CN112242591A - Oily functional slurry, lithium battery diaphragm and preparation method and application of lithium battery diaphragm - Google Patents
Oily functional slurry, lithium battery diaphragm and preparation method and application of lithium battery diaphragm Download PDFInfo
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Abstract
The invention belongs to the technical field of battery materials, and discloses an oily functional slurry, a lithium battery diaphragm, a preparation method and an application thereof. The preparation method of the oily functional slurry disclosed by the invention is a manufacturing process capable of realizing continuous production, and the manufacturing process is simple, low in cost and suitable for large-scale production. The oily functional slurry obtained by the invention has excellent storage stability and quality stability, and can be placed for 60 days without obvious sedimentation. In addition, the oily functional slurry can be used as one of preparation raw materials of the lithium battery diaphragm, can be coated on a polyolefin diaphragm or a ceramic diaphragm of a lithium ion battery, and can be dried to obtain the lithium battery diaphragm, so that the oily functional slurry is suitable for high-rate 3C and power lithium batteries, and has a wide application prospect.
Description
Technical Field
The invention belongs to the technical field of battery materials, and particularly relates to an oily functional slurry, a lithium battery diaphragm, and a preparation method and application thereof.
Background
With the increasing energy crisis and the environmental pollution, the new energy industry which is vigorously developed to be green and environment-friendly has become the mainstream consensus in the world. China is a large automobile consumption country, the development of new energy automobiles is the most important direction for the development of new energy industry in China, and the development of new energy automobiles is also a necessary way for turning the large automobile country into a strong automobile country. At present, the important factor for limiting the development of new energy automobiles is the vehicle-mounted power lithium battery. Generally, a lithium ion battery is mainly composed of four key components, namely, a positive electrode, a negative electrode, a separator and an electrolyte. The diaphragm is mainly used in the lithium battery to prevent short circuit caused by contact of the positive electrode and the negative electrode in the battery, and simultaneously provides a transmission channel of lithium ions between the positive electrode and the negative electrode, so that the quality of the diaphragm directly influences the internal resistance, capacity, cycle life, safety and other performances of the whole lithium ion battery although the diaphragm is not an active component of the lithium ion battery, and therefore, the functional slurry applied to the coating of the lithium battery diaphragm is particularly critical.
At present, functional slurry applied to coating of lithium battery diaphragms mainly has two main types: one is coating slurry taking inorganic materials as functional components, and the form of aqueous slurry is more; the other type is coating slurry taking organic macromolecules as functional components, and the type is oily slurry. Wherein, the inorganic functional components are ceramic powder such as alumina, boehmite, magnesium oxide and the like, and the main function of the inorganic functional components is to improve the thermal stability of the polyolefin diaphragm; the organic functional components comprise high-molecular polymers such as PMMA (polymethyl methacrylate), PVDF (polyvinylidene fluoride), PVDH-HPF (polyvinylidene fluoride-hexafluoropropylene copolymer), aramid fiber and the like, different functional components are selected to prepare different functional slurry, and the lithium battery diaphragms with different functions are obtained after coating. The organic functional polymer coating diaphragm has good wettability and liquid retention to electrolyte, can effectively bond the diaphragm and a pole piece, increases the cycle performance of the battery, and obviously improves the safety of the battery.
However, the existing lithium ion battery organic functional polymer coating diaphragm is generally coated by aqueous functional slurry, and the aqueous organic functional polymer slurry usually adopts water as a solvent, so that the problems of poor storage performance, short quality guarantee period and the like of a slurry system exist; and the aqueous polymer functional slurry uses more wetting dispersant, so that the bonding property is weakened, and the battery core prepared by coating the diaphragm has the problems of softness, poor hot-pressing bonding property with a pole piece and the like. Therefore, in recent years, oil-based functional pastes have come into wide use, and have good coating adhesion, and conventional oil-based pastes often contain N-methylpyrrolidone, dimethylacetamide, or the like as an organic solvent, but tend to cause clogging and poor air permeability.
Therefore, research and optimization of the formula design and preparation process of the oily polymer functional slurry are needed, the stability of the slurry is improved, and the binding power is improved, so that the problems of hole blocking and poor ventilation existing in the oily slurry are solved, and the comprehensive performance of the oily polymer functional slurry can be further improved when the oily polymer functional slurry is used for a lithium battery diaphragm.
Disclosure of Invention
The invention provides an oily functional slurry, a lithium battery diaphragm, and a preparation method and application thereof, which are used for solving one or more technical problems in the prior art and providing at least one beneficial choice or creation condition.
In order to overcome the technical problems, the technical scheme adopted by the invention is as follows:
the oily functional slurry is mainly prepared from a functional material, an oily solvent and a pore-forming aid, wherein the functional material is a high-molecular polymer.
As a further improvement of the scheme, the oily functional slurry is mainly prepared from 3-15% of a functional material, 10-20% of a pore-forming aid and 65-87% of an oily solvent in percentage by weight; preferably, the material is mainly prepared from 5-8% of functional materials, 12-15% of pore-forming aids and 77-83% of oily solvents.
As a further improvement of the above scheme, the molecular weight of the high molecular polymer is 20 to 100 ten thousand; the high molecular polymer is at least one selected from polyvinylidene fluoride homopolymer, polyvinylidene fluoride copolymer, aramid fiber and polyethylene oxide, preferably one or two selected from polyvinylidene fluoride homopolymer and polyvinylidene fluoride copolymer synthesized by emulsion.
Further preferably, the high molecular polymer is selected from one or two of polyvinylidene fluoride homopolymer and polyvinylidene fluoride copolymer synthesized by emulsion, wherein the homogeneity of the raw material is ensured by emulsion synthesis.
As a further improvement of the scheme, the melting point of the polyvinylidene fluoride homopolymer is 150-170 ℃, the primary particle size is 90-120nm, and the secondary particle size is 10-20 mu m; the melting point of the polyvinylidene fluoride copolymer is 90-160 ℃, the primary particle size is 100-200nm, and the secondary particle size is 10-20 mu m.
Here, the primary particle diameter and the secondary particle diameter are explained, and in general, the particle diameter of individual fine crystal grains is called a primary particle diameter, which is also called a primary particle diameter, and the particle diameter of secondary particles formed by agglomeration is called a secondary particle diameter. When the crystal is very fine, the surface energy of the crystal grains is very large, and the fine crystal grains are easily combined together due to weak interaction force, so that the crystal grains are agglomerated, namely a plurality of fine crystal grains are agglomerated, and larger secondary particles are formed, namely secondary particle sizes.
As a further improvement of the scheme, the pore-forming assistant is a low-boiling-point alcohol or alkane solvent, the boiling point is 45-100 ℃, and the pore-forming assistant is mainly selected from at least one of ethanol, n-heptane, n-butanol and n-propanol, preferably one or two of ethanol and n-heptane; the oily solvent is selected from at least one of acetone, n-heptane or n-propanol.
A preparation method of oily functional slurry comprises the following steps: weighing raw materials according to the raw material formula of the oily functional slurry, mixing, stirring, heating, condensing and refluxing an oily solvent to an original reaction system, sequentially adding a functional material, the oily solvent and a pore-forming aid under the stirring condition, heating, condensing and refluxing the oily solvent to the original reaction system, and thus obtaining the oily functional slurry.
Preferably, the functional material, the oily solvent and the pore-forming assistant are sequentially added under the stirring condition, and when the raw materials are added according to the sequence, the dissolution time of the raw materials is shortest.
As a further improvement of the above scheme, in the stirring process, the adopted stirrer comprises a low-speed stirrer with a high-speed dispersion plate, the tank body is provided with a low-speed frame type stirring and a high-speed dispersion plate, and the tank body and the high-speed dispersion plate can rotate independently in the same tank body; wherein, in the stirring process, high-speed dispersion and low-speed stirring are adopted; wherein the rotating speed of the low-speed stirring is 50-100r/min, preferably 50-60 r/min; the high-speed dispersion rotating speed is 1000-; the stirring time is 60-120min, preferably 70-90 min; the temperature during stirring is 30 to 55 ℃, preferably 42 to 48 ℃.
It is worth noting that the raw materials of the oily functional slurry have certain solubility of the oily solvent to the functional materials, and the oily functional slurry has obvious difficulty in dispersing if no dispersant is added in the conventional method, however, the invention is realized by adopting a low-speed stirrer with a high-speed dispersion disc and combining the modes of heating dissolution and condensation reflux, the dissolution and dispersion of the raw materials can be realized quickly without adding the dispersant, and the oily slurry with excellent storage stability and quality stability can be obtained.
The lithium battery diaphragm comprises a base material and a coating coated on the base material, wherein the coating is formed by coating the composite slurry on the base material and drying.
A preparation method of a lithium battery diaphragm comprises the following steps: the oily functional coating is coated on a ceramic diaphragm or a lithium ion battery polyolefin diaphragm, and then the oily functional coating diaphragm is obtained after drying.
A battery comprising a lithium battery separator according to the invention.
The invention has the beneficial effects that:
(1) the invention provides an oily functional slurry, which comprises main raw materials of a functional material, an oily solvent and a pore-forming assistant, wherein the functional material is a crystalline high polymer, and the crystalline high polymer has high strength, high toughness, corrosion resistance and friction resistance at low temperature, so that when the crystalline high polymer is used for preparing the functional slurry, the crystalline high polymer can be helpful for improving the volatilization rate of the pore-forming assistant with low boiling point during drying so as to form large pores, and meanwhile, the oily solvent can be easy to form small pores when the volatilization rate is slightly low, so that the obtained oily functional slurry can form a high-molecular coating with a net structure after being dried. Meanwhile, when the functional slurry is used for preparing the obtained slurry, the adhesion between the lithium battery diaphragm and the pole piece can be increased when a thin battery cell is manufactured, the hardness is ensured, the liquid retention amount is also ensured, and the full cycle performance is further realized.
It should be noted that the "liquid retention amount" in (1), that is, the electrolyte retention amount, is an important parameter for keeping the cell from jumping out at the later cycle stage, and there is a special parameter, called the liquid retention coefficient, when the liquid retention amount of the cell is good or bad, which is the liquid retention amount/cell capacity.
(2) The invention also provides a preparation method of the oily functional slurry, which is a manufacturing process capable of realizing continuous production, has simple manufacturing flow and low cost, and is suitable for large-scale production. The oily functional slurry obtained by the invention has excellent storage stability and quality stability, and can be placed for 60 days without obvious sedimentation.
(3) In addition, the oily functional slurry can also be used as one of raw materials for preparing a lithium battery diaphragm, and can be coated on a lithium ion battery polyolefin diaphragm or a ceramic diaphragm and then dried to obtain the lithium battery diaphragm.
(4) The lithium battery diaphragm obtained by the invention has good wettability and liquid retention for electrolyte in a lithium battery, and meanwhile, the safety performance of the lithium battery is greatly improved due to strong bonding force with a pole piece, so that the lithium battery diaphragm is suitable for batteries, especially high-rate 3C and power lithium batteries, and has wide application prospect.
Drawings
In order to more clearly illustrate the technical solution in the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly described below. It is clear that the described figures are only some embodiments of the invention, not all embodiments, and that a person skilled in the art can also derive other designs and figures from them without inventive effort.
FIG. 1 is a photograph of comparative example finished products 1-2 and oily functional slurry example finished products 1-4 on days 1, 10, 30 and 60 of storage;
FIG. 2 is a scanning electron microscope image of finished product 1 of the lithium battery diaphragm example;
FIG. 3 is a scanning electron microscope image of a lithium battery separator comparative example product 1;
fig. 4 is a scanning electron microscope image of a lithium battery separator comparative example product 2.
Detailed Description
The present invention is specifically described below with reference to examples in order to facilitate understanding of the present invention by those skilled in the art. It should be particularly noted that the examples are given solely for the purpose of illustration and are not to be construed as limitations on the scope of the invention, as non-essential improvements and modifications to the invention may occur to those skilled in the art, which fall within the scope of the invention as defined by the appended claims. Meanwhile, the raw materials mentioned below are not specified in detail and are all commercially available products; the process steps or extraction methods not mentioned in detail are all process steps or extraction methods known to the person skilled in the art.
Example 1 preparation of oily functional slurry and lithium battery separator
(1) Preparing oily functional slurry: 5.5kg of polyvinylidene fluoride copolymer powder (with the molecular weight of 20-30 ten thousand), 81kg of acetone and 13.5kg of ethanol are sequentially added into a production cylinder matched with the oily slurry, the rotating speed of a stirrer is set to be 50 revolutions per minute, the speed of a dispersion disc is set to be 1500 revolutions per minute, and the oily functional slurry is dispersed for 80 minutes to obtain a finished product 1 of the oily functional slurry example.
(2) Coating the oily functional slurry to prepare the lithium battery diaphragm: and (3) coating the coating of the finished product 1 of the 2um oily functional slurry embodiment on the 9+3um ceramic diaphragm in a wire rod spin coating mode, and baking the coating in a full-suspension oven to obtain the finished product 1 of the lithium battery diaphragm embodiment.
Example 2 preparation of oily functional slurry and lithium battery separator
(1) Preparing oily functional slurry: 5.5kg of polyvinylidene fluoride homopolymer powder (with the molecular weight of 20-40 ten thousand), 81kg of acetone and 13.5kg of normal propyl alcohol are sequentially added into a production cylinder matched with the oily slurry, the rotating speed of a stirrer is set to be 50 revolutions per minute, the speed of a dispersion disc is set to be 1500 revolutions per minute, and the oily functional slurry is dispersed for 80 minutes to prepare a finished product 2 of an oily functional slurry embodiment.
(2) Coating the oily functional slurry to prepare the lithium battery diaphragm: and (3) coating the coating of the 2um oily functional slurry embodiment finished product 2 on the 9+3um ceramic diaphragm in a wire rod spin coating mode, and baking the coating in a full-suspension oven to obtain the lithium battery diaphragm embodiment finished product 2.
Example 3 preparation of oily functional slurry and lithium battery separator
(1) Preparing oily functional slurry: adding 7.8kg of polyvinylidene fluoride copolymer powder (molecular weight is 20-40 ten thousand), 78kg of acetone and 14.2kg of n-butanol into a production cylinder matched with the oily slurry in sequence, setting the rotating speed of a stirrer to be 50 revolutions per minute and the speed of a dispersion disc to be 1500 revolutions per minute, and dispersing for 80 minutes to prepare a finished product 3 of the oily functional slurry in the embodiment.
(2) Coating the oily functional slurry to prepare the lithium battery diaphragm: and (3) coating the coating of the 2um oily functional slurry embodiment finished product 3 on the 9+3um ceramic diaphragm in a wire rod spin coating mode, and baking the coating by using a full-suspension oven to obtain the lithium battery diaphragm embodiment finished product 3.
Example 4 preparation of oily functional slurry and lithium battery separator
(1) Preparing oily functional slurry: adding 7.8kg of polyvinylidene fluoride copolymer powder (molecular weight is 30-50 ten thousand), 78kg of acetone and 14.2kg of ethanol into a production cylinder matched with the oily slurry in sequence, setting the rotating speed of a stirrer to be 50 revolutions per minute and the speed of a dispersion disc to be 1500 revolutions per minute, and dispersing for 80 minutes to obtain a finished product 4 of the oily functional slurry in the embodiment.
(2) Coating the oily functional slurry to prepare the lithium battery diaphragm: and (3) coating the coating of the 2um oily functional slurry embodiment finished product 4 on the 9+3um ceramic diaphragm in a wire rod spin coating mode, and baking the coating in a full-suspension oven to obtain the lithium battery diaphragm embodiment finished product 4.
Comparative example 1
(1) The oily polyvinylidene fluoride functional slurry for coating the lithium ion lithium battery diaphragm in the market is D-04 (the molecular weight is 40-70 ten thousand) and is marked as finished product 1 of the oily functional slurry comparative example.
(2) Coating a separator: and (3) coating the coating of the 2um oily functional slurry comparative example finished product 1 on the 9+3um ceramic coating diaphragm in a wire rod spin coating mode, and baking the coating in a full-suspension oven to obtain the oily functional coating diaphragm which is marked as a lithium battery diaphragm comparative example finished product 1.
Comparative example 2
(1) The oily functional slurry is prepared by adopting an oily polyvinylidene fluoride slurry formula which is mainstream in the industry, and the formula comprises the following components: 4.5% polyvinylidene fluoride LBG-D01 (molecular weight 40-60 ten thousand), 1.1% polyvinylidene fluoride powder 75130-D05 (molecular weight 80-100 ten thousand), 94.4% acetone (chemical purity) B-01, the preparation method is the same as example 1, and the obtained product is marked as oily functional slurry comparative example 2.
(2) Coating a separator: and (3) coating the coating of the 2um oily functional slurry comparative example finished product 2 on the 9+3um ceramic coating diaphragm in a wire rod spin coating mode, and baking the coating in a full-suspension oven to obtain the oily functional coating diaphragm which is marked as a lithium battery diaphragm comparative example finished product 2.
Product performance detection
1. Storage stability of the slurries
Oily functional slurry obtained in comparative examples 1 to 2 and examples 1 to 4 comparative examples 1 to 2 (the finished product of comparative example 1 was stored in a bottle labeled with "D-04" and the finished product of comparative example 2 was stored in a bottle labeled with "LBG") and the finished products of oily functional slurry examples 1 to 4 (corresponding to the products labeled with i, ii, iii, iv from left to right, respectively, on the body of the bottle in fig. 1) were stored in 100ml jars, respectively, and observed and photographed for the conditions of day 1 (shown in a in fig. 1), day 10 (shown in b in fig. 1), day 30 (shown in c in fig. 1) and day 60 (shown in D in fig. 1), respectively, to obtain fig. 1.
As is clear from fig. 1, day one: comparative examples 1 to 2, which were completely dispersed and in a clear state as in examples 1 to 4;
the tenth day: the turbidity began to appear in comparative examples 1-2, and examples 1-4 remained clear;
thirty-day: the turbidity aggravated in comparative examples 1-2 and the delamination in comparative example 2, a slight turbidity started to appear in example 4 and example 1/2/3 was still clear;
sixty days: the turbidity and delamination of comparative examples 1-2 are increased, example 4 is still slightly turbid, and example 1/2/3 is clear;
therefore, the finished products 1 to 4 of the oily functional slurry obtained in the invention have excellent storage stability.
2. Basic performance test of lithium battery diaphragm
The lithium battery diaphragm comparative example finished products 1-2 obtained in comparative examples 1-2 and example 1 and the lithium battery diaphragm example finished product 1 respectively are subjected to basic performance data tests such as thickness, air permeability value, surface density, thermal shrinkage, coating peel strength and the like, and the test method is tested by referring to a national standard GBT36363-2018 or an enterprise standard test method (the test is carried out by adopting a known prior art). The test results of the lithium battery separator of example 1, comparative example 1 and comparative example 2 are shown in the following table 1:
table 1 test results of finished products 1 of lithium battery separator examples and finished products 1 to 2 of lithium battery separator comparative examples
As can be seen from table 1, the oily functional coating lithium ion battery separator prepared in example 1 of the present invention is superior to comparative examples 1 and 2 in thickness increase value, air permeability value, electrolyte liquid absorption rate, peel strength, SEM microstructure, etc. when coated with the same ceramic membrane.
3. Scanning electron microscope
And (3) respectively carrying out scanning electron microscopy on the oily functional slurry finished products 1-2 obtained in comparative examples 1-2 and the oily functional slurry finished product 1 obtained in example 1 to obtain figures 2-4, wherein figure 2 is a scanning electron microscopy image of the lithium battery diaphragm example finished product 1 under different multiples, figure 3 is a scanning electron microscopy image of the lithium battery diaphragm comparative example finished product 1 under different multiples, and figure 4 is a scanning electron microscopy image of the lithium battery diaphragm comparative example finished product 2 under different multiples.
4. Testing basic performance of lithium battery diaphragm after being wound into battery cell
The lithium battery diaphragm finished products obtained in example 1, comparative example 1 and comparative example 2 are respectively prepared into soft packaging battery cells with the specification of 506090, and the battery cells are detected as follows, and the detection results are shown in the following table 2:
the dry pressing refers to winding the positive plate, the oily functional coating diaphragm and the negative plate, placing the positive plate, the oily functional coating diaphragm and the negative plate in an aluminum-plastic film, packaging the positive plate, hot-pressing the positive plate, the oily functional coating diaphragm and the negative plate for 30 minutes at 65 ℃ and under the pressure of 1MPa, and testing the hardness of the battery cell and the cohesive force of the pole plate after cooling.
The wet pressing indicates that a slurry positive plate, an oily functional coating diaphragm and a negative plate are wound, then the obtained product is placed in an aluminum-plastic film, 9g of 1mol/L LiPF6 electrolyte (the solvent is ethylene carbonate: diethyl carbonate: methyl ethyl carbonate: 1:1 in volume ratio) is injected, then the obtained product is packaged, hot pressing is carried out for 30 minutes at 65 ℃ and under the pressure of 1MPa, and the test of the hardness of the battery core and the bonding force of the pole piece is carried out after cooling.
The cell hardness test is to apply 1kg of force to press down the cell by using a round-head needle with the diameter of 1mm, measure the indentation depth value, and the larger the value is, the softer the cell is, otherwise, the smaller the value is, the harder the cell is.
Table 2 results of performance measurements of finished products 1 and comparative examples 1 to 2 of lithium battery separators
As can be seen from Table 2, the hardness, internal resistance, capacity, multiplying power and high-temperature storage of the battery cell in the example 1 are superior to those of the battery cells in the comparative examples 1-2, the pole piece adhesion is far greater than those of the battery cells in the comparative examples 1-2, and the battery cell obtained in the example 1 is stable in structural performance and higher in safety.
It will be obvious to those skilled in the art that many simple derivations or substitutions can be made without inventive effort without departing from the inventive concept. Therefore, simple modifications to the present invention by those skilled in the art according to the present disclosure should be within the scope of the present invention. The above embodiments are preferred embodiments of the present invention, and all similar processes and equivalent variations to those of the present invention should fall within the scope of the present invention.
Claims (10)
1. The oily functional slurry is characterized by being mainly prepared from a functional material, an oily solvent and a pore-forming aid, wherein the functional material is a high-molecular polymer.
2. The oily functional slurry according to claim 1, which is mainly prepared from 3-15% of functional materials, 10-20% of pore-forming aids and 65-87% of oily solvents by weight percentage; preferably, the material is mainly prepared from 5-8% of functional materials, 12-15% of pore-forming aids and 77-83% of oily solvents.
3. The oily functional slurry according to claim 1, wherein the molecular weight of the high molecular polymer is 20 to 100 ten thousand; the high molecular polymer is at least one of polyvinylidene fluoride homopolymer, polyvinylidene fluoride copolymer, aramid fiber and polyethylene oxide; preferably one or two selected from polyvinylidene fluoride homopolymer and polyvinylidene fluoride copolymer.
4. The oily functional slurry as claimed in claim 3, wherein the melting point of the polyvinylidene fluoride homopolymer is 150-170 ℃, the primary particle size is 90-120nm, and the secondary particle size is 10-20 μm; the melting point of the polyvinylidene fluoride copolymer is 90-160 ℃, the primary particle size is 100-200nm, and the secondary particle size is 10-20 mu m.
5. The oily functional slurry according to claim 1, wherein the pore-forming assistant is an alcohol or alkane solvent with a boiling point of 45-100 ℃, preferably one or two of ethanol and n-heptane; the oily solvent is selected from at least one of acetone, n-heptane or n-propanol.
6. A method for preparing the oily functional slurry according to any one of claims 1 to 5, characterized by comprising the steps of: weighing the raw materials according to the raw material formula of the oily functional slurry, mixing, stirring, heating, and obtaining the oily functional slurry after the oily solvent is condensed and reflowed to the original reaction system.
7. The production method according to claim 6, wherein in the stirring process, high-speed dispersion and low-speed stirring are adopted; wherein the rotating speed of the low-speed stirring is 50-100r/min, preferably 50-60 r/min; the high-speed dispersion rotating speed is 1000-; the stirring time is 60-120min, preferably 70-90 min; the temperature during stirring is 30 to 55 ℃, preferably 42 to 48 ℃.
8. A lithium battery separator comprising a substrate and a coating layer coated on the substrate, wherein the coating layer is formed by coating the composite paste according to any one of claims 1 to 5 on the substrate and then drying the coated substrate.
9. A method of making a lithium battery separator according to claim 8, comprising the steps of: and coating the oily functional coating on a ceramic diaphragm or a lithium ion battery polyolefin diaphragm, and drying to obtain the lithium ion battery diaphragm.
10. A battery comprising the lithium battery separator of claim 8.
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Application publication date: 20210119 |
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