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WO2021223115A1 - Electrolyte resistance testing method for adhesive tape - Google Patents

Electrolyte resistance testing method for adhesive tape Download PDF

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Publication number
WO2021223115A1
WO2021223115A1 PCT/CN2020/088817 CN2020088817W WO2021223115A1 WO 2021223115 A1 WO2021223115 A1 WO 2021223115A1 CN 2020088817 W CN2020088817 W CN 2020088817W WO 2021223115 A1 WO2021223115 A1 WO 2021223115A1
Authority
WO
WIPO (PCT)
Prior art keywords
adhesive tape
electrolyte
test
peel strength
resistance
Prior art date
Application number
PCT/CN2020/088817
Other languages
French (fr)
Chinese (zh)
Inventor
吴伟卿
Original Assignee
河源新之源粘贴技术有限公司
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by 河源新之源粘贴技术有限公司 filed Critical 河源新之源粘贴技术有限公司
Priority to PCT/CN2020/088817 priority Critical patent/WO2021223115A1/en
Publication of WO2021223115A1 publication Critical patent/WO2021223115A1/en

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Classifications

    • CCHEMISTRY; METALLURGY
    • C09DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
    • C09JADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
    • C09J7/00Adhesives in the form of films or foils
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N17/00Investigating resistance of materials to the weather, to corrosion, or to light
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N19/00Investigating materials by mechanical methods
    • G01N19/04Measuring adhesive force between materials, e.g. of sealing tape, of coating

Definitions

  • the invention relates to the field of quality inspection standards, in particular to a method for testing the resistance of an adhesive tape to electrolyte.
  • rechargeable secondary lithium-ion batteries have many advantages such as high energy density, high working voltage, long cycle life, no memory effect, green environmental protection, and flexible design according to actual needs. More and more electrical equipment are selected as power sources, especially mobile electrical equipment, energy storage stations and new energy vehicles. The wide range of applications has been driving the rapid development of lithium-ion batteries.
  • Lithium batteries include a positive electrode, a negative electrode, and an electrolyte.
  • the electrolyte is one of the core components of lithium-ion batteries, and its main components include lithium hexafluorophosphate, ethylene carbonate, diethyl carbonate, dimethyl carbonate and ethyl methyl carbonate, etc., which have corrosive properties. Therefore, the working environment is electrolyte, and the adhesive tape used for fixing and insulating the positive and negative materials in the battery needs to have the performance of resistance to the electrolyte of the lithium ion battery, and the electrolyte resistance test is also a necessary basic test item.
  • the current testing method of adhesive tape resistance to electrolyte is to directly paste the adhesive tape on a thin aluminum foil and put it in the electrolyte. After a period of time, observe whether the adhesive tape is arched, shifted, or penetrated. , Whether the electrolyte has faded, and whether the adhesive remains after tearing off the tape, etc., to determine the impact of the electrolyte on the adhesive tape, and further determine whether the adhesive tape is qualified.
  • This method is simple and direct. However, the above method is greatly affected by subjective factors, and the test method is not standardized. At the same time, the test method lacks quantitative indicators, which is not conducive to accurately judging whether the adhesive tape product is qualified or not, and the experimental results are difficult to reproduce.
  • the present invention provides a test method for the resistance of the adhesive tape to electrolyte.
  • the tools and materials used in the electrolyte resistance test process are standardized and standardized.
  • the peel strength change of the test board is used as the evaluation standard, and a quantitative method is implemented to accurately determine whether the adhesive tape product is qualified or not.
  • the above-mentioned test method is reproducible, intuitive, and convenient for discrimination.
  • a testing method for the resistance of an adhesive tape to electrolyte includes the following steps:
  • test piece immerse the test piece in the electrolyte, place it at 45°C-95°C for 4h-24h, take it out, absorb the electrolyte and leave it for 10min-30min;
  • the change rate of the electrolyte of the adhesive tape is used as the judgment basis, and the standards or requirements of the adhesive tape are compared to determine whether the electrolyte resistance test of the adhesive tape to be tested is qualified;
  • the calculation method of the change rate of the electrolyte of the adhesive tape is: peel strength I/peel strength II ⁇ 100%.
  • the attenuation rate of the electrolyte of the adhesive tape is used as the judgment basis, and the standards or requirements of the adhesive tape are compared to determine whether the electrolyte resistance test of the adhesive tape to be tested is qualified;
  • the calculation method of the attenuation rate is: (peel strength II-peel strength I)/peel strength II ⁇ 100%.
  • the standard test plate is selected from stainless steel plate, glass plate, aluminum-plastic plate, aluminum plate, aluminum foil, copper foil, copper-plastic plate or copper plate.
  • the thickness of the standard test board is 5 ⁇ m-400 ⁇ m.
  • the method of immersing the test piece in the electrolyte is: placing the test piece in a container, and adding the electrolyte into the container.
  • the container is a straight wide-mouth bottle with a communicating spacer layer inside.
  • the material of the container is selected from polytetrafluoroethylene, polyethylene, polypropylene, polystyrene, polyphenylene ether, polyphenylene sulfide, polyamide or glass.
  • the test piece is placed for at least 10 minutes and then immersed in the standard electrolyte.
  • the peeling angle when measuring the peel strength between the adhesive tape to be tested and the standard test plate of the test piece after the electrolyte is dried, the peeling angle is 180 degrees.
  • the peel angle is 180 degrees.
  • the present invention has the following beneficial effects:
  • the change in the peel strength of the adhesive tape and the test board before and after immersion in the electrolyte is used as the evaluation standard, and the adhesive tape standards or requirements are compared with the implementation of quantitative means to accurately determine whether the adhesive tape product is qualified or not.
  • the above-mentioned Wu's method is used to test the adhesive tape's resistance to electrolyte, which has good reproducibility, intuitiveness, and facilitates discrimination.
  • the present invention also provides for the standard test board (named “Wu's plate”), a container for containing the electrolytic solution (named “Wu's bottle”), and tools, materials, test procedures, and test procedures during the electrolyte resistance test.
  • the evaluation method is standardized and standardized, with standardized test procedures, standardized test methods, standardized data processing, and standardized evaluation standards, which minimize the influence of subjective factors during the adhesive tape testing process and facilitate promotion in the industry.
  • the existing testing methods for the resistance of adhesive tapes to electrolyte are largely affected by subjective factors and are not standardized. At the same time, the testing methods do not use quantitative means, the experimental results are difficult to reproduce, and it is not conducive to accurately judging whether the adhesive tape products are qualified or not.
  • the invention provides a test method for the resistance of an adhesive tape to electrolyte, which is also called "Wu's method”.
  • a testing method for the resistance of an adhesive tape to electrolyte includes the following steps:
  • test piece immerse the test piece in the electrolyte, place it at 45°C-95°C for 4h-24h, take it out, absorb the electrolyte and leave it for 10min-30min;
  • the method of attaching the adhesive tape to be tested to the standard test board can be as follows:
  • test group One group is subjected to the electrolyte resistance test, which is called the test group, the test piece is called the test piece, and the other group is placed in a constant temperature and humidity test environment.
  • control group correspondingly, the test piece is called the control piece.
  • the adhesive tape to be tested and the standard test board can be placed in a standard environment of constant temperature and humidity for no less than 30 minutes to adjust the state.
  • the standard environment of constant temperature and humidity may be an environment of 23 ⁇ 1° C. and 50 ⁇ 5% RH (relative humidity).
  • the standard test board can also be cleaned before bonding.
  • the standard test plate is selected from stainless steel plate, glass plate, aluminum-plastic plate, aluminum plate, aluminum foil, copper foil, copper-plastic plate or copper plate, and the standard test plate is named "Wu's plate” .
  • the thickness of the standard test board is 5 ⁇ m-400 ⁇ m.
  • the thickness of the standard test plate is preferably 100 ⁇ m-400 ⁇ m.
  • the thickness of the standard test board is preferably 5 ⁇ m-20 ⁇ m.
  • the test piece after bonding, the test piece is placed for at least 10 minutes, and then immersed in the electrolyte.
  • the test piece is placed in a standard environment of constant temperature and humidity for at least 10 minutes, and then immersed in the electrolyte.
  • the standard environment of constant temperature and humidity may be an environment of 23 ⁇ 1° C. and 50 ⁇ 5% RH (relative humidity).
  • test piece is placed in a container, the electrolyte is added to the container, and the container containing the discharge solution is named "Wu's bottle”.
  • the container may be a straight wide-mouth bottle.
  • the interior of the straight wide-mouth bottle may be designed with a communicating spacer layer, or without a spacer layer.
  • the container is a straight wide-mouth bottle with a communicating spacer layer inside.
  • the design of the spacer layer can perform electrolyte resistance tests on multiple adhesive tapes to be tested at the same time, which is convenient for multiple tests.
  • the parts are separated to prevent the test parts from overlapping, which will affect the full immersion of the electrolyte.
  • the material of the container is selected from polytetrafluoroethylene, polyethylene, polypropylene, polystyrene, polyphenylene ether, polyphenylene sulfide, polyamide or glass.
  • the electrolyte is a ternary lithium electrolyte, and a ternary lithium electrolyte commonly used in the field of lithium batteries can be used, and the present invention is not limited herein.
  • the electrolyte is lithium iron phosphate electrolyte, and lithium iron phosphate electrolyte commonly used in the field of lithium batteries can be used, and the present invention is not limited herein.
  • test piece is immersed in the electrolyte, placed at 45°C-95°C for 4h-24h, taken out and sucked up the electrolyte.
  • peel strength measurement needs to be completed within 30 minutes after the electrolyte is drained.
  • the test environment is a standard environment of constant temperature and humidity, and the standard environment of constant temperature and humidity may be an environment of 23 ⁇ 1° C. and 50 ⁇ 5% RH (relative humidity).
  • test the peel strength of the test piece and the control piece that have absorbed the electrolyte can refer to the national standard GB/T2792-2014 "Test Method for the Peel Strength of Adhesive Tapes".
  • the peel angle when measuring the peel strength between the adhesive tape to be tested and the standard test plate of the test piece after the electrolyte is dried, the peel angle is 180 degrees.
  • the peel angle is 180 degrees.
  • test piece is immersed in the electrolyte environment, and the control piece is placed in the constant temperature and humidity test environment. Except for this, the other operations should both be under the same conditions.
  • the peel strength between the adhesive tape to be tested and the standard test board of the test piece after the electrolyte is absorbed is measured to obtain the peel strength I; the adhesive tape to be tested and the standard test board of the control piece The peel strength between the two was measured, and the peel strength II was obtained.
  • the ratio of peel strength II to peel strength I can be used as the basis for judgment (peel strength II/peel strength I ⁇ 100%), and the adhesive tape standards or requirements can be compared to determine the adhesive tape’s performance Whether the electrolyte resistance test is qualified. That is, the electrolyte change rate of the adhesive tape is used to determine whether the test of the electrolyte resistance of the adhesive tape to be tested is qualified.
  • the specific ratio of judgment can be formulated according to the different performance requirements of the product.
  • the attenuation rate of the electrolyte of the adhesive tape can be used as the basis for judgment, and the standard or requirements of the adhesive tape can be compared to determine whether the electrolyte resistance test of the adhesive tape to be tested is qualified; the adhesive tape electrolysis
  • the calculation method of the liquid attenuation rate is: (Peel Strength II-Peel Strength I)/Peel Strength II ⁇ 100%. That is, the electrolyte decay rate method of the adhesive tape is used to determine whether the test of resistance to electrolyte of the adhesive tape to be tested is qualified.
  • the specific attenuation rate of the electrolyte of the adhesive tape can be determined according to the different performance requirements of the product.
  • the method of the present invention is used to judge whether it is qualified or not.
  • the percentage method peel strength II/peel strength The measured value of I
  • the measured value of I is greater than 20%, or the attenuation rate in the attenuation method is less than 80%.
  • the above-mentioned test method for the resistance of the adhesive tape to electrolyte also called "Wu's method" has a standardized test procedure, a standardized test method, a standardized data processing, and a standardized evaluation standard.
  • the electrolyte resistance test board, the electrolyte resistance test container, other tools, materials and the environment for the electrolyte resistance test used in the test process, the adhesive tape and the test board before and after immersion in the electrolyte are standardized and standardized.
  • the peel strength change is used as the evaluation standard.
  • the quantitative method is implemented to accurately judge whether the adhesive tape product is qualified or not.
  • the Wu's method is used to test the electrolyte resistance of the adhesive tape. The reproducibility is good, intuitive, and beneficial. Discriminate.
  • This embodiment provides a method for testing the resistance of an adhesive tape to electrolyte, which includes the following steps:
  • test pieces D, E, F are called test pieces D, E, F, and the other group is placed at constant temperature and humidity.
  • the control group is called control pieces A, B, and C.
  • Embodiment 1 provides a test method for the resistance of the adhesive tape to electrolyte.
  • the difference from Embodiment 1 is that the standard test board and its thickness and surface roughness are different from those in Embodiment 1, and specifically include the following steps:
  • test pieces Randomly and averagely divide the test pieces into two groups, each group has three pieces, one group is subjected to the electrolyte resistance test, which is called the test group, the test pieces are called test pieces d, e, f, and the other group is placed at constant temperature and humidity In the test environment, it is called the control group.
  • control pieces the test pieces are called control pieces a, b, and c.
  • a high-viscosity termination adhesive tape for lithium-ion batteries that was identified by the customer as unqualified during the production process is used as the adhesive tape to be tested, and the method of the present invention and the background art mentioned in the background technology are used respectively.
  • the current method for testing the resistance of adhesive tapes to electrolyte is carried out, and the specific steps are as follows:
  • test pieces IV, V, VI the test pieces
  • control pieces I, II, and III the test pieces
  • the change rate of the electrolyte of the adhesive tape is not less than 20% or the attenuation rate of the electrolyte of the adhesive tape is not higher than 80%, and the product is judged to be qualified, and the test results of the above-mentioned adhesive tape Among them, the adhesive tape electrolyte change rate was 3.05%, and the adhesive tape electrolyte attenuation rate was 96.95%. According to the judgment standard, the high-viscosity terminated adhesive tape product was a substandard product.

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Abstract

The present invention relates to an electrolyte resistance testing method for adhesive tape. The method comprises the following steps: respectively adhering adhesive tape to be tested to standard test boards to obtain a control piece and a test piece; immersing the test piece in an electrolyte, leaving same to stand at 45-95°C for 4-24 h, then taking out the test piece, completely soaking up the electrolyte, and then standing for 10-30 min; measuring the peel strength between said adhesive tape and the standard test board of the test piece from which the electrolyte has been completely soaked up, so as to obtain peel strength I; measuring the peel strength between said adhesive tape and the standard test board of the control piece, so as to obtain peel strength II; and taking changes in peel strength I and peel strength II as a determination basis, and contrasting same with a standard or requirement of the adhesive tape to determine whether an electrolyte resistance test for said adhesive tape is up to standard. In the method, a quantization means is implemented in conjunction with the standard or requirement for the adhesive tape, thereby facilitating the accurate determination of whether an adhesive tape product is up to standard. The method has a good reproducibility, and is intuitive.

Description

胶粘带耐电解液的测试方法Test method of adhesive tape resistance to electrolyte 技术领域Technical field
本发明涉及质量检测标准领域,特别是涉及胶粘带耐电解液的测试方法。The invention relates to the field of quality inspection standards, in particular to a method for testing the resistance of an adhesive tape to electrolyte.
背景技术Background technique
随着社会的发展,可充电的二次锂离子电池因具有能量密度高、工作电压高、循环寿命长、无记忆效应、绿色环保和尺寸形状大小可根据实际需求灵活设计等诸多优点,被越来越多的电器设备选为电源,尤其是移动电器设备、储能站和新能源汽车等。广阔的应用领域一直推动着锂离子电池在快速发展。With the development of society, rechargeable secondary lithium-ion batteries have many advantages such as high energy density, high working voltage, long cycle life, no memory effect, green environmental protection, and flexible design according to actual needs. More and more electrical equipment are selected as power sources, especially mobile electrical equipment, energy storage stations and new energy vehicles. The wide range of applications has been driving the rapid development of lithium-ion batteries.
锂电池包括正极、负极和电解液。其中,电解液是锂离子电池核心组成部分之一,其主要成分包括六氟磷酸锂、碳酸乙烯酯、碳酸二乙酯、碳酸二甲酯和碳酸甲乙酯等,具有腐蚀特性。因此,工作环境为电解液的,用于电池内正负材料的固定和绝缘的胶粘带,需要具有耐锂离子电池电解液的性能,耐电解液测试也是其必备的基本测试项目。Lithium batteries include a positive electrode, a negative electrode, and an electrolyte. Among them, the electrolyte is one of the core components of lithium-ion batteries, and its main components include lithium hexafluorophosphate, ethylene carbonate, diethyl carbonate, dimethyl carbonate and ethyl methyl carbonate, etc., which have corrosive properties. Therefore, the working environment is electrolyte, and the adhesive tape used for fixing and insulating the positive and negative materials in the battery needs to have the performance of resistance to the electrolyte of the lithium ion battery, and the electrolyte resistance test is also a necessary basic test item.
然而,现行的胶粘带耐电解液测试方法是直接将胶粘带粘贴于薄薄的铝箔上,再放入电解液中,一段时间后,观察胶粘带是否起拱,移位,穿透,电解液是否掉色,以及撕开胶带后是否残胶等,来判定电解液对胶粘带的影响,进一步来决定胶粘带是否合格。这种方法简单直接,但是,上述方法受主观因素影响较大,测试方法没有标准化,同时,测试方法缺乏量化指标,不利于准确判别胶粘带产品合格与否,实验结果难于重现。However, the current testing method of adhesive tape resistance to electrolyte is to directly paste the adhesive tape on a thin aluminum foil and put it in the electrolyte. After a period of time, observe whether the adhesive tape is arched, shifted, or penetrated. , Whether the electrolyte has faded, and whether the adhesive remains after tearing off the tape, etc., to determine the impact of the electrolyte on the adhesive tape, and further determine whether the adhesive tape is qualified. This method is simple and direct. However, the above method is greatly affected by subjective factors, and the test method is not standardized. At the same time, the test method lacks quantitative indicators, which is not conducive to accurately judging whether the adhesive tape product is qualified or not, and the experimental results are difficult to reproduce.
发明内容Summary of the invention
针对上述行业内存在的技术问题,本发明提供一种胶粘带耐电解液的测试方法,对耐电解液测试过程中的工具和物料进行了规范和标准化,以浸泡电解液前后胶粘带与测试板的剥离强度变化作为评价标准,实施量化手段准确判别胶粘带产品合格与否,上述测试方法重现性好,直观,利于判别。In view of the technical problems existing in the above-mentioned industries, the present invention provides a test method for the resistance of the adhesive tape to electrolyte. The tools and materials used in the electrolyte resistance test process are standardized and standardized. The peel strength change of the test board is used as the evaluation standard, and a quantitative method is implemented to accurately determine whether the adhesive tape product is qualified or not. The above-mentioned test method is reproducible, intuitive, and convenient for discrimination.
具体技术方案为:The specific technical solutions are:
一种胶粘带耐电解液的测试方法,包括以下步骤:A testing method for the resistance of an adhesive tape to electrolyte includes the following steps:
将待测胶粘带分别与标准测试板贴合,得对照件和试验件;Attach the adhesive tape to be tested to the standard test board to obtain the control part and the test part;
将所述试验件浸入电解液中,45℃-95℃下放置4h-24h,取出,吸干电解液后放置10min-30min;Immerse the test piece in the electrolyte, place it at 45°C-95°C for 4h-24h, take it out, absorb the electrolyte and leave it for 10min-30min;
对吸干电解液后的所述试验件的待测胶粘带和标准测试板之间的剥离强度进行测量,得剥离强度I;Measure the peel strength between the adhesive tape to be tested and the standard test plate of the test piece after the electrolyte is dried, and obtain the peel strength I;
对所述对照件的待测胶粘带和标准测试板之间的剥离强度进行测量,得剥离强度II;Measure the peel strength between the adhesive tape to be tested and the standard test board of the reference part, and obtain the peel strength II;
以所述剥离强度I和所述剥离强度II的变化作为判断依据,对照胶粘带标准或要求,判断待测胶粘带的耐电解液测试是否合格。Taking the change of the peeling strength I and the peeling strength II as the judgment basis, and comparing the adhesive tape standards or requirements, it is judged whether the electrolyte resistance test of the adhesive tape to be tested is qualified.
在一些优选的实施例中,以胶粘带电解液变化率作为判断依据,对照胶粘带标准或要求,判断待测胶粘带的耐电解液测试是否合格;In some preferred embodiments, the change rate of the electrolyte of the adhesive tape is used as the judgment basis, and the standards or requirements of the adhesive tape are compared to determine whether the electrolyte resistance test of the adhesive tape to be tested is qualified;
所述的胶粘带电解液变化率的计算方法为:剥离强度I/剥离强度II×100%。The calculation method of the change rate of the electrolyte of the adhesive tape is: peel strength I/peel strength II×100%.
在一些优选的实施例中,以胶粘带电解液衰减率作为判断依据,对照胶粘带标准或要求,判断待测胶粘带的耐电解液测试是否合格;In some preferred embodiments, the attenuation rate of the electrolyte of the adhesive tape is used as the judgment basis, and the standards or requirements of the adhesive tape are compared to determine whether the electrolyte resistance test of the adhesive tape to be tested is qualified;
所述的衰减率的计算方法为:(剥离强度II-剥离强度I)/剥离强度II×100%。The calculation method of the attenuation rate is: (peel strength II-peel strength I)/peel strength II×100%.
在一些优选的实施例中,所述标准测试板选自不锈钢板、玻璃板、铝塑板、铝板、铝箔、铜箔、铜塑板或铜板。In some preferred embodiments, the standard test plate is selected from stainless steel plate, glass plate, aluminum-plastic plate, aluminum plate, aluminum foil, copper foil, copper-plastic plate or copper plate.
在一些优选的实施例中,所述标准测试板的厚度为5μm-400μm。In some preferred embodiments, the thickness of the standard test board is 5 μm-400 μm.
在一些优选的实施例中,将所述试验件浸入所述电解液中的方法为:将所述试验件置于容器内,向所述容器中加入所述电解液。In some preferred embodiments, the method of immersing the test piece in the electrolyte is: placing the test piece in a container, and adding the electrolyte into the container.
在一些优选的实施例中,所述容器为内部设计有相通间隔层的直筒宽口瓶。In some preferred embodiments, the container is a straight wide-mouth bottle with a communicating spacer layer inside.
在一些优选的实施例中,所述容器的材质选自聚四氟乙烯、聚乙烯、聚丙烯、聚苯乙烯、聚苯醚、聚苯硫醚、聚酰胺或玻璃。In some preferred embodiments, the material of the container is selected from polytetrafluoroethylene, polyethylene, polypropylene, polystyrene, polyphenylene ether, polyphenylene sulfide, polyamide or glass.
在一些优选的实施例中,所述贴合后,将所述试验件至少放置10min再浸入所述标准电解液中。In some preferred embodiments, after the bonding, the test piece is placed for at least 10 minutes and then immersed in the standard electrolyte.
在一些优选的实施例中,对吸干电解液后的所述试验件的待测胶粘带和标准测试板之间的剥离强度进行测量时,剥离角度为180度。In some preferred embodiments, when measuring the peel strength between the adhesive tape to be tested and the standard test plate of the test piece after the electrolyte is dried, the peeling angle is 180 degrees.
在一些优选的实施例中,对所述对照件的待测胶粘带和标准测试板之间的剥离强度进行测量时,剥离角度为180度。In some preferred embodiments, when the peel strength between the adhesive tape to be tested and the standard test plate of the control part is measured, the peel angle is 180 degrees.
与现有方案相比,本发明具有以下有益效果:Compared with the existing solutions, the present invention has the following beneficial effects:
本申请发明人以其在本领域的长期经验累积和大量创造性的实验,研究得到了一种胶粘带耐电解液的测试方法,也称“吴氏法”,其通过将待测胶粘带贴合于标准测试板上,然后浸入电解液中,45℃-95℃下放置4h-24h,取出,吸干电解液,对吸干电解液后的所述试验件的待测胶粘带和标准测试板之间的剥离强度进行测量,得剥离强度I,对所述对照件的待测胶粘带和标准测试板之间的剥离强度进行测量,得剥离强度II。以浸泡电解液前后胶粘带与测试板的剥离强度变化作为评价标准,对照胶粘带标准或要求,实施量化手段准确判别胶粘带产品合格与否。上述采用吴氏法对胶粘带耐电解液进行测试,重现性好,直观,利于判别。Based on his long-term experience in the field and a large number of creative experiments, the inventor of the present application has researched and obtained a test method for the resistance of the adhesive tape to electrolyte, also known as the "Wu's method", which passes the test of the adhesive tape Stick it on a standard test board, then immerse it in the electrolyte, place it at 45°C-95°C for 4h-24h, take it out, and blot the electrolyte. After blotting the electrolyte, the adhesive tape and the adhesive tape of the test piece to be tested The peel strength between the standard test plates is measured to obtain the peel strength I, and the peel strength between the adhesive tape to be tested and the standard test plate of the control part is measured to obtain the peel strength II. The change in the peel strength of the adhesive tape and the test board before and after immersion in the electrolyte is used as the evaluation standard, and the adhesive tape standards or requirements are compared with the implementation of quantitative means to accurately determine whether the adhesive tape product is qualified or not. The above-mentioned Wu's method is used to test the adhesive tape's resistance to electrolyte, which has good reproducibility, intuitiveness, and facilitates discrimination.
进一步地,本发明还对标准测试板(命名为“吴氏板”)、盛放电解液容器(命名为“吴氏瓶”),以及耐电解液测试过程中的工具、物料、试验流程和评判方法进行了规范和标准化,具有标准化的测试流程,标准化的试验方法,标准化的数据处理,以及标准化的评判标准,最大程度减少胶粘带测试过程中受主观因素影响,利于在行业内推广。Further, the present invention also provides for the standard test board (named "Wu's plate"), a container for containing the electrolytic solution (named "Wu's bottle"), and tools, materials, test procedures, and test procedures during the electrolyte resistance test. The evaluation method is standardized and standardized, with standardized test procedures, standardized test methods, standardized data processing, and standardized evaluation standards, which minimize the influence of subjective factors during the adhesive tape testing process and facilitate promotion in the industry.
具体实施方式Detailed ways
以下结合具体实施例对本发明作进一步详细的说明。本发明可以以许多不同的形式来实现,并不限于本文所描述的实施方式。相反地,提供这些实施方式的目的是使对本发明公开内容理解更加透彻全面。The present invention will be further described in detail below in conjunction with specific embodiments. The present invention can be implemented in many different forms and is not limited to the embodiments described herein. On the contrary, the purpose of providing these embodiments is to make the understanding of the disclosure of the present invention more thorough and comprehensive.
除非另有定义,本文所使用的所有的技术和科学术语与属于本发明的技术领域的技术人员通常理解的含义相同。本文中在本发明的说明书中所使用的术语只是为了描述具体的实施例的目的,不是旨在于限制本发明。本文所使用的术语“和/或”包括一个或多个相关的所列项目的任意的和所有的组合。Unless otherwise defined, all technical and scientific terms used herein have the same meaning as commonly understood by those skilled in the technical field of the present invention. The terms used in the specification of the present invention herein are only for the purpose of describing specific embodiments, and are not intended to limit the present invention. The term "and/or" as used herein includes any and all combinations of one or more related listed items.
针对现有的胶粘带耐电解液测试方法受主观因素影响较大,没有标准化,同时,测试方法没有采用量化手段,实验结果难于重现,也不利于准确判别胶粘带产品合格与否。本发明提供了一种胶粘带耐电解液的测试方法,也称“吴氏法”。The existing testing methods for the resistance of adhesive tapes to electrolyte are largely affected by subjective factors and are not standardized. At the same time, the testing methods do not use quantitative means, the experimental results are difficult to reproduce, and it is not conducive to accurately judging whether the adhesive tape products are qualified or not. The invention provides a test method for the resistance of an adhesive tape to electrolyte, which is also called "Wu's method".
具体技术方案为:The specific technical solutions are:
一种胶粘带耐电解液的测试方法,包括以下步骤:A testing method for the resistance of an adhesive tape to electrolyte includes the following steps:
将待测胶粘带分别与标准测试板贴合,得对照件和试验件;Attach the adhesive tape to be tested to the standard test board to obtain the control part and the test part;
将所述试验件浸入电解液中,45℃-95℃下放置4h-24h,取出,吸干电解液后放置10min-30min;Immerse the test piece in the electrolyte, place it at 45°C-95°C for 4h-24h, take it out, absorb the electrolyte and leave it for 10min-30min;
对吸干电解液后的所述试验件的待测胶粘带和标准测试板之间的剥离强度进行测量,得剥离强度I;Measure the peel strength between the adhesive tape to be tested and the standard test plate of the test piece after the electrolyte is dried, and obtain the peel strength I;
对所述对照件的待测胶粘带和标准测试板之间的剥离强度进行测量,得剥离强度II;Measure the peel strength between the adhesive tape to be tested and the standard test board of the reference part, and obtain the peel strength II;
以所述剥离强度I和所述剥离强度II的变化作为判断依据,对照胶粘带标准或要求,判断待测胶粘带的耐电解液测试是否合格。Taking the change of the peeling strength I and the peeling strength II as the judgment basis, and comparing the adhesive tape standards or requirements, it is judged whether the electrolyte resistance test of the adhesive tape to be tested is qualified.
具体地,将待测胶粘带与标准测试板贴合的方法可以为:Specifically, the method of attaching the adhesive tape to be tested to the standard test board can be as follows:
将待测胶粘带扯去三至四圈,裁切宽度25mm、长度300mm的胶粘带六条,选取其中一条裁切好的胶粘带,将胶粘带的一端粘贴在标准测试板的一端,使胶粘带自然地置于标准测试板上方,然后使用2KG压辊机以300mm/min的速度来回滚压三次,使待测胶粘带与标准测试板贴合,制得测试件。重复以上操作步骤,制得余下五件测试件。随机地、平均将测试件分为两组,每组三件,一组进行耐电解液试验,称为试验组,测试件称为试验件,另外一组置于恒温恒湿测试环境中,称为对照组,相应的,测试件称为对照件。Tear off three to four turns of the adhesive tape to be tested, and cut six adhesive tapes with a width of 25 mm and a length of 300 mm. Select one of the cut adhesive tapes and paste one end of the adhesive tape on one end of the standard test board , Place the adhesive tape on the standard test board naturally, and then use a 2KG roller machine to roll back and forth three times at a speed of 300mm/min, so that the adhesive tape to be tested is attached to the standard test board to obtain a test piece. Repeat the above steps to obtain the remaining five test pieces. Randomly and averagely divide the test pieces into two groups with three pieces in each group. One group is subjected to the electrolyte resistance test, which is called the test group, the test piece is called the test piece, and the other group is placed in a constant temperature and humidity test environment. For the control group, correspondingly, the test piece is called the control piece.
可以理解地,贴合前,可将待测胶粘带和标准测试板分别放置在恒温恒湿的标准环境下放置不低于30min,进行状态调整。所述恒温恒湿的标准环境可以为23±1℃、50±5%RH(相对湿度)的环境。Understandably, before lamination, the adhesive tape to be tested and the standard test board can be placed in a standard environment of constant temperature and humidity for no less than 30 minutes to adjust the state. The standard environment of constant temperature and humidity may be an environment of 23±1° C. and 50±5% RH (relative humidity).
此外,可以理解地,贴合前,还可对标准测试板进行清洗。In addition, it is understandable that the standard test board can also be cleaned before bonding.
在一些优选的实施例中,所述标准测试板选自不锈钢板、玻璃板、铝塑板、铝板、铝箔、铜箔、铜塑板或铜板,将该标准测试板命名为“吴氏板”。In some preferred embodiments, the standard test plate is selected from stainless steel plate, glass plate, aluminum-plastic plate, aluminum plate, aluminum foil, copper foil, copper-plastic plate or copper plate, and the standard test plate is named "Wu's plate" .
优选地,所述标准测试板的厚度为5μm-400μm。Preferably, the thickness of the standard test board is 5 μm-400 μm.
当所述标准测试板为不锈钢板、玻璃板、铝塑板、铝板、铜塑板或铜板时,所述标准测试板的厚度优选为100μm-400μm。When the standard test plate is a stainless steel plate, a glass plate, an aluminum-plastic plate, an aluminum plate, a copper-plastic plate or a copper plate, the thickness of the standard test plate is preferably 100 μm-400 μm.
当所述标准测试板为铝箔或铜箔时,所述标准测试板的厚度优选为5μm-20μm。When the standard test board is aluminum foil or copper foil, the thickness of the standard test board is preferably 5 μm-20 μm.
在一些优选的实施例中,贴合后,将所述试验件至少放置10min,再浸入所述电解液中。In some preferred embodiments, after bonding, the test piece is placed for at least 10 minutes, and then immersed in the electrolyte.
可以理解地,贴合后,将所述试验件放置于恒温恒湿的标准环境下至少放置10min,然后再浸入所述电解液中。所述恒温恒湿的标准环境可以为23±1℃、50±5%RH(相对湿度)的环境。Understandably, after bonding, the test piece is placed in a standard environment of constant temperature and humidity for at least 10 minutes, and then immersed in the electrolyte. The standard environment of constant temperature and humidity may be an environment of 23±1° C. and 50±5% RH (relative humidity).
在一些优选的实施例中,将所述试验件置于容器内,向所述容器中加入电解液,将盛放电解液容器命名为“吴氏瓶”。In some preferred embodiments, the test piece is placed in a container, the electrolyte is added to the container, and the container containing the discharge solution is named "Wu's bottle".
可以理解地,所述容器可以为直筒宽口瓶。Understandably, the container may be a straight wide-mouth bottle.
应当理解的是,直筒宽口瓶内部可以设计有相通间隔层,也可以不设计间隔层。It should be understood that the interior of the straight wide-mouth bottle may be designed with a communicating spacer layer, or without a spacer layer.
在一些优选的实施例中,所述容器为内部设计有相通间隔层的直筒宽口瓶,隔层的设计,可以同时对多个待测胶粘带进行耐电解液测试,方便将多个试验件分割开,防止试验件叠合,进而影响电解液的充分浸泡。In some preferred embodiments, the container is a straight wide-mouth bottle with a communicating spacer layer inside. The design of the spacer layer can perform electrolyte resistance tests on multiple adhesive tapes to be tested at the same time, which is convenient for multiple tests. The parts are separated to prevent the test parts from overlapping, which will affect the full immersion of the electrolyte.
在一些优选的实施例中,所述容器的材质选自聚四氟乙烯、聚乙烯、聚丙烯、聚苯乙烯、聚苯醚、聚苯硫醚、聚酰胺或玻璃。In some preferred embodiments, the material of the container is selected from polytetrafluoroethylene, polyethylene, polypropylene, polystyrene, polyphenylene ether, polyphenylene sulfide, polyamide or glass.
在一些优选的实施例中,所述电解液为三元锂电解液,可使用锂电池领域常用的三元锂电解液,本发明在此不做更多的限定。In some preferred embodiments, the electrolyte is a ternary lithium electrolyte, and a ternary lithium electrolyte commonly used in the field of lithium batteries can be used, and the present invention is not limited herein.
在一些优选的实施例中,所述电解液为磷酸铁锂电解液,可使用锂电池领域常用的磷酸铁锂电解液,本发明在此不做更多的限定。In some preferred embodiments, the electrolyte is lithium iron phosphate electrolyte, and lithium iron phosphate electrolyte commonly used in the field of lithium batteries can be used, and the present invention is not limited herein.
将所述测试试验件浸入电解液中,45℃-95℃下放置4h-24h,取出后吸干电解液。The test piece is immersed in the electrolyte, placed at 45°C-95°C for 4h-24h, taken out and sucked up the electrolyte.
可以理解地,取出后,用无尘纸先吸干试验件表面残留的电解液,然后在测试环境中放置10min-30min。Understandably, after taking it out, dry the remaining electrolyte on the surface of the test piece with dust-free paper, and then place it in the test environment for 10-30 minutes.
应当理解地,需在吸干电解液后的30min内完成剥离强度测量。It should be understood that the peel strength measurement needs to be completed within 30 minutes after the electrolyte is drained.
所述的测试环境为恒温恒湿的标准环境,所述恒温恒湿的标准环境可以为23±1℃、50±5%RH(相对湿度)的环境。The test environment is a standard environment of constant temperature and humidity, and the standard environment of constant temperature and humidity may be an environment of 23±1° C. and 50±5% RH (relative humidity).
对吸干电解液的试验件和对照件分别进行剥离强度的测试,剥离强度的测试方法可参考国家标准GB/T2792-2014《胶粘带剥离强度的试验方法》。Test the peel strength of the test piece and the control piece that have absorbed the electrolyte. The test method of the peel strength can refer to the national standard GB/T2792-2014 "Test Method for the Peel Strength of Adhesive Tapes".
在一些优选的实施例中,对吸干电解液后的所述试验件的待测胶粘带和标准测试板之间的剥离强度进行测量时,剥离角度为180度。In some preferred embodiments, when measuring the peel strength between the adhesive tape to be tested and the standard test plate of the test piece after the electrolyte is dried, the peel angle is 180 degrees.
在一些优选的实施例中,对所述对照件的待测胶粘带和标准测试板之间的剥离强度进行测量时,剥离角度为180度。In some preferred embodiments, when the peel strength between the adhesive tape to be tested and the standard test plate of the control part is measured, the peel angle is 180 degrees.
应当理解地,在整个测试过程中,试验件浸入电解液环境,对照件置于恒温恒湿测试环境中,除此之外,其余操作两者均应处于相同条件的环境下。It should be understood that during the entire test process, the test piece is immersed in the electrolyte environment, and the control piece is placed in the constant temperature and humidity test environment. Except for this, the other operations should both be under the same conditions.
对吸干电解液后的所述试验件的待测胶粘带和标准测试板之间的剥离强度进行测量,得剥离强度I;对所述对照件的待测胶粘带和标准测试板之间的剥离强度进行测量,得剥离强度II。The peel strength between the adhesive tape to be tested and the standard test board of the test piece after the electrolyte is absorbed is measured to obtain the peel strength I; the adhesive tape to be tested and the standard test board of the control piece The peel strength between the two was measured, and the peel strength II was obtained.
以所述剥离强度I和所述剥离强度II的变化作为判断依据,对照胶粘带标准或要求,判断待测胶粘带的耐电解液测试是否合格。Taking the change of the peeling strength I and the peeling strength II as the judgment basis, and comparing the adhesive tape standards or requirements, it is judged whether the electrolyte resistance test of the adhesive tape to be tested is qualified.
在一些优选的实施例中,可通过剥离强度II和剥离强度I的比值作为判断依据(剥离强度II/剥离强度I×100%),对照胶粘带标准或要求,判断待测胶粘带的耐电解液测试是否合格。即,通过胶粘带电解液变化率判断待测胶粘带的 耐电解液测试是否合格。判断的具体比值,可根据对产品的不同的性能要求来制定。In some preferred embodiments, the ratio of peel strength II to peel strength I can be used as the basis for judgment (peel strength II/peel strength I×100%), and the adhesive tape standards or requirements can be compared to determine the adhesive tape’s performance Whether the electrolyte resistance test is qualified. That is, the electrolyte change rate of the adhesive tape is used to determine whether the test of the electrolyte resistance of the adhesive tape to be tested is qualified. The specific ratio of judgment can be formulated according to the different performance requirements of the product.
在一些优选的实施例中,可通过胶粘带电解液衰减率作为判断依据,对照胶粘带标准或要求,判断待测胶粘带的耐电解液测试是否合格;所述的胶粘带电解液衰减率的计算方法为:(剥离强度II-剥离强度I)/剥离强度II×100%。即,通过胶粘带电解液衰减率法判断待测胶粘带的耐电解液测试是否合格。同样的,判断的具体胶粘带电解液衰减率,可根据对产品的不同的性能要求来制定。In some preferred embodiments, the attenuation rate of the electrolyte of the adhesive tape can be used as the basis for judgment, and the standard or requirements of the adhesive tape can be compared to determine whether the electrolyte resistance test of the adhesive tape to be tested is qualified; the adhesive tape electrolysis The calculation method of the liquid attenuation rate is: (Peel Strength II-Peel Strength I)/Peel Strength II×100%. That is, the electrolyte decay rate method of the adhesive tape is used to determine whether the test of resistance to electrolyte of the adhesive tape to be tested is qualified. Similarly, the specific attenuation rate of the electrolyte of the adhesive tape can be determined according to the different performance requirements of the product.
以应用于锂离子电池中的高粘终止胶粘带为例,根据客户对产品的性能要求,规定采用本发明所述方法判断其是否为合格的标准应为百分比法(剥离强度II/剥离强度I)的测定值大于20%,或衰减法中的衰减率低于80%。Taking the high-viscosity termination adhesive tape used in lithium-ion batteries as an example, according to the customer's performance requirements for the product, it is stipulated that the method of the present invention is used to judge whether it is qualified or not. The percentage method (peel strength II/peel strength The measured value of I) is greater than 20%, or the attenuation rate in the attenuation method is less than 80%.
上述胶粘带耐电解液的测试方法,也称“吴氏法”,具有标准化的测试流程,标准化的试验方法,标准化的数据处理,以及标准化的评判标准。通过对测试过程中使用的耐电解液测试板、耐电解液测试容器、耐电解液测试的其他工具、物料和环境都进行了规范化和标准化,并以浸泡电解液前后胶粘带与测试板的剥离强度变化作为评价标准,对照胶粘带标准或要求,实施量化手段准确判别胶粘带产品合格与否,采用吴氏法对胶粘带耐电解液进行测试,重现性好,直观,利于判别。The above-mentioned test method for the resistance of the adhesive tape to electrolyte, also called "Wu's method", has a standardized test procedure, a standardized test method, a standardized data processing, and a standardized evaluation standard. Through the standardization and standardization of the electrolyte resistance test board, the electrolyte resistance test container, other tools, materials and the environment for the electrolyte resistance test used in the test process, the adhesive tape and the test board before and after immersion in the electrolyte are standardized and standardized. The peel strength change is used as the evaluation standard. Compared with the standard or requirements of the adhesive tape, the quantitative method is implemented to accurately judge whether the adhesive tape product is qualified or not. The Wu's method is used to test the electrolyte resistance of the adhesive tape. The reproducibility is good, intuitive, and beneficial. Discriminate.
以下结合具体实施例进行说明,其中,具体实施例所涉及到的原料、仪器,若无特说明,均可来源于市售。The following description will be given in conjunction with specific embodiments, where the raw materials and instruments involved in the specific embodiments, unless otherwise specified, can all be commercially available.
实施例1Example 1
本实施例提供一种胶粘带耐电解液的测试方法,包括以下步骤:This embodiment provides a method for testing the resistance of an adhesive tape to electrolyte, which includes the following steps:
(1)取待测胶粘带,将其置于23±1℃、50±5%RH(相对湿度)的环境中24h,进行状态调节。(1) Take the adhesive tape to be tested and place it in an environment of 23±1°C and 50±5% RH (relative humidity) for 24 hours to adjust the state.
(2)取6块相同的SUS316标准测试钢板,用丙酮分别擦拭其表面4次,并晾置30min,所述SUS316标准测试钢板的厚度为200μm,表面粗糙度Ra为40nm。(2) Take 6 identical SUS316 standard test steel plates, wipe their surfaces 4 times with acetone, and leave them in the air for 30 minutes. The thickness of the SUS316 standard test steel plates is 200 μm, and the surface roughness Ra is 40 nm.
(3)将待测胶粘带扯去三至四圈,裁切宽度25mm长度300mm的胶粘带六条,选取其中一条裁切好的胶粘带,将胶粘带的一端粘贴在标准测试板的一端,使胶粘带自然地置于标准测试板上方,然后使用2KG压辊机以300mm/min的速度来回滚压三次,使待测胶粘带与标准测试板贴合,制得测试件。重复以上操作步骤,制得余下五件测试件。随机地、平均将测试件分为两组,每组三件,一组进行耐电解液试验,称为试验组,测试件称为试验件D、E、F,另外一组置于恒温恒湿测试环境中,称为对照组,相应的,测试件称为对照件A、B、C。(3) Pull off three to four turns of the adhesive tape to be tested, and cut six adhesive tapes with a width of 25mm and a length of 300mm. Select one of the cut adhesive tapes and paste one end of the adhesive tape on the standard test board. Place the adhesive tape on the standard test board naturally, and then use a 2KG roller machine to roll back and forth three times at a speed of 300mm/min, so that the adhesive tape to be tested is attached to the standard test board to obtain a test piece . Repeat the above steps to obtain the remaining five test pieces. Randomly and averagely divide the test pieces into two groups with three pieces in each group. One group is subjected to the electrolyte resistance test, which is called the test group, the test pieces are called test pieces D, E, F, and the other group is placed at constant temperature and humidity. In the test environment, it is called the control group. Correspondingly, the test pieces are called control pieces A, B, and C.
(4)贴合后,放置15min,将试验组3个试验件分别置于直筒宽口瓶的3个相通的不同隔层中,再向直筒宽口瓶中灌满电解液,于65℃下放置6h,将3个试验件取出,分别用无尘纸吸干电解液,然后放置10min。(4) After bonding, leave it for 15 minutes, put the 3 test pieces of the test group in 3 different compartments of the straight wide-mouth bottle, and then fill the straight wide-mouth bottle with electrolyte, and keep it at 65℃. Leave it for 6 hours, take out the 3 test pieces, dry the electrolyte with dust-free paper, and then leave it for 10 minutes.
(5)对3个对照件和吸干电解液后的3个试验件进行剥离强度试验,方法为:(5) Carry out the peel strength test on the 3 control parts and the 3 test parts after blotting the electrolyte, the method is as follows:
从不锈钢板的一端剥下25mm的胶粘带少许,把钢板的一端夹在拉力试验机的夹具里,胶粘带自由端夹到另一夹具里,使自由端胶粘带与不锈钢板呈现180度。在5±0.2mm/s的速率下180°连续剥离,负载夹具运转后,忽略第一个25mm胶粘带机械剥离时获得的值,以下一个50mm胶粘带获得的平均力值作为剥离力,转换为剥离强度。Peel off a little 25mm adhesive tape from one end of the stainless steel plate, clamp one end of the steel plate in the clamp of the tensile testing machine, and clamp the free end of the adhesive tape to another clamp to make the free end adhesive tape and the stainless steel plate appear 180 Spend. Continuous peeling at 180° at a rate of 5±0.2mm/s. After the load clamp is running, the value obtained when the first 25mm adhesive tape is mechanically peeled off is ignored. The average force value obtained by the next 50mm adhesive tape is used as the peeling force. Converted to peel strength.
3个对照件和3个试验件的剥离强度如表1所示。The peel strengths of 3 control pieces and 3 test pieces are shown in Table 1.
表1Table 1
Figure PCTCN2020088817-appb-000001
Figure PCTCN2020088817-appb-000001
在不同的时间,由不同的测试人员,重复上述实验,得到的结果如表2示。At different times, different testers repeated the above experiment, and the results obtained are shown in Table 2.
表2Table 2
Figure PCTCN2020088817-appb-000002
Figure PCTCN2020088817-appb-000002
Figure PCTCN2020088817-appb-000003
Figure PCTCN2020088817-appb-000003
由表1和表2可知,本实施方法的重现性好。It can be seen from Table 1 and Table 2 that the reproducibility of this implementation method is good.
实施例2Example 2
本实施例提供一种胶粘带耐电解液的测试方法,与实施例1的区别仅在于,标准测试板及其厚度和表面粗糙度与实施例1不同,具体包括以下步骤:This embodiment provides a test method for the resistance of the adhesive tape to electrolyte. The difference from Embodiment 1 is that the standard test board and its thickness and surface roughness are different from those in Embodiment 1, and specifically include the following steps:
(1)取与实施例1相同的待测胶粘带,将其置于23±1℃、50±5%RH(相对湿度)的环境中24h,进行状态调节。(1) Take the same adhesive tape to be tested as in Example 1, and place it in an environment of 23±1° C. and 50±5% RH (relative humidity) for 24 hours to adjust the state.
(2)取6块相同的铝塑板,用丙酮分别擦拭其表面4次,并晾置30min,所述铝塑板的厚度为110μm,表面粗糙度Ra为75nm。(2) Take 6 identical aluminum-plastic panels, wipe their surfaces 4 times with acetone, and leave them in the air for 30 minutes. The thickness of the aluminum-plastic panels is 110 μm, and the surface roughness Ra is 75 nm.
(3)将待测胶粘带扯去三至四圈,裁切宽度25mm长度300mm的胶粘带六条,选取其中一条裁切好的胶粘带,将胶粘带的一端粘贴在标准测试板的一端,使胶粘带自然地置于标准测试板上方,然后用2KG压辊机以300mm/min的速度来回滚压三次,使待测胶粘带与标准测试板贴合,制得测试件。重复以上操作步骤,制得余下五件测试件。随机地、平均将测试件分为两组,每组三件,一组进行耐电解液试验,称为试验组,测试件称为试验件d、e、f,另外一组置于恒温恒湿测试环境中,称为对照组,相应的,测试件称为对照件a、b、c。(3) Pull off three to four turns of the adhesive tape to be tested, and cut six adhesive tapes with a width of 25mm and a length of 300mm. Select one of the cut adhesive tapes and paste one end of the adhesive tape on the standard test board. Place the adhesive tape on the standard test board naturally, and then use a 2KG roller machine to roll back and forth three times at a speed of 300mm/min, so that the adhesive tape to be tested is attached to the standard test board to obtain a test piece . Repeat the above steps to obtain the remaining five test pieces. Randomly and averagely divide the test pieces into two groups, each group has three pieces, one group is subjected to the electrolyte resistance test, which is called the test group, the test pieces are called test pieces d, e, f, and the other group is placed at constant temperature and humidity In the test environment, it is called the control group. Correspondingly, the test pieces are called control pieces a, b, and c.
(4)贴合后,放置15min,将试验组的3个试验件分别置于直筒宽口瓶的3个相通不同隔层中,再向直筒宽口瓶中灌满电解液,于65℃下放置6h,将3个试验件取出,分别用无尘纸吸干电解液,然后放置10min。(4) After bonding, leave it for 15 minutes, put the 3 test pieces of the test group in the three different compartments of the straight wide-mouth bottle, and then fill the straight wide-mouth bottle with electrolyte, and keep it at 65℃. Leave it for 6 hours, take out the 3 test pieces, dry the electrolyte with dust-free paper, and then leave it for 10 minutes.
(5)对3个对照件和吸干电解液后的3个试验件进行剥离强度试验,方法为:(5) Carry out the peel strength test on the 3 control parts and the 3 test parts after blotting the electrolyte, the method is as follows:
从铝塑板的一端剥下25mm的胶粘带少许,把铝塑板的一端夹在拉力试验机的夹具里,胶粘带自由端夹到另一夹具里,使自由端胶粘带与铝塑板呈现180度。在5±0.2mm/s的速率下180°连续剥离,负载夹具运转后,忽略第一个25mm胶粘带机械剥离时获得的值,以下一个50mm胶粘带获得的平均力值作为剥离力,转换为剥离强度。Peel off a little 25mm adhesive tape from one end of the aluminum composite panel, clamp one end of the aluminum composite panel in the fixture of the tensile testing machine, and clamp the free end of the adhesive tape to the other fixture to make the free end adhesive tape and aluminum The plastic board presents 180 degrees. Continuous peeling at 180° at a rate of 5±0.2mm/s. After the load clamp is running, the value obtained when the first 25mm adhesive tape is mechanically peeled off is ignored. The average force value obtained by the next 50mm adhesive tape is used as the peeling force. Converted to peel strength.
3个对照件和3个试验件的剥离强度如表3所示。The peel strengths of 3 control pieces and 3 test pieces are shown in Table 3.
表3table 3
Figure PCTCN2020088817-appb-000004
Figure PCTCN2020088817-appb-000004
Figure PCTCN2020088817-appb-000005
Figure PCTCN2020088817-appb-000005
在不同的时间,由不同的测试人员,重复上述实验,得到的结果如表4所示。At different times, different testers repeated the above experiment, and the results obtained are shown in Table 4.
表4Table 4
Figure PCTCN2020088817-appb-000006
Figure PCTCN2020088817-appb-000006
由表3和表4可知,本实施的测试方法的重现性好。It can be seen from Table 3 and Table 4 that the test method in this implementation has good reproducibility.
实施例3Example 3
本实施例以一个在生产过程中,被客户认定为产品质量不合格的用于锂离子电池的高粘终止胶粘带作为待测胶粘带,分别采用本发明方法和背景技术所提及的现行的胶粘带耐电解液测试的方法进行试验,具体步骤如下:In this embodiment, a high-viscosity termination adhesive tape for lithium-ion batteries that was identified by the customer as unqualified during the production process is used as the adhesive tape to be tested, and the method of the present invention and the background art mentioned in the background technology are used respectively. The current method for testing the resistance of adhesive tapes to electrolyte is carried out, and the specific steps are as follows:
方法1method 1
(1)取该胶粘带,将其置于23±1℃、50±5%RH(相对湿度)的环境中24h,进行状态调节。(1) Take the adhesive tape and place it in an environment of 23±1°C and 50±5% RH (relative humidity) for 24 hours to adjust the state.
(2)取6片相同的铝箔,用丙酮分别擦拭其表面4次,并晾置30min,所述铝箔的厚度为11μm。(2) Take 6 pieces of the same aluminum foil, wipe their surfaces 4 times with acetone, and leave them in the air for 30 minutes. The thickness of the aluminum foil is 11 μm.
(3)将待测胶粘带扯去三至四圈,裁切宽度25mm长度300mm的胶粘带六条,选取其中一条裁切好的胶粘带,将胶粘带的一端粘贴在铝箔的一端,使胶粘带自然地置于铝箔上方,然后用2KG压辊机以300mm/min的速度来回滚 压三次,使待测胶粘带与铝箔贴合,制得测试件。重复以上操作步骤,制得余下五件测试件。随机地、平均将测试件分为两组,每组三件,一组进行耐电解液试验,称为试验组,测试件称为试验件IV、V、VI,另外一组置于恒温恒湿测试环境中,称为对照组,相应的,测试件称为对照件I、II、III。(3) Pull off three to four turns of the adhesive tape to be tested, and cut six adhesive tapes with a width of 25mm and a length of 300mm. Select one of the cut adhesive tapes and paste one end of the adhesive tape on one end of the aluminum foil , The adhesive tape is naturally placed on the aluminum foil, and then rolled back and forth three times at a speed of 300mm/min with a 2KG roller press, so that the adhesive tape to be tested is bonded to the aluminum foil to obtain a test piece. Repeat the above steps to obtain the remaining five test pieces. Randomly and averagely divide the test pieces into two groups, each group has three pieces, one group is subjected to the electrolyte resistance test, which is called the test group, the test pieces are called test pieces IV, V, VI, and the other group is placed at constant temperature and humidity. In the test environment, it is called the control group, and correspondingly, the test pieces are called control pieces I, II, and III.
(4)贴合后,放置15min,将3个试验件分别置于直筒宽口瓶的3个相通不同间隔层中,再向直筒宽口瓶中灌满电解液,于85℃下放置12h,将3个试验件取出,分别用无尘纸吸干电解液,然后放置10min。(4) After bonding, place it for 15 minutes, place the 3 test pieces in the three communicating layers of the straight wide-mouth bottle, and then fill the straight wide-mouth bottle with electrolyte, and place it at 85°C for 12 hours. Take out the 3 test pieces, dry the electrolyte with dust-free paper, and then leave them for 10 minutes.
(5)对3个对照件和吸干电解液后的3个试验件进行剥离强度试验,方法为:(5) Carry out the peel strength test on the 3 control parts and the 3 test parts after blotting the electrolyte, the method is as follows:
用强力双面胶粘带将试验件粘贴到不锈钢测试板上,从铝箔的一端剥下25mm的胶粘带少许,把铝箔连同钢板的一端夹在拉力试验机的夹具里,胶粘带自由端夹到另一夹具里,使自由端胶粘带与铝箔呈现180度。在5±0.2mm/s的速率下180°连续剥离,负载夹具运转后,忽略第一个25mm胶粘带机械剥离时获得的值,以下一个50mm胶粘带获得的平均力值作为剥离力,转换为剥离强度。Stick the test piece on the stainless steel test board with strong double-sided adhesive tape, peel off a little 25mm adhesive tape from one end of the aluminum foil, and clamp the aluminum foil and one end of the steel plate in the fixture of the tensile testing machine, the free end of the adhesive tape Clamp it into another fixture to make the free end adhesive tape and the aluminum foil appear 180 degrees. Continuous peeling at 180° at a rate of 5±0.2mm/s. After the load clamp is running, the value obtained when the first 25mm adhesive tape is mechanically peeled off is ignored. The average force value obtained by the next 50mm adhesive tape is used as the peeling force. Converted to peel strength.
3个对照件和3个试验件的剥离强度如表5所示。The peel strengths of 3 control pieces and 3 test pieces are shown in Table 5.
表5table 5
Figure PCTCN2020088817-appb-000007
Figure PCTCN2020088817-appb-000007
根据高粘终止胶粘带的判断标准,胶粘带电解液变化率不低于20%或胶粘带电解液衰减率不高于80%,判为产品合格,而上述胶粘带的测试结果中,胶粘带电解液变化率为3.05%,胶粘带电解液衰减率为96.95%,根据该判断标准,该高粘终止胶粘带产品为不合格产品。According to the judgment standard of high-viscosity terminated adhesive tape, the change rate of the electrolyte of the adhesive tape is not less than 20% or the attenuation rate of the electrolyte of the adhesive tape is not higher than 80%, and the product is judged to be qualified, and the test results of the above-mentioned adhesive tape Among them, the adhesive tape electrolyte change rate was 3.05%, and the adhesive tape electrolyte attenuation rate was 96.95%. According to the judgment standard, the high-viscosity terminated adhesive tape product was a substandard product.
方法2(背景技术中所介绍的现行的方法)Method 2 (the current method introduced in the background art)
(1)取同一胶粘带,将其置于23±1℃、50±5%RH(相对湿度)的环境中24h,进行状态调节。(1) Take the same adhesive tape and place it in an environment of 23±1°C and 50±5% RH (relative humidity) for 24 hours to adjust the state.
(2)裁取所述胶粘带,得到1个试样。(2) Cut the adhesive tape to obtain 1 sample.
(3)将宽度25mm的胶粘带试样粘贴于铝箔(厚度为11μm)上,用2KG压辊来回压滚一次,剪成20mm长度三片,浸入电解液中,85℃下放置12h,观察胶粘带是否起拱,移位,穿透,电解液是否掉色,以及撕开胶带后是否残胶。测试结果如表6所示。(3) Paste the adhesive tape sample with a width of 25mm on the aluminum foil (thickness of 11μm), roll it back and forth with a 2KG pressure roller, cut into three pieces of 20mm length, immerse them in the electrolyte, and place them at 85℃ for 12h, and observe Whether the adhesive tape is arched, displaced, penetrated, whether the electrolyte has faded, and whether the adhesive remains after the tape is torn off. The test results are shown in Table 6.
表6Table 6
 To 起拱Arching 移位Shift 穿透penetrate 脱色Bleaching 掉胶Glue drop
试验件Test piece no no no no no
由表6的测试结果可知,根据现行的胶粘带测试方法及判别标准,该胶粘带应为合格。可见,现行的胶粘带测试方法的测试结果存在一定弊端。本发明的测试方法结果更准确。It can be seen from the test results in Table 6 that the adhesive tape should be qualified according to the current adhesive tape testing method and judgment standard. It can be seen that the test results of the current adhesive tape test method have certain drawbacks. The result of the test method of the present invention is more accurate.
以上所述实施例的各技术特征可以进行任意的组合,为使描述简洁,未对上述实施例中的各个技术特征所有可能的组合都进行描述,然而,只要这些技术特征的组合不存在矛盾,都应当认为是本说明书记载的范围。The technical features of the above-mentioned embodiments can be combined arbitrarily. In order to make the description concise, all possible combinations of the various technical features in the above-mentioned embodiments are not described. However, as long as there is no contradiction in the combination of these technical features, All should be considered as the scope of this specification.
以上所述实施例仅表达了本发明的几种实施方式,其描述较为具体和详细,但并不能因此而理解为对本发明专利范围的限制。应当指出的是,对于本领域的普通技术人员来说,在不脱离本发明构思的前提下,还可以做出若干变形和改进,这些都属于本发明的保护范围。因此,本发明专利的保护范围应以所附权利要求为准。The above-mentioned embodiments only express several implementation modes of the present invention, and their description is relatively specific and detailed, but they should not be understood as a limitation on the patent scope of the present invention. It should be pointed out that for those of ordinary skill in the art, without departing from the concept of the present invention, several modifications and improvements can be made, and these all fall within the protection scope of the present invention. Therefore, the protection scope of the patent of the present invention should be subject to the appended claims.

Claims (10)

  1. 一种胶粘带耐电解液的测试方法,其特征在于,包括以下步骤:A method for testing the resistance of an adhesive tape to electrolyte, which is characterized in that it comprises the following steps:
    将待测胶粘带分别与标准测试板贴合,得对照件和试验件;Attach the adhesive tape to be tested to the standard test board to obtain the control part and the test part;
    将所述试验件浸入电解液中,45℃-95℃下放置4h-24h,取出,吸干电解液后放置10min-30min;Immerse the test piece in the electrolyte, place it at 45°C-95°C for 4h-24h, take it out, absorb the electrolyte and leave it for 10min-30min;
    对吸干电解液后的所述试验件的待测胶粘带和标准测试板之间的剥离强度进行测量,得剥离强度I;Measure the peel strength between the adhesive tape to be tested and the standard test plate of the test piece after the electrolyte is dried, and obtain the peel strength I;
    对所述对照件的待测胶粘带和标准测试板之间的剥离强度进行测量,得剥离强度II;Measure the peel strength between the adhesive tape to be tested and the standard test board of the reference part, and obtain the peel strength II;
    以所述剥离强度I和所述剥离强度II的变化作为判断依据,对照胶粘带标准或要求,判断待测胶粘带的耐电解液测试是否合格。Taking the change of the peeling strength I and the peeling strength II as the judgment basis, and comparing the adhesive tape standards or requirements, it is judged whether the electrolyte resistance test of the adhesive tape to be tested is qualified.
  2. 根据权利要求1所述的胶粘带耐电解液的测试方法,其特征在于,以胶粘带电解液变化率作为判断依据,对照胶粘带标准或要求,判断待测胶粘带的耐电解液测试是否合格;The test method for the resistance of the adhesive tape to electrolyte according to claim 1, wherein the change rate of the electrolyte of the adhesive tape is used as a judgment basis, and the standard or requirement of the adhesive tape is compared to determine the resistance of the adhesive tape to be tested. Whether the liquid test is qualified;
    所述的胶粘带电解液变化率的计算方法为:剥离强度I/剥离强度II×100%。The calculation method of the change rate of the electrolyte of the adhesive tape is: peel strength I/peel strength II×100%.
  3. 根据权利要求1所述的胶粘带耐电解液的测试方法,其特征在于,以胶粘带电解液衰减率作为判断依据,对照胶粘带标准或要求,判断待测胶粘带的耐电解液测试是否合格;The method for testing the resistance of the adhesive tape to electrolyte according to claim 1, wherein the attenuation rate of the electrolyte of the adhesive tape is used as a judgment basis, and the standards or requirements of the adhesive tape are compared to determine the resistance of the adhesive tape to be tested. Whether the liquid test is qualified;
    所述的胶粘带电解液衰减率的计算方法为:(剥离强度II-剥离强度I)/剥离强度II×100%。The calculation method of the attenuation rate of the electrolyte of the adhesive tape is: (peel strength II-peel strength I)/peel strength II×100%.
  4. 根据权利要求1所述的胶粘带耐电解液的测试方法,其特征在于,所述标准测试板选自不锈钢板、玻璃板、铝塑板、铝板、铝箔、铜箔、铜塑板或铜板。The method for testing the adhesive tape resistance to electrolyte according to claim 1, wherein the standard test board is selected from the group consisting of stainless steel plate, glass plate, aluminum-plastic plate, aluminum plate, aluminum foil, copper foil, copper-plastic plate or copper plate .
  5. 根据权利要求4所述的胶粘带耐电解液的测试方法,其特征在于,所述标准测试板的厚度为5μm-400μm。The method for testing the resistance of the adhesive tape to electrolyte according to claim 4, wherein the thickness of the standard test board is 5 μm-400 μm.
  6. 根据权利要求1-5任一项所述的胶粘带耐电解液的测试方法,其特征在于,将所述试验件浸入所述电解液中的方法为:将所述试验件置于容器内,向所述容器中加入所述电解液。The method for testing the adhesive tape resistance to electrolyte according to any one of claims 1-5, wherein the method of immersing the test piece in the electrolyte is: placing the test piece in a container , Add the electrolyte to the container.
  7. 根据权利要求6所述的胶粘带耐电解液的测试方法,其特征在于,所述容器为内部设计有相通间隔层的直筒宽口瓶。The method for testing the resistance of the adhesive tape to electrolyte according to claim 6, wherein the container is a straight wide-mouth bottle with a communicating spacer layer inside.
  8. 根据权利要求6所述的胶粘带耐电解液的测试方法,其特征在于,所述容器的材质选自聚四氟乙烯、聚乙烯、聚丙烯、聚苯乙烯、聚苯醚、聚苯硫醚、聚酰胺或玻璃。The method for testing the resistance of the adhesive tape to electrolyte according to claim 6, wherein the material of the container is selected from polytetrafluoroethylene, polyethylene, polypropylene, polystyrene, polyphenylene ether, polyphenylene sulfide Ether, polyamide or glass.
  9. 根据权利要求1-5任一项所述的胶粘带耐电解液的测试方法,其特征在于,所述贴合后,将所述试验件至少放置10min,再浸入所述电解液中。The method for testing the resistance of the adhesive tape to electrolyte according to any one of claims 1 to 5, characterized in that, after the bonding, the test piece is placed for at least 10 minutes, and then immersed in the electrolyte.
  10. 根据权利要求1-5任一项所述的胶粘带耐电解液的测试方法,其特征在于,对吸干电解液后的所述试验件的待测胶粘带和标准测试板之间的剥离强度进行测量时,剥离角度为180度;The method for testing the adhesive tape's resistance to electrolyte according to any one of claims 1-5, wherein the gap between the adhesive tape to be tested and the standard test board of the test piece after the electrolyte is absorbed When the peel strength is measured, the peel angle is 180 degrees;
    对所述对照件的待测胶粘带和标准测试板之间的剥离强度进行测量时,剥 离角度为180度。When measuring the peel strength between the adhesive tape to be tested and the standard test plate of the control piece, the peeling angle is 180 degrees.
PCT/CN2020/088817 2020-05-06 2020-05-06 Electrolyte resistance testing method for adhesive tape WO2021223115A1 (en)

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