CN105514328A - Ceramic diaphragm for lithium ion battery and preparation method of ceramic diaphragm - Google Patents
Ceramic diaphragm for lithium ion battery and preparation method of ceramic diaphragm Download PDFInfo
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- CN105514328A CN105514328A CN201610022662.8A CN201610022662A CN105514328A CN 105514328 A CN105514328 A CN 105514328A CN 201610022662 A CN201610022662 A CN 201610022662A CN 105514328 A CN105514328 A CN 105514328A
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- ceramic
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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
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
-
- 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
-
- 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
- H01M50/431—Inorganic material
-
- 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 invention discloses a ceramic diaphragm for a lithium ion battery. The ceramic diaphragm comprises a diaphragm base material and a ceramic coating on the surface of the diaphragm base material, wherein ceramic particles having a porous structure and a high specific surface area are selected for the ceramic coating. A preparation method includes the following steps of firstly, evenly mixing ceramic particles, binder and solvent to obtain coating slurry; secondly, evenly coating the surface of the diaphragm base material with the coating slurry, and conducting drying to form the ceramic diaphragm. Quite strong binding force exists between the porous ceramic powder and the binder, and the powder falling phenomenon is effectively avoided; meanwhile, the ceramic diaphragm has high electrolyte wettability and quite strong liquid absorption capacity, the cycle life and rate capability of the lithium ion battery are increased, and excellent electrochemical performance is achieved; in addition, under the same thickness, the mass of the porous ceramic coating is far lower than that of an ordinary ceramic coating, and the energy density of the battery is improved.
Description
Technical field
The invention belongs to technical field of lithium ion, be specifically related to a kind of lithium ion battery ceramic diaphragm and preparation method thereof.
Background technology
The major function of lithium ion battery septation is isolation both positive and negative polarity and stops electronics to pass, and lithium ion can be allowed to pass through simultaneously, thus in charge and discharge process, complete the fast transport of lithium ion between both positive and negative polarity.The quality of membrane properties directly affects the quality of the internal resistance of cell, discharge capacity, service life cycle and battery safety.Polyolefine material has excellent mechanical property, chemical stability and relatively inexpensive feature, just be used widely at the lithium battery research and development initial stage, and become the main flow direction of lithium electric separator, as single-layer polypropylene (PP) microporous barrier, monolayer polyethylene (PE) microporous barrier and three layers of PP/PE/PP composite membrane.But the thermal stability of this barrier film is poor, be at high temperature easy to shrink, cause both positive and negative polarity to contact, and then cause battery to disintegrate or blast.In addition, polyolefine material parent electrolyte ability, keeps electrolyte scarce capacity, causes the poor performance such as battery cycle life, high current charge-discharge, and these shortcomings limit its use at power energy-storage battery.
In order to improve the problems referred to above, relatively more conventional method is the surface-coated ceramic material at polyalkene diaphragm, even if barrier film base material there occurs contraction or melts like this, ceramic coating still can stop both positive and negative polarity to contact, and prevents large area short circuit, promotes security performance.
The Chinese patent literature being CN104538573A as publication number discloses a kind of diaphragm for lithium ion battery and preparation method thereof, wherein, comprise step: a, inorganic filler, binding agent and solvent to be mixed, use churned mechanically mode to be prepared into uniform slurry; B, slurry to be coated on barrier film uniformly, to dry 2h ~ 24h in the baking oven being then positioned over 50 DEG C ~ 80 DEG C, just can obtain the inorganic matter coated separator of lithium ion battery.
In prior art, usually adopt common ceramic powder to apply, specific area only has tens m
2/ g to tens of m
2/ g, imbibition ability is still limited, and adhesion between ceramic particle and binding agent is more weak, easily occurs dry linting phenomenon.
Summary of the invention
The invention provides a kind of lithium ion battery ceramic diaphragm and preparation method thereof, this ceramic diaphragm has stronger imbibition ability and stability.
To achieve these goals, the present invention adopts following technical scheme:
A kind of lithium ion battery ceramic diaphragm, comprise barrier film base material and be compounded in the ceramic coating on its at least one surface, described ceramic coating comprises the ceramic particle with loose structure.
As preferably, the specific area>=200m of described ceramic particle
2/ g, the porosity>=45%, the particle diameter of ceramic particle is 20nm ~ 1 μm.
In ceramic diaphragm, ceramic coating is compounded in the one side of barrier film base material, also can two-sided at barrier film base material.In actual production process, ceramic particle can be configured to coating fluid, be coated in the surface of barrier film base material subsequently again.The present invention adopts specific area to be greater than 200m
2the porous of/g, the porosity>=45%, the ceramic particle of high-specific surface area, can increase the compound of ceramic coating and barrier film base material, adhesion effect, strengthen the mechanical strength of described ceramic diaphragm, reduces ceramic particle dry linting, obscission; The tension force of electrolyte and barrier film can also be reduced, improve wetability and the water retainability of described barrier film, the stress of barrier film can also be reduced, the thermal stability of the ceramic diaphragm obtained by raising simultaneously.
Described barrier film base material is polyolefin microporous film, as preferably, described barrier film base material is polyethylene (PE) monofilm, polypropylene (PP) monofilm or PP/PE/PP sandwich diaphragm, and the porosity of barrier film base material is 35 ~ 60%, and aperture is 30-500nm.
Described ceramic particle selects at least one in porous silica, alundum (Al2O3), titanium dioxide, zirconium dioxide.The particle diameter of described ceramic particle is 20nm ~ 1 μm.
The thickness of described ceramic coating is 1 ~ 10 μm.Under the thickness of this ceramic coating, the thickness of barrier film base material preferably 10 ~ 30 μm.
Further preferably, the specific area of described ceramic particle is 300-800m
2/ g, porosity 55-90%, the particle diameter of ceramic particle is 50 ~ 500nm.
As preferably, described ceramic particle is silicon dioxide and/or alundum (Al2O3), and specific area is 400-600m
2/ g, the porosity is 60 ~ 80%, and the particle diameter of ceramic particle is 60nm ~ 300nm.
Know by experiment, adopt the silicon dioxide of mixing and aluminum oxide ceramic particle can improve the thermal stability of described ceramic diaphragm and the wettability to electrolyte further, further preferably, the weight ratio of silicon dioxide and alundum (Al2O3) is 1:3-3:1.
The present invention also comprises the preparation method of above-mentioned lithium ion battery ceramic diaphragm, comprises the steps:
Step (1): ceramic particle, binding agent and solvent are mixed, obtains applying slurry;
Step (2): coating slurry is evenly coated in barrier film substrate surface, forms ceramic diaphragm through super-dry.
Preferably, described solvent is at least one in water, 1-METHYLPYRROLIDONE and DMF.
Further preferably, when solvent is water, binding agent is at least one in sodium carboxymethylcellulose (CMC)/butadiene-styrene rubber (SBR), gelatin/polyvinyl alcohol (PVA) and polyacrylate based terpolymers latex (LA132, LA133);
When solvent is 1-METHYLPYRROLIDONE or N, during dinethylformamide, binding agent is at least one in Kynoar (PVDF), Kynoar-hexafluoropropylene (PVDF-HFP), polymethyl methacrylate (PMMA), polyacrylonitrile (PAN).
When the water soluble polymer compositions such as the mixture of the mixture of sodium carboxymethylcellulose (CMC) and butadiene-styrene rubber (SBR), gelatin and polyvinyl alcohol (PVA) make binding agent, the performance of the multilayer composite membrane obtained by ratio regular meeting impact of each composition, when binding agent is CMC and SBR, the weight ratio of CMC:SBR is preferably 1:2 ~ 2:1.
When binding agent be gelatin and PVA time, the weight ratio of gelatin: PVA is preferably 1:5 ~ 1:20.
In described coating slurry, the ratio of ceramic particle and binding agent is 1:1 ~ 49:1, and the mass fraction of solvent is 40-90%.
The thickness that the slurry prepared according to the method described above is coated on base material is preferably 2-20 μm, and again through vacuum heat (drying) solidification after being coated with, as preferably, vacuum degree is 0.01MPa-0.1MPa, and heat treatment temperature is 70-90 DEG C.Drying time is 2 ~ 24 hours.
As preferably, described preparation method, comprises the steps:
Step (1): ceramic particle, binding agent and solvent are mixed, obtains applying slurry; Described solvent is water, and described binding agent is sodium carboxymethylcellulose (CMC)/butadiene-styrene rubber (SBR) or gelatin/polyvinyl alcohol (PVA); Wherein, the weight ratio of CMC:SBR is 1:2 ~ 2:1, and the weight ratio of gelatin: PVA is preferably 1:20 ~ 1:5; In described coating slurry, the ratio of ceramic particle and binding agent is 3:1 ~ 19:1, and the mass fraction of solvent is 60-80%.Described ceramic particle selects at least one of silicon dioxide, alundum (Al2O3), and the particle diameter of described ceramic particle is 50 ~ 500nm, and specific area is 400-600m
2/ g;
Step (2): coating slurry is evenly coated in barrier film substrate surface, coating thickness is 2 ~ 20 μm, forms ceramic diaphragm through vacuumize.Heat treatment temperature is 70 ~ 90 DEG C; Vacuum degree is 0.01 ~ 0.03MPa, and drying time is 8 ~ 10 hours.
As preferably, described preparation method, comprises the steps:
Step (1): ceramic particle, binding agent and solvent are mixed, obtains applying slurry; Described solvent is NMP or DMF, and described binding agent is Kynoar (PVDF) or Kynoar-hexafluoropropylene (PVDF-HFP); In described coating slurry, the ratio of ceramic particle and binding agent is 3:1 ~ 19:1, and the mass fraction of solvent is 60-80%.Described ceramic particle selects at least one of silicon dioxide, alundum (Al2O3), and the particle diameter of described ceramic particle is 50 ~ 500nm, and specific area is 400-600m
2/ g;
Step (2): coating slurry is evenly coated in barrier film substrate surface, coating thickness is 2 ~ 20 μm, forms ceramic diaphragm through vacuumize.Heat treatment temperature is 70 ~ 90 DEG C; Vacuum degree is 0.01 ~ 0.03MPa, and drying time is 8 ~ 10 hours.
Because ceramic coating in the present invention adopts the ceramic particle with loose structure, this ceramic particle has very high specific area, compared with existing ceramic diaphragm, has following beneficial effect:
(1) ceramic coating has good electrolyte wettability and extremely strong imbibition ability, improves cycle life and the high rate performance of lithium ion battery.
(2) adhesion between ceramic particle and binding agent strengthens greatly, effectively prevent dry linting phenomenon, enhances the stability of barrier film.
(3) under same thickness, the quality of porous ceramic coating, far below Ordinary ceramic coatings, improves the energy density of battery.
Embodiment
For making the present invention easier to understand, below in conjunction with embodiment, the invention will be further described.
In the present invention, the preparation method of porous alumina is as follows:
Using CTAB (softex kw) aqueous solution of 1g/L to prepare mass fraction is respectively the aluminum nitrate solution of 18% and the ammonium bicarbonate soln of 8%.Slowly be added drop-wise in aluminum nitrate solution by ammonium bicarbonate soln, rapid stirring forms colloidal sol, by colloidal sol vacuumize after standing a period of time, obtains white powder, is calcined by white powder and obtain porous alumina in 2 hours under 550 DEG C of conditions.It is obtained that porous alumina particle diameter is about 100nm, specific area is 432m
2/ g.
In the present invention, the preparation method of porous silica is as follows:
Ammoniacal liquor, 50g absolute ethyl alcohol that 2gCTAB, 10g concentration is 32% is added successively in 50mL deionized water, after being uniformly mixed, add 3.6g tetraethoxysilane, stir 2 hours, filtered by white precipitate and spend deionized water for several times, after drying, under 600 DEG C of conditions, calcining obtains porous silica in 6 hours; Obtained porous silica particle diameter is about 200nm, specific area is 576m
2/ g.
Embodiment 1
1,1g particle diameter is about 100nm, specific area is 432m
2the porous alumina powder of/g, 0.3g Kynoar (PVDF) and 7.5gN-methyl pyrrolidone (NMP) mix, and obtain ceramic coated slurry.
2, ceramic coated slurry is evenly coated in by coating machine the one side that thickness is polyethylene (PE) barrier film of 20 μm, under 80 DEG C of conditions, vacuum (vacuum degree 0.01MPa) is dried, and forms the ceramic diaphragm A1 that coating layer thickness is 3 μm.
Embodiment 2
1,1.5g particle diameter is about 200nm, specific area is 576m
2the porous silica silicon powder of/g, 0.1g sodium carboxymethylcellulose (CMC), 0.1g butadiene-styrene rubber (SBR) and 8g deionized water mix, and obtain ceramic coated slurry.
2, ceramic coated slurry is evenly coated in by coating machine the one side that thickness is polypropylene (PP) barrier film of 20 μm, under 80 DEG C of conditions, vacuum (vacuum degree 0.01MPa) is dried, and forms the ceramic diaphragm A2 that coating layer thickness is 4 μm.
Embodiment 3
1,2.4g particle diameter is about 200nm, specific area is 576m
2the porous silica silicon powder of/g, 0.7g polyvinyl alcohol (PVA), 0.1g gelatin and 12g deionized water mix, and obtain ceramic coated slurry
2, ceramic coated slurry is evenly coated in by coating machine the one side that thickness is the PP/PE/PP sandwich diaphragm of 20 μm, under 80 DEG C of conditions, vacuum (vacuum degree 0.01MPa) is dried, and forms the ceramic diaphragm A3 that coating layer thickness is 2 μm.
Embodiment 4
Compare with embodiment 2, difference is, in step 2, the porous alumina of employing weight ratio 3:1 and porous silica silicon powder, as ceramic particle, obtain ceramic diaphragm A4.The specification of porous alumina and porous silica is identical with embodiment 1 and embodiment 2 respectively.
Comparative example 1
Experimental procedure is with embodiment 1, and being changed into by the alundum (Al2O3) powder of porous than particle diameter 100nm, surface area is 28m
2the common alundum (Al2O3) powder of/g, other conditions are constant, obtain ceramic diaphragm B1.
Comparative example 2
The silicon-dioxide powdery of porous, with embodiment 2, is changed into particle diameter 200nm, specific area is 22m by experimental procedure
2the general silica powder of/g, other conditions are constant, obtain ceramic diaphragm B2.
Pick up is tested:
Select with LiPF
6as solute, the solution be dissolved in EC and DEC mixed solvent makes electrolyte, weighs the change of ceramic diaphragm quality before and after immersion liquid, and calculate pick up, result is as table 1:
Table 1
| Sample | A1 | A2 | A3 | A4 | B1 | B2 |
| Pick up/% | 825 | 886 | 732 | 916 | 215 | 233 |
Known by pick up test result, have employed the ceramic diaphragm that there is loose structure and high-specific surface area ceramic powder and carry out applying, its pick up will far away higher than the conventional ceramic barrier film using the coating of conventional ceramic powder, and high pick up will contribute to extending cycle life, improving high rate performance.
Charge-discharge test:
Make positive pole with nickle cobalt lithium manganate (NCM532), lithium sheet makes negative pole, and the barrier film prepared by embodiment and comparative example is assembled into button cell.Test as follows respectively: (1) charge and discharge cycles 100 times under 0.5C multiplying power, calculated capacity conservation rate, result is as table 2; (2) first discharge and recharge 5 times under 0.2C multiplying power, then discharge and recharge 5 times under 1C multiplying power, calculate high rate performance (the 10th discharge capacity/the 5th discharge capacity), result is as table 3.
Table 2
| Sample | A1 | A2 | A3 | A4 | B1 | B2 |
| Capability retention/% | 87.3 | 88.4 | 86.7 | 88.9 | 81.6 | 82.1 |
Table 3
| Sample | A1 | A2 | A3 | A4 | B1 | B2 |
| High rate performance/% | 86.3 | 86.9 | 85.5 | 87.8 | 82.2 | 83.3 |
From table 2 and table 3, the ceramic diaphragm cycle performance of embodiment and high rate performance all obviously will be better than comparative example.Above result shows, the ceramic powder of choice for use porous type, high-specific surface area carries out to barrier film the chemical property that surface-coated obviously can improve barrier film, and effect is better than conventional ceramic powder.
Claims (9)
1. a lithium ion battery ceramic diaphragm, is characterized in that, comprise barrier film base material and be compounded in the ceramic coating on its at least one surface, described ceramic coating comprises the ceramic particle with loose structure.
2. lithium ion battery ceramic diaphragm according to claim 1, the specific area>=200m of described ceramic particle
2/ g, the porosity>=45%, the particle diameter of ceramic particle is 20nm ~ 1 μm.
3. lithium ion battery ceramic diaphragm according to claim 1, the thickness of described ceramic coating is 1 ~ 10 μm.
4. lithium ion battery ceramic diaphragm according to claim 1, is characterized in that, described barrier film base material is polyethylene monolayer film, polypropylene monofilm or PP/PE/PP sandwich diaphragm, and the porosity of barrier film base material is 35 ~ 60%, and aperture is 30-500nm.
5. lithium ion battery ceramic diaphragm according to claim 1, is characterized in that, described ceramic particle selects at least one in porous silica, alundum (Al2O3), titanium dioxide, zirconium dioxide.
6. the preparation method of lithium ion battery ceramic diaphragm as described in claim as arbitrary in Claims 1 to 5, is characterized in that, comprise the steps:
Step (1): ceramic particle, binding agent and solvent are mixed, obtains applying slurry;
Step (2): coating slurry is evenly coated in barrier film substrate surface, forms ceramic diaphragm through super-dry.
7. the preparation method of lithium ion battery ceramic diaphragm according to claim 6, it is characterized in that, described solvent is at least one in water, 1-METHYLPYRROLIDONE and DMF.
8. the preparation method of lithium ion battery ceramic diaphragm according to claim 7, it is characterized in that, when solvent is water, binding agent is at least one in sodium carboxymethylcellulose/butadiene-styrene rubber mixture, gelatin/polyvinyl alcohol mixture, polyacrylate based terpolymers latex;
When solvent be 1-METHYLPYRROLIDONE or DMF time, binding agent is at least one in Kynoar, Kynoar-hexafluoropropylene and polymethyl methacrylate.
9. the preparation method of lithium ion battery ceramic diaphragm according to claim 6, it is characterized in that, in described coating slurry, the ratio of ceramic particle and binding agent is 1:1 ~ 49:1, and the mass fraction of solvent is 40-90%.
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