CN104600231A - Diaphragm provided with active nano boron nitride coating, and preparation method of diaphragm - Google Patents
Diaphragm provided with active nano boron nitride coating, and preparation method of diaphragm Download PDFInfo
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- CN104600231A CN104600231A CN201410853236.XA CN201410853236A CN104600231A CN 104600231 A CN104600231 A CN 104600231A CN 201410853236 A CN201410853236 A CN 201410853236A CN 104600231 A CN104600231 A CN 104600231A
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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
- H01M50/431—Inorganic 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
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- 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
- H01M50/449—Separators, membranes or diaphragms characterised by the material having a layered structure
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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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- Materials Engineering (AREA)
- Inorganic Chemistry (AREA)
- Cell Separators (AREA)
Abstract
The invention belongs to the field of battery material, and provides a diaphragm provided with an active nano boron nitride coating. The diaphragm comprises a polyolefin film of a base layer and the active nano boron nitride coating, wherein the base layer is coated with the active nano boron nitride coating; the thickness of the single layer of coating is 1-3% of that of the base layer, and the thickness of the two layers of coating is 2-5% of that the base layer. The diaphragm provided with the flaky nano boron nitride coating has heat resistance and mechanical property, but a composite polymer system does not have the heat resistance and the mechanical property; compared with the traditional diaphragm provided with an aluminum oxide coating, the diaphragm provided with the active nano boron nitride coating has more excellent liquid absorbing/ liquid retaining capacity as well as ionic conductivity. Furthermore, the diaphragm provided with the boron nitride coating has the advantages of being thin in thickness, low in battery internal resistance, high in porosity and the like, is capable of enabling a lithium ion battery to have higher capacity when the battery is charged and discharged at high rate, and has excellent high-rate performance and cycle performance.
Description
Technical field
The invention belongs to battery material field, be specifically related to barrier film of a kind of lithium ion battery and preparation method thereof.
Background technology
Along with haze weather increases the weight of and energy crisis Step wise approximation day by day, new-energy automobile starts to enter public view, and obtains Rapid Popularization, and future just becomes day by day urgent to the demand of lithium ion battery material.And barrier film is as one of key component in power lithium-ion battery, play isolation both positive and negative polarity, allow the key effect that lithium ion reciprocates through between both positive and negative polarity, the quality of its gas permeability, paracentesis resistance and heat-shrinkable directly affects capacity and the cycle performance of lithium ion battery simultaneously.
At present, 3 layers of microporous compound film that traditional lithium ion battery separator extensively adopts polyethene microporous membrane (PP), microporous polypropylene membrane (PE) and is made up of polypropylene, polyethylene, polypropylene.It has that mechanical strength is excellent, fire prevention, chemical-resistant reagent, acid-alkali-corrosive-resisting are good, good biocompatibility, the advantage such as nontoxic.But the thermal contraction at high temperature of this barrier film can cause positive/negative plate to contact, bring local heat release rapidly, thus have huge potential safety hazard; Simultaneously poor, the puncture-resistant poor-performing of the wettability of TPO barrier film to polarity electrolyte.And add the polyolefin complex barrier film that nano aluminium oxide prepares, although the conductance of polymer dielectric film can be improved, improve its thermal endurance and imbibition/liquid-keeping property, but nano aluminium oxide crystal belongs to close-packed structure, be coated in by alumina powder on barrier film, on the one hand, alumina particle may block the space of barrier film, be unfavorable for the embedding of lithium ion and deviate from, cause efficiency for charge-discharge to reduce and capacitance loss.On the other hand, aluminum oxide coating layer significantly increases battery diaphragm thickness, not only increase the internal resistance of battery, and hindering the flowing of electrolyte, conductance declines, and after circulation, the internal resistance of cell increases speed quickening, heating is many, temperature raises and causes electrolyte to decompose rapidly generation gas, and barrier film melts, and causes the short circuit of battery inflatable to explode.
Therefore, at present in the urgent need to developing a kind of barrier film containing excellent coating, it can solve the safety problem of above battery, can ensure the lifting of the chemical property of lithium ion battery and the prolongation in useful life simultaneously.
Summary of the invention
For the problem existing for this area, a kind of barrier film having active nano boron nitride coating is proposed.
Another object of the present invention is the preparation method proposing described barrier film.
3rd object of the present invention proposes the lithium ion battery containing described barrier film.
The technical scheme realizing above-mentioned purpose of the present invention is:
There is a barrier film for active nano boron nitride coating, the polyolefin film that described barrier film comprises basic unit and the active nano boron nitride coating be coated on basic unit's one or both sides; In basic unit's one side, the thickness of coating is the 1-3% of groundwork thickness, and on basic unit two sides, the thickness of coating is altogether the 2-5% of groundwork thickness.
Wherein, described polyolefin film is the one in the microporous compound film of polyethene microporous membrane, microporous polypropylene membrane, polyethylene film and polypropylene screen composition, and the thickness of described polyolefin film is 25 μm-40 μm, and porosity is 45-55%.
Prepare the method having active nano boron nitride coating barrier film of the present invention, comprise step:
1) slurry is prepared: slurry is grouped into by the following one-tenth of mass parts: boron nitride powder: bonding agent PVDF: organic solvent NMP: surface modifier dimethicone=20-75:1-5:15-80:0.1-5;
In pulper, first add organic solvent, after bonding agent is joined in organic solvent, dissolve with the rotating speed high-speed stirred 0.5-3h of 10-10000r/min; Add boron nitride powder and surface modifier again, then with the rotating speed high-speed stirred 1-10h of 10-10000r/min, make coating slurry;
2) with coating machine by step 1) obtained coating slurry is coated on polyolefin film, the thickness of slurry coating is 0.5-5 μm, then coated polyolefin film is placed on 60-100 DEG C of insulation 1-6h in baking oven.
Wherein, described boron nitride powder is the boron nitride powder of hexagonal structure; Particle diameter is 200-300nm.Further, described boron nitride powder is by water heat transfer.
Described nm-class boron nitride powder is lamellar structure, is coated on barrier film, and thin layer is conducive to the thickness reducing barrier film, reduces the internal resistance of lithium ion battery to a certain extent, ensures the optimization of battery high-rate discharge ability and cycle performance.Due to boron nitride sheet interlayer and and barrier film between have larger space, this is just conducive to the flowing of electrolyte and the embedding of lithium ion and deviates from, and is conducive to afterwards improving the efficiency for charge-discharge of lithium ion battery and capacity.
Wherein, described bonding agent is the PVDF emulsion of solid content 40%-60%.
Wherein, described organic solvent is one or more in NMP (1-METHYLPYRROLIDONE), DMF (dimethyl formamide), DMAC (dimethylacetylamide).
Wherein, described surface modifier is one or more in sorbester p17, dimethicone, Emulsifier EL-60, glycerin monostearate.
Further, described slurry is grouped into by the following one-tenth of mass parts: boron nitride powder: binding agent: organic solvent: surface modifier=20-75:1-5:15-80:0.1-5.
Lithium ion battery containing barrier film of the present invention.The positive electrode of described battery can be cobalt acid lithium, LiMn2O4, LiFePO4 or the cobalt acid lithium, LiMn2O4, the LiFePO4 that are doped with iron, nickel, manganese, magnesium, titanium.The negative material of described battery is carbon materials.Preferably, positive electrode is LiNi
1/3co
1/3mn
1/3o
2material and acetylene black, PTFE in mass ratio 16:3:1 mix obtained positive electrode, and electrolyte is LiPF
6with the mixture of DMC+EMC+EC (volume ratio of dimethyl carbonate+methyl ethyl carbonate+ethylene carbonate is 1:1:1).
Beneficial effect of the present invention is:
Compared with prior art, the barrier film of nano-sheet boron nitride coating provided by the invention provides the thermal endurance and mechanical performance that complex polymer system do not have, and also demonstrates the imbibition/liquid-keeping property more excellent than the barrier film of conventional oxidation aluminized coating and ionic conductivity.In addition, the barrier film of boron nitride coating has that membrane thicknesses is little, the internal resistance of cell is low, porosity advantages of higher, and can ensure lithium ion battery under high magnification during discharge and recharge, capacity is higher, shows outstanding multiplying power property and cycle performance.
The diaphragm material that the present invention proposes, the electrode diaphragm that effectively can solve conventional aluminium oxide coated separator often has melts the battery short circuit problem caused, avoid the generation of security incident, good security performance can be had, ensure that the long-time normal of lithium ion battery uses.
Accompanying drawing explanation
Fig. 1 is the polyalkene diaphragm structure diagram of one side coating boron nitride powder.
Fig. 2 is the polyalkene diaphragm structure diagram of double spread boron nitride powder.
In figure, 1 is polyalkene diaphragm, and 2 is boron nitride coating.
Fig. 3 is embodiment 1-5 charge-discharge property curve.
Fig. 4 is the charge and discharge cycles volume change curve of embodiment 1-5.
Fig. 5 is the SEM figure of boron nitride powder.
Embodiment
Following examples for illustration of the present invention, but are not used for limiting the scope of the invention.
Boron nitride powder is water heat transfer, and Fig. 5 is shown in by its SEM photo.Particle diameter is about 260nm.
Embodiment 1
Prepare slurry.The proportioning of slurry is: the boron nitride powder of 20kg, the dimethicone of the NMP of the PVDF of 1kg, 78.9kg, 0.1kg.
First, in pulper, first add NMP, after PVDF is joined in NMP, with the rotating speed of 10r/min stir 0.5h dissolve; Add boron nitride powder and dimethicone again, stir 1h, make coating slurry.The barrier film slurry be stirred is on coating machine, at pre-prepd polyethene microporous membrane (film thickness 30 μm, porosity is 50%) on carry out single coating operation (wherein slurry coating thickness in monolayer is 0.5 μm), the membrane configuration obtained is as Fig. 1, then coated barrier film is placed on 100 DEG C of insulation 1h in baking oven, obtains barrier film sample S1.
Prepare button cell.By homemade LiNi
1/3co
1/3mn
1/3o
2material and acetylene black, PTFE in mass ratio (16:3:1) mix ultrasonic and stir and obtain positive electrode, and put into 120 DEG C, baking oven insulation half an hour, roll-in obtains positive plate.Using metal lithium sheet as to electrode, 1mol/LLiPF
6/ DMC+EMC+EC (volume ratio is 1:1:1) is electrolyte, is assembled into button cell, obtains battery sample B1 in the glove box being full of argon gas.
Performance test is carried out to barrier film sample S1 and battery sample B1.
Embodiment 2
Prepare slurry.Wet end furnish is: the boron nitride powder of 40kg, the dimethicone of the NMP of the PVDF of 5kg, 50kg, 5kg.First in pulper, first add NMP, after PVDF is joined in NMP, dissolve with the rotating speed high-speed stirred 3h of 10000r/min; Add boron nitride powder and dimethicone again, high-speed stirred 10h, make coating slurry.The barrier film slurry be stirred is on coating machine, at pre-prepd polyethene microporous membrane, (film thickness is 30 μm, porosity is 50%) on carry out single coating operation (slurry coating thickness in monolayer is 1 μm), then coated barrier film is placed on 60 DEG C of insulation 6h in baking oven, obtains barrier film sample S2.
Adopt the step identical with embodiment 1 to prepare button cell sample B2, and performance test is carried out to barrier film sample S2 and battery sample B2.
Embodiment 3
Prepare slurry.Wet end furnish is: the boron nitride powder of 75kg, the dimethicone of the NMP of the PVDF of 5kg, 15kg, 5kg.First, in pulper, first add NMP, after PVDF is joined in NMP, dissolve with the rotating speed high-speed stirred 2.5h of 6000r/min; Add boron nitride powder and dimethicone again, high-speed stirred 7h, make coating slurry.The barrier film slurry be stirred is on coating machine, at pre-prepd microporous polypropylene membrane (film thickness 30 μm, porosity is 50%) one side on carry out painting work (slurry coating thickness is 2 μm), then coated barrier film is placed on 70 DEG C of insulation 4h in baking oven, obtains barrier film sample S3.
Adopt the step identical with embodiment 1 to prepare button cell sample B3, and performance test is carried out to barrier film sample S3 and battery sample B3.
Embodiment 4
Prepare slurry.Wet end furnish is: the boron nitride powder of 75kg, the dimethicone of the NMP of the PVDF of 5kg, 15kg, 5kg.First, in pulper, first add NMP, after PVDF is joined in NMP, dissolve with the rotating speed high-speed stirred 2.5h of 6000r/min; Add boron nitride powder and dimethicone again, high-speed stirred 7h, make coating slurry.The barrier film slurry be stirred is on coating machine, at pre-prepd microporous polypropylene membrane (film thickness 30 μm, porosity is 50%) two sides on carry out the identical painting work of thickness (slurry coating two layers of thickness is 5 μm altogether), then coated barrier film is placed on 70 DEG C of insulation 4h in baking oven, obtains barrier film sample S4.The structure of barrier film is see Fig. 2.
Adopt the step identical with embodiment 1 to prepare button cell sample B4, and performance test is carried out to barrier film sample S4 and battery sample B4.
Comparative example
Prepare slurry.Wet end furnish is: 75kg's is alumina powder jointed, the dimethicone of the NMP of the PVDF of 5kg, 15kg, 5kg.First, in pulper, first add NMP, after PVDF is joined in NMP, dissolve with the rotating speed high-speed stirred 2.5h of 6000r/min; Add alumina powder jointed and dimethicone again, high-speed stirred 7h, make coating slurry.The barrier film slurry be stirred is on coating machine, at pre-prepd microporous polypropylene membrane (film thickness 30 μm, porosity is 50%) painting work (slurry coating two layers of thickness is altogether 5 μm) is carried out on two sides, then coated barrier film is placed on 70 DEG C of insulation 4h in baking oven, obtains barrier film sample S5.
Adopt the step identical with embodiment 1 to prepare button cell sample B5, and performance test is carried out to barrier film sample S5 and battery sample B5.
Performance test:
1, battery diaphragm test
Adopt thickness and the porosity of contact thickness gauge and mercury injection apparatus test battery barrier film sample S1-S5, test result is as shown in table 1.
Table 1
| Sample | Membrane thicknesses (μm) | Barrier film porosity (%) |
| S1 | 30.45 | 40 |
| S2 | 30.78 | 42 |
| S3 | 31.43 | 46 |
| S4 | 34.65 | 47 |
| S5 | 34.83 | 43 |
2, battery performance test
Charge-discharge property and cycle performance test are carried out to lithium ion battery sample B1-B5.Carry out the charge and discharge cycles experiment (1C charging 2C electric discharge) of 1C/2C at 20 DEG C, test loop number of times is 100 times.Test result as shown in Figure 3, Figure 4.
The present invention adopts the diaphragm design of nano-sheet boron nitride coating, and boron nitride coating 2 is coated in polyalkene diaphragm 1 surface, greatly reduces, containing the thickness of coated separator, on average to thicken less than 5 μm, and ensure the porosity of barrier film 40% and more than.Meanwhile, buckle electricity B1, B2, B3 of being made up of the barrier film of nano-sheet boron nitride coating put specific capacitance first all at about 140mAh/g, and through 100 these cycle charge-discharges, capability retention can reach 87.86%, 91.14%, 92.27% respectively.Especially, detain the first discharge specific capacity of electric B4 up to 146.2mAh/g, capability retention is 93.32%.
And the first discharge specific capacity of the button electricity B5 that nano aluminium oxide coated separator is made is 144.1mAh/g, capability retention is 92.34%.In visible equal pulp furnish situation; the electrochemical properties that boron nitride coating barrier film is more excellent than conventional aluminium oxide coated separator; and better to protect due to duplex coating and to support the upper and lower surface structures of basic unit's barrier film; make the embedding of lithium ion and deviate from more smooth and easy; also be conducive to the flowing of electrolyte, the chemical property of made button electricity is made compared with signal layer coating barrier film, and to buckle electricity more excellent.
Above embodiment is only be described the preferred embodiment of the present invention; not scope of the present invention is limited; under not departing from the present invention and designing the prerequisite of spirit; the various modification that the common engineers and technicians in this area make technical scheme of the present invention and improvement, all should fall in protection range that claims of the present invention determine.
Claims (9)
1. there is a barrier film for active nano boron nitride coating, it is characterized in that, the polyolefin film that described barrier film comprises basic unit and the active nano boron nitride coating be coated on basic unit's one or both sides; In basic unit's one side, the thickness of coating is the 1-3% of groundwork thickness, and on basic unit two sides, the thickness of coating is altogether the 2-5% of groundwork thickness.
2. barrier film according to claim 1, it is characterized in that, described polyolefin film is the one in the microporous compound film of polyethene microporous membrane, microporous polypropylene membrane, polyethylene film and polypropylene screen composition, and the thickness of described polyolefin film is 25 μm-40 μm, and porosity is 45-55%.
3. the method that have active nano boron nitride coating barrier film of preparation described in claim 1 or 2, is characterized in that, comprise step:
1) slurry is prepared: slurry is grouped into by the following one-tenth of mass parts: boron nitride powder: bonding agent: organic solvent: surface modifier=20-75:1-5:15-80:0.1-5;
In pulper, first add organic solvent, after bonding agent is joined in organic solvent, dissolve with the rotating speed high-speed stirred 0.5-3h of 10-10000r/min; Add boron nitride powder and surface modifier again, then with the rotating speed high-speed stirred 1-10h of 10-10000r/min, make coating slurry;
2) with coating machine by step 1) obtained coating slurry is coated on polyolefin film one or both sides, the thickness of slurry coating is 0.5-5 μm, then coated polyolefin film is placed on 60-100 DEG C of insulation 1-6h in baking oven.
4. method according to claim 3, is characterized in that, described boron nitride powder is the boron nitride powder of hexagonal structure; Particle diameter is 200-300nm.
5. method according to claim 3, is characterized in that, described bonding agent is the PVDF emulsion of solid content 40%-60%.
6. method according to claim 3, is characterized in that, described organic solvent is one or more in NMP, DMF, DMAC.
7. method according to claim 3, is characterized in that, described surface modifier is one or more in sorbester p17, dimethicone, Emulsifier EL-60, glycerin monostearate.
8., according to the arbitrary described method of claim 3-7, it is characterized in that, described slurry is grouped into by the following one-tenth of mass parts: boron nitride powder: bonding agent: organic solvent: surface modifier=40-75:5:50-80:0.1-5.
9. the lithium ion battery containing barrier film described in claim 1 or 2.
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| CN105776157A (en) * | 2016-05-04 | 2016-07-20 | 合肥国轩高科动力能源有限公司 | Preparation method of boron nitride colloids for coating lithium-ion battery separators |
| CN106058321A (en) * | 2016-07-14 | 2016-10-26 | 中夏新能源（上海）有限公司 | Explosion-proof lithium ion battery for military police and automobiles |
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