Quickly determine the method and its application of polypropylene film for capacitor thermal-electrical aging and tests
Card method
Technical field
The present invention relates to capacitor preparation fields, more particularly to determine the polypropylene film electricity for being used as capacitor insulation material
The method and its application and verification method of heat ageing.
Background technique
With the rapid development of industry, either rail traffic, SVG, photovoltaic, smart grid, household electrical appliance etc.
Demand of the field to capacitor is increasing, and polypropylene film is widely used as the insulating dielectric materials in capacitor.It is poly-
Polypropylene film using and storage process in will inevitably by illumination, oxidation, thermal degradation the effects of, undergo aging
Journey.Film performance after aging declines, and has seriously affected the service performance of polypropylene plastics.Due to answering for its agine mechaism
Polygamy is also difficult to the variation of film performance caused by directly researching various senile causes at present, but is analyzed by testing
Research.Current degradation is mainly accelerated aging test method, it is to utilize ageing oven simulating natural environment in laboratory
Under certain aging actions carry out degradation, the method for obtaining test result.Currently, the general detection side of polypropylene film
Performance indicator in method " GB/T 13542.2-2009 electric insulation film part 2: test method " can not be intuitively anti-
Answer the aging as caused by electric stress and thermal stress in capacitor use process.Want electricity, the heat of accurate evaluation polypropylene film old
Change the long-duration experiments for needing for polypropylene film to be made capacitor and carrying out heating power-up.Such as made with polypropylene film
The voltage-capacity of the capacitor of insulating materials is 2200VDC-1000 μ F, and operating temperature is 70 DEG C, then according to " GB/T
17702-2013 power electronic capacitor " standard, durability experiment there are two types of method, a kind of method be under the conditions of 70 DEG C,
It is tested 500 hours under the conditions of 2200*1.4=3080VDC, another method is 2200*1.3=2860VDC item under the conditions of 70 DEG C
It is tested 1000 hours under part, if after experiment, condenser capacity decaying≤3% then judges durability qualification.And durability
What is mainly examined is exactly resistance to electric, the heat-resisting ability of polypropylene film.This has delayed finally sentencing for polypropylene film performance significantly
It is fixed, verifying expense is improved, the risk for increasing production and using.
Chinese invention patent publication number CN104749128A discloses a kind of old using infrared spectrum measurement polypropylene plastics
Change the method for time, comprising the following steps: (1) prepare two groups of polypropylene plastics samples;(2) first group is measured according to a conventional method to gather
The ageing time of each polypropylene plastics sample in Acrylic plastic sample;(3) using infrared spectrometer to each poly- in second group of sample
Acrylic plastic sample carries out infrared spectrum analysis, acquires spectral data, is drawn according to characteristic peak peak height and antioxidant content relationship
Standard curve calculates fit equation with Partial Least Squares founding mathematical models, that is, determines antioxidant content infrared spectroscopy point
Analyse equation;(4) polypropylene plastics to be measured is scanned with infrared spectrometer, the feature peak height of sample to be tested is substituted into antioxidant content
Infrared spectrum analysis equation, calculates antioxidant content, and reference standard data can determine polypropylene plastics ageing time.It should
Invention calculates polypropylene plastics ageing time using the oxidation preventive content that infrared spectrum measurement comes out, and the data obtained can only
For the durability estimation of polypropylene plastics under normality, the resistance to of (heating, power-up) polypropylene plastics is not used under specified conditions
Long property estimation.
Summary of the invention
The technical problem to be solved by the present invention is to the indexs of existing evaluation polypropylene film can not all reflect capacitor
With the electricity of polypropylene film, heat aging performance, after polypropylene film that capacitor is made, then establishing criteria needs 500 or 1000
Hour can just obtain polypropylene film for capacitor durability index whether He Ge conclusion, improve verifying expense, increase
Production and the risk used, applicant just thinks whether the verification time can be shortened thus, then that three groups of polypropylene are thin
Film is denoted as A group, B group and C group, and every group of polypropylene film is cut into two parts, and a part production capacitor is denoted as A1 group, B1 group and C1
Group, another part, which keeps sample, is denoted as A2 group, B2 group and C2 group, and wherein A1 group and B1 group are that the polypropylene through code test qualification is thin
Film, C1 group are underproof polypropylene films, and a variety of tests of A2 group, B2 group and C2 group are found, when experimental condition is with one
Determining A2 group and B2 group when temperature heating certain time, there is no variations, and the polypropylene film of C2 group hardens, and should add
500h needed for the hot time is far smaller than code test or 1000h, consequently found that polypropylene film harden temperature when
Contacting between intermediate node and the capacity attenuation rate of capacitor, and the mechanism hardened is the polypropylene film of C2 group by polypropylene
Certain macromolecular chains fragment into small molecule chain during polypropylene film is made in particle, these small molecule chains are specifically heating
Under the conditions of can volatilize, cause polypropylene film to be hardened, thus using the capacity attenuation rate of capacitor as measure polypropylene film it is resistance to
Polypropylene film for capacitor be individually heat-treated and then judges whether its bent angle alpha is greater than by the basis of long property index
30 °, the capacity attenuation rate of the bending angle and capacitor is established into corresponding relationship, this is core of the invention innovative point,
A kind of method and its application for quickly determining polypropylene film thermal-electrical aging are provided thus.
The technical scheme is that quickly determine polypropylene film thermal-electrical aging method, it the following steps are included:
(1), 10 layers or more of polypropylene film is cut to the sample block that length and width are (200-500) * (10-300) mm;(2), by polypropylene
Film sample block is put into 120 DEG C -150 DEG C of baking oven heat treatment 10min-6000min;(3), by the polypropylene film through Overheating Treatment
Sample block is placed on testing stand, and being placed on testing stand length is L1, the polypropylene film sample block length of L1≤1/3, and poly- third
Briquetting, the minimum point of part L2 of the observation polypropylene film sample block beyond testing stand and the company of highest point are placed on alkene film sample block
Angle α between line and testing stand horizontal plane illustrates that the thermal-electrical aging performance of polypropylene film is unqualified if α≤30 °.
The application of the method for above-mentioned quick judgement polypropylene film thermal-electrical aging, it uses NMR spectrum for assessing
The thermal-electrical aging performance of electrician's grade bidirectional stretching polypropylene film of the polypropylene particles production of isotacticity >=97% of method test,
In other words the method for above-mentioned quick judgement polypropylene film thermal-electrical aging is suitable for polypropylene made of high temperature polypropylene particles
Film.
The present invention also provides a kind of thermal-electrical aging judgements suitable for polypropylene film made of plain polypropylene particle
Method, i.e., for assess using nuclear magnetic resonance spectroscopy test isotacticity 94%-97% polypropylene particles produce electrician
The thermal-electrical aging performance of grade bidirectional stretching polypropylene film, it the following steps are included: (1), by 10 layers or more of polypropylene film
It is cut to the sample block that length and width are (200-500) * (10-300) mm;(2), polypropylene film sample block is put into 90 DEG C -130 DEG C of baking
Case is heat-treated 10min-3000min;(3), the polypropylene film sample block through Overheating Treatment is placed on testing stand, is placed on examination
Testing on platform length is L1, the polypropylene film sample block length of L1≤1/3, and briquetting is placed on polypropylene film sample block, and observation is poly-
Polypropylene film sample block is beyond the angle between the minimum point of part L2 and the line of highest point and testing stand horizontal plane of testing stand
α illustrates that the thermal-electrical aging performance of polypropylene film is unqualified if α≤30 °.
Quickly determine the verification method of the method for polypropylene film thermal-electrical aging, it is the following steps are included: thin by polypropylene
Film cuts into two groups, and one group is observed α after the operation of the step (1) to step (3), after another group is made fabricated capacitors
Carry out the test of condenser capacity attenuation rate, the corresponding capacitor electricity of discovery polypropylene film if α≤30 ° in step (3)
Capacity attenuation rate is above standard value.
The beneficial effects of the invention are as follows change when whether test polypropylene film durability index is qualified in the past to make
The drawbacks of just can be carried out 500 or 1000 hours verification experimental verifications after fabricated capacitors passes through after polypropylene film is individually carried out sample preparation
The heat treatment for spending several hours can quickly judge whether the polypropylene film is qualified on durability index, substantially reduces and tests
The time is demonstrate,proved, reduces verifying expense, and then improve the yields of capacitor.
Detailed description of the invention
Fig. 1 is the photo after the underproof polypropylene film of durability is heat-treated;
Fig. 2 is the photo after the polypropylene film of durability qualification is heat-treated.
Specific embodiment
Below with reference to embodiment, technical scheme in the embodiment of the invention is clearly and completely described.Obviously, institute
The embodiment of description is only a part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention,
Those of ordinary skill in the art's every other embodiment without making creative work, belongs to protection of the invention
Range.
Embodiment 1: quickly determine polypropylene film thermal-electrical aging method, it the following steps are included: (1), by 10 layers
Polypropylene film is cut to the sample block that length and width are 200*10mm;(2), polypropylene film sample block is put at 120 DEG C of baking oven heat
Manage 6000min;(3), the polypropylene film sample block through Overheating Treatment is placed on testing stand, the length being placed on testing stand
For L1, the polypropylene film sample block length of L1≤1/3, and briquetting is placed on polypropylene film sample block, observe polypropylene film sample
Block is beyond the angle α between the minimum point of part L2 and the line of highest point and testing stand horizontal plane of testing stand, if α≤30 °
Then illustrate that the thermal-electrical aging performance of polypropylene film is unqualified, polypropylene film is as shown in Figure 1;The polypropylene film if 30 ° of α >
As shown in Figure 2.
Embodiment 2: quickly determine polypropylene film thermal-electrical aging method, it the following steps are included: (1), by 30 layers
Polypropylene film is cut to the sample block that length and width are 200*300mm;(2), polypropylene film sample block is put at 130 DEG C of baking oven heat
Manage 800min;(3), the polypropylene film sample block through Overheating Treatment is placed on testing stand, the length being placed on testing stand
For L1, the polypropylene film sample block length of L1≤1/3, and briquetting is placed on polypropylene film sample block, observe polypropylene film sample
Block illustrates the thermal-electrical aging of polypropylene film beyond the angle α between the part L2 and testing stand of testing stand if α≤30 °
It can be unqualified.
Embodiment 3: quickly determine polypropylene film thermal-electrical aging method, it the following steps are included: (1), by 60 layers
Polypropylene film is cut to the sample block that length and width are 500*10mm;(2), polypropylene film sample block is put at 140 DEG C of baking oven heat
Manage 360min;(3), the polypropylene film sample block through Overheating Treatment is placed on testing stand, the length being placed on testing stand
For L1, the polypropylene film sample block length of L1≤1/3, and briquetting is placed on polypropylene film sample block, observe polypropylene film sample
Block is beyond the angle α between the minimum point of part L2 and the line of highest point and testing stand horizontal plane of testing stand, if α≤30 °
Then illustrate that the thermal-electrical aging performance of polypropylene film is unqualified.
Embodiment 4: quickly determine polypropylene film thermal-electrical aging method, it the following steps are included: (1), by 100 layers
Polypropylene film is cut to the sample block that length and width are 500*300mm;(2), polypropylene film sample block is put at 150 DEG C of baking oven heat
Manage 10min;(3), the polypropylene film sample block through Overheating Treatment is placed on testing stand, the length being placed on testing stand is
The polypropylene film sample block length of L1, L1≤1/3, and briquetting is placed on polypropylene film sample block, observe polypropylene film sample block
Angle α between the minimum point of part L2 and the line of highest point and testing stand horizontal plane beyond testing stand, if α≤30 °
Illustrate that the thermal-electrical aging performance of polypropylene film is unqualified.
The object that above-described embodiment 1-4 determines is the polypropylene for isotacticity >=97% tested using nuclear magnetic resonance spectroscopy
Electrician's grade bidirectional stretching polypropylene film of particle production.
Embodiment 5: the difference from embodiment 1 is that the heat treatment temperature of step (2) is 90 DEG C, heat treatment time is
3000min。
Embodiment 6: the difference from example 2 is that the heat treatment temperature of step (2) is 100 DEG C, heat treatment time is
300min。
Embodiment 7: the difference with embodiment 3 is that the heat treatment temperature of step (2) is 110 DEG C, and heat treatment time is
100min。
Embodiment 8: the difference with embodiment 4 is that the heat treatment temperature of step (2) is 130 DEG C, and heat treatment time is
10min。
The object that embodiment 5-8 determines is the polypropylene grain of the isotacticity 94%-97% tested using nuclear magnetic resonance spectroscopy
Electrician's grade bidirectional stretching polypropylene film of son production.
The present invention detects capacitor to traditional heat-resisting resistance to electric test of polypropylene film is passed through by up to a hundred experiments, discovery
Device capacity attenuation rate sample not up to standard, capacitors self-healing is excessive, and the dielectric strength of thin film dielectrics all decreases, and illustrates not reach
Have the defects that inside the thin film dielectrics of standard specimen product certain.Defect inside these thin film dielectrics should be processed in thin-film material
It is generated in journey, macromolecular chain fracture is caused in film manufacturing process, is degraded into small-molecule substance, is formed and is lacked inside thin film dielectrics
It falls into.After heating power-up, thin film dielectrics defect further speeds up amplification under the action of electric stress, thermal stress, and insulation is strong
Degree decline, capacitance fall-off expand.And the sample that condenser capacity attenuation rate is up to standard, thin film dielectrics dielectric strength do not change,
Illustrate that there is no problem for sample itself material, does not form defect in thin film dielectrics process.Thus expect polypropylene is thin
Film individually carries out the heat treatment of certain time and certain temperature, if the existing small molecule defect degraded of polypropylene film itself
If, it can gradually be evaporated at a certain temperature, and the state of film itself, which will be varied, (to be occurred a degree of hard
Change warpage).By test of many times, discovery by step (3) if part L2 of the detection polypropylene film beyond testing stand with
Then corresponding condenser capacity attenuation rate is less than standard value when angle α > 30 ° between testing stand, has thereby determined that quick detection
Determine polypropylene film thermal-electrical aging, that is, polypropylene film durability index method.
Verification process of the invention is as follows: polypropylene film being cut into two groups, one group by the step (1) to step
(3) α is observed after operation, another group is made progress capacitor capacitance attenuation rate test after fabricated capacitors, by repeatedly comparing
Test, discovery corresponding condenser capacity attenuation rate of the polypropylene film if α≤30 ° in step (3) are above standard value, say
Bright mode of operation of the invention is as a result, accurate believable.
Verification method of the invention is suitable for assessing the polypropylene for isotacticity >=97% tested using nuclear magnetic resonance spectroscopy
The electrician's grade bidirectional stretching polypropylene film (high temperature polypropylene particles) and use nuclear magnetic resonance spectroscopy test that particle produces
Electrician's grade bidirectional stretching polypropylene film (plain polypropylene particle) electric heating of the polypropylene particles production of isotacticity 94%-97% is old
Change performance.Need to only carry out directly observing can determine whether the thermal-electrical aging performance of polypropylene film is qualified, it is efficiently convenient.
The standard value referred in the present invention is different according to its standard value of different types of capacitor, such as power electronics capacitor
The capacitance fall-off rate standard value of device is ± 3%, and the capacitance fall-off rate standard value of capacitor for ac motor is ± 3%, high pressure
The capacitance fall-off rate standard value of DC transmission system converter valve braking absorption circuit electricity container is ± 2%.