CN113012937A - Metallized film for humidity-resistant and heat-resistant capacitor - Google Patents
Metallized film for humidity-resistant and heat-resistant capacitor Download PDFInfo
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- CN113012937A CN113012937A CN201911326802.0A CN201911326802A CN113012937A CN 113012937 A CN113012937 A CN 113012937A CN 201911326802 A CN201911326802 A CN 201911326802A CN 113012937 A CN113012937 A CN 113012937A
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- 239000003990 capacitor Substances 0.000 title claims abstract description 87
- 239000011104 metalized film Substances 0.000 title claims abstract description 74
- 239000011241 protective layer Substances 0.000 claims abstract description 71
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910052710 silicon Inorganic materials 0.000 claims abstract description 34
- 239000010703 silicon Substances 0.000 claims abstract description 34
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 32
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 32
- 239000001301 oxygen Substances 0.000 claims abstract description 32
- 229910020489 SiO3 Inorganic materials 0.000 claims abstract description 28
- 229910052681 coesite Inorganic materials 0.000 claims abstract description 27
- 229910052906 cristobalite Inorganic materials 0.000 claims abstract description 27
- 239000000377 silicon dioxide Substances 0.000 claims abstract description 27
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims abstract description 27
- 229910052682 stishovite Inorganic materials 0.000 claims abstract description 27
- 229910052905 tridymite Inorganic materials 0.000 claims abstract description 27
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 3
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 3
- 239000010410 layer Substances 0.000 claims description 41
- 230000008859 change Effects 0.000 claims description 32
- 239000002184 metal Substances 0.000 claims description 25
- 229910052751 metal Inorganic materials 0.000 claims description 25
- -1 polypropylene Polymers 0.000 claims description 8
- 239000004743 Polypropylene Substances 0.000 claims description 3
- 239000011701 zinc Substances 0.000 claims description 3
- HCHKCACWOHOZIP-UHFFFAOYSA-N Zinc Chemical compound [Zn] HCHKCACWOHOZIP-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229920001155 polypropylene Polymers 0.000 claims description 2
- 238000005011 time of flight secondary ion mass spectroscopy Methods 0.000 claims description 2
- 229910052725 zinc Inorganic materials 0.000 claims description 2
- 238000001228 spectrum Methods 0.000 abstract description 23
- 239000010408 film Substances 0.000 abstract description 15
- 230000001105 regulatory effect Effects 0.000 abstract 1
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- 238000009832 plasma treatment Methods 0.000 description 10
- 238000012360 testing method Methods 0.000 description 9
- 238000000034 method Methods 0.000 description 7
- 238000000151 deposition Methods 0.000 description 6
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- 238000001704 evaporation Methods 0.000 description 2
- 230000003993 interaction Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 description 2
- 229920003216 poly(methylphenylsiloxane) Polymers 0.000 description 2
- 229920000647 polyepoxide Polymers 0.000 description 2
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- BLRPTPMANUNPDV-UHFFFAOYSA-N Silane Chemical group [SiH4] BLRPTPMANUNPDV-UHFFFAOYSA-N 0.000 description 1
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- FJMNNXLGOUYVHO-UHFFFAOYSA-N aluminum zinc Chemical compound [Al].[Zn] FJMNNXLGOUYVHO-UHFFFAOYSA-N 0.000 description 1
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- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000005484 gravity Effects 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 238000007731 hot pressing Methods 0.000 description 1
- 125000002887 hydroxy group Chemical group [H]O* 0.000 description 1
- 239000011229 interlayer Substances 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
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- 238000001883 metal evaporation Methods 0.000 description 1
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- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 230000000144 pharmacologic effect Effects 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 229920000642 polymer Polymers 0.000 description 1
- 238000004382 potting Methods 0.000 description 1
- 238000007789 sealing Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
- 238000003466 welding Methods 0.000 description 1
- 230000037303 wrinkles Effects 0.000 description 1
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Classifications
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/018—Dielectrics
- H01G4/06—Solid dielectrics
- H01G4/14—Organic dielectrics
- H01G4/18—Organic dielectrics of synthetic material, e.g. derivatives of cellulose
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/005—Electrodes
- H01G4/008—Selection of materials
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/002—Details
- H01G4/224—Housing; Encapsulation
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/32—Wound capacitors
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-SENSITIVE DEVICES OF THE ELECTROLYTIC TYPE
- H01G4/00—Fixed capacitors; Processes of their manufacture
- H01G4/33—Thin- or thick-film capacitors
Landscapes
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Manufacturing & Machinery (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Fixed Capacitors And Capacitor Manufacturing Machines (AREA)
Abstract
A moisture-and heat-resistant metallized film for capacitors, which has a compressive strength in the range of 0 to 0.25MPa when wound into a capacitor core of 0.47 μ F for 2 hr. The metallized film has a protective layer with regulated components, the protective layer contains one or more of silicon, oxygen or carbon elements, wherein the relative atomic percentage of the oxygen element is more than 20 percent, and the protective layer contains the oxygen element76SiO3 ‑Number of radicals and75SiO2CH3 ‑the ratio of the number of groups (TOF-SMIS spectrum) is more than or equal to 0.02, and the surface density of silicon element is 0.02-0.25 mu g/cm2In the meantime. The metallizationThe capacitor made of the film has good humidity and heat resistance.
Description
Technical Field
The invention relates to the field of metallized films, which comprises a novel composition structure of a metallized film, wherein a film capacitor made of the metallized film has good humidity and heat resistance.
Background
The film capacitor is applied to the fields of household appliances, electric automobiles and charging equipment, and plays the roles of relieving current impact and filtering an alternating circuit. The principle is to store electric charges in two thin metal layers which are insulated and opposite to each other; wherein the metal thin layer is arranged on the surface of the polymer film and is wound together with the polymer film to form a laminated structure of metal layers and polymer layers, and because the thickness of each layer is very thin, the film capacitor can provide a large enough surface for storing charges.
Thin film capacitors that do not have manufacturing defects also fail during use. The failure reason is mainly that the resistance is increased due to the oxidation of the metal layer, and the metal layer generates a large amount of heat under the condition that the capacitor is loaded with alternating current, so that the capacitor is deformed, melted through and even exploded. Under the popularization of high-energy electronic equipment and electric automobiles, the performance stability of the film capacitor is gradually improved, and the stable operation under long-time and extreme conditions becomes the necessary requirement of the performance of the current capacitor.
The vapor-deposited oil layer can be used for manufacturing the humidity-resistant and heat-resistant capacitor film, the oil layer is small in using amount and low in cost, and the method is a common method for producing the humidity-resistant and heat-resistant capacitor film at present. The oil layer covers the surface of the metal layer, and because the oil layer has better hydrophobicity than metal, the oil layer can prevent water vapor from directly contacting the metal surface and prevent the metal from being oxidized. The method of evaporating the oil layer is also deficient. The oil layer is liquid and has the characteristics of agglomeration and transfer, so that the form of the oil layer on the surface of the metal layer is unstable, and the exposed part of the metal layer is easily corroded by moisture (application number: PCT/CN 2019/083601). The stability of the oil layer is one of the factors that restrict the resistance to moist heat of the film capacitor.
Disclosure of Invention
Aiming at the problem that the humidity resistance and heat resistance of a common capacitor film are unstable, the invention provides a novel humidity resistance metallized film composition structure. The scheme has low cost and can improve the humidity and heat resistance of the metallized film.
The technical scheme of the invention is as follows:
a moisture and heat resistant metallized film for a capacitor, which has a compressive strength in the range of 0 to 0.25MPa when the metallized film is wound into a capacitor core of 0.47 muF for 2 hr.
Due to the requirement for substantial resistance to moist heat, it is preferred that the metallized film comprises a dielectric layer, a metal layer, and a protective layer.
The compressive strength is one of the apparent properties of the protective layer used in the present invention, and when the value is greater than 0.25MPa, it indicates that the interaction between the metal surface side of the metallized film and the insulating layer side of the counterpart metallized film is large, i.e., the difference in surface energy is large, since the metal surface is not sufficiently covered with the protective layer, and the presence of the metal increases the surface energy of the surface of the metallized film, in which case moisture penetrates into the exposed site of the metal layer, and the moisture and heat resistance of the metallized film is lowered. Because the compressive strength needs to be maintained at a relatively low level to prevent interlayer gaps, wrinkles and sliding difficulties, the insulating medium layer needs to have a relatively thin thickness, good mechanical strength and high pressure resistance, and preferably comprises polypropylene; the thickness is less than or equal to 10 mu m.
Since the compressive strength is required to have good stability over time and the interface composition between layers is required to be relatively stable, the metal layer is required to have corrosion resistance and easy processability, and it is preferable that the metal layer contains one or more of aluminum or zinc.
Since it is required that the smaller the compressive strength is, the better the lubricity of the organic substance is, it is preferable that the protective layer contains one or more of elemental silicon, oxygen, or carbon; the relative atomic percent of the oxygen element is more than 20 percent; said protective layer when analyzed using TOF-SIMS,76SiO3 -number of radicals and75SiO2CH3 -the ratio of the number of the groups is more than or equal to 0.02. The protective layer is post-treated with oxygen plasma to produce inorganic cross-linking sites, i.e.76SiO3 -As a raw material for the protective layer, a modified silicone oil having one or more of a silylhydride group, an epoxy group, a hydroxyl group, a phenyl group, a carboxyl group, an amino group, a vinyl group, a mercapto group, an alkyl group having 4 or more carbon atoms, or an acid anhydride group is generally used in order to increase the yield of the crosslinking point, and a general methyl silicone oil or methyl phenyl silicone oil can be also realized by adjusting the plasma treatment conditions76SiO3 -Number of radicals and75SiO2CH3 -the ratio of the number of groups (TOF-SMIS spectrum) is more than or equal to 0.02.
Since the content of the protective layer on the surface of the metallized film can affect the sliding behavior between layers of the metallized film, namely the compressive strength, the surface density of the silicon element in the protective layer is preferably 0.02-0.25 mug/cm2In the meantime. When the surface density of the silicon element of the protective layer reaches 0.02 mu g/cm2When the surface density of silicon element in the protective layer exceeds 0.25 mu g/cm, the moisture and heat resistance of the metallized film capacitor can reach less than 20 percent2In time, the manufacturing cost of the metallized film starts to increase.
In addition, the molecular weight of the protective layer is also limited in order to meet the requirements for compressive strength. The number average molecular weight of the raw materials is required to be 600-5000 g/mol. The general evaporation oil has the number average molecular weight less than 600g/mol, and is not suitable for being used as the raw material of the protective layer, because the low molecular weight oil has low adhesion to the surface of the metal layer, and the oil layer structure cannot be stable for a long time; however, the vapor deposition oil having a number average molecular weight of more than 5000g/mol has good adhesion to the surface of the metal layer, but the cohesive force of the oil molecule increases with the increase of the number average molecular weight, and the vapor deposition oil has an excessively high molecular weight, so that the molecules are easily agglomerated and voids appear in the protective layer.
The invention also discloses a capacitor, which comprises the metalized film.
Because the metallized film has good humidity resistance, under the premise of packaging by using non-humidity-resistant heat-sealing potting adhesive, the capacitor is preferably tested for 1500hr under the conditions of 310VAC, 85 ℃ and 85% RH, and the capacity change rate is less than or equal to 20%.
The invention has the beneficial effects that:
(1) the invention discloses a metallized film with a stable protective layer structure, which can improve the humidity and heat resistance of the metallized film.
(2) The invention has the advantages of wide source of raw materials, easy acquisition and low consumption, and reduces the material cost of the moisture-proof thermal capacitor.
(3) The film capacitor manufactured by the invention is suitable for high-temperature and high-humidity environment, and can prolong the service life of electrical equipment.
Drawings
Fig. 1 and 2 are schematic diagrams of compressive strength analysis methods.
Detailed Description
The present invention is described in more detail by the following examples, which are not intended to limit the present invention.
The analytical methods used in the examples and comparative examples are as follows:
(1) compressive strength analysis
The metallized film was wound into a cylindrical core in accordance with the capacitor specification of 0.47 μ F, and the compressive strength was measured using a push-pull dynamometer (model GNS-SC, Jinnosheng technologies, Inc., Shenzhen).
During testing, the core is compressed downwards by a distance of half of the inner diameter, and the peak value index f in the process is recorded in unit kg. The inside diameter D, outside diameter D, width a, in mm, of the core were measured with a vernier caliper. The compressive strength δ is calculated according to the following formula:
δ＝(f×g)/[a×(D-d)]
wherein, delta is the compression strength and the unit MPa; f is the peak reading in kg; g is gravity acceleration in m/s2(ii) a a is the inner diameter of the core in mm; d is the outer diameter of the core in mm; d is the core inside diameter in mm. In the examples and comparative examples, g is 9.8m/s2The value of a is 14.60mm, the value of D is 11.10mm, and the value of D is 3.00 mm.
(2) Number average molecular weight analysis
A small amount of the protective layer material was diluted and tested by GPC using THF mobile phase to obtain the number average molecular weight.
(3) Relative atomic percent of oxygen
The relative atomic percent of oxygen on the surface of the protective layer of the metallized film was measured using K-Alpha + XPS from Thermo Scientific to excite the X-ray source Monoc hromic Al K α1,2A laid line (1486.6eV), X-ray region 400 μm, and the inclination angle of the detector with respect to the sample surface was 90 °.
(4)76SiO3 2-Number of radicals and75SiO2CH3 -ratio of the number of radicals
(5) Metallized film protective layerIs/are as follows76SiO3 -Number of radicals and75SiO2CH3 -the ratio of the number of radicals was analyzed using a TOF-SIMS5 time-of-flight secondary ION mass spectrometer from ION-TOF corporation, 1 ION Bi3+ +, 2 IONs negative in polarity. Areal density analysis of silicon element
The silicon element surface density represents the content of the silicon oil, and the surface density of the silicon element of the metallized film is measured by an X-ray fluorescence spectrometer (pharmacological ZSX Primus III +) with the unit of mu g/cm2。
(6) Analysis of humidity and heat resistance of capacitor
The manufactured capacitor is placed in an environment with 310VAC, 85 ℃ and 85% RH for 1500hr, the capacity before and after treatment is measured, and the capacity change rate is calculated as follows:
capacity change rate ═ C1500 hr-C0 hr)/C0 hr×100％
In the formula, C1500 hr、C0 hrThe capacitor capacities after the wet heat treatment and before the treatment were measured.
The raw material compositions of the protective layers used in the examples and comparative examples are shown in table 1:
TABLE 1
Example 1:
firstly, a layer of aluminum-zinc alloy is vapor-plated on a PP basal membrane, Zn/Al is 95/5, the impedance of a thickening surface is controlled to be about 3 omega, and the impedance of a working surface is controlled to be about 10 omega; then a layer of epoxy modified silicone oil D is evaporated on the metal evaporation surface, the modified silicone oil is volatile component fractionated at 140 ℃, and the Si content is controlled at 0.06 mug/cm by controlling the temperature of an oil box2And on the left and right, applying oxygen plasma post-treatment on the evaporated oil layer by using a rod type plasma treatment electrode, wherein the power is 3.5kW, and the film traveling speed is 600-.
Winding and cutting the post-treated metallized film to prepare a film disc with the width of 14mm, and mounting the film disc on a winding machine for winding for about 330 circles to obtain a cylinderA capacitor core having an inner diameter of 3mm and an outer diameter of 11mm, and a pressure of 25kg/cm at 105 deg.C2And then, hot-pressing the section of the cylindrical capacitor core into an oval shape for 300s, wrapping a layer of paper on the outer ring of the oval core, spraying gold and welding wires on two end parts, removing the wrapping paper, putting the core into a polybutylene terephthalate rubber shell, pouring a small amount of epoxy resin (non-moisture-heat-resistant type encapsulation adhesive), putting the core into an oven for curing, filling the residual space in the rubber shell with the epoxy resin, and putting the rubber shell into the oven for curing to obtain the 0.47 mu F capacitor.
GPC analysis was performed on the raw material silicone oil to measure the number average molecular weight (g/mol); XPS analysis, flight time secondary ion mass spectrum surface analysis and X-ray fluorescence spectrum analysis are carried out on the surface of the protective layer, and the relative atomic percentage content of oxygen element,76SiO3 -Number of radicals and75SiO2CH3 -the ratio of the number of radicals (TOF-SMIS spectra) and the areal density of the silicon element; analyzing the compression strength of the cylindrical capacitor core; the capacitor was placed at 310VAC, 85 ℃ and 85% RH for 1500hr, and the rate of change in capacity (%) was measured.
Example 2:
example 2 in addition to example 1, the Si content of the surface of the protective layer was adjusted to 0.03. mu.g/cm by adjusting the deposition temperature2And preparing a metallized film. XPS analysis, flight time secondary ion mass spectrum surface analysis and X-ray fluorescence spectrum analysis are carried out on the surface of the protective layer, and the relative atomic percentage content of oxygen element,76SiO3 -Number of radicals and75SiO2CH3 -the ratio of the number of radicals (TOF-SMIS spectra) and the areal density of the silicon element; analyzing the compression strength of the cylindrical capacitor core; the capacitor was placed at 310VAC, 85 ℃ and 85% RH for 1500hr, and the rate of change in capacity (%) was measured.
Example 3:
example 3 in addition to example 1, the Si content of the surface of the protective layer was adjusted to 0.14. mu.g/cm by adjusting the deposition temperature2And preparing a metallized film. XPS analysis and flying of the surface of the protective layerPerforming line time secondary ion mass spectrum surface analysis and X-ray fluorescence spectrum analysis, and measuring the relative atomic percentage content of oxygen element,76SiO3 -Number of radicals and75SiO2CH3 -the ratio of the number of radicals (TOF-SMIS spectra) and the areal density of the silicon element; analyzing the compression strength of the cylindrical capacitor core; the capacitor was placed at 310VAC, 85 ℃ and 85% RH for 1500hr, and the rate of change in capacity (%) was measured.
Example 4:
example 4 a metallized film was prepared by changing the protective layer component to a silanol-modified polysiloxane in addition to example 1. XPS analysis, flight time secondary ion mass spectrum surface analysis and X-ray fluorescence spectrum analysis are carried out on the surface of the protective layer, and the relative atomic percentage content of oxygen element,76SiO3 -Number of radicals and75SiO2CH3 -the ratio of the number of radicals (TOF-SMIS spectra) and the areal density of the silicon element; analyzing the compression strength of the cylindrical capacitor core; the capacitor was placed at 310VAC, 85 ℃ and 85% RH for 1500hr, and the rate of change in capacity (%) was measured.
Example 5:
example 5 in addition to example 4, the Si content of the surface of the protective layer was adjusted to 0.03. mu.g/cm by adjusting the deposition temperature2And preparing a metallized film. XPS analysis, flight time secondary ion mass spectrum surface analysis and X-ray fluorescence spectrum analysis are carried out on the surface of the protective layer, and the relative atomic percentage content of oxygen element,76SiO3 -Number of radicals and75SiO2CH3 -the ratio of the number of radicals (TOF-SMIS spectra) and the areal density of the silicon element; analyzing the compression strength of the cylindrical capacitor core; the capacitor was placed at 310VAC, 85 ℃ and 85% RH for 1500hr, and the rate of change in capacity (%) was measured.
Example 6:
example 6 in addition to example 1, the protective layer component was changed to polydimethylsiloxane, the plasma treatment power was increased to 5.5kW, and a metallized film was prepared. XPS analysis, flight time secondary ion mass spectrum surface analysis and X-ray fluorescence spectrum analysis are carried out on the surface of the protective layer, and the relative atomic percentage content of oxygen element,76SiO3 -Number of radicals and75SiO2CH3 -the ratio of the number of radicals (TOF-SMIS spectra) and the areal density of the silicon element; analyzing the compression strength of the cylindrical capacitor core; the capacitor was placed at 310VAC, 85 ℃ and 85% RH for 1500hr, and the rate of change in capacity (%) was measured.
Example 7:
example 7 in addition to example 6, the Si content of the surface of the protective layer was adjusted to 0.03. mu.g/cm by adjusting the deposition temperature2And increasing the plasma treatment power to 5.5kW, and preparing the metallized film. XPS analysis, flight time secondary ion mass spectrum surface analysis and X-ray fluorescence spectrum analysis are carried out on the surface of the protective layer, and the relative atomic percentage content of oxygen element,76SiO3 -Number of radicals and75SiO2CH3 -the ratio of the number of radicals (TOF-SMIS spectra) and the areal density of the silicon element; analyzing the compression strength of the cylindrical capacitor core; the capacitor was placed at 310VAC, 85 ℃ and 85% RH for 1500hr, and the rate of change in capacity (%) was measured.
Example 8:
example 8 a metallized film was prepared by providing protective layers on both the front and back surfaces of the metallized film in addition to example 1. XPS analysis, flight time secondary ion mass spectrum surface analysis and X-ray fluorescence spectrum analysis are carried out on the surface of the protective layer, and the relative atomic percentage content of oxygen element,76SiO3 -Number of radicals and75SiO2CH3 -the ratio of the number of radicals (TOF-SMIS spectra) and the areal density of the silicon element; analyzing the compression strength of the cylindrical capacitor core; the capacitor was placed at 310VAC, 85 ℃ and 85% RH for 1500hr, and the rate of change in capacity (%) was measured.
Example 9:
example 9 the surface of the metallized film was treated in addition to example 2And arranging protective layers on the front surface and the back surface, and preparing the metallized film. XPS analysis, flight time secondary ion mass spectrum surface analysis and X-ray fluorescence spectrum analysis are carried out on the surface of the protective layer, and the relative atomic percentage content of oxygen element,76SiO3 -Number of radicals and75SiO2CH3 -the ratio of the number of radicals (TOF-SMIS spectra) and the areal density of the silicon element; analyzing the compression strength of the cylindrical capacitor core; the capacitor was placed at 310VAC, 85 ℃ and 85% RH for 1500hr, and the rate of change in capacity (%) was measured.
Example 10:
example 10 a metallized film was prepared by providing protective layers on both the front and back surfaces of the metallized film based on example 4. XPS analysis, flight time secondary ion mass spectrum surface analysis and X-ray fluorescence spectrum analysis are carried out on the surface of the protective layer, and the relative atomic percentage content of oxygen element,76SiO3 -Number of radicals and75SiO2CH3 -the ratio of the number of radicals (TOF-SMIS spectra) and the areal density of the silicon element; analyzing the compression strength of the cylindrical capacitor core; the capacitor was placed at 310VAC, 85 ℃ and 85% RH for 1500hr, and the rate of change in capacity (%) was measured.
Example 11:
example 11 a metallized film was prepared by providing protective layers on both the front and back surfaces of a metallized film based on example 5. XPS analysis, flight time secondary ion mass spectrum surface analysis and X-ray fluorescence spectrum analysis are carried out on the surface of the protective layer, and the relative atomic percentage content of oxygen element,76SiO3 -Number of radicals and75SiO2CH3 -the ratio of the number of radicals (TOF-SMIS spectra) and the areal density of the silicon element; analyzing the compression strength of the cylindrical capacitor core; the capacitor was placed at 310VAC, 85 ℃ and 85% RH for 1500hr, and the rate of change in capacity (%) was measured.
Example 12:
example 12 the surface of the metallized film was coated with a metal oxide filmAnd (4) arranging protective layers on the back surfaces of the two layers to prepare the metallized film. XPS analysis, flight time secondary ion mass spectrum surface analysis and X-ray fluorescence spectrum analysis are carried out on the surface of the protective layer, and the relative atomic percentage content of oxygen element,76SiO3 -Number of radicals and75SiO2CH3 -the ratio of the number of radicals (TOF-SMIS spectra) and the areal density of the silicon element; analyzing the compression strength of the cylindrical capacitor core; the capacitor was placed at 310VAC, 85 ℃ and 85% RH for 1500hr, and the rate of change in capacity (%) was measured.
Example 13:
example 13 a metallized film was prepared by providing protective layers on both the front and back surfaces of a metallized film based on example 7. XPS analysis, flight time secondary ion mass spectrum surface analysis and X-ray fluorescence spectrum analysis are carried out on the surface of the protective layer, and the relative atomic percentage content of oxygen element,76SiO3 -Number of radicals and75SiO2CH3 -the ratio of the number of radicals (TOF-SMIS spectra) and the areal density of the silicon element; analyzing the compression strength of the cylindrical capacitor core; the capacitor was placed at 310VAC, 85 ℃ and 85% RH for 1500hr, and the rate of change in capacity (%) was measured.
The following comparative examples were prepared by the same procedure as in the preparation of the metallized film without using the preparation conditions of the present invention, and data were collected.
Comparative example 1
Comparative example 1 a metallized film was prepared by changing the protective layer component to a high molecular weight epoxy-modified polysiloxane in addition to example 1. XPS analysis, flight time secondary ion mass spectrum surface analysis and X-ray fluorescence spectrum analysis are carried out on the surface of the protective layer, and the relative atomic percentage content of oxygen element,76SiO3 -Number of radicals and75SiO2CH3 -the ratio of the number of radicals (TOF-SMIS spectra) and the areal density of the silicon element; analyzing the compression strength of the cylindrical capacitor core; the capacitor was placed at 310VAC, 85 ℃ and 85% RH for 1500hr, and the rate of change in capacity (%) was measured.
Comparative example 2
Comparative example 2 in addition to comparative example 1, the Si content of the surface of the protective layer was adjusted to 0.03. mu.g/cm by adjusting the deposition temperature2And preparing a metallized film. XPS analysis, flight time secondary ion mass spectrum surface analysis and X-ray fluorescence spectrum analysis are carried out on the surface of the protective layer, and the relative atomic percentage content of oxygen element,76SiO3 -Number of radicals and75SiO2CH3 -the ratio of the number of radicals (TOF-SMIS spectra) and the areal density of the silicon element; analyzing the compression strength of the cylindrical capacitor core; the capacitor was placed at 310VAC, 85 ℃ and 85% RH for 1500hr, and the rate of change in capacity (%) was measured.
Comparative example 3
Comparative example 3 a metallized film was prepared by changing the protective layer component to methyl phenyl silicone oil in addition to example 1. XPS analysis, flight time secondary ion mass spectrum surface analysis and X-ray fluorescence spectrum analysis are carried out on the surface of the protective layer, and the relative atomic percentage content of oxygen element,76SiO3 -Number of radicals and75SiO2CH3 -the ratio of the number of radicals (TOF-SMIS spectra) and the areal density of the silicon element; analyzing the compression strength of the cylindrical capacitor core; the capacitor was placed at 310VAC, 85 ℃ and 85% RH for 1500hr, and the rate of change in capacity (%) was measured.
Comparative example 4
Comparative example 4 in addition to example 1, the protective layer was changed to a high molecular weight silanol-modified polysiloxane as a component, and the Si content on the surface of the protective layer was 0.04. mu.g/cm2And preparing a metallized film. XPS analysis, flight time secondary ion mass spectrum surface analysis and X-ray fluorescence spectrum analysis are carried out on the surface of the protective layer, and the relative atomic percentage content of oxygen element,76SiO3 -Number of radicals and75SiO2CH3 -the ratio of the number of radicals (TOF-SMIS spectra) and the areal density of the silicon element; analyzing the compression strength of the cylindrical capacitor core; the capacitor is placed at 310VAC, 85 ℃ and 85 percentThe test was carried out for 1500hr under RH conditions, and the rate of change in capacity (%) was measured.
Comparative example 5
Comparative example 5 in addition to comparative example 4, the Si content of the surface of the protective layer was adjusted to 0.10. mu.g/cm by adjusting the deposition temperature2And preparing a metallized film. XPS analysis, flight time secondary ion mass spectrum surface analysis and X-ray fluorescence spectrum analysis are carried out on the surface of the protective layer, and the relative atomic percentage content of oxygen element,76SiO3 -Number of radicals and75SiO2CH3 -the ratio of the number of radicals (TOF-SMIS spectra) and the areal density of the silicon element; analyzing the compression strength of the cylindrical capacitor core; the capacitor was placed at 310VAC, 85 ℃ and 85% RH for 1500hr, and the rate of change in capacity (%) was measured.
Comparative example 6
Comparative example 6 on the basis of example 6, the metallized film was prepared by reducing the plasma treatment power to 3.5 kW. XPS analysis, flight time secondary ion mass spectrum surface analysis and X-ray fluorescence spectrum analysis are carried out on the surface of the protective layer, and the relative atomic percentage content of oxygen element,76SiO3 -Number of radicals and75SiO2CH3 -the ratio of the number of radicals (TOF-SMIS spectra) and the areal density of the silicon element; analyzing the compression strength of the cylindrical capacitor core; the capacitor was placed at 310VAC, 85 ℃ and 85% RH for 1500hr, and the rate of change in capacity (%) was measured.
Comparative example 7
Comparative example 7 on the basis of example 1, the plasma treatment process was removed, and a metallized film was prepared. XPS analysis, flight time secondary ion mass spectrum surface analysis and X-ray fluorescence spectrum analysis are carried out on the surface of the protective layer, and the relative atomic percentage content of oxygen element,76SiO3 -Number of radicals and75SiO2CH3 -the ratio of the number of radicals (TOF-SMIS spectra) and the areal density of the silicon element; analyzing the compression strength of the cylindrical capacitor core; placing the capacitor under 310VAC, 85 deg.C, 85% RH for 1500hr, and measuring capacityRate of change (%).
Comparative example 8
Comparative example 8 instead of epoxy-modified polysiloxane (DY-E701 Shandong Dai chemical Co., Ltd.), plasma treatment was carried out at 5.5kW and the Si content of the surface of the protective layer was adjusted to 0.80. mu.g/cm by adjusting the vapor deposition temperature2And preparing a metallized film. XPS analysis, flight time secondary ion mass spectrum surface analysis and X-ray fluorescence spectrum analysis are carried out on the surface of the protective layer, and the relative atomic percentage content of oxygen element,76SiO3 -Number of radicals and75SiO2CH3 -the ratio of the number of radicals (TOF-SMIS spectra) and the areal density of the silicon element; analyzing the compression strength of the cylindrical capacitor core; the capacitor was placed at 310VAC, 85 ℃ and 85% RH for 1500hr, and the rate of change in capacity (%) was measured.
The analytical data for the above examples and comparative examples are shown in tables 2 to 6, respectively:
TABLE 2
TABLE 3
TABLE 4
TABLE 5
TABLE 6
As can be seen from examples 1-7, the metallized film prepared by controlling the areal density of the silicon element has a compressive strength of the cylindrical core of less than 0.25MPa and a capacity change rate of less than 20% in the capacitor at 1500hr of the damp heat test.
As can be seen from examples 6 and 7 and comparative example 6, in the case of the silicone oil having no reactive group, it is necessary to control the plasma treatment power so high that the compressive strength of the cylindrical core becomes less than 0.25MPa, and the capacity change rate of the capacitor at 1500hr in the wet heat test becomes less than 20%.
It can be seen from examples 8-13 that the protective layers were provided on both sides of the metallized film so that the compressive strength of the cylindrical core was less than 0.25MPa, and the rate of change in the capacity of the capacitor in the damp heat test for 1500hr was less than 20%.
Comparative examples 1, 2, 4 and 5 use a high molecular weight silicone oil as a protective layer for the metallized film, and the compressive strength of the cylindrical core was greater than 0.25MPa, at which time the rate of change in capacity of the capacitor in the damp heat test for 1500hr was greater than 20%. The cohesion of the molecular chain of the high molecular weight silicone oil is large, an oil layer is not easy to spread, metal is partially exposed, the surface energy of the protective layer is increased, the interaction between one surface of the protective layer of the metallized film and the back surface of the matched metallized film is enhanced, and the compression strength of the core is improved; meanwhile, the moisture and heat resistance of the metallized film is poor due to poor covering effect of the protective layer.
Comparative example 3 a silicone oil having a molecular weight of less than 600g/mol was used as a protective layer for a metallized film, and the compressive strength of the cylindrical core was greater than 0.25MPa, at which time the rate of change of the capacity of the capacitor in a damp heat test for 1500hr was greater than 20%. The low molecular weight silicone oil film has poor stability, resulting in poor hiding, metal exposure, resulting in increased core compressive strength and poor wet heat resistance of the metallized film.
Comparative example 7 the plasma treatment process was removed from example 1 and the compressive strength of the cylindrical core was greater than 0.25MPa, at which time the rate of change of the capacity of the capacitor was greater than 20% at 1500hr of the damp heat test. The removal of the plasma treatment process weakens the stability of the silicone oil film, resulting in poor coverage, metal exposure, resulting in increased core compressive strength and poor moisture and heat resistance of the metallized film.
Comparative example 8 used a silicone oil containing a large amount of high molecular weight components, for the same reason as in comparative examples 1, 2, 4 and 5, so that the compressive strength of the cylindrical core was more than 0.25MPa, at which time the rate of change in capacity of the capacitor in the wet heat test for 1500hr was more than 20%.
In summary, the above examples and comparative examples show that when the compressive strength of the capacitor core is too high, the protective effect of the reflective protective layer is poor and the moisture and heat resistance is poor.
The embodiments are not limited to the above 13 types, and other combinations according to the claims and the teaching of the present application are included in the scope of protection of the present patent.
Claims (8)
1. A moisture-resistant and heat-resistant metallized film for capacitors, characterized in that:
the compressive strength was measured to be in the range of 0-0.25MPa at 2hr after the metallized film was wound into a capacitor core of 0.47. mu.F.
2. The metallized film of claim 1, wherein: the metallized film comprises an insulating dielectric layer, a metal layer and a protective layer.
3. The metallized film of claim 2, wherein: the insulating medium layer comprises polypropylene; the thickness is less than or equal to 10 mu m.
4. The metallized film of claim 2, wherein: the metal layer includes one or more of aluminum or zinc.
5. The metallized film of claim 2, wherein: the protective layer comprises one or more of silicon, oxygen or carbon elements; the relative atomic percent of the oxygen element is more than 20 percent; said protective layer when analyzed using TOF-SIMS,76SiO3 -number of radicals and75SiO2CH3 -the ratio of the number of the groups is more than or equal to 0.02.
6. The metallized film of claim 2 or 5, wherein: the surface density of silicon element in the protective layer is 0.02-0.25 mu g/cm2In the meantime.
7. A capacitor, characterized by: the capacitor comprising the metallized film of claim 1.
8. The capacitor of claim 7, wherein: the capacitor is tested for 1500hr under the conditions of 310VAC, 85 ℃ and 85% RH, and the capacity change rate is less than or equal to 20%.
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|---|---|---|---|---|
| JP2005159169A (en) * | 2003-11-27 | 2005-06-16 | Kyocera Corp | Thin film capacitor |
| CN204067066U (en) * | 2014-04-18 | 2014-12-31 | 扬州日精电子有限公司 | A kind of metallic film capacitor |
| CN105869890A (en) * | 2016-05-23 | 2016-08-17 | 郑州航空工业管理学院 | Evaporation technology of metallized polypropylene film dielectric capacitor |
| CN206742085U (en) * | 2017-03-16 | 2017-12-12 | 东莞市国灿电子科技有限公司 | It is resistant to the resistance-capacitance depressurization thin film capacitor of hygrothermal environment |
| CN207624554U (en) * | 2017-12-21 | 2018-07-17 | 东丽薄膜加工（中山）有限公司 | Metallized film and capacitor containing the metallized film |
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- 2019-12-20 CN CN201911326802.0A patent/CN113012937A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2005159169A (en) * | 2003-11-27 | 2005-06-16 | Kyocera Corp | Thin film capacitor |
| CN204067066U (en) * | 2014-04-18 | 2014-12-31 | 扬州日精电子有限公司 | A kind of metallic film capacitor |
| CN105869890A (en) * | 2016-05-23 | 2016-08-17 | 郑州航空工业管理学院 | Evaporation technology of metallized polypropylene film dielectric capacitor |
| CN206742085U (en) * | 2017-03-16 | 2017-12-12 | 东莞市国灿电子科技有限公司 | It is resistant to the resistance-capacitance depressurization thin film capacitor of hygrothermal environment |
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