JP2892620B2 - Vacuum evaporation method for optical parts using porous ceramics sintered compact impregnated with organic film-forming substance for optical parts - Google Patents

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a method for vacuum deposition of optical parts, and more particularly to a method of using a porous ceramic sintered body impregnated and solidified with an organic film-forming substance for optical parts. And a vacuum deposition method for an optical component. More specifically, the present invention, after vacuum-depositing an optical component with an inorganic deposition material in a vacuum deposition apparatus,
The present invention relates to a vacuum evaporation method characterized by heating a porous ceramic sintered body in the apparatus as it is, performing vacuum evaporation with an inorganic evaporation material, and further forming an organic protective film.

[0002]

2. Description of the Related Art Generally, a chemical substance has a melting point and a boiling point. In particular, the boiling point has a pressure dependency and is high at a high pressure and low at a reduced pressure side. For this reason, a substance that is difficult to boil under normal pressure can be easily evaporated by reducing the pressure. At this time, the solid is present in the path of the evaporant, so that the surface thereof is covered with the precipitate of the evaporate. This is the principle of vacuum evaporation.

When an optical component is processed by vacuum evaporation, very small and severe irregularities are generated on the surface of an object to be processed due to adhesion of crystals of an inorganic evaporation material due to the nature of the processing. It is necessary to fill the gaps of the irregularities to make the gap smooth, and to form a protective film without impairing the optical properties. In the case of spectacle lenses, the outermost surface of the multi-coat (multi-layer anti-reflection film) is a silicon dioxide film, which easily becomes cloudy due to moisture or splashing water in the air, and becomes a so-called white burn, so it is water repellent By applying a coating, it is possible to prevent whitening. In addition, a protective coating is used to protect against contamination caused by touching a finger or the like.

It is known that applying a film-forming substance as a solution has a certain effect. However, since a very thin film has to be formed, the solution is diluted with a large amount of a solvent. The solvent used in the prior art is a so-called chlorofluorocarbon-based ozone layer depleting substance, and a recently developed non-fluorocarbon-based solvent is also an organic fluorine-based or organic chlorine-based compound that is considered as a subject of study on regulated substances in the future.

In the prior art, a film is formed in a separately prepared process after being taken out of a vapor deposition apparatus. The process is divided into solution concentration adjustment, coating, and drying. The inside of the device is released to the atmospheric pressure immediately after the end of the vapor deposition, and the product is taken out. At this time, the crystalline substance deposited on the surface of the object to be treated adheres to the surface in the form of particles, so it is extremely resistant to external contamination. In addition to being in a weak state, the vapors generated by the introduction of air or nitrogen gas when released to the atmosphere cause the vapor deposition material deposited in the device to fly up and re-adhere to the workpiece, so the next process It is well known that there is a problem that a wet cleaning step is indispensable.

[0006]

As described above, it is well known that the conventional formation of a protective film has a problem of environmental pollution due to the solvent used and a problem of surface cleaning caused by the process. An object of the present invention is to eliminate the drawbacks of using a solvent which has been conventionally regarded as indispensable and of using a wet cleaning step, and in particular, evaporating an organic film-forming substance without using a solvent at all. It is intended to be solidified by adhesion.

The present invention uses a porous ceramic sintered body which has been subjected to a vacuum evaporation treatment with an inorganic evaporation material and then impregnated and solidified with an organic film-forming material for an optical component in the vacuum evaporation apparatus. It is an object of the present invention to provide a vacuum deposition method for an optical component in which an organic protective film is formed on the optical component without using any solvent.

[0008]

According to the present invention, an organic protective film is formed on an optical component by using a porous ceramic sintered body impregnated and solidified with an organic film-forming substance for an optical component. This is a vacuum deposition method for optical components.

That is, the present invention is to evaporate and solidify an organic film-forming substance by a solvent-free principle which completely eliminates the use of a solvent, which has been regarded as indispensable until now. A medium that can easily absorb the melt or solution of the film-forming substance and does not evaporate in vacuum is required. For this purpose, it is generally desirable to use a porous ceramic body.

[0010] The porous ceramic body is preferably a sintered ceramic body. The shape of the porous ceramics sintered body is not particularly limited, and is a plate-shaped body having a size of 15 × 15 × 1 mm, a disc-shaped body having a diameter of φ17 × 7 mm, a spherical body having a diameter of φ15 mm, a cylindrical body having a diameter of φ12 × 10, Examples thereof include those crushed into irregular shapes.

As the organic film-forming substance which can be vaporized in a vacuum, any substance can be used as long as it can form an organic film on the surface of optical parts represented by lenses such as glasses and cameras. Waxes and silicone resin compounds are exemplified.

The organic film-forming substance is brought into a molten state or a solution state and is impregnated and solidified in the porous ceramic sintered body. Although the film-forming substance is absorbed by the porous ceramics sintered body, the organic compound may be solvent-free without any problem. Even when a solvent is used, it can be recovered before the ceramic sintered body manufacturing process.

The present invention is a method for vacuum-depositing an optical component, wherein the porous ceramic sintered body is used in a vacuum deposition apparatus for an optical component.

The above-mentioned vacuum vapor deposition apparatus is a normal vacuum vapor deposition apparatus having means for forming an inorganic-based vapor-deposited film, into which the above-mentioned specific porous ceramics sintered body is inserted. The porous ceramics sintered body is heated to evaporate the organic film-forming substance. The optical component is vacuum-deposited with an inorganic deposition material, and an organic protective film is further formed. The organic protective film is formed by heating a porous ceramic sintered body impregnated and solidified with an organic film-forming substance that can be vaporized in a vacuum.
As described above, since the protective film is formed in the same apparatus after the vapor deposition, an intermediate cleaning step is not required. Therefore, the use of a solvent is unnecessary in the vapor deposition processing step. That is, since the protective coating of the present invention is formed in the vapor deposition apparatus as it is after the ordinary vacuum vapor deposition operation, the object to be processed is not taken out of the vapor deposition apparatus, and dust and contamination generated by being taken out are removed. The cleaning step does not require a cleaning step before the protective film forming process, which has been conventionally performed.

According to the present invention, an optical component is vacuum-deposited with an inorganic deposition material in a vacuum deposition apparatus, and then is impregnated with an organic film-forming substance for an optical component which can be vaporized in a vacuum in the apparatus. A vacuum evaporation method for optical parts, characterized in that an organic protective film is formed by heating a porous ceramic sintered body.

The amount of the film-forming substance can be adjusted by adjusting the size of the ceramic sintered body, the viscosity of the solution, etc. for the porous ceramic sintered body to be used. A constant amount can always be supplied to a vacuum evaporation apparatus having a constant amount of. Especially when the required amount is very small, it is difficult to measure with pure film-forming substance alone and skill is required. Easy. Therefore, if the treatment is carried out by an evaporator adjusted so as to completely eliminate this, the required amount is naturally evaporated. Further, according to this method, it is easy to heat the object to be processed, so that it is possible to form a film by polymerizing the object to be processed.

[0017]

EXAMPLES The present invention will be described with reference to examples. The present invention is not limited by this embodiment.

Example 1 Polyethylene wax was melted as a vapor-depositing substance which is an organic film-forming substance, and was sufficiently dried beforehand.
Absorbed in 5 × 15 × 1 mm porous ceramics. The increase of this ceramic is 0.20 per piece
Gram.

One of the ceramics obtained here was used for a diameter φ60.
It was inserted into a 0 mm vacuum evaporation apparatus and heated to 85 ° C. to evaporate after a normal evaporation operation. The film thickness measured by the interferometry was 0.03 micrometers. The thickness of the water-repellent film formed on the lens of the spectacles was 0.03 μm when measured by an interference method.
This is a thickness that sufficiently functions as a protective film.

Example 2 A solution of a silicone resin compound (perfluoroalkylsilazane) was used as a vapor-depositing substance which is an organic film-forming substance. The evaporation residue of this product was 3%. Diameter φ1
A 5 mm spherical porous ceramic sintered body was prepared, sufficiently dried in advance, absorbed with a silicone resin solution, and dried under reduced pressure to 10 ^-6 torr by a drying apparatus equipped with a solvent recovery apparatus to remove volatile substances. . The amount of ceramics increased by this operation was 0.50 g per piece.

After inserting these two ceramics into a vacuum evaporation apparatus having a diameter of 800 mm,
Heat to 50 ° C. and evaporate. The thickness of the water-repellent film formed on the lenses of the glasses was measured to be 0.08 micrometers by an interference method. This is a thickness that sufficiently functions as a protective film. Perfluoroalkylsilazane has an unstable and easily decomposable portion, and is usually stored in a large amount of solvent. Since this is concentrated, stability becomes a problem. However, in the method of this embodiment, the chemical component of the ceramic sintered body and one part of perfluoroalkylsilazane are chemically bonded and stably held until evaporated by heating. You.

Example 3 A deammonified urethane monomer was used as a vapor-deposited substance which is an organic-based film-forming substance. The evaporation residue of this product was 25%. This product was crushed into an irregular shape, absorbed into a sufficiently dried porous ceramic, and dried using the drying apparatus used in Example 2. Ceramics by this operation 1.
The weight gain per gram was 0.2 grams or 20%. 2 grams of this ceramic was separated and the diameter was 80
After inserting into a 0 mm vacuum evaporation apparatus and performing a normal evaporation operation, it was heated to 80 ° C. to evaporate.

In order to promote the reaction on the object, the object was kept at 150 ° C. by another heating device. When the vacuum deposition apparatus was opened after the vapor deposition process, it was confirmed that ammonia odor was emitted and a deammonification reaction had occurred. The film thickness was measured by the interferometry to be 0.05 micrometers. This is a thickness that sufficiently functions as a protective film. There is a word called water contact angle in the number that is a measure of water repellency,
When perfluoroalkylsilazane is deposited, the temperature is reduced from 110 degrees or less in the conventional method to about 120 degrees in the method of the present invention.

[0024]

According to the present invention, the amount of the film-forming substance can be adjusted, the skilled artisan needs no skill in the vacuum deposition apparatus, and can always supply a fixed amount (even a small amount) of the film-forming substance, and put it in a container or the like for heating. Thus, a new method of using an organic film-forming substance that can be used more easily can be provided.

Cleaning Step The present invention can provide a vacuum vapor deposition method in which the coating step is a single step including the vapor deposition step, and further, fine adjustment for forming a film is not required.

The ratio of the amount of the film-forming substance contained in the ceramic sintered body can be adjusted by adjusting the size of the ceramic sintered body or the concentration of the solution when the ceramic sintered body is contained.
The number of objects to be processed by a single vacuum evaporation apparatus is substantially determined by the size of the vacuum evaporation apparatus for processing the same, especially by the diameter, and therefore the amount of the film-forming substance is also determined by the size of the vacuum evaporation apparatus. In the method of the present invention, a constant amount of the film-forming substance can be supplied according to the size of the vacuum deposition apparatus.
In particular, when the amount of the film-forming substance is very small, it is necessary to use only the film-forming substance to perform the measurement. There is no. Therefore, if a necessary number of ceramic sintered bodies are put into an evaporator in which a heating mechanism is adjusted so that the film-forming substance is completely eliminated, the necessary amount is evaporated even if a small amount is required.

Further, according to this method, it is easy to heat the object to be processed, so that it is possible to form a film by polymerizing on the object to be processed.

Further, since the protective film of the present invention is formed in the vapor deposition apparatus after the ordinary vacuum vapor deposition operation, the object to be processed is not taken out of the vapor deposition apparatus but is produced by taking it out. There is no need for a conventional cleaning step before the protective film forming process for cleaning dust and contamination. After the vapor deposition, the protective film is formed in the same vacuum vapor deposition apparatus, so that an intermediate cleaning step is not required, and the use of a solvent in the vapor deposition step is not required. The solvent is used only in the manufacturing process, and is easily recovered in this process, so that there is an advantage that the product carried out of the factory is completely solvent-free.

──────────────────────────────────────────────────続 き Continued on the front page (58) Field surveyed (Int.Cl. ⁶ , DB name) C23C 14/00-14/58 G02B 1/10

Claims (4)

(57) [Claims] 1. A vacuum deposition of an optical component, wherein an organic protective film is formed on the optical component by using a porous ceramic sintered body impregnated and solidified with an organic film-forming substance for an optical component. Method. 2. An optical component is vacuum-deposited with an inorganic deposition material in a vacuum deposition apparatus, and then impregnated and solidified with an organic film-forming substance for an optical component which can be vaporized in vacuum in the apparatus. 2. The method of claim 1, wherein the porous ceramic sintered body is heated to form an organic protective film. 3. The method according to claim 1, wherein the organic film-forming substance impregnated and solidified in the porous ceramics sintered body is polyethylene wax. 4. The method according to claim 1, wherein the organic film-forming substance impregnated and solidified in the porous ceramic sintered body is a silicone resin compound.