JPH08209346A - Conductive cooling roll and production of vapor deposited film - Google Patents

Abstract

PURPOSE: To improve the adhesion property of a plastic film and a material for vapor deposition by specifying the dielectric breakdown voltage of an electrical insulating layer formed on the outer peripheral surface of a cooling roll to a specific value or above and specifying the heat pass rate of this conductive cooling roll to a specific value. CONSTITUTION: A long-sized plastic film is continuously unwound and while this film is made to travel in a manner as to hold the conductive cooling roll 1 thereon, the film is made into a vapor deposited film by an ion plating method. The outer peripheral surface of the cooling roll 1 is provided with the electrical insulating layer 2 in tight contact therewith. The electrical insulating layer 2 is provided thereon with a conductive layer 3 in tight contact therewith, by which the conductive cooling roll is formed. The electrical insulating layer 2 is a ceramic coating layer having a thickness of 0.1 to 5mm and the dielectric breakdown voltage thereof is specified to >=0.2kV. The heat pass rate of the conductive cooling roll 1 is specified to 10 to 100000W/m<2> .K. The sufficient cooling of the plastic film is possible and the accelerated irradiation of the film with the ionized material for vapor deposition without allowing the impressed voltage to escape is possible.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a vapor-deposited substance strongly adhered to an entire long film by applying a voltage to a conductive chill roll in an ion plating device, resulting in uniform quality and excellent oxygen barrier properties. And a method for producing a transparent vapor-deposited film having a water vapor barrier property.

[0002]

2. Description of the Related Art Generally, a plastic film having a low water vapor or oxygen permeability is used as a packaging material for foods, pharmaceuticals, chemicals, etc. in order to prevent the deterioration of the contents. Above all, as a transparent plastic film having a high gas barrier property, a film in which a silicon oxide is vapor-deposited on a base film such as a biaxially stretched polyester film has been proposed (see Japanese Patent Publication No. 53-12953). .

However, in the case of producing such a vapor-deposited film, even if the silicon oxide is vapor-deposited directly on the substrate film, the gas-barrier property of the obtained vapor-deposited film is insufficient, and There is a problem that the adhesion to the vapor deposition film is weak. Vacuum deposition, sputtering, and ion plating have been proposed as methods for producing a vapor-deposited film. Among them, as a method capable of forming a thin film having excellent adhesion strength between a vapor-deposited substance and a plastic film, ion plating is used. A method for producing a vapor-deposited film by the coating method has been proposed (JP-A-5-9709).
JP-A-5-65644 and JP-A-5-29
5528, etc.).

The ion plating method is a technique in which a part of vaporized particles is activated and vaporized as ionized or excited particles by using gas plasma in principle.
Since the operation is performed in plasma, the first condition is to obtain stable plasma, and low temperature plasma by weakly ionized plasma in a low gas pressure region is often used. As a method for generating plasma, a method utilizing collision of thermoelectrons,
There are a type using a high frequency wave and a microwave electric field, a type using a plasma arc, and the like, but a high frequency type that can always stably maintain a low-pressure gas discharge is generally adopted.

In the high frequency system, an oscillating electric field of 13.56 MHz which is a permissible band by the radio wave method is usually used to utilize gas multiplication action to ionize gas molecules. The excited or ionized gas molecules react with the vaporized particles, and the vaporized particles are also excited or ionized. Since these particles are activated, a dense and hard film is formed as compared with the conventional vacuum deposition method in which most of the particles are neutral particles. Further, since the ions generated by applying the electric field can be accelerated, the adhesion of the vaporized particles to the base material is improved.

Also in this method, since the vapor deposition material is put into the crucible and heated, the plastic film is cooled and ionized in order to prevent damage to the plastic film due to heat from the crucible and condensation heat of the vapor deposition material. Need to accelerate. However, usually
Since the chill roll is made of metal, the voltage escapes even if a voltage is applied to accelerate the ionized vapor deposition material.
Therefore, even if the bearing of the cooling roll is insulated, it is difficult to completely insulate it because water or the like is passed inside to cool the bearing, and the voltage escapes even when a voltage is applied as in the former case. There is a problem that the adhesion is weak, the vapor-deposited film obtained is incomplete, and a uniform and stable thin film cannot be formed continuously.

[0007]

SUMMARY OF THE INVENTION The present invention has been made in view of the above circumstances, and is an electrically conductive cooling roll having a function of cooling a plastic film in an ion plating device and a function of holding a potential on the roll surface. Another object of the present invention is to provide a method for producing a vapor-deposited film in which a thin film of a metal or a metal compound is formed on a plastic film continuously and stably by the ion plating method with strong adhesion.

[0008]

In order to solve the above-mentioned problems, in the invention described in claim 1 of the present invention, the electric insulating layer 2 is provided in close contact with the outer peripheral surface of the cooling roll 1, and the electric insulating layer is provided. In a conductive cooling roll in which the conductive layer 3 is closely provided on the above, the dielectric breakdown voltage of the electric insulating layer 2 is 0.2 kV or more, and the heat transmission rate of the conductive cooling roll is 10 to 100.
The present invention relates to a conductive cooling roll in an ion plating device, which is characterized in that it has a power of 000 W / m ² · K.

Further, in the invention according to claim 5 of the present invention, in the ion plating method, a metal or metal compound thin film is formed on at least one surface of a long transparent plastic film and vapor deposition is performed. In manufacturing the film, the dielectric breakdown voltage of the electric insulating layer 2 was set to 0.
2 kV or more, and the heat transmission rate of the conductive cooling roll is 10
A means of cooling the plastic film by applying a voltage to the conductive layer 3 of the conductive cooling roll of -100,000 W / m ² · K to hold it at a negative potential and passing a cooling medium through the cooling roll 1 is used. is there.

Hereinafter, the present invention will be described in detail. The present invention will be described in detail with reference to the drawings, but the present invention is not limited to the following examples unless it exceeds the gist. FIG. 1 is a schematic sectional view of an ion plating apparatus for producing a vapor-deposited film according to the present invention, and FIGS. 2 to 5 are perspective views showing an example of a conductive cooling roll according to the present invention.

In the drawings, 1 is a cooling roll, 2 is an electrically insulating layer, 3 is a conductive layer, 4 is a power supply tool, 5 is an introduction terminal, 6 is a bearing, 10 is a conductive cooling roll, 20 is a plastic film, and 21 is a Unwinding film, 22 winding film, 23 guide roll, 30 vacuum chamber, 31
Is an exhaust system, 40 is a crucible, 41 is a vapor deposition material, 50 is a high frequency coil, 51 is a matching box, 52 is a power supply, and 6
Reference numeral 0 indicates a gas introduction unit, 61 indicates a flow rate adjusting device, and 62 indicates an introduction gas.

The ion plating method according to the present invention will be described with reference to FIG. First, the inside of the vacuum chamber 30 is evacuated by an exhaust system 31 (for example, a vacuum pump or the like), and then an introduction gas 62 is introduced from the gas introduction unit 60 via the flow rate adjusting device 61 to obtain a vacuum of 10 ⁻³ to 10 ⁻⁶ Torr. To maintain. Next, high frequency power is supplied from the power source 52 to the high frequency coil 50 arranged between the conductive cooling roll 10 and the crucible 40 via the matching box 51 to start discharge. Ionization of the vapor deposition material 41 and the introduction gas 62 which are vaporized by heating the vapor deposition material 41 accommodated in the crucible 40 arranged immediately below the conductive cooling roll 10 when passing through the high frequency coil. To be done. By applying a voltage to the conductive layer 3 and holding it at a negative potential, the ionized vapor deposition material 41 and the introduced gas 62 are
Are accelerated toward the conductive chill roll 10.

At this time, the long transparent plastic film 20 was continuously unwound from the unwinding roll 21, passed through the guide roll 23, and ionized while traveling so as to hold the conductive cooling roll 10. The vapor deposition material 41 and the introduced gas 62 collide with and adhere to the surface of the plastic film,
Then, it is cooled and condensed on the surface of a long transparent plastic film to form a thin film. The plastic film on which the thin film is formed is wound around the winding roll 22 via the guide roll 23.

As the introduction gas, an inert gas such as argon or helium, oxygen, ozone, nitrogen or the like can be used. Further, as a method for heating the vapor deposition material, methods such as electron beam irradiation, resistance heating and induction heating can be adopted. In the ion plating method of the present invention, by applying a voltage to the conductive layer 3 and holding it at a negative potential, it is possible to accelerate the ionized vapor deposition material by high-frequency power, and to adhere the plastic film and the vapor deposition material. A vapor-deposited film having good properties can be obtained. The voltage applied to the conductive layer 3 may be a voltage capable of accelerating the ionized vapor deposition material to bring it into close contact with the plastic film, and preferably in the range of 1 to 10 kV.

As a method of applying a voltage to the conductive layer 3,
A method of applying a voltage by directly contacting the power supply tool 4 with the conductive layer 3, and a method in which a conductive tubular object is attached to the shaft of the cooling roll 1 after being insulated with an insulator or the like, and the tubular object and the conductive layer 3 are provided with a conductive wire. Then, a method of contacting the tubular object with the power supply tool 4 and indirectly applying a voltage or the like can be adopted. The power supply tool 4 may be made of a conductive material, and may have a brush-like shape, a plate-like shape, a roll-like shape, or any other structure capable of applying a voltage.

In the present invention, a transparent plastic film is used as the base film. Specific examples of the base film include polyolefin resins such as homopolymers or copolymers of ethylene, propylene and butene, polyester resins such as polyethylene terephthalate, polybutylene terephthalate and polyethylene-2,6-naphthalate. Polyamide resins such as nylon, nylon 6, nylon 12, aromatic nylon, copolymer nylon, vinyl alcohol resins such as polyvinyl alcohol and ethylene-vinyl alcohol copolymer, polyimide resins, polyetherimide resins, polysulfone resins, polyethers Examples include films of sulfone resins, polyetherketone resins, polycarbonate resins, polyvinyl butyral resins, and the like, and mixtures thereof.

In addition, known additives for the base film,
For example, an antistatic agent, an ultraviolet absorber, a plasticizer, a lubricant, a coloring agent and the like can be added. The base film may be an unstretched film or a stretched film, and may be a single layer or a laminated film of different resin films. Of these, a stretched film is preferable from the viewpoints of strength, elongation and thermal characteristics.

The method for producing the base film is not particularly limited, and extrusion molding methods such as T-die method and inflation method,
The film may be calendered or the like, and the film may be unstretched or biaxially stretched. The biaxially stretched film may be produced by either a simultaneous biaxial stretching method or a sequential biaxial stretching method. The thickness, width and length of the base film in the method of the present invention are not particularly limited and can be appropriately selected depending on the application. For example, the length is 500 m or more, and the thickness is 3 to 400 μm, and particularly preferably 5 to 200 μm from the viewpoint of mechanical strength and flexibility.

The base film is subjected to surface treatment by a conventionally known method such as corona discharge treatment, flame treatment, plasma treatment, glow discharge treatment and surface roughening treatment before forming a thin film by the ion plating method. be able to. In the present invention, a thin film of metal or metal compound is formed on the base film. This thin film has a function of imparting oxygen barrier properties and water vapor barrier properties to the finally obtained plastic film.

The vapor deposition material for forming the thin film in the method of the present invention is a metal or a metal compound. Specific examples of the metal include metals such as aluminum, iron, silver, tungsten, zirconium, tin, magnesium, titanium, silicon, zinc, copper and nickel, stainless steel, Zn-Ni.
Alloys such as alloys, Zn-Al alloys, Zn-Fe alloys, Fe-Al alloys, Ti-Ni alloys and Cu-Zn-Al alloys can be mentioned. In addition, specific examples of the metal compound include oxides, hydroxides, sulfides, carbides, nitrides and fluorides of the above metals. As the vapor deposition material, the above metals or metal compounds may be used alone or in combination of two or more, and a trace amount of a metal or metal compound other than the above may be contained as an impurity.

According to the experiments by the present inventors, the reason why the adhesion between the vapor deposition material of the vapor deposition film obtained by the ion plating method and the plastic film is weak and a stable thin film is not formed is that the conventional cooling roll is It was found that this is because the ionized vapor deposition material is difficult to accelerate because the applied voltage escapes. Then, in order to effectively achieve the object of the present invention, a vapor deposition film having a strong adhesion between a vapor deposition material and a plastic film by applying a voltage to a conductive cooling roll provided with an insulating layer in an ion plating method. It has been found that can be continuously and stably formed.

The conductive cooling roll 10 of the present invention is
The dielectric breakdown voltage of the electric insulation layer 2 is 0.2 kV or more, and
The heat transmission rate of the conductive cooling roll 10 is 10 to 100,000.
W / m ² · K is required, so that the plastic film can be sufficiently cooled,
Since the ionized vapor deposition material is accelerated without letting the applied voltage escape, a vapor deposition film having strong adhesion between the vapor deposition material and the plastic film can be obtained. Dielectric breakdown voltage is 1kV or more, heat transmission rate is 50 to 50000W
/ M ² · K is particularly preferable.

With respect to the dielectric breakdown voltage, referring to ASTM D149, the cooling roll 1 of the conductive cooling roll 10 is grounded under the condition of the temperature of 33 ° C. and the relative humidity of 60%, and the conductive layer 3 has a voltage of 50.
It is a value obtained by measuring a voltage when a voltage is applied and a current is applied at a speed of 0 V / s. In the conductive cooling roll 10, the heat transfer rate is such that thermocouples are installed so that one point on the inner surface of the cooling roll 1 and a point on the conductive layer 3 side at that point are aligned with each other, The inner surface of the cooling roll 1 was heated with a heater, the surface of the conductive layer was cooled with water, and the temperature difference caused thereby was measured. It is a value obtained by calculating the amount of heat from the voltage and current value applied to the heater at that time and calculating the heat transmission rate from Equation 1.

[0024]

## EQU00001 ## h = Q.ln (D2 / D1) / [2.pi.L. (t1-t2). (D2-D1)] ... Equation 1

In Equation 1, h is the heat transmission rate (W / m ² · K),
Q is the amount of heat (W), t is the temperature (° C), D is the diameter (m), L
Indicates a cooling roll length (m), 1 indicates an inner surface of the cooling roll, and 2 indicates an outer surface of the conductive layer. Breakdown voltage is 0.2kV
When it is less than 1, even if a voltage is applied to the conductive layer 3, the ionized vapor deposition material is not accelerated, and only a vapor deposition film having poor adhesion between the plastic film and the vapor deposition material is obtained, and the heat transmission rate is 10 W / m ² If it is less than K, the cooling ability of the plastic film is weak and the plastic film is easily damaged by the heat from the crucible and the condensation heat of the vapor deposition material, and if it exceeds 100000 W / m ² · K, the thickness of the conductive cooling roll 10 itself. Since the thickness becomes thin, it is easily deformed and the strength becomes insufficient, which is not preferable.

In the present invention, the electrically conductive chill roll 10 having a dielectric breakdown voltage of 0.2 kV or more and a heat transmission rate of the electrically conductive chill roll 10 of 10 to 100,000 W / m ² · K is insulated. It can be produced by appropriately selecting the materials and thicknesses of the layers and the conductive layer. The insulating layer 2 is provided in close contact with the outer peripheral surface of the cooling roll 1, and the conductive layer is provided in close contact with the insulating layer 2. This is a structure provided with 3.

The cooling roll 1 has a function of cooling the heated plastic film. As the metal material of the cooling roll 1, stainless steel, copper, iron or the like can be used, and as the shape, a well-known hollow type, jacket type or the like, or a structure in which a refrigerant is passed inside can be used. Any liquid can be used as the cooling medium as long as it has a function of cooling the cooling roll, and a mixture of ethylene glycol and water cooled to −20 ° C. can be usually used.

The electrical insulating layer 2 has the function of blocking the conduction of electricity between the cooling roll 1 and the conductive layer 3 and conducting heat. The thickness of the electric insulating layer 2 depends on the type of material, but may be a thickness that hinders the conduction of electricity, and is 0.1 mm or more, preferably 0.1 to 5 mm.
The electric insulating layer 2 is provided so as to be uniformly intimately contacted with the outer peripheral surface of the cooling roll 1 in order to suppress a decrease in heat transfer.
As a material of the electric insulation layer 2, a conventionally known ceramic,
Examples thereof include Teflon and fluorine. As a method for providing the electric insulation layer 2, a generally known method such as a ceramic spraying method, a Teflon processing method, or a fluorine processing method can be adopted. For example, as the ceramic spray processing method, methods such as a plasma spray method, an explosion spray method, an arc spray method, and a powder flame spray method can be adopted.

Among them, the plasma spraying method is a method of melting the powdered ceramics at a high temperature and spraying the powdery ceramics on the surface of the base material to provide the electric insulating layer 2, and the adhesive strength between the sprayed ceramic and the base material is strong. It is preferable because a dense and uniform film can be obtained. As a raw material of the ceramic, one having a low electric conductivity and a high thermal conductivity, such as alumina, can be used. Further, it is preferable to perform a sealing treatment on the ceramic surface.

The conductive layer 3 has a function of holding a potential on the surface of the conductive cooling roll 10. The conductive layer 3 is
A conductive substance is formed so as to be in close contact with the electric insulating layer 2 in order to suppress a decrease in heat conductivity. As a method for forming the conductive layer 3 on the insulating layer 2, a coating process such as winding a metal foil or a plate directly on the electric insulating layer 2, shrink fitting a metal tube on the electric insulating layer 2, or the like, or Alternatively, a method of spraying a metal or a conductive ceramic on the insulating layer can be adopted.

Specific examples of the electrically conductive cooling roll having the dielectric breakdown voltage and the heat transmission rate in the above ranges include, for example, FIGS. The hatched portions in FIGS. 2 to 5 indicate the electric insulating layer 2 portion. Such a conductive cooling roll can be obtained by taking the following means. First, when forming the conductive layer 3 on the electric insulating layer 2, it is necessary to have a structure in which a voltage does not escape. One is a conductive layer having a width smaller than that of the cooling roll 1 provided with the electric insulating layer 2. By closely setting 3. It is preferably 2 mm or more from both ends of the cooling roll 1, and more preferably 3 mm or more.
The conductive layer 3 having a small width of -30 mm is provided.

On the other hand, a conductive layer 3 having the same width as that of the cooling roll 1 provided with the electric insulating layer 2 is formed, and further, the end face of the cooling roll 1 or the end face of the conductive layer 3 or both are closely contacted to form the electric insulating layer. 2 is a means of providing an insulating layer continuous with 2. Cooling roll 1 provided with the former electric insulation layer 2
As a method of providing the conductive layer 3 having a smaller width, as a coating method, a method of winding a metal foil or a plate having a width smaller than that of the cooling roll 1 so as to be located closer to the center side than both ends, or a method of forming a smaller width than the cooling roll 1 As a thermal spraying method, such as a method of shrink-fitting a metal tube so that it is located closer to the center than both ends, a method of spraying metal or conductive ceramic with a width smaller than that of the cooling roll 1, winding insulating tape around both ends, or using plastic or It can be formed by a method of applying an insulating material such as ceramics.

As a method of providing the conductive layer 3 having the same width as the cooling roll 1 provided with the electric insulating layer 2 of the latter, the conductive layer 3 having the same width as the cooling roll 1 is formed by the above-mentioned coating processing method or thermal spraying processing method. To form. After that, an insulating tape may be attached to the end surface of the cooling roll 1, the end surface of the conductive layer 3, or both, and an insulating material such as plastic or ceramic may be applied, or ceramic may be sprayed.

The conductive cooling roll 10 in the present invention is
Since it can cool the plastic film sufficiently and has the function of holding the electric potential, it can be used for an ion plating device that forms a thin film of a metal or a metal compound on a long transparent plastic film. it can. Further, since the vapor-deposited film obtained by this ion plating method has excellent oxygen barrier properties and water vapor barrier properties, it can be used as a packaging material for foods, medical products, chemicals, EL devices and the like.

[0035]

EXAMPLES The contents and effects of the present invention will be described below in more detail with reference to Examples, but the present invention is not limited to the following examples as long as the gist thereof is not exceeded. The breakdown voltage, heat transfer rate, adhesion strength, and appearance were evaluated and calculated by the methods described below, and the results are summarized in Table 1.

<Dielectric Breakdown Voltage (kV)> ASTM D1
49, the temperature of 33 ℃, relative humidity of 60%,
The inner surface of the cooling roll 1 of the conductive cooling roll 10 is grounded,
When a voltage was applied to the conductive layer 3 at a rate of 500 V / s, the applied voltage was measured. <Heat transmission rate (W / m ² · K)> In the conductive cooling roll 10, a point on the inner surface of the cooling roll 1 and a point on the conductive layer 3 side at that point are paired with each other. Thus, the thermocouple was installed, the inner surface of the cooling roll 1 was heated with a heater, the conductive layer surface was cooled with water, and the temperature difference caused thereby was measured. The amount of heat was obtained from the voltage and current value applied to the heater at that time, and the heat transmission rate was calculated from Equation 1.

[0037]

[Number 2] h = Q · ln (D2 / D1) / in [2πL · (t1-t2) · (D2-D1)] ··· Equation 1 Equation 1, h is the heat transfer coefficient (W / m ² · K) and Q are amounts of heat (W), t is temperature (° C.), D is outer diameter (m), L is cooling roll length (m), 1 is the cooling roll inner surface, and 2 is the conductive layer outer surface. .

<Appearance> The vapor-deposited film is visually observed for wrinkles, slack, and heat damage, and wrinkles, slack, and
When none of the phenomena of heat damage was present, it was evaluated as ◯, and when any of these phenomena was present, it was evaluated as x. <Adhesive strength (g / 15 mm)> A urethane adhesive (AD-900: AD-RT5 = 10: 1.5 mixture) manufactured by Toyo Morton Co., Ltd. is applied to the vapor deposition surface of the vapor deposition film as an adhesive. Then, a polypropylene film (RXC-7, manufactured by Tokyo Cellophane Paper Co., Ltd.) having a thickness of 50 μm was dry laminated and aged at 60 ° C. for 3 days. Next, this laminated film was subjected to hot water treatment at 120 ° C. for 30 minutes and cut into strips having a width of 15 mm and a length of 100 mm to obtain test pieces.

One end of the interface between the vapor-deposited film and the polypropylene film of this test piece was peeled off by 50 mm in advance, and both peeled surfaces were autographed (a test apparatus according to JIS K7127, DSS-10 manufactured by Shimadzu Corporation).
Attached to the fixed and movable grips of 0) with a distance between grips of 100 mm, and pulling the movable grips at a pulling speed of 3
The value of the center line of the wavy curve of the tensile load recorded on the strain gauge during this was moved 60 mm at 00 mm / min, and the average value of the three test pieces was taken as the adhesion strength. When the test piece was broken during the pulling (this is called film breakage), the tensile load at this time was taken as the adhesion strength.

Example 1 (1) Preparation of Conductive Cooling Roll Alumina (LA-6, manufactured by Prax Air Engineering Co., Ltd.) was thickly formed on the entire outer peripheral surface of a stainless single-row spiral cooling roll having an outer diameter of 778 mm and a width of 610 mm. It was sprayed to a thickness of 1 mm and a sealing treatment was performed. Alumina-treated stainless single-roll spiral cooling roll, outer diameter 799 mm, wall thickness 10 mm, width 57
A 0 mm stainless-cylindrical tube was shrink-fitted by 20 mm inside from both ends of the spiral cooling roll.
The entire outer peripheral surface of the shrink-fitted stainless steel cylindrical tube was subjected to a plating treatment to prepare a conductive cooling roll.

(2) Method for producing vapor-deposited film In the ion plating apparatus shown in FIG. 1, the conductive cooling roll 10 produced in the above (1) was used to attach a brush made of copper to the tip of the conductive wire. Was brought into contact with the outer peripheral surface of the conductive cooling roll 10 and a voltage of 5 kV was applied to maintain the negative potential. The conductive cooling roll 10 was cooled by passing a mixture of ethylene glycol and water at −20 ° C. as a cooling medium. The introduction gas, argon gas, (the gas pressure: 1 × 10 ^{over 4} torr), as the deposition material, a sintered body of SiO the (Sumitomo Sitix (Ltd.)) 1.2 kg was heated at putting resistive heating in a crucible , 13.56MH for high frequency coil
High frequency power of z, 1 kW was supplied.

Next, as shown in FIG. 1, a biaxially stretched polyethylene terephthalate film (H-100 manufactured by Diafoil Hoechst Co., Ltd.) having a thickness of 12 μm, a width of 500 mm and a length of 4000 m was used, as shown in FIG.
3, the conductive cooling roll 10, the guide roll 23 in this order 2
By running at a speed of 00 mm / min, a vapor deposition film having a vapor deposition film thickness of 300 Å was obtained. The dielectric breakdown voltage of the conductive cooling roll prepared in (1) was measured, the heat transmission rate was calculated, and the adhesion strength of the obtained vapor deposition film was measured. The results of evaluating the appearance are shown in Table 1.

Example 2 and Example 3 A conductive cooling roll was prepared by the procedure described in Example 1 except that the thickness of alumina of the conductive cooling roll was changed as shown in Table 1 in Example 1. Then, a vapor deposition film was obtained. The dielectric breakdown voltage of each of the prepared conductive cooling rolls was measured, the results of calculating the heat transmission rate and the adhesion strength of the vapor deposition film obtained were measured, and the results of evaluating the appearance are shown in Table 1.

Example 4 In Example 1, 1 kV was applied to the outer peripheral surface of the conductive cooling roll.
A vapor-deposited film was obtained by the procedure described in Example 1 except that the voltage was applied. The dielectric breakdown voltage of the produced conductive cooling roll was measured, the heat transmission rate was calculated, and the adhesion strength of the obtained vapor deposition film was measured. The results of evaluating the appearance are shown in Table 1.

Example 5 In Example 1, the conductive cooling roll made of stainless steel 1 was used.
A conductive cooling roll was produced by the procedure described in Example 1 except that both the strip spiral cooling roll and the stainless steel cylindrical tube to be shrink-fitted were replaced with copper, and a vapor deposition film was obtained. The dielectric breakdown voltage of the produced conductive cooling roll was measured, the heat transmission rate was calculated, and the adhesion strength of the obtained vapor deposition film was measured. The results of evaluating the appearance are shown in Table 1.

Comparative Example 1 In Example 1, the conductive cooling roll was made of stainless steel 1.
A vapor-deposited film was obtained by the procedure described in Example 1 except that the strip spiral cooling roll (the one not subjected to the alumina treatment and the shrink fitting treatment) was used. Table 1 shows the results of calculating the heat transmission rate of the stainless single-roll spiral cooling roll and the adhesion strength of the obtained vapor deposition film, and evaluating the appearance.

Comparative Example 2 In the example described in Example 1, the outer diameter was 801 mm and the wall thickness was 10
A conductive cooling roll was produced by the procedure described in Example 1, except that a stainless steel cylindrical tube having a width of 570 mm and a width of 570 mm was shrink-fitted inward by 20 mm from both ends of the spiral cooling roll. The produced conductive cooling roll was not intimate because a gap was generated between the alumina-treated stainless single-row spiral cooling roll and the shrink-fitted stainless steel cylindrical tube. Also, an attempt was made to produce a vapor-deposited film by the procedure described in Example 1, but a good vapor-deposited film capable of measuring the adhesion strength could not be obtained. Table 1 shows the results of measuring the dielectric breakdown voltage of the produced conductive cooling roll, calculating the heat transmission rate, and evaluating the appearance of the vapor deposition film obtained.

Comparative Example 3 In the example described in Example 1, conductive cooling was conducted by the procedure described in Example 1 except that a stainless steel cylindrical tube having the same width as the spiral cooling roll of the conductive cooling roll was shrink-fitted. A roll was prepared and a vapor deposition film was obtained. The conductive chill roll thus prepared had the alumina-treated portion entirely hidden by a stainless steel cylindrical tube. Table 1 shows the results of measuring the dielectric breakdown voltage of the produced conductive cooling roll, calculating the heat transmission rate, and evaluating the appearance of the vapor deposition film obtained.

[0049]

[Table 1]

The following can be seen from Table 1. (1) The vapor-deposited film obtained by using the conductive cooling roll of the present invention is free from wrinkles, slack, and heat, and the vapor deposition material is adhered to the base film side when measuring the adhesion strength. It can be seen that the adhesion between the base material film of the vapor deposition film and the vapor deposition material is strong because the polypropylene film is peeled off and the polypropylene film is broken (see Examples 1 to 5). (2) The vapor-deposited film obtained by using the conductive cooling rolls in Comparative Examples 1 and 3 has a voltage that escapes even when a voltage is applied to the conductive cooling roll. It was peeled off from the polypropylene film side where was attached. It can be seen that the adhesion between the base material film of the vapor deposition film and the vapor deposition material is weak. (3) The vapor-deposited film obtained by using the conductive cooling roll in Comparative Example 2 suffers from wrinkles, sagging, and heat damage due to insufficient cooling of the plastic film due to a decrease in heat conduction from the cooling roll. A good vapor-deposited film could not be obtained.

[0051]

Since the conductive cooling roll of the present invention has a function of cooling the plastic film and a function of holding the potential on the roll surface, the vapor deposition film obtained by the ion plating method is a plastic film and a vapor deposition film. A vapor-deposited film having strong adhesion to a material has a particularly advantageous effect that it can be industrially advantageously produced, and its industrial utility value is extremely large.

[Brief description of drawings]

FIG. 1 is a schematic cross-sectional view of an ion plating apparatus for producing a vapor deposited film according to the present invention.

FIG. 2 is a perspective view of an example of a conductive cooling roll according to the present invention.

FIG. 3 is a perspective view of an example of a conductive cooling roll according to the present invention.

FIG. 4 is a perspective view of an example of a conductive cooling roll according to the present invention.

FIG. 5 is a perspective view of an example of a conductive cooling roll according to the present invention.

[Explanation of symbols]

 1 Cooling Roll 2 Electric Insulating Layer 3 Conductive Layer 4 Power Supply Tool 5 Introducing Terminal 6 Bearing 10 Conductive Cooling Roll 20 Plastic Film 21 Unwinding Film 22 Winding Film 23 Guide Roll 30 Vacuum Chamber 31 Exhaust System 40 Crucible 41 Vapor Deposition Material 50 High Frequency Coil 51 Matching Box 52 Power Supply 60 Gas Introducing Section 61 Flow Control Device 62 Introducing Gas

 ─────────────────────────────────────────────────── ─── Continuation of the front page (72) Inventor Kenji Takamatsu 1000, Higashihuinana-cho, Ushiku-shi, Ibaraki Mitsubishi Chemical Corporation Tsukuba Plant

Claims (5)

[Claims] 1. A conductive cooling roll having a cooling roll 1 provided with an electrically insulating layer 2 in close contact with an outer peripheral surface thereof, and an electrically conductive layer 3 provided in close contact with the electrically insulating layer, wherein insulation of the electrically insulating layer 2 is achieved. A conductive cooling roll for use in an ion plating apparatus, which has a breakdown voltage of 0.2 kV or more and a heat transmission rate of the conductive cooling roll of 10 to 100,000 W / m ² · K. 2. An electric insulating layer 2 is provided in close contact with the outer peripheral surface of the cooling roll 1, and a conductive layer 3 having a width smaller than that of the cooling roll 1 is provided in close contact with the electric insulating layer 2. The conductive cooling roll according to claim 1. 3. A conductive layer having an electric insulating layer 2 which is in close contact and continuous with the outer peripheral surface of the cooling roll 1 and has the same width as the cooling roll 1 on a layer corresponding to the outer peripheral surface of the electric insulating layer 2. Three
2. The conductive cooling roll according to claim 1, wherein the insulating layer is provided in close contact with the end face of the cooling roll 1, the end face of the conductive layer 3 or both, and an insulating layer continuous with the electric insulating layer 2 is provided. . 4. The electrically conductive cooling roll according to claim 1, wherein the electrically insulating layer 2 is a ceramic coating layer having a thickness of 0.1 to 5 mm. 5. In the ion plating method, when a vapor-deposited film is manufactured by forming a thin film of a metal or a metal compound on at least one surface of a long and transparent plastic film, a dielectric breakdown of the electric insulation layer 2 is produced. A voltage is applied to the conductive layer 3 of the conductive cooling roll having a voltage of 0.2 kV or more and a heat transmission rate of the conductive cooling roll of 10 to 100,000 W / m ² · K, and kept at a negative potential, and
A method for producing a vapor-deposited film, comprising cooling a plastic film by passing a cooling medium through a cooling roll 1.