CN111129405A - Mixed coating diaphragm slurry and preparation method thereof, mixed coating diaphragm and lithium battery - Google Patents
Mixed coating diaphragm slurry and preparation method thereof, mixed coating diaphragm and lithium battery Download PDFInfo
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- CN111129405A CN111129405A CN201911400866.0A CN201911400866A CN111129405A CN 111129405 A CN111129405 A CN 111129405A CN 201911400866 A CN201911400866 A CN 201911400866A CN 111129405 A CN111129405 A CN 111129405A
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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
- H01M50/446—Composite material consisting of a mixture of organic and inorganic materials
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
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- 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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Abstract
The invention discloses a mixed coating diaphragm slurry which comprises the following components in parts by weight: 100 parts of deionized water, 0.5-1.0 part of dispersant, 0.5-10.0 parts of thickener, 5-7 parts of binder, 5-30 parts of alumina powder and 6-10 parts of PVDF emulsion. Compared with the traditional mixed coating diaphragm slurry, the mixed coating diaphragm slurry has the advantages that PVDF particles are smaller and are more uniformly mixed with alumina powder, the stacking density of a coating formed by the mixed coating diaphragm slurry is greatly improved, the thermal shrinkage at 130 ℃ for 1h is 0.5-1.5%, the mixed coating diaphragm slurry is far smaller than the traditional mixed coating diaphragm, and the high temperature resistance and the needling strength of the obtained diaphragm are improved.
Description
Technical Field
The invention relates to the technical field of lithium battery diaphragms, in particular to a mixed coating diaphragm slurry, a mixed coating diaphragm and a lithium battery.
Background
And the mixed coating membrane is an alumina and PVDF mixed coating membrane. It is intended that the high temperature resistance of alumina and the adhesion properties of PVDF be combined. However, the conventional mixed coating diaphragm has no high temperature resistance of alumina, and the adhesive force performance of PVDF is weakened.
Because the common mixed coating diaphragm has overlarge thermal shrinkage at 130 ℃, the advantages of the mixed coating diaphragm do not exist, the high temperature resistance of the alumina is not existed, and the adhesive force performance between the PVDF and the battery pole piece is reduced.
Disclosure of Invention
The invention aims to provide mixed coating diaphragm slurry aiming at the defect of excessive thermal shrinkage at 130 ℃ of a mixed coating diaphragm in the prior art.
The invention also aims to provide a preparation method of the mixed coating diaphragm slurry.
It is another object of the present invention to provide a hybrid coated separator.
Another object of the present invention is to provide a lithium battery.
The technical scheme adopted for realizing the purpose of the invention is as follows:
the mixed coating diaphragm slurry comprises the following components in parts by weight: 100 parts of deionized water, 0.5-1.0 part of dispersant, 0.5-10 parts of thickener, 5-7 parts of binder, 5-30 parts of alumina powder and 6-10 parts of PVDF emulsion.
In the above technical solution, preferably, the composition comprises the following components in parts by weight: 100 parts of deionized water, 0.6-0.8 part of dispersant, 0.5-0.7 part of thickener, 5-7 parts of binder, 9-11 parts of alumina powder and 8-10 parts of PVDF emulsion.
In the technical scheme, the particle size of the alumina powder is 0.5-2.5 um; the particle size of PVDF in the PVDF emulsion is 100-200 nm.
In the technical scheme, the dispersing agent is one or a mixture of modified polyether polymer, fatty alcohol, sodium polyethylene glycol alkyl aryl ether sulfonate, alkylphenol polyethenoxy ether, polyoxyethylene alkylphenol ether and sodium polyacrylate in any proportion;
the thickening agent is one or a mixture of PVA (polyvinyl alcohol), PEG (polyethylene glycol), PVP (polyvinylpyrrolidone) and CMC (sodium carboxymethylcellulose) in any proportion;
the binder is one of polymethyl acrylate and xanthan gum or a mixture of the polymethyl acrylate and the xanthan gum in any proportion.
In another aspect of the present invention, the preparation method of the mixed coating diaphragm slurry comprises the following steps:
step 1: adding a dispersing agent into deionized water, adding alumina powder after uniformly stirring, and sanding after uniformly stirring at a high speed;
step 2: adding PVDF emulsion and stirring uniformly;
and step 3: adding the thickening agent and the binder, and uniformly stirring.
In the above technical solution, in step 1, the high-speed stirring condition is that a stirrer is used to stir at a high speed of 800-; the sanding condition is that a sand mill is used for sanding for 3-15min at the speed of 500-1200 r/min.
In another aspect of the present invention, a method for preparing a mixed coating diaphragm slurry includes the following steps:
step 1: adding a dispersing agent into deionized water, adding alumina powder after uniformly stirring, and sanding after uniformly stirring at a high speed;
step 2: adding PVDF emulsion and stirring uniformly;
and step 3: adding the thickening agent and the binder, and uniformly stirring.
In another aspect of the invention, a mixed coating diaphragm comprises a base film and a coating layer formed after the mixed coating diaphragm slurry is coated on one side or two sides of the base film; the base film is made of a PP film or a PE film, the thickness of the base film is 5-25 mu m, and the thickness of the coating on each side is 1-5 mu m.
In another aspect of the invention, the mixed coating diaphragm is applied to a lithium battery.
In another aspect of the invention, a lithium battery includes a positive electrode, a negative electrode, an electrolyte, and the above mixed coating separator.
Compared with the prior art, the invention has the beneficial effects that:
1. the mixed coating diaphragm slurry provided by the invention uses PVDF emulsion as a raw material instead of PVDF powder, and is matched with a certain formula proportion, so that the dispersibility is better, the PVDF emulsion is distributed in small particles in the slurry, the particle size distribution is small and concentrated, and the bulk density of the formed coating is greatly improved.
2. The thermal shrinkage of the mixed coating diaphragm at 130 ℃ for 1h is 0.5-1.5%, which is smaller than that of the traditional mixed coating diaphragm, the tensile strength of 200-230Mpa is improved compared with that of the traditional mixed coating diaphragm, and the high temperature resistance and the needling strength of the obtained diaphragm are improved.
Drawings
FIG. 1 is an SEM image of a hybrid coated membrane of example 1.
Fig. 2 is an SEM image of the separator in comparative example 1.
Detailed Description
The present invention will be described in further detail with reference to specific examples. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
The mixed coating diaphragm slurry comprises the following components in parts by weight: 100 parts of deionized water, 1.0 part of dispersant, 0.5 part of thickener, 7 parts of binder, 30 parts of alumina powder and 10 parts of PVDF emulsion.
A preparation method of mixed coating diaphragm slurry comprises the following steps:
step 1: 0.3kg of polyethylene glycol alkyl aryl ether sodium sulfonate is added into 30kg of deionized water, stirred by a stirrer (double-planet stirrer) at a speed of 40r/min for 15min, then 9kg of alumina powder is added, stirred by the stirrer at a high speed of 1500r/min for 30min, and then ground by a sand mill at a speed of 800r/min for 10 min.
Step 2: adding 3.0kg of PVDF emulsion and stirring at a high speed of 1500r/min for 30min by using a stirrer;
and step 3: adding 0.15kg of PVA and 2.1kg of polymethyl acrylate, and stirring for 5-25min at the speed of 25-50r/min by using a stirrer to obtain the mixed coating diaphragm slurry.
Wherein the particle size of the alumina powder is 1.2-2.5um, and the manufacturer is Shandong China porcelain; the particle size of PVDF in the PVDF emulsion is 100-200nm, and the manufacturer is Achima.
A mixed coating diaphragm comprises a base film and a coating formed by coating the mixed coating diaphragm slurry on two sides of the base film through a micro gravure roller coating process, then drying the base film in a baking oven at 75 ℃ for 1.5 min. Wherein the base film is made of a PE film, the thickness of the base film is 9 micrometers, and the thickness of each side coating is 2 micrometers.
The SEM image of the hybrid coating membrane is shown in fig. 1.
The mixed coating membrane has the air permeability value of 115s/100ml, the areal density of 9.4 g/square meter, the needling strength of 5.5N and the tensile strength of 230Mpa (MD direction); baking at 130 deg.C for 1 hr under 200Mpa (TD direction), heat shrinkage of 1.2% (MD) and 0.5(TD), water content of 578ppm, and film breaking temperature of 156 deg.C.
The lithium battery manufactured by applying the diaphragm comprises: the positive electrode is made of a ternary material, the negative electrode is made of graphite, the electrolyte is EC/DMC/EMC (1: 1: 1), the standard electrolyte with the concentration of 1mol/L lithium hexafluorophosphate is assembled into a half battery, after the half battery is cycled for 100 circles under the multiplying power of 0.5C, the specific capacity is 156mAh/g, the capacity retention rate is 95.55%, and the average coulombic efficiency is 98.8%.
Comparative example 1
Comparative example 1 compared to example 1, the PVDF emulsion was changed to PVDF powder.
A diaphragm slurry comprises the following components in parts by weight: 100 parts of deionized water, 1.0 part of dispersant, 0.5 part of thickener, 7 parts of binder, 30 parts of alumina powder and 10 parts of PVDF powder.
A preparation method of mixed coating diaphragm slurry comprises the following steps:
step 1: 0.3kg of polyethylene glycol alkyl aryl ether sodium sulfonate is added into 30kg of deionized water, stirred by a stirrer at a speed of 40r/min for 15min, then 9kg of alumina powder is added, stirred by the stirrer at a high speed of 1500r/min for 30min, and then ground by a sand mill at a speed of 800r/min for 10 min.
Step 2: adding 3.0kg of PVDF powder and stirring at a high speed of 1500r/min for 30min by using a stirrer;
and step 3: adding 0.15kg PVA and 2.1kg polymethyl acrylate, and stirring with a stirrer at a speed of 25-50r/min for 5-25min to obtain the diaphragm slurry.
Wherein the particle size of the alumina powder is 1.2-2.5um, and the manufacturer is Shandong China porcelain. The stirrer is a double-planet stirrer and is a stirring system with a dispersion disc. The inner part is divided into a stirring paddle and a dispersing paddle. If the stirring is performed uniformly, the stirring paddle is 20-50 r/min; if ceramic powder or PVDF powder is added for dispersion, high-speed dispersion slurry needs to be started, namely 800-2000 r/min.
A diaphragm comprises a base film and a coating formed by coating the diaphragm slurry on two sides of the base film through a micro gravure roller coating process, then passing through a 75 ℃ oven, and baking and drying for 1.5 min. Wherein the base film is made of a PE film, the thickness of the base film is 9 micrometers, and the thickness of each side coating is 2 micrometers.
The SEM image of the separator is shown in fig. 2. Comparing fig. 1 and 2, the bulk density of the coating layer of the hybrid coating membrane of example 1 is far higher than that of the hybrid coating membrane of comparative example 1, which is also the reason for the improved high temperature resistance of the hybrid coating membrane of the present invention.
The air permeability value of the diaphragm is 130s/100ml, the area density is 6.4 g/square meter, the needling strength is 5.0N, and the tensile strength is 200Mpa (MD direction); 180Mpa (TD direction), baking at 130 ℃ for 1h, respectively having heat shrinkage of 8.5% (MD) and 5.5(TD direction), moisture content of 513ppm, and rupture temperature of 148 ℃.
It can be seen that the mixed coating diaphragm prepared from the mixed coating diaphragm slurry improved according to the invention (example 1) has a significantly increased areal density due to the increased bulk density, i.e., the coverage of the base film by the coating layer is increased, the thermal insulation effect is increased, and the thermal shrinkage performance is improved, compared to the diaphragm before the improvement (comparative example 1), and the thermal shrinkage at 130 ℃ for 1h in example 1 is 1.2% (MD) and 0.5(TD), which is far better than the diaphragm in comparative example 1. The tensile strength and the rupture temperature are obviously improved compared with those before the improvement, and in addition, the needling strength and the air permeability are also improved.
The lithium battery manufactured by applying the diaphragm comprises: the positive electrode is made of a ternary material, the negative electrode is made of graphite, the electrolyte is EC/DMC/EMC (1: 1: 1), the standard electrolyte with the concentration of 1mol/L lithium hexafluorophosphate is assembled into a half battery, after the half battery is cycled for 100 circles under the multiplying power of 0.5C, the specific capacity is 152mAh/g, the capacity retention rate is 93.21%, and the average coulombic efficiency is 98.7%.
Example 2
The mixed coating diaphragm slurry comprises the following components in parts by weight: 100 parts of deionized water, 0.5 part of dispersant, 0.7 part of thickener, 5 parts of binder, 5 parts of alumina powder and 6 parts of PVDF emulsion.
A preparation method of mixed coating diaphragm slurry comprises the following steps:
step 1: 0.15kg of alkylphenol polyvinyl ether is added into 30kg of deionized water, stirred for 15min at the speed of 40r/min by using a stirrer, then 1.5kg of alumina powder is added, stirred for 30min at the speed of 1500r/min by using the stirrer at a high speed, and then ground for 10min at the speed of 800r/min by using a sand mill.
Step 2: adding 1.8kg of PVDF emulsion and stirring at a high speed of 800r/min for 30min by using a stirrer;
and step 3: adding 0.15kg of CMC and 1.5kg of xanthan gum, and stirring for 5-25min at the speed of 25-50r/min by using a stirrer to obtain the mixed coating diaphragm slurry.
Wherein the particle size of the alumina powder is 1.2-2.5um, and the manufacturer is Shandong China porcelain; the particle size of PVDF in the PVDF emulsion is 100-200nm, and the manufacturer is Achima.
A mixed coating diaphragm comprises a base film and a coating formed by coating the mixed coating diaphragm slurry on two sides of the base film through a micro gravure roller coating process, then drying the base film in a baking oven at 75 ℃ for 1.5 min. The base film is made of a PP film, the thickness of the base film is 15 micrometers, and the thickness of each side coating is 3 micrometers.
The mixed coating membrane has the air permeability value of 118s/100ml, the areal density of 9.3 g/square meter, the needling strength of 5.7N and the tensile strength of 220Mpa (MD direction); 215MPa (in TD direction), baked at 130 ℃ for 1h, the heat shrinkage rates are 1.5% (MD) and 0.8(TD), the moisture content is 520ppm, and the film breaking temperature is 149 ℃.
The lithium battery manufactured by applying the diaphragm comprises: the positive electrode is made of a ternary material, the negative electrode is made of graphite, the electrolyte is EC/DMC/EMC (1: 1: 1), the standard electrolyte with the concentration of 1mol/L lithium hexafluorophosphate is assembled into a half battery, after the half battery is cycled for 100 circles under the multiplying power of 0.5C, the specific capacity is 154mAh/g, the capacity retention rate is 95.23%, and the average coulombic efficiency is 97.5%.
The inventor also tries to use the PVDF emulsion to match with the formula components outside the range of the formula components of the application, and cannot achieve better experimental effect.
The slurry of the present invention was prepared with process parameter adjustments according to the present disclosure and exhibited substantially the same properties as in example 1.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. The mixed coating diaphragm slurry is characterized by comprising the following components in parts by weight: 100 parts of deionized water, 0.5-1.0 part of dispersant, 0.5-10 parts of thickener, 5-7 parts of binder, 5-30 parts of alumina powder and 6-10 parts of PVDF emulsion.
2. The mix-coated separator slurry according to claim 1, comprising, in parts by weight: 100 parts of deionized water, 0.6-0.8 part of dispersant, 0.5-0.7 part of thickener, 5-7 parts of binder, 9-11 parts of alumina powder and 8-10 parts of PVDF emulsion.
3. The mix-coated separator slurry according to claim 1, wherein the alumina powder has a particle size of 1.2-2.5 um; the particle size of PVDF in the PVDF emulsion is 100-200 nm.
4. The mix-coated separator slurry according to claim 1,
the dispersing agent is one or a mixture of modified polyether polymer, fatty alcohol, polyethylene glycol alkyl aryl ether sodium sulfonate, alkylphenol polyethenoxy ether, polyoxyethylene alkyl phenol ether and sodium polyacrylate in any proportion;
the thickening agent is one or a mixture of PVA, PEG, PVP and CMC in any proportion;
the binder is one of polymethyl acrylate and xanthan gum or a mixture of the polymethyl acrylate and the xanthan gum in any proportion.
5. The method for preparing a mix coating separator paste according to any of claims 1 to 4, comprising the steps of:
step 1: adding a dispersing agent into deionized water, adding alumina powder after uniformly stirring, and sanding after uniformly stirring at a high speed;
step 2: adding PVDF emulsion and stirring uniformly;
and step 3: adding the thickening agent and the binder, and uniformly stirring.
6. The method as claimed in claim 5, wherein in step 1, the high speed stirring condition is that a stirrer is used to stir at a high speed of 800-; the sanding condition is that a sand mill is used for sanding for 3-15min at the speed of 500-1200 r/min.
7. The preparation method of the mixed coating diaphragm slurry is characterized by comprising the following steps:
step 1: adding a dispersing agent into deionized water, adding alumina powder after uniformly stirring, and sanding after uniformly stirring at a high speed;
step 2: adding PVDF emulsion and stirring uniformly;
and step 3: adding the thickening agent and the binder, and uniformly stirring.
8. A hybrid coating separator comprising a base film and a coating layer formed after the hybrid coating separator slurry according to any one of claims 1 to 4 is coated on one side or both sides of the base film; the base film is made of a PP film or a PE film, the thickness of the base film is 5-25 mu m, and the thickness of the coating on each side is 1-5 mu m.
9. Use of the hybrid coated separator of claim 8 in a lithium battery.
10. A lithium battery comprising a positive electrode, a negative electrode, an electrolyte, and the hybrid coated separator of claim 8.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111613759A (en) * | 2020-05-27 | 2020-09-01 | 湖北亿纬动力有限公司 | Diaphragm slurry, preparation method thereof, diaphragm and lithium ion battery |
| CN111883726A (en) * | 2020-08-28 | 2020-11-03 | 芜湖天弋能源科技有限公司 | Lithium ion battery diaphragm slurry and preparation method and application thereof |
| CN111933865A (en) * | 2020-06-30 | 2020-11-13 | 河北金力新能源科技股份有限公司 | Preparation method of lithium battery composite coating diaphragm slurry, diaphragm and high-nickel system lithium battery |
| WO2023082911A1 (en) * | 2021-11-11 | 2023-05-19 | 上海巴洛特新材料研究有限公司 | Thermal insulation coating, preparation method therefor and application method thereof |
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| CN111613759A (en) * | 2020-05-27 | 2020-09-01 | 湖北亿纬动力有限公司 | Diaphragm slurry, preparation method thereof, diaphragm and lithium ion battery |
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