certain hot strength and puncture-resistant intensity, to prevent battery short circuit.Meanwhile, it also offers the passage that lithium ion between both positive and negative polarity penetrates, there is electrolyte and absorb and hold facility, achieve the normal circulation of lithium ion battery.
Commercial lithium-ion batteries barrier film conventional is at present the single or multiple lift film of polyethylene (Polyethylene), polypropylene (Polypropylene).Because the fusing point of conventional polyolefins barrier film is lower, after being heated, there will be contraction, cause battery plus-negative plate contact short circuit; And not good to electrolyte wettability, therefore people are studied exploitation to new types of diaphragm material.
Also the ceramic diaphragm for lithium ion battery has been engendered in the market.Common ceramic coating pottery used is nano alumina particles.The problem such as but some ceramic diaphragms exist dry linting and uniformity is low, its main cause is that the specific surface energy of superfine alumina powder is on the one hand large, surface activity is high, single ultra-fine grain often plays pendulum, reunite because of attracting each other between particle, form larger agglomerated particle, harmful effect is produced to follow-up coating process; Be that coating accuracy controls existing defects on the other hand, coating layer thickness is uneven, and coating quality is not high.
Summary of the invention
In view of this, the object of the present invention is to provide a kind ofly have that high security, electrolyte wetability are strong, the energy-storage lithium battery ceramic coating membrane that can improve lithium battery cycle life and preparation method thereof.
For achieving the above object, concrete technical scheme is as follows:
On the one hand, a kind of lithium battery ceramic coating membrane is provided, comprise ceramic coating and base material barrier film, described ceramic coating is made up at base material membrane surface of ceramic coated slurry even application, described ceramic coated slurry comprises: the aluminium oxide of 10 ~ 30wt%, the bonding agent of 0.5 ~ 3wt%, the additive of 0.2 ~ 1.0wt% and the auxiliary agent of 0.01 ~ 0.1wt%, and described aluminium oxide is that particle diameter compares D
1/ D
2be 0.10 ~ 0.20 nano alumina powder jointed.
Preferably, described nano alumina powder jointed middle Large stone D2 is greater than 0.1um, and is less than 1.0um, and Large stone alumina content is 50% ~ 90% of alumina powder jointed gross mass; Small particle diameter D1 is less than 0.1um, and small particle diameter alumina content is 10% ~ 50% of alumina powder jointed gross mass.
Preferably, the thickness of the ceramic coating of described base material membrane surface coating is 2.0 ~ 5.0um.
Preferably, described base material barrier film is polyethylene diagrams or polypropylene diaphragm.
Preferably, the bonding agent in described ceramic coated slurry comprises one or more in styrene-butadiene emulsion, polymethyl methacrylate-polybutylacrylate latex, Polyphenylethylene-butyl acrylate emulsion, ptfe emulsion, polyvinylidene fluoride emulsion.
Preferably, the additive in described ceramic coated slurry is water-soluble macromolecule, comprises one or more in sodium carboxymethylcellulose, hydroxyethylcellulose, hydroxypropyl methylcellulose, polyvinyl alcohol, polyethylene glycol, polyacrylamide.
Preferably, the auxiliary agent in described ceramic coated slurry comprises one or more in tertiary alkyl polyalcohol polyvinylether, sulfonic group di-isooctyl sodium, alkylnaphthalene sulfonate, polyether modified silicon oil, polypropylene glycol-oxirane, polyethers stearate dimethyl siloxane, polyoxyethylene polyoxypropylene pentaerythrite ether, polyoxyethylene glycerol ether, polyoxyethylene polyoxy propyl alcohol amidogen ether.
On the other hand, provide a kind of preparation method of lithium battery ceramic coating membrane, comprise the steps:
Step 1, gets particle diameter and compares D
1/ D
2be 0.10 ~ 0.20 nano alumina powder jointed, be dispersed in deionized water water, prepare nano aluminium oxide aqueous dispersions;
Step 2, mixes described nano aluminium oxide aqueous dispersions with bonding agent, additive and auxiliary agent, configuration ceramic coated slurry, wherein aluminium oxide: the mass ratio of bonding agent is 5 ~ 20:1;
Step 3, by described ceramic coated slurry even application at base material membrane surface, obtains lithium battery ceramic coating membrane.
Preferably, in described step 1, the solid content of nano aluminium oxide aqueous dispersions is 20 ~ 40%, and regulates its pH value to be 4.0 ~ 5.0.
Preferably, also comprise the dispersant of 0.1-1.0wt% in described step 1 in nano aluminium oxide aqueous dispersions, described dispersant comprises one or more in neopelex, lauryl sodium sulfate, dodecyl sodium sulfate, calgon, polyacrylic acid, softex kw, octylphenolpolyoxyethylene, polyethylene glycol.
Relative to prior art, technical scheme tool of the present invention has the following advantages:
1, ceramic coating membrane air permeability is good, and the air permeability of more uncoated base material barrier film adds 10%;
2, the peeling force of ceramic coating is high, and ceramic coating membrane can not dry linting;
3, ceramic coating has very strong absorption and keeps electrolyte ability, and coating can not come off in the electrolytic solution, still keeps cementability;
4, the thermal contraction performance of ceramic coating membrane, more uncoated base material barrier film is greatly improved;
5, ceramic coating is conducive to the lifting of the capability retention of battery, improves cycle life.
Accompanying drawing explanation
The accompanying drawing forming a part of the present invention is used to provide a further understanding of the present invention, and schematic description and description of the present invention, for explaining the present invention, does not form inappropriate limitation of the present invention.In the accompanying drawings:
Fig. 1 is the scanning electron microscope (SEM) photograph of the ceramic coating membrane that the embodiment of the present invention obtains;
Fig. 2 is the scanning electron microscope (SEM) photograph of polyalkene diaphragm in the comparative example of the embodiment of the present invention;
Fig. 3 is the cycle-index-discharge capacity under the 1C multiplying power of the button cell of the polyalkene diaphragm assembling of the ceramic diaphragm prepared of the embodiment of the present invention and comparative example;
Fig. 4 is that embodiment of the present invention gained ceramic coating membrane compares with the electrolyte wetability of the polyethylene base material barrier film of comparative example.
Embodiment
Below in conjunction with the accompanying drawing in the embodiment of the present invention, be clearly and completely described the technical scheme in the embodiment of the present invention, obviously, described embodiment is only the present invention's part embodiment, instead of whole embodiments.Based on the embodiment in the present invention, those of ordinary skill in the art, not making the every other embodiment obtained under creative work prerequisite, belong to the scope of protection of the invention.
It should be noted that, when not conflicting, the embodiment in the present invention and the feature in embodiment can combine mutually.
Below with reference to accompanying drawing, concrete explaination is done to embodiments of the invention.
A kind of lithium battery ceramic coating membrane of embodiments of the invention, comprises ceramic coating and base material barrier film.Ceramic coating is made up at base material membrane surface of ceramic coated slurry even application.Ceramic coated slurry comprises: the aluminium oxide of 10 ~ 30wt%, the bonding agent of 0.5 ~ 3wt%, the additive of 0.2 ~ 1.0wt% and the auxiliary agent of 0.01 ~ 0.1wt%.Aluminium oxide is that particle diameter compares D
1/ D
2be 0.10 ~ 0.20 nano alumina powder jointed.
Its preparation method, comprises the steps:
Step 1, gets particle diameter and compares D
1/ D
2be 0.10 ~ 0.20 nano alumina powder jointed, be dispersed in deionized water water, prepare nano aluminium oxide aqueous dispersions;
Step 2, mixes nano aluminium oxide aqueous dispersions and bonding agent, additive, reduction slurry surface tension and the auxiliary agent of eliminating small vacuole, configuration ceramic coated slurry, wherein aluminium oxide: the mass ratio of bonding agent is 5 ~ 20:1;
Step 3, by ceramic coated slurry even application at base material membrane surface, obtains lithium battery ceramic coating membrane.
The air permeability of embodiments of the invention is good, peeling force is high, have very strong absorption and maintenance electrolyte ability, thermal contraction performance, is conducive to the lifting of the capability retention of battery, improves the cycle life of battery.
In an embodiment of the present invention, preferential oxidation aluminum nanopowder adopts method that is ultrasonic and high-speed stirred to disperse in deionized water, adds a certain amount of dispersant, high-speed stirred and ultrasonic process 1h under normal temperature.And a certain amount of hydrochloric acid and sodium hydroxide solution is added in above-mentioned aluminium oxide aqueous dispersions, regulate the pH value of dispersion liquid to maintain 4.0 ~ 5.0, to obtain stable alumina fluid dispersion.
And preferably adopt micro gravure printing machine, above-mentioned ceramic coated slurry is evenly coated in the surface of base material barrier film, through the heated-air drying of 40 ~ 60 DEG C, obtains lithium battery ceramic coating membrane.And to control thickness of ceramic coating be that 2.0 ~ 5.0um is controlled, within coating precision controlling 0.5um.Wherein, base material barrier film both can be dry method polyethylene diagrams, polypropylene diaphragm, also can be wet method polyalkene diaphragm.
Embodiment 1
The preparation method of energy-storage lithium battery ceramic coating membrane, comprises the steps;
Step 1, get the aluminium oxide 2g that D1 is 50nm, D2 is the aluminium oxide 8g of 400nm, joins in 40g deionized water, first high-speed stirred 30min, then ultrasonic disperse 30min, obtains the pre-dispersed liquid of nano aluminium oxide.Add in pre-dispersed liquid mass fraction be 0.5% dispersant comprise: neopelex 0.125g, octylphenolpolyoxyethylene 0.063g and polyacrylic acid 0.063g, the amount ratio of three is 2:1:1.High-speed stirred pre-dispersed liquid 30min, then the pH value adding a small amount of hydrochloric acid weak solution and dilute solution of sodium hydroxide adjustment dispersion liquid wherein remains on 4-5;
Above-mentioned pre-dispersed liquid carries out ball-milling treatment 2h in ball mill, obtains uniform and stable nano aluminium oxide aqueous dispersions.
Step 2, in step 1 gained nano aluminium oxide aqueous dispersions, add styrene-butadiene emulsion (solid content is 50%) 2g, sodium carboxymethylcellulose (mass fraction is 5%) 2g and tertiary alkyl polyalcohol polyvinylether 0.05g, carry out low rate mixing evenly after, with 400 order stainless steel sift net filtrations, obtain aqueous ceramic coating slurry.
Step 3, employing micro gravure printing machine, above-mentioned aqueous ceramic coating slurry is evenly coated on polyethylene diagrams, the base material barrier film speed of service is 0.5m/min, and heated-air drying temperature is 50 DEG C, prepares the ceramic coating membrane that one side thickness of ceramic coating is 3.0 ± 0.5um.
As shown in fig. 1, in the present invention, the ceramic coating on the ceramic coating membrane surface of embodiment 1 is very even, and aluminium oxide defines many holes,
As shown in Figure 2, polyethylene (PE) barrier film of use in embodiment 1 is adopted as a comparison case, its thickness 16.0um.
Commercial polyethylene (PE) barrier film of the ceramic coating membrane prepared by embodiment in the present invention 1 and comparison example is compared test, and experimental result is as shown in table 1.Lifting is to a certain degree had before the mechanical performance of the lithium battery ceramic coating membrane that the embodiment of the present invention 1 obtains comparatively applies,
And as shown in Figure 3, wherein, the chain-dotted line relatively gone up along ordinate is the cycle-index-discharge capacity performance of ceramic coated film and ceramic diaphragm, along ordinate relatively under a chain-dotted line be the cycle-index-discharge capacity performance of basement membrane and polyalkene diaphragm, as can be seen from Figure, the ceramic diaphragm that prepared by embodiment 1 compares the cycle-index-discharge capacity performance enhancement under the 1C multiplying power of the button cell of the polyalkene diaphragm assembling of ratio.As shown in Figure 4, wherein the left side is polyethylene base material barrier film, and the right is ceramic coating membrane, and embodiment 1 gained ceramic coating membrane compares the electrolyte wetability performance enhancement of the polyethylene base material barrier film of ratio.
Table 1:
Embodiment 2
Energy-storage lithium battery ceramic coating membrane and preparation method thereof, comprises the steps;
Step 1, get the aluminium oxide 4g that D1 is 80nm, D2 is the aluminium oxide 6g of 500nm, joins in 30g deionized water, first high-speed stirred 30min, then ultrasonic disperse 30min, obtains the pre-dispersed liquid of nano aluminium oxide.Add in pre-dispersed liquid mass fraction be 1.0% dispersant comprise: neopelex 0.20g, octylphenolpolyoxyethylene 0.10g and polyacrylic acid 0.10g, the amount ratio of three is 2:1:1.High-speed stirred pre-dispersed liquid 30min, then the pH value adding a small amount of hydrochloric acid weak solution and dilute solution of sodium hydroxide adjustment dispersion liquid wherein remains on 4-5;
Above-mentioned pre-dispersed liquid carries out ball-milling treatment 2h in ball mill, obtains uniform and stable nano aluminium oxide aqueous dispersions.
Step 2, polymethyl methacrylate-polybutylacrylate latex (solid content is 40%) 2.50g, polyacrylamide (mass fraction is 5%) 1.6g and polyethers stearate dimethyl siloxane 0.04g is added in step 1 gained nano aluminium oxide aqueous dispersions, carry out low rate mixing evenly after, with 400 order stainless steel sift net filtrations, obtain aqueous ceramic coating slurry.
Step 3, adopt micro gravure printing machine, be evenly coated on polyethylene diagrams by above-mentioned aqueous ceramic coating slurry, the base material barrier film speed of service is 1.0m/min, heated-air drying temperature is 60 DEG C, prepares the ceramic coating membrane that one side thickness of ceramic coating is 4.0 ± 0.5um.
Be described in detail specific embodiments of the invention above, but it is just as example, the present invention is not restricted to specific embodiment described above.To those skilled in the art, any equivalent modifications that the present invention is carried out and substituting also all among category of the present invention.Therefore, equalization conversion done without departing from the spirit and scope of the invention and amendment, all should contain within the scope of the invention.
Claims (10)
1. a lithium battery ceramic coating membrane, it is characterized in that, comprise ceramic coating and base material barrier film, described ceramic coating applies slurry even application by aqueous ceramic and makes at base material membrane surface, described aqueous ceramic coating slurry comprises: the aluminium oxide of 10 ~ 30wt%, the bonding agent of 0.5 ~ 3wt%, the additive of 0.2 ~ 1.0wt% and the auxiliary agent of 0.01 ~ 0.1wt%, described aluminium oxide is that particle diameter compares D
1/ D
2be 0.10 ~ 0.20 nano alumina powder jointed.
2. lithium battery ceramic coating membrane as claimed in claim 1, it is characterized in that, described nano alumina powder jointed middle Large stone D2 is greater than 0.1um, and is less than 1.0um, and Large stone alumina content is 50% ~ 90% of alumina powder jointed gross mass; Small particle diameter D1 is less than 0.1um, and small particle diameter alumina content is 10% ~ 50% of alumina powder jointed gross mass.
3. lithium battery ceramic coating membrane as claimed in claim 2, is characterized in that, the thickness of the ceramic coating of described base material membrane surface coating is 2.0 ~ 5.0um.
4. lithium battery ceramic coating membrane as claimed in claim 3, it is characterized in that, described base material barrier film is polyethylene diagrams or polypropylene diaphragm.
5. lithium battery ceramic coating membrane as claimed in claim 4, it is characterized in that, the bonding agent in described ceramic coated slurry comprises one or more in styrene-butadiene emulsion, polymethyl methacrylate-polybutylacrylate latex, Polyphenylethylene-butyl acrylate emulsion, ptfe emulsion, polyvinylidene fluoride emulsion.
6. lithium battery ceramic coating membrane as claimed in claim 5, it is characterized in that, additive in described ceramic coated slurry is water-soluble macromolecule, comprises one or more in sodium carboxymethylcellulose, hydroxyethylcellulose, hydroxypropyl methylcellulose, polyvinyl alcohol, polyethylene glycol, polyacrylamide.
7. lithium battery ceramic coating membrane as claimed in claim 6, it is characterized in that, the auxiliary agent in described ceramic coated slurry comprises one or more in tertiary alkyl polyalcohol polyvinylether, sulfonic group di-isooctyl sodium, alkylnaphthalene sulfonate, polyether modified silicon oil, polypropylene glycol-oxirane, polyethers stearate dimethyl siloxane, polyoxyethylene polyoxypropylene pentaerythrite ether, polyoxyethylene glycerol ether, polyoxyethylene polyoxy propyl alcohol amidogen ether.
8. a preparation method for lithium battery ceramic coating membrane, is characterized in that, comprises the steps:
Step 1, gets particle diameter and compares D
1/ D
2be 0.10 ~ 0.20 nano alumina powder jointed, be dispersed in deionized water water, prepare nano aluminium oxide aqueous dispersions;
Step 2, mixes described nano aluminium oxide aqueous dispersions with bonding agent, additive and auxiliary agent, configuration ceramic coated slurry, wherein aluminium oxide: the mass ratio of bonding agent is 5 ~ 20:1;
Step 3, by described ceramic coated slurry even application at base material membrane surface, obtains lithium battery ceramic coating membrane.
9. the preparation method of lithium battery ceramic coating membrane as claimed in claim 8, it is characterized in that, in described step 1, the solid content of nano aluminium oxide aqueous dispersions is 20 ~ 40%, and regulates its pH value to be 4.0 ~ 5.0.
10. the preparation method of lithium battery ceramic coating membrane as claimed in claim 9, it is characterized in that, also comprise the dispersant of 0.1-1.0wt% in described step 1 in nano aluminium oxide aqueous dispersions, described dispersant comprises one or more in neopelex, lauryl sodium sulfate, dodecyl sodium sulfate, calgon, polyacrylic acid, softex kw, octylphenolpolyoxyethylene, polyethylene glycol.
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