CN109269866B - Method for rapidly judging electric heating aging of polypropylene film for capacitor and application and verification method thereof - Google Patents
Method for rapidly judging electric heating aging of polypropylene film for capacitor and application and verification method thereof Download PDFInfo
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- CN109269866B CN109269866B CN201811085533.9A CN201811085533A CN109269866B CN 109269866 B CN109269866 B CN 109269866B CN 201811085533 A CN201811085533 A CN 201811085533A CN 109269866 B CN109269866 B CN 109269866B
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- 239000004743 Polypropylene Substances 0.000 title claims abstract description 151
- -1 polypropylene Polymers 0.000 title claims abstract description 151
- 229920001155 polypropylene Polymers 0.000 title claims abstract description 151
- 230000032683 aging Effects 0.000 title claims abstract description 46
- 239000003990 capacitor Substances 0.000 title claims abstract description 45
- 238000000034 method Methods 0.000 title claims abstract description 42
- 238000012795 verification Methods 0.000 title claims abstract description 15
- 238000005485 electric heating Methods 0.000 title description 2
- 238000010438 heat treatment Methods 0.000 claims abstract description 36
- 238000005520 cutting process Methods 0.000 claims abstract description 11
- 238000012360 testing method Methods 0.000 claims description 48
- 239000002245 particle Substances 0.000 claims description 13
- 238000005481 NMR spectroscopy Methods 0.000 claims description 8
- 229920006378 biaxially oriented polypropylene Polymers 0.000 claims description 8
- 239000011127 biaxially oriented polypropylene Substances 0.000 claims description 8
- 238000003825 pressing Methods 0.000 claims description 7
- 230000007547 defect Effects 0.000 abstract description 8
- 238000002360 preparation method Methods 0.000 abstract description 2
- 210000000697 sensory organ Anatomy 0.000 abstract 1
- 239000010408 film Substances 0.000 description 118
- 239000004033 plastic Substances 0.000 description 11
- 239000003963 antioxidant agent Substances 0.000 description 5
- 230000003078 antioxidant effect Effects 0.000 description 5
- 230000008569 process Effects 0.000 description 5
- 238000004458 analytical method Methods 0.000 description 3
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 238000002329 infrared spectrum Methods 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 239000010409 thin film Substances 0.000 description 3
- 238000004566 IR spectroscopy Methods 0.000 description 2
- 238000005452 bending Methods 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 239000011810 insulating material Substances 0.000 description 2
- 238000009413 insulation Methods 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000007246 mechanism Effects 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- 230000035882 stress Effects 0.000 description 2
- 238000010998 test method Methods 0.000 description 2
- 238000003878 thermal aging Methods 0.000 description 2
- 230000008646 thermal stress Effects 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000002238 attenuated effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000013016 damping Methods 0.000 description 1
- 230000001934 delay Effects 0.000 description 1
- 238000001514 detection method Methods 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 238000010292 electrical insulation Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 230000007774 longterm Effects 0.000 description 1
- 238000013178 mathematical model Methods 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
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- 239000000126 substance Substances 0.000 description 1
- 238000010200 validation analysis Methods 0.000 description 1
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01R—MEASURING ELECTRIC VARIABLES; MEASURING MAGNETIC VARIABLES
- G01R31/00—Arrangements for testing electric properties; Arrangements for locating electric faults; Arrangements for electrical testing characterised by what is being tested not provided for elsewhere
- G01R31/003—Environmental or reliability tests
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- Engineering & Computer Science (AREA)
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- General Physics & Mathematics (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
Abstract
The invention discloses a method for rapidly judging the electrothermal aging of a polypropylene film for a capacitor and an application and verification method thereof, which comprises the following steps: (1) cutting 10-100 layers of polypropylene films into sample blocks; (2) putting the polypropylene film sample block into an oven for heat treatment; (3) and observing the surface condition of the polypropylene film sample block subjected to heat treatment to judge whether the electrothermal aging performance of the polypropylene film is qualified. The invention has the advantages that the defect that 500 or 1000 hours can be carried out after a finished product capacitor is manufactured when the durability index of the polypropylene film is qualified is changed, whether the durability index of the polypropylene film is qualified or not can be quickly judged by sense organ through heat treatment for several hours after the polypropylene film is singly subjected to sample preparation, the verification time is greatly shortened, the verification cost is reduced, and the yield of the capacitor is further improved.
Description
Technical Field
The invention relates to the field of capacitor preparation, in particular to a method for judging the electrothermal aging of a polypropylene film used as a capacitor insulating material and an application and verification method thereof.
Background
With the rapid development of industry, the demand of the fields such as rail transit, SVG, solar photovoltaic, smart grid, household appliances and the like for capacitance is increasing, and the polypropylene film is widely used as an insulating medium material in the capacitor. The polypropylene film will inevitably be exposed to light, oxidation, thermal degradation, etc. during use and storage, undergoing an aging process. The performance of the aged film is reduced, and the service performance of the polypropylene plastic is seriously influenced. Due to the complexity of the aging mechanism, it is difficult to directly study the change of the film performance caused by various aging reasons, and the change is analyzed and studied through experiments. The current aging test is mainly an artificial aging test method, which is a method for simulating certain aging factors under natural environment by using an aging box in a laboratory to obtain a test result. At present, the general detection method of polypropylene films, GB/T13542.2-2009 film part 2 for electrical insulation: the performance indexes in the test method can not intuitively reflect the aging of the capacitor caused by electric stress and thermal stress in the using process. To accurately evaluate the electrical and thermal aging of polypropylene films requires long-term durability tests in which polypropylene films are formed into capacitors and heated and energized. For example, the voltage-capacity of a capacitor using a polypropylene film as an insulating material is 2200VDC-1000 muF, the working temperature is 70 ℃, and the durability test has two methods according to the GB/T17702-2013 power electronic capacitor standard, wherein one method is to test for 500 hours under the condition of 2200 x 1.4=3080VDC under the condition of 70 ℃, the other method is to test for 1000 hours under the condition of 2200 x 1.3=2860VDC under the condition of 70 ℃, and the durability is judged to be qualified if the capacitor capacity is attenuated to be less than or equal to 3% after the test is finished. The durability is mainly evaluated by the electric resistance and the heat resistance of the polypropylene film. This greatly delays the final determination of the polypropylene film properties, increases the validation costs and increases the risks of production and use.
Chinese patent publication No. CN104749128A discloses a method for measuring aging time of polypropylene plastic by using infrared spectroscopy, which comprises the following steps: (1) two sets of polypropylene plastic samples were prepared; (2) measuring the aging time of each polypropylene plastic sample in the first group of polypropylene plastic samples according to a conventional method; (3) performing infrared spectrum analysis on each polypropylene plastic sample in the second group of samples by using an infrared spectrometer, collecting spectrogram data, drawing a standard curve according to the relation between the characteristic peak height and the antioxidant content, establishing a mathematical model by using a partial least square method, and calculating a fitting equation, namely determining an antioxidant content infrared spectrum analysis equation; (4) scanning the polypropylene plastic to be detected by using an infrared spectrometer, substituting the characteristic peak height of a sample to be detected into an antioxidant content infrared spectrum analysis equation, calculating the antioxidant content, and contrasting standard data to determine the aging time of the polypropylene plastic. The aging time of the polypropylene plastic is calculated by using the antioxidant content measured by infrared spectroscopy, and the obtained data can only be used for estimating the durability of the polypropylene plastic in a normal state and cannot be used for estimating the durability of the polypropylene plastic under specific conditions (heating and electrifying).
Disclosure of Invention
The invention aims to solve the technical problem that the existing indexes for evaluating the polypropylene film cannot reflect the electrical and thermal aging performance of the polypropylene film for the capacitor, and after the polypropylene film is made into the capacitor, the conclusion of whether the durability index of the polypropylene film for the capacitor is qualified or not can be obtained according to the standard within 500 or 1000 hours, thereby improving the verification cost and increasing the production and use risks, so that the applicant wants to shorten the verification time, therefore, three groups of polypropylene films are marked as A group, B group and C group, each group of polypropylene films is cut into two parts, one part of the three groups of polypropylene films is made into capacitors marked as A1 group, B1 group and C1 group, the other part of the three groups is marked as A2 group, B2 group and C2 group, wherein the A1 group and the B1 group are polypropylene films qualified by the standard test, the C1 group is unqualified polypropylene films, the A2 group, the B2 group and the C2 group are discovered by various tests, when the test condition is that the A2 group and the B2 group are not changed when the polypropylene film of the C2 group is heated for a certain time at a certain temperature, and the heating time is far shorter than 500h or 1000h required by a standard test, the relation between the temperature time node at which the polypropylene film is hardened and the capacity attenuation rate of the capacitor is found, and the hardening mechanism is that certain macromolecular chains of the polypropylene film of the C2 group are broken into small molecular chains in the process of preparing the polypropylene film from polypropylene particles, and the small molecular chains are volatilized under a specific heating condition to cause the hardening of the polypropylene film, so that the capacity attenuation rate of the capacitor is used as a basis for measuring the durability index of the polypropylene film, the polypropylene film for the capacitor is subjected to single heat treatment to judge whether the bending angle alpha is larger than 30 degrees or not, and the corresponding relation is established between the bending angle and the capacity attenuation rate of the capacitor, the invention is the core innovation point of the invention, and provides a method for rapidly judging the electrothermal aging of the polypropylene film and application thereof.
The technical scheme of the invention is as follows: the method for rapidly judging the electrothermal aging of the polypropylene film comprises the following steps: (1) cutting the polypropylene film with more than 10 layers into sample blocks with the length and width of (200-; (2) putting the polypropylene film sample block into a baking oven with the temperature of 120-150 ℃ for heat treatment for 10-6000 min; (3) placing the polypropylene film sample block subjected to heat treatment on a test bed, wherein the length of the polypropylene film sample block placed on the test bed is L1, the length of the polypropylene film sample block is L1-1/3, placing a pressing block on the polypropylene film sample block, observing an included angle alpha between a connecting line of the lowest point and the highest point of a part L2 of the polypropylene film sample block exceeding the test bed and the horizontal plane of the test bed, and if the alpha is less than or equal to 30 degrees, determining that the electrothermal aging performance of the polypropylene film is unqualified.
The application of the method for rapidly judging the electrothermal aging of the polypropylene film is used for evaluating the electrothermal aging performance of an electrical biaxially oriented polypropylene film produced by polypropylene particles with isotacticity of more than or equal to 97 percent tested by a nuclear magnetic resonance spectroscopy, in other words, the method for rapidly judging the electrothermal aging of the polypropylene film is suitable for the polypropylene film made of high-temperature polypropylene particles.
The invention also provides a method for judging the electrothermal aging of a polypropylene film made of common polypropylene particles, namely the method is used for evaluating the electrothermal aging performance of an electrical biaxially oriented polypropylene film produced by polypropylene particles with the isotacticity of 94-97 percent and tested by a nuclear magnetic resonance spectroscopy method and comprises the following steps: (1) cutting the polypropylene film with more than 10 layers into sample blocks with the length and width of (200-; (2) putting the polypropylene film sample block into an oven with the temperature of 90-130 ℃ for heat treatment for 10-3000 min; (3) placing the polypropylene film sample block subjected to heat treatment on a test bed, wherein the length of the polypropylene film sample block placed on the test bed is L1, the length of the polypropylene film sample block is L1-1/3, placing a pressing block on the polypropylene film sample block, observing an included angle alpha between a connecting line of the lowest point and the highest point of a part L2 of the polypropylene film sample block exceeding the test bed and the horizontal plane of the test bed, and if the alpha is less than or equal to 30 degrees, determining that the electrothermal aging performance of the polypropylene film is unqualified.
The verification method for rapidly judging the electrothermal aging of the polypropylene film comprises the following steps: and (3) cutting the polypropylene film into two groups, observing alpha after the operation of the steps (1) to (3) on one group, and testing the capacitance attenuation rate of the capacitor after the other group is made into a finished capacitor, wherein the capacitance attenuation rate of the capacitor corresponding to the polypropylene film exceeds a standard value if the alpha in the step (3) is less than or equal to 30 degrees.
The invention has the advantages that the defect that the test verification for 500 or 1000 hours can be carried out only after the finished capacitor is made when the durability index of the polypropylene film is qualified is changed, and the polypropylene film can be rapidly judged whether to be qualified on the durability index by heat treatment for several hours after the polypropylene film is singly sampled, so that the verification time is greatly shortened, the verification cost is reduced, and the yield of the capacitor is improved.
Drawings
FIG. 1 is a photograph of a polypropylene film having an unacceptable durability after heat treatment;
FIG. 2 is a photograph of a polypropylene film having satisfactory durability after heat treatment.
Detailed Description
The technical scheme in the embodiment of the invention is clearly and completely described below by combining the embodiment. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments based on the embodiments in the present invention, without any inventive work, will be apparent to those skilled in the art from the following description.
Example 1: the method for rapidly judging the electrothermal aging of the polypropylene film comprises the following steps: (1) cutting 10 layers of polypropylene films into sample blocks with the length and the width of 200 x 10 mm; (2) putting the polypropylene film sample block into a 120 ℃ oven for heat treatment for 6000 min; (3) placing the polypropylene film sample block subjected to heat treatment on a test bed, wherein the length of the polypropylene film sample block placed on the test bed is L1, the length of the polypropylene film sample block is L1-1/3, placing a pressing block on the polypropylene film sample block, observing an included angle alpha between a connecting line of the lowest point and the highest point of a part L2 of the polypropylene film sample block exceeding the test bed and the horizontal plane of the test bed, and if the alpha is less than or equal to 30 degrees, determining that the electrothermal aging performance of the polypropylene film is unqualified, wherein the polypropylene film is shown in figure 1; if α >30 ° the polypropylene film is as shown in figure 2.
Example 2: the method for rapidly judging the electrothermal aging of the polypropylene film comprises the following steps: (1) cutting the 30 layers of polypropylene films into sample blocks with the length and the width of 200 x 300 mm; (2) putting the polypropylene film sample block into an oven at 130 ℃ for heat treatment for 800 min; (3) placing the polypropylene film sample block subjected to heat treatment on a test bed, wherein the length of the polypropylene film sample block placed on the test bed is L1, the length of the polypropylene film sample block is L1-1/3, placing a pressing block on the polypropylene film sample block, observing an included angle alpha between the part L2 of the polypropylene film sample block, which exceeds the test bed, and if the angle alpha is less than or equal to 30 degrees, determining that the electrothermal aging performance of the polypropylene film is unqualified.
Example 3: the method for rapidly judging the electrothermal aging of the polypropylene film comprises the following steps: (1) cutting 60 layers of polypropylene films into sample blocks with the length and the width of 500 x 10 mm; (2) putting the polypropylene film sample block into a baking oven with the temperature of 140 ℃ for heat treatment for 360 min; (3) placing the polypropylene film sample block subjected to heat treatment on a test bed, wherein the length of the polypropylene film sample block placed on the test bed is L1, the length of the polypropylene film sample block is L1-1/3, placing a pressing block on the polypropylene film sample block, observing an included angle alpha between a connecting line of the lowest point and the highest point of a part L2 of the polypropylene film sample block exceeding the test bed and the horizontal plane of the test bed, and if the alpha is less than or equal to 30 degrees, determining that the electrothermal aging performance of the polypropylene film is unqualified.
Example 4: the method for rapidly judging the electrothermal aging of the polypropylene film comprises the following steps: (1) cutting 100 layers of polypropylene films into sample blocks with the length and the width of 500 x 300 mm; (2) putting the polypropylene film sample block into a drying oven at 150 ℃ for heat treatment for 10 min; (3) placing the polypropylene film sample block subjected to heat treatment on a test bed, wherein the length of the polypropylene film sample block placed on the test bed is L1, the length of the polypropylene film sample block is L1-1/3, placing a pressing block on the polypropylene film sample block, observing an included angle alpha between a connecting line of the lowest point and the highest point of a part L2 of the polypropylene film sample block exceeding the test bed and the horizontal plane of the test bed, and if the alpha is less than or equal to 30 degrees, determining that the electrothermal aging performance of the polypropylene film is unqualified.
The objects judged in examples 1 to 4 above were electrical grade biaxially oriented polypropylene films produced using polypropylene particles having an isotacticity of 97% or more as measured by nuclear magnetic resonance spectroscopy.
Example 5: the difference from example 1 is that the heat treatment temperature in step (2) was 90 ℃ and the heat treatment time was 3000 min.
Example 6: the difference from example 2 is that the heat treatment temperature in step (2) was 100 ℃ and the heat treatment time was 300 min.
Example 7: the difference from example 3 is that the heat treatment temperature in step (2) was 110 ℃ and the heat treatment time was 100 min.
Example 8: the difference from example 4 is that the heat treatment temperature in step (2) was 130 ℃ and the heat treatment time was 10 min.
Examples 5-8 identified objects were electrical grade biaxially oriented polypropylene films produced using polypropylene particles with isotacticity of 94% -97% as measured by nuclear magnetic resonance spectroscopy.
Through hundreds of experiments, the invention discovers that the self-healing of the capacitor is excessive and the insulation strength of the film medium is reduced for a sample which passes through the traditional heat-resistant and electricity-resistant test of the polypropylene film and detects that the capacity attenuation rate of the capacitor does not reach the standard, which indicates that certain defects exist in the film medium of the sample which does not reach the standard. These defects in the thin film medium should be generated during the thin film material processing process, which causes the breakage and degradation of macromolecular chains into small molecular substances, and the formation of defects in the thin film medium. After heating and power-up, the defects of the film medium are further accelerated and amplified under the action of electric stress and thermal stress, the insulating strength is reduced, and the capacitance attenuation is enlarged. And the insulation strength of the film medium of the sample with the capacitor capacity attenuation rate up to the standard is not changed, which shows that the material of the sample is not problematic, and no defect is formed in the processing process of the film medium. Therefore, it is thought that if the polypropylene film is subjected to a heat treatment for a certain period of time and at a certain temperature, if the polypropylene film itself has a small molecular defect of degradation, it gradually volatilizes at a certain temperature, and the state of the film itself changes (a certain degree of hardening warpage occurs). After a plurality of tests, the method for rapidly detecting and judging the electrothermal aging of the polypropylene film, namely the durability index of the polypropylene film is determined by finding that the corresponding capacitor capacity attenuation rate is smaller than a standard value if the polypropylene film exceeds the part L2 of the test bed and the included angle alpha between the test bed and the test bed in the step (3) is larger than 30 degrees.
The verification process of the invention is as follows: and (3) cutting the polypropylene film into two groups, observing alpha after the operation of the steps (1) to (3) on one group, testing the capacitance attenuation rate of the capacitor after the finished capacitor is manufactured on the other group, and finding that the capacitance attenuation rate of the capacitor corresponding to the polypropylene film exceeds a standard value if alpha is less than or equal to 30 degrees in the step (3) through a plurality of comparison tests, thereby indicating that the operation mode of the invention has accurate and credible results.
The verification method is suitable for evaluating the electrothermal aging performance of the electrical-grade biaxially oriented polypropylene film (high-temperature polypropylene particles) produced by polypropylene particles with isotacticity of more than or equal to 97 percent tested by a nuclear magnetic resonance spectroscopy and the electrical-grade biaxially oriented polypropylene film (common polypropylene particles) produced by polypropylene particles with isotacticity of 94-97 percent tested by the nuclear magnetic resonance spectroscopy. Whether the electrothermal aging performance of the polypropylene film is qualified or not can be determined only by direct observation, and the method is efficient and convenient.
The standard value mentioned in the invention is different according to different types of capacitors, for example, the standard value of the capacitance attenuation rate of a power electronic capacitor is +/-3%, the standard value of the capacitance attenuation rate of an alternating current motor capacitor is +/-3%, and the standard value of the capacitance attenuation rate of a capacitor for a converter valve damping absorption loop of a high-voltage direct current transmission system is +/-2%.
Claims (5)
1. The method for rapidly judging the electrothermal aging of the polypropylene film for the capacitor is characterized by comprising the following steps of: (1) cutting the polypropylene film with more than 10 layers into sample blocks with the length and width of (200-; (2) putting the polypropylene film sample block into a baking oven with the temperature of 120-150 ℃ for heat treatment for 10-6000 min; (3) placing the polypropylene film sample block subjected to heat treatment on a test bed, wherein the length of the polypropylene film sample block placed on the test bed is L1, the length of the polypropylene film sample block is L1-1/3, placing a pressing block on the polypropylene film sample block, observing an included angle alpha between a connecting line of the lowest point and the highest point of a part L2 of the polypropylene film sample block exceeding the test bed and the horizontal plane of the test bed, and if the alpha is less than or equal to 30 degrees, determining that the electrothermal aging performance of the polypropylene film is unqualified.
2. The method for rapidly judging the electrothermal aging of a polypropylene film for capacitors as claimed in claim 1, wherein the heat treatment temperature in said step (2) is 120 ℃ to 130 ℃ and the heat treatment time is 10min to 3000 min.
3. The use of the method for rapidly determining the electrothermal aging of a polypropylene film for capacitors as claimed in claim 1, wherein: the method is used for evaluating the electrothermal aging performance of the electrical biaxially oriented polypropylene film produced by polypropylene particles with isotacticity of more than or equal to 97 percent tested by a nuclear magnetic resonance spectroscopy.
4. The use of the method for rapidly determining the electrothermal aging of a polypropylene film for capacitors as claimed in claim 2, wherein: used for evaluating the electrothermal aging performance of an electrical grade biaxially oriented polypropylene film produced from polypropylene particles with an isotacticity of 94% -97% tested by nuclear magnetic resonance spectroscopy.
5. The verification method of the method for rapidly judging the electrothermal aging of a polypropylene film for capacitors as claimed in claim 1 or 2, wherein: the method comprises the following steps: and (3) cutting the polypropylene film into two groups, observing alpha after the operation of the steps (1) to (3) on one group, and testing the capacitor capacitance attenuation rate after the finished capacitor is manufactured on the other group, wherein the capacitor capacitance attenuation rate corresponding to the polypropylene film exceeds a standard value if the alpha in the step (3) is less than or equal to 30 degrees.
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| CN110031302A (en) * | 2019-04-19 | 2019-07-19 | 国网四川省电力公司电力科学研究院 | A kind of capacitor BOPP film ageing properties test method |
| CN113358159A (en) * | 2021-07-08 | 2021-09-07 | 无锡市电力滤波有限公司 | Method for inspecting metallized polypropylene film for direct-current support capacitor |
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2018
- 2018-09-18 CN CN201811085533.9A patent/CN109269866B/en active Active
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