CN112710669A - Method for rapidly evaluating crystal points of hard elastic diaphragm of homo-polypropylene lithium battery - Google Patents
Method for rapidly evaluating crystal points of hard elastic diaphragm of homo-polypropylene lithium battery Download PDFInfo
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- CN112710669A CN112710669A CN202011453564.2A CN202011453564A CN112710669A CN 112710669 A CN112710669 A CN 112710669A CN 202011453564 A CN202011453564 A CN 202011453564A CN 112710669 A CN112710669 A CN 112710669A
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- 239000013078 crystal Substances 0.000 title claims abstract description 60
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 title claims abstract description 45
- 229910052744 lithium Inorganic materials 0.000 title claims abstract description 45
- 229920005629 polypropylene homopolymer Polymers 0.000 title claims abstract description 24
- 238000000034 method Methods 0.000 title claims abstract description 21
- 238000005266 casting Methods 0.000 claims abstract description 24
- 239000000463 material Substances 0.000 claims abstract description 24
- 238000012545 processing Methods 0.000 claims abstract description 11
- 238000001125 extrusion Methods 0.000 claims abstract description 5
- 238000005096 rolling process Methods 0.000 claims abstract description 4
- 230000007547 defect Effects 0.000 claims description 19
- 239000012528 membrane Substances 0.000 claims description 18
- -1 polypropylene lithium Polymers 0.000 claims description 10
- 238000001514 detection method Methods 0.000 claims description 6
- 230000007704 transition Effects 0.000 claims description 5
- 238000004804 winding Methods 0.000 claims description 4
- 239000002245 particle Substances 0.000 claims description 3
- 238000009966 trimming Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 2
- 238000011156 evaluation Methods 0.000 abstract description 11
- 239000002952 polymeric resin Substances 0.000 abstract description 2
- 229920003002 synthetic resin Polymers 0.000 abstract description 2
- 230000005540 biological transmission Effects 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 6
- 239000002994 raw material Substances 0.000 description 6
- 238000012360 testing method Methods 0.000 description 6
- 210000003128 head Anatomy 0.000 description 4
- 230000003749 cleanliness Effects 0.000 description 3
- 239000004743 Polypropylene Substances 0.000 description 2
- 238000004458 analytical method Methods 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000000155 melt Substances 0.000 description 2
- 230000000704 physical effect Effects 0.000 description 2
- 229920001155 polypropylene Polymers 0.000 description 2
- 239000007787 solid Substances 0.000 description 2
- 241000251468 Actinopterygii Species 0.000 description 1
- 241000519995 Stachys sylvatica Species 0.000 description 1
- 238000000137 annealing Methods 0.000 description 1
- 239000002131 composite material Substances 0.000 description 1
- 230000002950 deficient Effects 0.000 description 1
- 238000009826 distribution Methods 0.000 description 1
- 239000000428 dust Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000007373 indentation Methods 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000012797 qualification Methods 0.000 description 1
- 238000011897 real-time detection Methods 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
- G01N21/88—Investigating the presence of flaws or contamination
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/84—Systems specially adapted for particular applications
- G01N2021/8411—Application to online plant, process monitoring
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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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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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Abstract
The invention relates to the field of polymer resin evaluation, in particular to an evaluation method of hard elastic diaphragm crystal points of a homo-polypropylene lithium battery. The method comprises the following steps: extruding the special material for the lithium battery diaphragm through a casting roller by using a double-screw extruder for casting; before the hard elastic film is rolled, an online flaw detector is arranged at a position after the extrusion processing is finished in advance; before traction and rolling, the casting film is wound and extended in multiple layers, stretched and flattened between the last two groups of casting rollers to form a hard elastic film, crystal points of the hard elastic diaphragm of the lithium battery are detected through an online flaw detector, crystal point data are collected, and the product quality is estimated according to the classified collection quantity of the crystal points. According to the invention, the relationship between the crystal point of the product and the ash content, the rebound rate and the transmission performance of the filter screen is obtained through the online flaw detector, the product evaluation time is shortened, the performance of the special material for the lithium battery film can be preliminarily judged in the process of preparing the hard elastic film of the lithium battery, and the evaluation efficiency is greatly improved.
Description
Technical Field
The invention relates to the field of polymer resin evaluation, in particular to an evaluation method of hard elastic diaphragm crystal points of a homo-polypropylene lithium battery.
Technical Field
The polymer is changed from solid raw material into melt and then changed from the melt into solid sheets and films, namely, the materials are subjected to a series of phase changes in the process of processing.
In the production process of the homo-polypropylene lithium battery film, due to raw materials, equipment, processing parameters and the like, many problems in appearance, such as crystal points, white spots, fish eyes, transverse striations, mottling, unstretched traces and the like, are generated. Even if the fineness of the filter screen of the extruder is improved, large crystal points on the film can be reduced to a certain extent, but small crystal points still pass through the filter screen, so that the pressure of the filter is increased, and the frequency and the cost for replacing the filter screen are increased.
Therefore, in order to ensure the product quality, the crystal point condition of the hard elastic film is monitored in real time in the production process, which is very necessary.
Disclosure of Invention
The invention aims to provide an evaluation method for rapidly evaluating the crystal points of the hard elastic diaphragm of the homo-polypropylene lithium battery, which can realize real-time detection of the crystal points in the preparation process, monitor the product quality, effectively shorten the test time and ensure the stability and reliability of the product quality.
In order to achieve the purpose, the invention provides an evaluation method of a hard elastic diaphragm crystal point of a homo-polypropylene lithium battery, which comprises the following specific steps:
firstly, extruding and casting the special material for the lithium battery diaphragm by a twin-screw extruder through a casting roller;
secondly, before the hard elastic film is rolled, an online flaw detector is arranged at a position after the extrusion processing is finished in advance;
before traction and rolling, the casting film is wound and extended in multiple layers and stretched and flattened between the last two groups of casting rollers to form a hard elastic film, crystal points of the hard elastic diaphragm of the lithium battery are detected through an online flaw detector, crystal point data are collected, and the product quality is estimated according to the classified collection quantity of the crystal points.
Further, in the first step, the processing temperature range of each zone of the double-screw extruder is 150-230 ℃.
Further, in the first step, the temperature of the casting roller is 80-120 ℃.
Further, in the first step, the winding speed of the casting roller is 10-40 m/min.
Further, the hard elastic film thickness was maintained at 15 to 30 μm.
Further, each zone of the double-screw extruder comprises 1-9 charging barrels, 3 transition temperature zones and 3 die head temperature zones.
Further, in the step one, the special material for the lithium battery diaphragm is a special material for a lithium wafer battery diaphragm, or is formed by mixing the special material for the lithium wafer battery diaphragm and at least one of special materials S801, S802H and S802M for a homo-polypropylene lithium battery diaphragm according to a proportion.
Further, the third step further comprises:
3.1 presetting a crystal point size threshold of the hard elastic diaphragm;
3.2 the online flaw detector judges whether the edge of the hard elastic diaphragm of the polypropylene lithium battery is detected according to the brightness acquired by the image acquisition assembly;
3.3 determining the width of the hard elastic film, and calculating the total length to be measured;
the calibrated width is an area between the starting edge and the ending edge of the area to be detected; the edge is retracted into the part of the edge of the hard elastic diaphragm needing trimming;
3.4 according to 100m2And (4) total detection area, detecting the hard elastic membrane by using an online flaw detector, counting the total number of flaws on the hard elastic membrane with the measured length, and classifying the quality of the hard elastic membrane product according to a flaw judgment standard according to a preset crystal point size threshold of the hard elastic membrane.
Further, hard elastic diaphragm grain size threshold:
further, the flaw determination criteria are classified as follows:
superior products:
the total number of defects is less than 600/100 m2The total number of the small crystal points and the small black points is less than or equal to 300;
qualified products:
600 is less than or equal to 1000/100m2And 300/100m2Total of < small crystal point, small black pointThe number is less than or equal to 500/100m2；
Grade 2 qualified product:
1000 is less than or equal to 2000 pieces/100 m2And 500/100m2Less than small crystal points and less than or equal to 1000 small black points/100 m2；
Grade 3 qualified product:
2000 < total number less than or equal to 3000/100 m2And 1000/100m2Less than small crystal points and less than or equal to 1500 small black points per 100m2；
Unqualified products: the total number is more than 3000/100 m2And the total number of small crystal points and small black points is more than 1500/100 m2。
The invention has the advantages that:
the online flaw detector is used for classifying the crystal points of the hard elastic film and counting the total amount to preliminarily judge indexes such as ash content, cleanliness and the like of the product, so that the product quality detection and continuous closed-loop control of production can be realized; the online flaw detector is arranged after melt extrusion and before the hard elastic diaphragm is rolled, the diaphragm does not need to be subjected to secondary annealing treatment in the testing process, the experimental steps are simple, the testing result is visual, and the evaluation time is saved.
Drawings
FIG. 1 is a top level illustration;
FIG. 2 is a diagram illustrating a second-level qualification;
FIG. 3 is a diagram illustrating a reject;
FIG. 4 is a graphical illustration of various defect images of a homo-polypropylene lithium battery separator.
Detailed Description
In order to make the content and use of the invention clearer, the invention is described in further detail below with reference to examples.
Selecting different raw materials to carry out preliminary judgment on the appearance, comprising the following steps: black spots, visible impurities and dust by naked eyes, the size uniformity of polypropylene particles and the like;
the physical properties of the raw materials are analyzed and tested, and the method mainly comprises the following steps: melt index, ash, rebound, etc.;
the evaluation of the special material crystal points of the homo-polypropylene lithium battery diaphragm is realized through the following process;
firstly, extruding and casting the special material for the lithium battery diaphragm by a double-screw extruder through a casting roller.
Each zone of the double-screw extruder comprises a charging barrel with 1-9 zones, 3 transition temperature zones and 3 die head temperature zones. Preferably, the processing temperature range of the twin-screw extruder is as follows: 150 ℃ to 230 ℃; specifically, the method comprises the following steps:
the 3 transition temperature zones include zone 1: 175-200 ℃; zone 2: 175-200 ℃; zone 3: 175-200 ℃;
the die head temperature zone comprises a zone 1: 175-200 ℃; zone 2: 180 ℃ and 205 ℃; zone 3: 185 ℃ C. about.205 ℃.
Preferably, the material special for the lithium battery diaphragm is melted and extruded through a charging barrel with 1-9 areas and 3 transition temperature areas, after casting through 3T-shaped die head channels, a casting film is cooled, wound and extended at 4 levels, stretched and flattened between the last two groups of casting rollers to form a hard elastic film, and the thickness of the hard elastic film is kept at 15-30 mu m. The temperature of the casting roller is 80-120 ℃, and the winding speed of the casting roller is 10-40 m/min.
And secondly, mounting the online flaw detector at a position before the hard elastic film is rolled and after the extrusion processing is finished.
The online flaw detector comprises a light source assembly, an image acquisition assembly and a rear-end server connected with the image acquisition assembly;
the light source assembly of the online flaw detector is arranged below the hard elastic film, and the image acquisition assembly is arranged above the hard elastic film and is opposite to the light source assembly below the hard elastic film.
Before traction and rolling, after the hard elastic membrane is effectively extended through 4 layers of winding, the hard elastic membrane is stretched and flattened between the last two groups of rollers to form the hard elastic membrane, defect detection is carried out on the hard elastic membrane of the lithium battery through an online flaw detector, crystal points are calculated according to the hole surface, and the number of the crystal points is monitored in real time.
The light source subassembly of hard elastic membrane below sends out light and passes through hard elastic membrane below, and the image acquisition subassembly of hard elastic membrane top is shot the film, if have defect points such as brilliant point on the hard elastic membrane, the light beam that the light source sent just can not see through hard elastic membrane.
The specific process is as follows:
3.1 the crystal point size threshold of the hard elastic diaphragm of the polypropylene lithium battery is preset, as shown in the following table 1.
TABLE 1 specific parameters of crystal point size threshold of hard elastic diaphragm of polypropylene lithium battery
Remarking: a maximum value of 0 indicates no upper limit for the maximum value.
Wherein, the hardware area refers to the area of the defect measured and calculated by software; the hardware dark area is the sum of dark areas contained in the defects measured and calculated by software; the hardware dark area is the sum of the bright areas contained within the defect as measured by the software.
3.2 the online flaw detector judges whether the edge of the hard elastic diaphragm of the polypropylene lithium battery is detected through the brightness acquired by the camera.
And reflecting the irradiated area into a dynamic image distribution area of the online flaw detector, wherein a high-frequency broken line fracture area is the edge of the diaphragm, so that the edge of the hard and elastic diaphragm of the polypropylene lithium battery on the casting and stretching equipment is matched with a to-be-detected area of the online flaw detector.
The area to be detected is determined by the start edge and the end edge, and the system does not detect beyond the two edges.
After the debugging image page of the online flaw detector is opened, two dotted lines are arranged on the interface, the left dotted line represents a starting edge, the right dotted line represents an ending edge, the left dotted line and the right dotted line are manually adjusted to be placed on the inner sides of high-frequency broken line marks, namely the starting edge and the ending edge are determined, and the width after calibration is obtained.
In actual production, because the edge part is often defective, the edge of the material is often required to be trimmed, and the defect of the edge part is irrelevant, an edge indentation value can be set, so that the edge part is shielded and not detected by an online flaw detector.
After the width of the hard elastic film of the polypropylene lithium battery is determined, the total length to be measured is calculated according to an area formula SRectangleLength and width, the formula is as follows:
the calibrated width is an area between the starting edge and the ending edge of the area to be detected; the edge is indented into the portion of the hard elastomeric membrane edge that requires trimming.
3.3 random inspection of 100m by means of an on-line flaw detector2The method comprises the steps of counting the total number of flaws on a hard elastic diaphragm with a measured length, classifying the quality of hard elastic diaphragm products according to a flaw judgment standard according to a preset crystal point size threshold value of the hard elastic diaphragm, preliminarily evaluating the cleanliness of the special material for the homo-polypropylene lithium battery diaphragm, comparing the cleanliness with data obtained by experimental analysis and detection, and verifying the reliability of the rapid evaluation method.
And counting the total number of large black spots, medium black spots, crystal spots, small black spots and small crystal spots counted by the software as the total number of the defects, and then classifying the product grades.
The specific criteria are as follows:
superior products:
the total number of defects is less than 600/100 m2And the total number of the small crystal points and the small black points is less than or equal to 300, as shown in figure 1.
Qualified products:
the total number of defects is more than 600 and less than or equal to 1000/100m2And 300/100m2Less than small crystal points and less than or equal to 500 small black points/100 m2。
Grade 2 qualified product:
the total number of defects is more than 1000 and less than or equal to 2000/100 m2And 500/100m2Less than small crystal points and less than or equal to 1000 small black points/100 m2As shown in fig. 2.
Grade 3 qualified product:
the total number of defects is more than 2000 and less than or equal to 3000/100 m2And 1000/100m2Less than small crystal points and less than or equal to 1500 small black points per 100m2。
Unqualified products: the total number is more than 3000/100 m2And the total number of small crystal points and small black points is more than 1500/100 m2As shown in fig. 3.
The invention proves that the total flaw detection number is 3000/100 m through repeated experiments2Or the total number of crystal points and small black points exceeds 1500/100 m2Can be judged as a special material not conforming to the production of the polypropylene lithium battery diaphragm. FIG. 4 shows an image legend of defects of a homo-polypropylene lithium battery diaphragm, and Table 2 shows a physical property test result of a material special for the homo-polypropylene lithium battery diaphragm.
TABLE 2 Property test results of the material specially used for homo-polypropylene lithium battery diaphragm
From the defect classification of the sample, the total number of the defects of the No. 1 raw material is minimum, the ash content in the corresponding physical analysis is minimum, the melt index is ideal, the rebound resilience also presents a proportional corresponding relation, and the production and the processing of the lithium battery film are easier; the number of the 3# raw material defects is the largest, the special material for the lithium battery diaphragm is preliminarily judged to be unqualified, and then the ash content is obviously increased through comparison with the ash content and the rebound rate, the elastic recovery rate is lower, the processing of the lithium battery diaphragm is not facilitated, and the test result is met.
The above is merely an exemplary embodiment and is not intended to limit the present invention, and those skilled in the art are within the spirit and scope of the present invention, and the field of this application also relates to composite lithium battery films, polypropylene separator special materials, and the like.
Claims (10)
1. A method for evaluating a material crystal point special for a homo-polypropylene lithium battery diaphragm is characterized by comprising the following steps:
firstly, extruding and casting the special material for the lithium battery diaphragm by a twin-screw extruder through a casting roller;
secondly, before the hard elastic film is rolled, an online flaw detector is arranged at a position after the extrusion processing is finished in advance;
before traction and rolling, the casting film is wound and extended in multiple layers and stretched and flattened between the last two groups of casting rollers to form a hard elastic film, crystal points of the hard elastic diaphragm of the lithium battery are detected through an online flaw detector, crystal point data are collected, and the product quality is estimated according to the classified collection quantity of the crystal points.
2. The method for evaluating the crystal point special for the homo-polypropylene lithium battery diaphragm as claimed in claim 1, wherein in the first step, the processing temperature of each zone of the twin-screw extruder is in the range of 150 ℃ to 230 ℃.
3. The method for evaluating a crystal point special for a homo-polypropylene lithium battery separator according to claim 2, wherein in the first step, the temperature of the casting roll is 80-120 ℃.
4. The method for evaluating a crystal particle special for a homo-polypropylene lithium battery separator as claimed in claim 3, wherein in the first step, the winding speed of the casting roll is 10-40 m/min.
5. The method for evaluating a crystal particle dedicated to a homo-polypropylene lithium battery separator according to claim 4, wherein the thickness of the hard elastic film is maintained at 15 to 30 μm.
6. The method for evaluating a crystal point special for a homo-polypropylene lithium battery diaphragm as claimed in claim 2, wherein each zone of the twin-screw extruder comprises 1-9 zones of the charging barrel, 3 transition temperature zones and 3 die head temperature zones.
7. The method according to claim 1, wherein in the first step, the material special for the lithium battery separator is a material special for a lithium Huajin battery film, or is formed by mixing at least one of the materials special for the lithium Huajin battery film and the material special for the lithium homo-polypropylene battery film in proportion S801, S802H and S802M.
8. The method for evaluating the crystal grain special for the homo-polypropylene lithium battery diaphragm as claimed in claim 1, wherein the third step further comprises:
3.1 presetting a crystal point size threshold of the hard elastic diaphragm;
3.2 the online flaw detector judges whether the edge of the hard elastic diaphragm of the polypropylene lithium battery is detected according to the brightness acquired by the image acquisition assembly;
3.3 determining the width of the hard elastic film, and calculating the total length to be measured;
the calibrated width is an area between the starting edge and the ending edge of the area to be detected; the edge is retracted into the part of the edge of the hard elastic diaphragm needing trimming;
3.4 according to 100m2And (4) total detection area, detecting the hard elastic membrane by using an online flaw detector, counting the total number of flaws on the hard elastic membrane with the measured length, and classifying the quality of the hard elastic membrane product according to a flaw judgment standard according to a preset crystal point size threshold of the hard elastic membrane.
9. The method for evaluating a crystal point special for a homo-polypropylene lithium battery diaphragm as claimed in claim 8, wherein the size threshold of the hard elastic diaphragm crystal point is as follows:
10. the method for evaluating the crystal point special for the homo-polypropylene lithium battery diaphragm as claimed in claim 9, wherein the defect judgment criteria are classified as follows:
superior products:
the total number of defects is less than 600/100 m2The total number of the small crystal points and the small black points is less than or equal to 300;
qualified products:
grade 1 qualified product:
600 is less than or equal to 1000/100m2And 300/100m2Less than small crystal points and less than or equal to 500 small black points/100 m2；
Grade 2 qualified product:
1000 is less than or equal to 2000 pieces/100 m2And 500/100m2Less than small crystal points and less than or equal to 1000 small black points/100 m2；
Grade 3 qualified product:
2000 < total number less than or equal to 3000/100 m2And 1000/100m2Less than small crystal points and less than or equal to 1500 small black points per 100m2；
Unqualified products: the total number is more than 3000/100 m2And the total number of small crystal points and small black points is more than 1500/100 m2。
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2020
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