JPH07331418A - Vacuum deposition apparatus and vacuum deposition method - Google Patents

Abstract

(57) [Abstract] [Purpose] To provide a vacuum vapor deposition apparatus and a vacuum vapor deposition method for continuously supplying an evaporation raw material to obtain a high productivity and stable high quality vapor deposition film. A vaporization material supply / discharge guide capable of continuously supplying and discharging the vaporization material is provided with a discharge hole for at least one vaporization particle in addition to the vaporization source, and the vaporization raw material between the discharge hole and the vaporization source. A vacuum vapor deposition apparatus and a vacuum vapor deposition method, characterized in that a supply / discharge guide is heated to a temperature equal to or higher than the vaporization temperature of vaporized particles. [Effect] Vacuum deposition can be performed without causing troubles such as breakage of the raw material molding, generation of splash due to bumping, rapid gas release, rise in pressure in the vacuum tank, mixing of impurities and fluctuation of evaporation rate, and high quality. The vapor-deposited film can be manufactured with high productivity.

Description

Detailed Description of the Invention

[0001]

FIELD OF THE INVENTION The present invention relates to a vacuum deposition of a flexible plastic film having various functions, which can be used in the fields of food packaging, pharmaceutical packaging, electronic device component packaging, tobacco packaging, photoengraving, photosensitive photographic materials and the like. The present invention relates to a vacuum vapor deposition apparatus and a vacuum vapor deposition method that are preferably used for processing.

[0002]

2. Description of the Related Art In recent years, the surface of a flexible plastic film is coated with a metal or a metal oxide by a vacuum vapor deposition method to improve decorative properties, gas barrier properties, chemical resistance, wetting properties, magnetic properties, electrical conductivity, dimensional stability, etc. With added functionality, it has come to be used in fields such as food packaging, pharmaceutical packaging, electronic device component packaging, tobacco packaging, photoengraving and photosensitive photographic materials. In particular, aluminum vapor-deposited films have come to be widely used for decoration and packaging. Recently, research and development of silicon oxide vapor deposition film has been actively carried out as a transparent high barrier material with little environmental pollution, and it is expected that it will be widely spread, and the demand for the development of metal oxide vapor deposition technology is increasing day by day. It's getting stronger.

In response to the spread of these applications, it has become necessary to reduce mass production and processing costs. Therefore, it is practical to reduce the processing time by increasing the evaporation temperature to increase the processing speed, increase the area that can be produced in one processing step by increasing the width of the film to be attached, and extend the processing length. As a result, vapor deposition machines have become larger. In order to extend the processing length, the evaporation material crucible must be enlarged so that a large amount of evaporation material can be charged at one time, or a storage space for evaporation material can be provided in the vacuum chamber so that it can be continuously supplied. It has been. When a sublimable evaporation material such as silicon oxide is used, a method of continuously supplying the evaporation material heated to a sublimation temperature or higher by an electron beam heating method as shown in FIG. A device as shown in FIG. 6 (Japanese Patent Laid-Open No. 1-252768)
Japanese Patent Laid-Open No. 2-277774), a method of continuously supplying an evaporation raw material has been used.

The apparatus disclosed in Japanese Unexamined Patent Publication No. 1-252768 is very effective for stable quality and improvement in productivity due to long-time processing, especially in vapor deposition of silicon oxide or the like. However, when the evaporation source has a structure in which a part of the tube is open as shown in FIG. 5, this method also has the following drawbacks. Evaporative particles flying from a continuously supplied cylindrical evaporation source in an evaporation source basically uniformly fly in all directions. The vaporized particles pass through the opening of the tube directly or while repeatedly colliding several times, fly toward the upper film direction, and further adhere to the film to become a vapor deposition film. However, since the evaporation source has a structure in which a part of the tube is open, evaporated particles also fly in the longitudinal direction of the tube. The evaporative particles flying in the longitudinal direction of the tube repeatedly adhere to the inner wall portion of the heated tube, re-evaporate and redeposit, and finally adhere to the portion of the inner wall of the tube below the sublimation temperature of the evaporative particles, accumulate. As a result, a part of the inner wall of the pipe is blocked, and smooth continuous supply / discharge of the vaporized raw material is hindered. In other words, if vaporized particles adhere to and accumulate on the inner wall of the vaporization source, the columnar vaporized raw material that is continuously supplied / discharged comes into contact with the deposited portion, causing the vaporized raw material to meander or clog. ", And had to stop the continuous supply of evaporation raw material.

When the supply of the evaporation raw material is stopped, the evaporation raw material is cracked, the evaporation rate fluctuates, and a splash is generated, and the fluctuation of the evaporation rate causes irregularity in each heating heater of the evaporation sources arranged in a plurality. The control of the thickness and the like becomes unstable, and the occurrence of splash causes the defects of the vapor deposition film, the damage of the base film, and the phenomenon of inclusion of foreign matter as described above. As described above, as a result, the quality of the vapor deposition film deteriorates. In the conventional vacuum vapor deposition apparatus that continuously supplies / discharges the evaporation raw material, if the supply of the evaporation raw material is stopped, the quality of the vapor deposition film is remarkably deteriorated, and thus the vapor deposition process must be stopped.
There is a problem that productivity is significantly reduced.

[0006]

SUMMARY OF THE INVENTION It is an object of the present invention to provide a vacuum vapor deposition apparatus and a vacuum vapor deposition method for continuously supplying an evaporation raw material to obtain a vapor-deposited film having high productivity and stable high quality vapor deposition film.

[0007]

SUMMARY OF THE INVENTION An object of the present invention is to provide an evaporation source supply / discharge guide capable of continuously supplying and discharging an evaporation source with at least one discharge hole for evaporation particles in addition to an evaporation source, and This can be achieved by a vacuum vapor deposition device characterized in that an evaporation source supply / exhaust guide between the exhaust hole and the evaporation source is heated to an evaporation temperature of the evaporation particles or higher. Further, an object of the present invention is to provide an evaporation source supply / discharge guide capable of continuously supplying and discharging an evaporation source with a discharge hole for at least one evaporation particle in addition to the evaporation source, and to connect the discharge hole and the evaporation source. This can be achieved by a vacuum vapor deposition method characterized in that the evaporation source supply / exhaust guide in between is heated to the evaporation temperature of the evaporating particles or higher, and the evaporating particles are discharged from the discharge hole.

In the present invention, as a vacuum vapor deposition apparatus having a mechanism for continuously supplying and discharging an evaporation raw material, as shown in FIG. 6, JP-A-1-252768 and JP-A-2-2
The device described in Japanese Patent No. 77774 can be used. As the evaporation source supply / discharge guide capable of continuously supplying and discharging the evaporation source, a structure having an integrated evaporation source as shown in FIG. 1 or an evaporation source as shown in FIG. 2 is provided separately. The thing of a structure is mentioned. Further, the shape of the evaporative material supply / discharge guide may be either a circular tube or a rectangular tube. The holes for discharging evaporated particles other than the evaporation source may be circular, elliptical, or rectangular as shown in FIG. Further, as shown in FIG. 2, when the tubular evaporation source is separated, it may be used as a discharge hole by providing a gap between the evaporation source and the evaporation source.

Between the evacuation particle discharge hole and the evaporation source, it is necessary to keep the evaporation temperature of the evaporation particles or higher so that the evaporation particles do not adhere and accumulate. The space between the discharge hole for the evaporated particles and the evaporation source may be heated by a conventionally known method, but the temperature may be raised to the evaporation temperature of the evaporated particles or higher by heat conduction from the evaporation source. The evaporation temperature of evaporation particles depends on the evaporation material and the degree of vacuum. For example, when vapor-depositing SiO or a mixture of Si and SiO ₂ as a vapor deposition raw material under a pressure of 1 × 10 ⁻² Pa, the temperature is 873 ° C. or higher. The heating method for the evaporation material supply / discharge guide is not particularly limited as long as it can be used in a vacuum state and the evaporation material can be heated to a predetermined temperature within a predetermined time, and direct resistance heating, indirect resistance Conventionally known methods such as heating, direct high frequency induction heating, indirect high frequency induction heating, radiant heating, and electron beam heating can be used.

As a method for directly controlling the temperature between the discharge hole of the evaporation particles and the evaporation source to be higher than the evaporation temperature of the evaporation particles, there are methods such as PID control, proportional control and fuzzy control. As a temperature measuring method therefor, a method using a conventionally known thermometer such as a thermocouple thermometer or a radiation thermometer can be used. In the case of the evaporating material supply / discharge guide having the structure in which the evaporation sources are integrated as shown in FIG. 1, the temperature between the evacuation particle discharge hole and the evaporation source should be indirectly controlled to be equal to or higher than the evaporation temperature of the evaporation particles. You can That is, since the temperature of the evaporation source itself is temperature controlled, by correctly grasping the temperature difference between the evaporation source temperature and the evaporation material supply / discharge guide,
In effect, temperature control of the evaporative feedstock supply and discharge guide between the evacuation particle discharge hole and the evaporation source is realized.

As the evaporation source, Si, SiO, Si
SiOx containing ₃ O ₄ , Si ₂ O ₃ and SiO ₂ (X = 1
2) and the like, a mixture of one or more substances selected from silicon and silicon oxides, a mixture of silicon and / or silicon oxides and a metal compound, and a chemical bond. Examples of the metal compound include metal oxides and metal fluorides. Examples of the metal oxide include magnesium oxide, calcium oxide, barium oxide, aluminum oxide, titanium oxide, zirconia oxide, sodium oxide, potassium oxide, tin oxide, indium oxide, magnesium oxide-dioxide. Examples thereof include silicon co-oxides (forsterite, steatite), aluminum oxide-silicon dioxide co-oxides (mullite), and the like. Examples of the metal fluorides include alkaline earth metal fluorides such as magnesium fluoride, calcium fluoride, and barium fluoride, and alkali metal fluorides such as sodium fluoride and potassium fluoride.

[0012]

The present invention will be described in more detail based on the following examples, but the invention is not intended to be limited to the following examples without departing from the gist thereof. In addition, the test method of the vapor deposition film obtained in the example is as follows.
Oxygen barrier property: According to ASTM D 3985, the oxygen gas permeability was measured using OXTRAN-TWIN manufactured by Modern Controls, Inc., USA. Appearance: Defects in the deposited film of the obtained deposited film and inclusion of foreign matter were visually evaluated.

[Embodiment 1] As shown in FIG. 3, holes having a diameter of 10 mm are provided at two locations on an evaporation source supply / discharge guide of a vacuum vapor deposition apparatus described in Japanese Patent Laid-Open No. 1-252768.
Four were provided at intervals of 8 °, for a total of eight. FIG. 1 shows a side view of the evaporation material supply / discharge guide. The evaporation source was heated by a resistance heating method, and the temperature was controlled by a radiation thermometer. Further, the temperature between the discharge hole of the evaporation raw material and the evaporation source was measured using a radiation thermometer. Next, an equimolar mixture of silicon and silicon dioxide (amorphous) was compression molded to give a diameter of 4
A cylindrical molded product having a height of 0 mm and a height of 35 mm was obtained. The obtained molded product was continuously supplied at a supply rate of 5 mm / min from a supply port of an evaporation material supply / discharge guide (made of a boron nitride composite sintered body), and an evaporation source was set under a vacuum of 1 × 10 ^-2 Pa. It was heated to 1350 ° C. by resistance heating, and silicon oxide was vacuum-deposited on a polyethylene terephthalate film having a thickness of 12 μm. The temperature between the discharge hole of the evaporation material and the evaporation source is 900 to 110.
It was 0 ° C. Under the conditions, the processing speed was 50 m / min, and vacuum deposition processing was performed for 1 hour. The thickness of the vapor-deposited film was measured by using a quartz-type film thickness monitor, and it was about 1000 Å.

[Comparative Example 1] The same procedure as in Example 1 was carried out except that the evaporation material supply / discharge guide of the vacuum vapor deposition apparatus used in Example 1 was not provided with holes. Twenty-five minutes after the start of vapor deposition processing, a trouble occurred due to clogging of the vaporized raw material that was continuously supplied, so the raw material supply was stopped, the processing was continued for 5 minutes thereafter, and the vapor deposition processing was stopped.

The vapor-deposited films obtained in Examples and Comparative Examples were evaluated for oxygen barrier property and appearance. The results are shown in Table 1.

[Table 1]

[0016]

According to the present invention, the vaporized raw material can be smoothly supplied and discharged without the vaporized particles adhering to and depositing on the inner wall of the vaporizing raw material supply / discharge guide. Therefore, it is possible to perform vacuum deposition without causing troubles such as breakage of the raw material molded product, generation of splash due to bumping, rapid gas release, increase in pressure in the vacuum chamber, mixing of impurities and fluctuation of evaporation rate, and high-quality evaporation. The film can be produced with high productivity.

[0017]

[Brief description of drawings]

FIG. 1 is a side view of an evaporation source supply / discharge guide of the present invention in which an evaporation source is integrated.

FIG. 2 is a side view of an evaporation source supply / discharge guide of the present invention in which an evaporation source is provided separately.

FIG. 3 is a cross-sectional view of an evaporation source supply / discharge guide provided with a discharge hole for evaporated particles.

FIG. 4 is a perspective view of an evaporation source supply / discharge guide provided with a discharge hole for evaporated particles.

FIG. 5 is a perspective view of an evaporation source having a structure in which a part of a tube is opened.

FIG. 6 is a side view of a conventional evaporation source supply / discharge guide.

FIG. 7 is a side view of a conventional vacuum vapor deposition apparatus using an electron beam heating method.

[Explanation of symbols]

1: evaporation source 2: evaporation material
3: Evaporation material supply mechanism 4: Evaporation particle discharge hole 5: Electron beam
6: Electrode 7: Evaporative material supply / discharge guide
8: Radiation thermometer 9: PID temperature controller 10: Electron gun

Claims (2)

[Claims] 1. An evaporation source supply / discharge guide capable of continuously supplying and discharging an evaporation source is provided with an emission hole for at least one evaporation particle in addition to the evaporation source, and between the discharge hole and the evaporation source. A vacuum vapor deposition apparatus, characterized in that an evaporation source supply / discharge guide is heated to an evaporation temperature of evaporation particles or higher. 2. An evaporation source supply / discharge guide capable of continuously supplying and discharging an evaporation source is provided with a discharge hole for at least one evaporation particle in addition to the evaporation source, and between the discharge hole and the evaporation source. A vacuum vapor deposition method, characterized in that an evaporation material supply / discharge guide is heated to a temperature equal to or higher than an evaporation temperature of evaporation particles and the evaporation particles are discharged from a discharge hole.