CN1152035A - Method for making zinc metallized film for film capacitors exhibiting improved adhesion and thereby having excellent anti-oxidation characteristics - Google Patents
Method for making zinc metallized film for film capacitors exhibiting improved adhesion and thereby having excellent anti-oxidation characteristics Download PDFInfo
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- CN1152035A CN1152035A CN 95120817 CN95120817A CN1152035A CN 1152035 A CN1152035 A CN 1152035A CN 95120817 CN95120817 CN 95120817 CN 95120817 A CN95120817 A CN 95120817A CN 1152035 A CN1152035 A CN 1152035A
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Abstract
A method for making a zinc metallized film for a film capacitor, being capable of protecting the zinc film from moisture and thereby preventing it from oxidizing. The method includes treating a surface of a polymer film with a metal having a high bonding force by use of glow discharge or sputtering process or evaporating a seed layer of aluminum, tin or chromium over the polymer film surface by use of a thermal evaporation process. The seed layer as an intermediate layer between the polymer film and zinc film provides a high bonding force between the polymer film and zinc film. By this high bonding force, the zinc metallized film exhibits an improved anti-oxidation property, a superior electrical characteristic and an lengthened use life.
Description
The present invention relates to a method for manufacturing a zinc-plated film which can improve the adhesion between zinc and a polymer film in a film capacitor and has excellent oxidation resistance.
Since most of electric and electronic devices have a compact and fine structure, the use of thin film capacitors using a metal plating film has recently been greatly increased. In particular, such a cover film capacitor exhibits very high reliability because it has excellent high-frequency characteristics and self-repairing ability to repair damage to the electrode surface film or defects that may be caused by self-contamination. They also have many advantages over conventional electrolytic capacitors in terms of manufacturing and cost. For these reasons, the use of thin film capacitors using metal deposition (metallization) films has increased.
The metallized films of capacitors are classified into: pure aluminum (Al) deposition type, aluminum-zinc (Al-Zn) deposition type, and zinc (Zn) deposition type.
The metal-plated capacitor using a zinc-plated film (hereinafter referred to as MF-Zn capacitor) has more excellent electrical characteristics than those using a thin film deposited of aluminum (hereinafter referred to as MF-Al capacitor). However, MF-Zn capacitors have limited applications due to their more or less poor moisture resistance and self-healing properties.
On the other hand, since aluminum has higher conductivity than a zinc-plated film, the thickness of an aluminum deposited film is small, thereby exhibiting excellent self-healing properties. In particular, the film has very good oxidation resistance because of the presence of a layer of alumina on the surface of the aluminized film, which contributes to the chemical stability of the filmProperties and therefore storage advantages. However, such aluminum-plated films also have disadvantages: over time, its capacitance decreases. It is disadvantageous from the viewpoint of cost because it requires 1.33X 10-2To 1.33X 10-3Handkerchief (10)-4To 10-5Torr) and an evaporation temperature as high as 1,500 c to 1,800 c as its deposition conditions, the deposited film is too thin (100 to 250 Å) to make contact with lead wires, and it is difficult for the deposited film to have a thick edge due to such a small thickness.
In contrast, the capacity of the zinc-plated film capacitor increases little or no over time. Deposition at low temperature of about 600 ℃ of 1.33 to 1.33X 10-1Handkerchief (10)-2To 10-3Torr) is achieved. Since the zinc plating film is thicker than the aluminum plating film, zinc oxide is formed on the surface of the film in contact with the lead wire, thereby reducing the contact resistance between the lead wire and the electrode. Such films also have cost advantages over aluminized films. Because of these advantages, galvanized films have been widely used.
However, zinc has a high oxidation activity and its adhesion to polymer films made of insulating materials is weak, such as polyethylene terephthalate (PET), oriented polypropylene (OPP), Polyethylene (PE), or Polycarbonate (PC). For the above reasons, the zinc layer exhibits low surface adhesive strength. Therefore, the zinc plating film has a disadvantage that the zinc layer thereof is easily scratched.
Typically, the oxidation of the zinc plated film is accomplished in a continuous manner in two steps as moisture and oxygen penetrate the film. Oxidation continues as long as moisture is present in the film.
The oxidation of the first step is achieved in the following way: and the second oxidation is carried out in the following manner: . Moisture permeation occurs through A, B, C three pathways as shown in figure 2. Through the route A, moisture in the air is combined with the zinc plating film; by way B, zinc-plated films and polymer films of capacitorsThe contained water is combined; by way of route C, the zinc-coated film also combines with moisture that permeates through the polymer film. The degree of binding of moisture to the zinc-plated film is the greatest in pathway A and the smallest in pathway C.
The galvanized film has the following properties: namely, the property of rapid oxidation in air and the fact that oxidation continues from after film deposition until the beginning of the immersion process in the capacitor manufacturing process, the application thereof is limited despite the excellent electrical properties. Problems also exist when stored for extended periods of time. In order to improve the adhesion properties of the deposited films while still maintaining the advantages of zinc-plated films, British patent No.1,754,064 proposes a method relating to the deposition of metal oxides, for example Al-coating of polymer films2O3And galvanizing is performed on the metal oxide layer, so that the oxidation resistance of the galvanized film is improved. In german patent No.0,083,137, another method is disclosed in which a zinc-based alloy, such as a Zn-Al alloy, is deposited in a monolayer form on a plastic film instead of a multilayer film, thereby improving oxidation resistance. In fact, when a metal, such as Cr, is deposited on the zinc layer, the oxidation resistance is improved. But in this case high temperature and high vacuum are required to deposit Cr. For this reason, this method is still not practical.
Accordingly, it is an object of the present invention to provide a method of manufacturing a zinc metal film for a thin film capacitor, which has excellent oxidation resistance, i.e., a metal film is isolated from moisture by increasing the surface tension of a polymer film through surface treatment of the polymer film on which the zinc metal film is deposited, or the object is achieved by depositing a metal having high binding energy on the zinc film.
In one aspect, the present invention provides a method for manufacturing a zinc-plated film for a thin film capacitor having excellent oxidation resistance, the method comprising the steps of: (a) the surface of the polymer film is treated with a metal having a high binding energy by a vacuum spray method of evaporating a seed layer of aluminum, tin or silver, and a metal layer having a single-layer or multi-layer structure is formed on the surface of the polymer film by thermal evaporation. (b) Depositing zinc or a zinc-aluminum alloy on the film obtained in step (a) to obtain 2 to 10. omega./m2(ohm/square meter) total surface resistance.
In another aspect, the method further comprises: before depositing the zinc or zinc-aluminium alloyDepositing a seed layer of a metal comprising aluminum, silver or titanium having a higher oxidation activity than zinc to give a concentration of 3.5 to 10 Ω/m on the film obtained in step (a)2And depositing aluminum on the seed layer in a continuous process.
In another aspect, the present invention provides a method for manufacturing a zinc-plated film for a thin film capacitor having excellent oxidation resistance, comprising the steps of: in the presence of O2In air, i.e. as O2+ Ar or O2+N2Generating oxygen anions (O-) on the surface of the polymer film by glow discharge in the mixed gas of + Ar; zinc is deposited as an electrode metal on the polymer film without a metal seed layer to obtain 2 to 10 omega/m2Total surface resistance of (a); a protective film for preventing oxidation of zinc is formed on the zinc film by glow discharge or sputtering.
Other uses and aspects of the invention will become apparent from the following description of the embodiments with reference to the accompanying drawings.
Fig. 1 is a diagram illustrating a state of zinc deposition in the present invention.
FIG. 2 is a graphical representation of the different pathways for moisture to pass through the metallized film.
FIG. 3 is a sectional view of a zinc-plated film produced by the method of the present invention.
FIG. 4 is a diagram of a vacuum heating furnace used for producing a zinc-plated film in the present invention.
FIG. 5 is a graph comparing the oxidation resistance of the zinc-plated film of the present invention with that of the conventional film.
When a metal-plated film is formed on a polymer film by a thermal resistance evaporation method, a porous structure is generated, and when the film is exposed to air, moisture in the air easily permeates into the film, in which case the film reduces adhesion, possibly resulting in sudden oxidation of the film. In order to improve the oxidation resistance of the metal film to prevent such oxidation, a seed layer composed of a metal or an oxide having high adhesion to the polymer film is plated on the polymer film before zinc is deposited on the polymer film. The adhesion and oxidation of the metal film may depend on the kind of the seed layer. When the bonding force between the seed layer and the polymer film is low, the seed layer is not uniformly deposited due to the surface tension energy of the seed layer, and a block is formed. In this case, the adhesion of the zinc plating film covering the seed layerAnd decreases. This tendency is particularly pronounced when polypropylene or polycarbonate films are used. The adhesion of the deposited layer to the polymer film has a great influence on the oxidation resistance and oxidation mechanism of the deposited layer. In particular, biaxially stretched polypropylene films (OPP films) which are widely used as polymer films for capacitors are, due to their relatively low adhesion, e.g. 3.2X 103Newton per square meter (32 dyne/cm)2) (while the adhesion of the Polyester (PET) film was 4.8X 103Newton per square meter (48 dyne/cm)2) Exhibit reduced adhesion to the zinc layer, and films such as these therefore need to be subjected to special treatment, for example corona discharge treatment, to increase their adhesion tension to not less than 3.8-4.2X 103Newton/square meter (38-42 dyne/cm)2) The level of (c).
According to the present invention, a method for producing a zinc-plated film comprises: aluminum having excellent oxidation resistance is plated as a seed layer on a capacitor polymer film having a thickness of 1.5 to 20 μm so that the surface resistance of the aluminum layer is 100 to 300. omega./m2Or by glow discharge or vacuum sprayingTreating the polymer film and then plating zinc on the film obtained by the above method to give a film having 3-4.0. omega./m2The total surface resistance of (a). The formation of the zinc plating film is carried out in a vacuum heating furnace in a continuous operation. As shown in fig. 4, the vacuum heating furnace includes: an upper chamber 9 and a lower chamber 10, the upper chamber 9 being maintained at 2.66 Pa (2X 10)-2Torr) and the lower chamber 10 is maintained at 2.66 x 10-2Handkerchief (2X 10)-4Torr). In particular, aluminizing is performed in an aluminizing zone 5 in a vacuum heating furnace, while galvanizing is performed in a galvanizing zone 6 in the vacuum heating furnace. On the other hand, the processing of the polymer film is performed in the plasma region 4 in the vacuum chamber.
In the vacuum chamber shown in fig. 4, the capacitor polymer film is continuously fed from the base film roll to the cooling drum 1 at a speed of not less than 6 m/sec, after which the polymer film is fed along the cooling drum 1 while the polymer film is in contact with the cooling drum 1, and then wound on a roll 3 for winding the film. As the polymer film is fed along the cooling drum 1 through the galvanizing station 6, hot zinc vapour at 600 to 800 c in the station 6 sticks to the polymer film. Then, the zinc-plated film is rapidly cooled by a cooling drum 1 maintained at a temperature of-25 to-10 ℃. A metal seed layer is formed on the polymer film or the polymer film metal electrode fed at a high speed. The metal seed layer is formed by generating a metal plasma having a high oxidation rate in a plasma region 4, the plasma region 4 being a vacuum vessel of a batch type, the plasma being generated by glow discharge or vacuum sputtering using a Direct Current (DC) or Radio Frequency (RF) power supply when an inert gas and oxygen or nitrogen are supplied to the plasma region 4 in a certain ratio. An alternative method of forming the metal seed layer is by a thermal evaporation method in the aluminized region 5. An oxidation resistant film having high bonding energy can be formed on the polymer film or the metal electrode through the metal seed layer.
Because the zinc-plated film has a micro-polycrystal structure, there is an atomic bonding force between the zinc-plated film and the polymer film. However, this bonding force is not sufficient because energy consumption is caused by conversion of thermal energy into adsorption energy. Polyethylene terephthalate for forming insulating polymer filmThe alcohol ester (PET) and oriented polypropylene (OPP) have the following molecular structures, respectively:
when a metal having high oxidation is deposited on PET as a seed layer, the PET shows strong adhesion with the metal seed layer due to oxygen atoms in the molecular structure of the PET. I.e. the bonding force is generated between the oxygen atoms and the metal seed layer atoms. Because of the strong metallic bond between the metallic seed layer and the zinc, a uniform and dense zinc film is produced when the zinc is deposited on the seed layer. Thereby improving oxidation resistance.
However, such properties are not observed in polymers having no oxygen groups, such as polypropylene, and accordingly, it is necessary to treat such polymers by vacuum sputtering or glow discharge in a plasma atmosphere containing a small amount of oxygen. When the polymer film is subjected to such surface treatment, molecules having oxygen-containing groups are present on the surface thereof. Then, a layer of metal with high oxidation activity is formed on the polymer film subjected to surface treatment by vacuum sputtering or ion plating. In this case, a uniform and dense zinc layer is deposited on the polymer film by the above-described process similar to the process of treating PET, and thus, it is possible to obtain a capacitor having high bonding force and excellent oxidation resistance. This surface treatment and the coating of the highly oxidizing metal are achieved by a continuous process. Accordingly, the present invention is directed to prevent oxidation of a metal electrode by forming an oxide or nitride layer using a plasma oxidation or nitridation process using a Direct Current (DC) power source or depositing a metal having high oxidation properties by a vacuum sputtering method.
The process of the invention is suitably carried out at 10-2To 10-6One or both surfaces of the metal electrode or the polymer film are treated under a vacuum of torr/cc to increase the bonding force between the film and the electrode to improve the adhesion, which improves the oxidation resistance.
According to the method used in the present invention, an oxide or nitride film is coated on a thin film metal electrode, the film being formed on one side or both sides of the surface of the polymer film in a continuous deposition manner and having a thickness of 100 to 1,500 Å, in a plasma atmosphere formed by an electric field of DC or RF voltage of 400 to 1,000V, the plasma atmosphere being generated by a mixture of an inert gas and oxygen or nitrogen through a gas control valve (MFC: mass flow controller). in the plasma atmosphere, oxygen or nitrogen reacts with a target material, that is, a material on which an oxide or nitride is deposited, to form an oxide or nitride coating having a thickness of 50 to 200 Å on the metal electrode.
In order to prevent the zinc film from being oxidized by moisture or oxygen, a layer composed of a material having a high oxidation activity, such as chromium, titanium, niobium, or aluminum, is formed on the zinc film, thereby forming a dense oxide film. Due to the oxide film, the zinc film has superior oxidation resistance.
According to a first embodiment of the present invention, an OPP film is applied to a capacitor by increasing the surface tension of a polymer film to increase the bonding force between the polymer film and a metal deposition film, the metal plating film and the polymer film are firmly bonded together due to the increase of the bonding force, and the polymer film is treated by plasma generated by a glow discharge process in a vacuum deposition apparatus in order to increase the surface tension energy, a seed layer having a thickness of from 20 to several tens of thousands of angstroms (Å) is formed on the polymer film by the plasma treatment, thereby activating the polymer film (Zn-O-C, Zn-N-C, Al-O-C or Al-N-C) as follows:
then, a metal such as Cr, Ti, Al, Ag or an aluminum alloy in which both metals have high oxidation activity is uniformly deposited on the seed layer as a film having a thickness of from 5 to more than several hundred angstroms (a). Zn or a Zn-Al alloy is deposited on the resulting film, thereby obtaining a multilayer film structure.
According to a second embodiment of the invention, Ar + O is generated by a DC or RF power source2Or Ar + N2In the atmosphere, a seed layer is formed on the polymer film by using Cr, Ti, Al, Ag or Zr as a target material by a vacuum sputtering method. At the same time, oxygen and nitrogen groups are generated on the surface of the polymer film. Then, Zn or Zn-Al alloy is used as the phase of the first embodimentThe same method is deposited on the resulting film, according to the practice of this embodiment, to improve oxidation resistance and bonding force. Since the dense oxide or nitride layer helps to shield the metal film from exposure toIn addition, the oxide or nitride forms a film with a thickness of 50 to 100 Å on the metal electrode, which also helps to prevent the metal-plated electrode from being oxidized by moisture in the air.
According to a third embodiment of the present invention, a metal having higher oxidation activity than zinc is deposited on a polymer film as an intermediate layer having a thickness of 20 to 50 Å by a thermal evaporation method, and then, a zinc film is deposited on the resulting film, the intermediate layer is oxidized before the zinc film because the zinc film is in a reduced potential state, thereby obtaining an oxide film having a dense structure, in the intermediate layer composed of aluminum, the aluminum is in an oxidized potential state and the zinc is in a reduced potential state because the aluminum potential is-1.662 volts and the zinc potential is-0.763 volts, and the aluminum film is oxidized earlier than the zinc film, and further, the primary cell is not formed because the aluminum is oxidized to form aluminum.
Interlayer metal (Al)+3) Through the electrode metal, i.e. zinc (Zn)+2) Migrate to the polymer surface so that it combines with oxygen before the zinc film, thus forming a dense oxide film with a thickness of 20 to 50A. This oxide film helps to protect the zinc film from oxidation by moisture in the air that permeates through the polymer film.
According to the invention, another method suitable for high-voltage capacitors can also be used. The method comprises coating a polymer film with an oxidation resistant film, depositing zinc as an electrode metal on a zinc film, and then depositing a protective metal layer on the zinc film to protect the zinc film from oxidation. According to this method, zinc is deposited on the polymer film to give 4 to 100. omega./m2The surface resistance of (1). Deposition of protective metal on zinc film by continuous operationTo obtain 2 to 10. omega./m2The surface resistance of (1). Thus, a multilayer structure is obtained by means of successive depositions.
According to the above-mentioned method, it is possible to obtain a zinc film having superior oxidation resistance and many advantages.
The invention will be more readily understood by reference to the following examples; these examples are intended to illustrate the invention and are not to be construed as limiting the scope of the invention. Example 1:
under a vacuum of 2.66 Pa (2X 10)-2Torr) and vacuum of 2.66 x 10-2Handkerchief (2X 10)-4Torr), aluminum is deposited on a polypropylene film with a thickness of 4-6 μm and treated by corona discharge as a seed layer, and 100-300 Ω/m is obtained by the deposition2The surface resistance of (1). Zinc is deposited on the aluminum film to obtain 3-4 omega/m2Thus obtaining a metallized capacitor film structure.
Then, the capacitor film structure was maintained in a constant temperature and humidity container, the temperature was maintained at 60 ℃ and the relative humidity was maintained at 80% for 2, 8, 12, and 20 hours, and the surface resistance of the film structure was measured and the degree of oxidation of the film was measured from the measured surface resistance, and the results are shown in FIG. 5. Example 2:
a capacitor film structure was fabricated in the same manner as in example 1, and then aluminum was deposited on the zinc film of the capacitor film structure to have a thickness of 3. omega./m2The surface resistance of the capacitor film structure thus obtained was measured in the same manner as in example 1, and the results are shown in fig. 5. Example 3:
a6 μm thick polypropylene film without corona treatment was prepared and then evacuated at a top chamber vacuum of 2.66 Pa (2X 10)-2Torr) and bottom end chamber vacuum of 2.66 x 10-2Handkerchief (2X 10)-4Torr), the polypropylene film formed Ar (60%) + O in the upper chamber2(40%) was subjected to glow discharge treatment in an atmosphere with aluminum deposited as a seed layerOn the polypropylene film, zinc was deposited on the aluminum film in a continuous operation to obtain a surface resistance of 3. omega./m2. This gave a metallized capacitor film structure, which was subjected to the same test as in example 1 to measure the degree of oxidation, and the results are shown in FIG. 5. Example 4:
a metallized capacitor film structure was prepared in the same manner as in example 3, except that no seed layer was formed on the polypropylene film. The same test as in example 1 was carried out on this capacitor film structure to measure the degree of oxidation, and the results are shown in fig. 5. Example 5:
in the same way as in example 3, aluminium and zinc were deposited in a continuous operation on the same polypropylene film as in example 3. Then aluminum is deposited on the zinc film by continuous operation to obtain 10 omega/m2So that the total surface resistance is about 2.5. omega./m2. This results in a metallized capacitor film structure. The same test as in example 1 was carried out on this capacitor film structure to measure the degree of oxidation, and the results are shown in fig. 5. Example 6:
aluminum and zinc were deposited in the same continuous operation as in example 3 on the same polypropylene film as in example 3, and then the zinc film was treated by glow discharge in the lower chamber to give a concentration of 4-5.5. omega./m2The total surface resistance of (a). Thus, a metallized capacitor film structure is obtained. The same test as in example 1 was carried out on this capacitor film structure to measure the degree of oxidation, and the results are shown in fig. 5. Comparative example:
zinc is deposited on a polypropylene film or polyethylene terephthalate film to obtain a film of 3.5 omega/m2The total surface resistance of (a). This gave a deposited capacitor film structure, and the same test as in example 1 was carried out to measure the degree of oxidation of the capacitor film structure, with the results shown in FIG. 5.
Referring to fig. 5, it can be found that the capacitor film structures of examples 1 to 6 have higher oxidation resistance than the capacitor film structure in the comparative example. It can also be seen that the capacitor film structures of examples 1 to 6 are also improved in electrical properties (improved reliability in long-term use and reduced capacitance attenuation).
Although the preferred embodiments of the present invention have been disclosed for illustrative purposes, those skilled in the art will appreciate that various modifications, additions and substitutions are possible, without departing from the scope and spirit of the invention as disclosed in the accompanying claims.
Claims (3)
1. A method for plating a zinc metal film having excellent oxidation resistance on a film capacitor, comprising the steps of:
(a) the surface of the polymer film is treated with a metal having high binding energy using a vacuum sputtering method or an evaporation method, and aluminum, tin or silver is covered on the surface of the polymer film as a seed layer having a single-layer or multi-layer structure using a thermal evaporation method.
(b) Depositing a layer of zinc or zinc-aluminium alloy on the structure obtained in step (a) to obtain 2 to 10 Ω/m2The total surface resistance of (a).
2. The method according to claim 1, further comprising the steps of: depositing a seed layer of a metal having a higher oxidation activity than zinc, such as aluminum, silver, titanium, onto the structure obtained in step (a) before depositing zinc or a zinc-aluminum alloy, to obtain a concentration of 3.5 to 10 Ω/m2Then depositing aluminum on the seed layer in a continuous operation.
3. A method for plating a zinc metal film having an excellent oxidation resistance on a film capacitor, comprising the steps of:
using glow discharge at O2、O2+N2In + Ar atmosphere, negative oxygen ion groups are generated on the surface of a polymer film.
Depositing zinc on the surface of the polymer film without the metal seed layer as electrode metal to obtain 2-10 omega/m2The total surface resistance of (a).
An oxide film for protecting zinc is formed on the zinc film by glow discharge or vacuum sputtering.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 95120817 CN1195885C (en) | 1995-12-13 | 1995-12-13 | Method for making zinc metallized film for film capacitors exhibiting improved adhesion and thereby having excellent anti-oxidation characteristics |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 95120817 CN1195885C (en) | 1995-12-13 | 1995-12-13 | Method for making zinc metallized film for film capacitors exhibiting improved adhesion and thereby having excellent anti-oxidation characteristics |
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| CN1152035A true CN1152035A (en) | 1997-06-18 |
| CN1195885C CN1195885C (en) | 2005-04-06 |
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| CN 95120817 Expired - Fee Related CN1195885C (en) | 1995-12-13 | 1995-12-13 | Method for making zinc metallized film for film capacitors exhibiting improved adhesion and thereby having excellent anti-oxidation characteristics |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106298242A (en) * | 2016-09-30 | 2017-01-04 | 铜陵市超越电子有限公司 | A kind of metallized film production technology |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN106298242A (en) * | 2016-09-30 | 2017-01-04 | 铜陵市超越电子有限公司 | A kind of metallized film production technology |
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