JPH0559563A - Film formation on one surface of planar body - Google Patents

Abstract

PURPOSE:To subject one surface of two sheets of planar bodies to a film forming treatment with excellent productivity by disposing these planar bodies to face each other apart a spacing, crimping an elastic packing material on the entire periphery at the end faces of the planar bodies and discharging the internal space of the two planar bodies to form a double-layered planar body, then subjecting the planar body to dipping film formation by the sol-gel method. CONSTITUTION:Two sheets of the planar bodies 1, 2, such as sheet glass, the surfaces of which are cleaned, are disposed to face each other apart the specified spacing in such a manner that the film forming surfaces exist on the outer side. The packing material 3 made of silicone rubber or the like provided with a tube 6 for suction having a valve 5 is gripped on the peripheral edge of the planar bodies on the spacing side to form the internal space between the two planar bodies 1 and 2. The internal space is internally evacuated to a reduced pressure by the suction tube 6 to form the double-layered planar body 7 having the hermetic reduced pressure space. This plate body is immersed into a sol-gel soln. and is dried and heat treated after pulling up to form the film by the sol-gel liquid on the outer surface of the two planar bodies 1 and 2. The plate body formed with the film only on one surface without being formed with the film on the internal space side surface of the double-layered plate body 7 is produced under the excellent productivity.

Description

Detailed Description of the Invention

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention is useful for forming a film on one surface of a plate-like body such as a glass plate or a resin plate by dipping by a wet method, especially a sol-gel method, etc. In particular, in a wide range of fields, such as UV-shielding glass, privacy glass, decorative glass, glass for copying machine top plate with transparent conductive film, architectural glass and related materials, vehicle glass or various optical glasses. This is a film forming method on one surface of a plate-like body that can be adopted.

[0002]

2. Description of the Related Art Conventionally, when a dipping film is formed by wet method such as a sol-gel method on one side of a plate-like body such as a plate glass or a resin plate, as a pre-processing operation, for example, both sides of the plate-like body are processed. In order to prevent the film from being covered, it is necessary to perform masking on one side and peel it off, or to perform manual work such as wiping one side after film formation on both sides of the plate-like body, or work close to it. Met.

The above-mentioned operations are very difficult and extremely complicated and require a lot of man-hours as the plate-shaped body of a large size such as a sheet glass for vehicles or a sheet glass for construction is used. It is inefficient, and it is likely to be unsafe if it is a little.In addition, it often happens that, for example, it leaks from the masking and stains the non-film-forming surface, and it is not perfect. However, it may not be said to be sufficient, because the quality may be deteriorated.

[0004]

The present invention has been made in view of the above-mentioned drawbacks of the prior art. For example, the masking or wiping is not necessary, and two plate-like bodies are simultaneously formed into a film. In addition, it is possible to drastically reduce stain removal work, etc. without surface scratches, it is easy to control the film thickness and improve quality, it is easy to line up and safety is improved, and it becomes more efficient on one side of plate A film forming method is provided.

That is, according to the present invention, when the film is formed by wet dipping on one surface of the plate-shaped body, the two plate-shaped bodies are opposed to each other with a space therebetween, and the edge of the plate-shaped body on the side of the facing surface is opposed. A packing material having suction ports at at least one location is sandwiched and / or gripped around the entire circumference or / and the entire end surfaces of the two plate-like bodies to form an internal space, and degassing is performed from the suction ports. The inner space is made into a double-layered glass like a decompressed closed space, and at the same time, a hanging jig is arranged to perform an integral hanging jig to perform the dipping operation to coat the film, followed by a drying operation or / And a film-forming method on one side of a plate-like body, characterized in that the heat-treatment operation is performed in the state of the double-layer glass or in a single plate state under reduced pressure. Also, in the above-mentioned double-layer glass-like internal space, a buffer spacer is provided in the internal space, wherein the film formation method on one side of the plate-like body is characterized.
Further, the film forming method on one surface of the plate-like body described above, characterized in that the suction port is provided at least at one place so as to be on the upper side of the double glazing. Furthermore, the packing material and the suspending tool are integrated, and by suspending the packing material, the multi-layer glass-like is suspended. Is.

[0006] Here, as described above, the reason why the packing material is used to form a double-layered glass in which two plate-like members are sandwiched under reduced pressure is that the sealing effect of the packing material is sufficiently exerted and the non-forming This is because it is possible to prevent the film surface from being soiled at all, and because two plate-shaped bodies can be simultaneously formed into a film, which leads to high productivity, and further, manual work such as attaching and detaching masking and removing dirt is unnecessary. This is because it is easy to make lines and labor is saved.

The packing material is silicone rubber, fluororubber, polyethylene, soft vinyl chloride, viton, butyl rubber, or the like, and is preferably silicone rubber or fluororubber (for example, sepular soft (made by Central Glass)). ..

In addition to the double-layer glass,
At the same time, it is possible to perform dipping operation with a hanging jig that deploys a hanging tool and is integrated.
This is because the film coated on the outer surface of the one plate-shaped body has uniform and uniform optical characteristics and does not cause defects such as scratches. Further, for example, the film-forming surface of the two plate-shaped bodies is Of course, even on the end face on the film-forming surface side, the above-mentioned optical characteristics are made uniform and uniform and the prevention of defects is made more effective by not contacting the above-mentioned suspending tool, and further, the above-mentioned packing material and the above-mentioned suspending tool. It is preferable to integrally or integrally integrate the packing material and the hanger and combine them with the hanging jig to substantially support the entire double glazing. It is more preferable to carry out vertical movement and transportation. Needless to say, for example, a conventional tongs-shaped hanging device can be used, or a pad plate or a rod can be provided on the lower part.

Further, when the internal space is formed and degassed from the suction port provided at at least one place to form a depressurized closed space, it is preferable to dispose the suction port at two places if possible on the upper side. The degree depends on the shape, size, thickness or weight of the plate glass, etc.
It is important to stop as much as possible so that surface deflection does not appear, and if it is large, it is necessary to provide a buffer spacer, for example, of the same thickness as the packing material in the internal space in order to reduce the pressure sufficiently. It is preferable for obtaining it.

Further, the plate-like body is an inorganic plate-like body such as a colorless or colored transparent plate glass or the like, and an organic plate-like body such as a resin plate such as a PC plate, for example, a flat plate or a plate having various shapes and sizes. Bent flat glass, further tempered glass or strength-up glass, etc., and can be used not only as a single plate but also as multi-layer glass.

[0011]

As described above, according to the present invention, a packing material having a suction port is provided at the peripheral edge portions of two plate-shaped members facing each other so as to form a double-layered glass, and a suspender is integrally provided. Then, by connecting to a hanging jig, for example, after dipping in a sol-gel solution and drying, a film is formed on one side of the plate by heat treatment, so that the sealing effect can be sufficiently exerted It can be said that it will never be soiled, and manual work such as wiping to remove stains and putting on and taking off masking is unnecessary, and moreover, two plate-like bodies can be simultaneously formed into a film and mechanized, so that the tact It is possible to increase the production efficiency and productivity, and it is easy to make a line and labor saving. It is easy to control the film thickness, the optical characteristics are uniform and uniform, and defects such as scratches are drastically reduced. A film forming method on one side of a plate-like body, which can be adopted and useful in a wide range of fields, including the sol-gel method, which improves work efficiency and safety and enables high quality and low cost. Is.

[0012]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS An embodiment of the present invention will be specifically described below with reference to the drawings. However, the present invention is not limited to the embodiment.

Example 1 FIG. 1 shows a method for forming a film on one surface of a plate-shaped body of the present invention.
FIG. 2 is a schematic perspective view showing an embodiment of a double-layer glass-like structure composed of two sheet glasses and a packing material, and FIG. 2 is a double-layer glass in the film forming method on one surface of the plate-shaped body of the present invention. FIG. 6 is a schematic perspective view showing an example of a configuration in which the above-mentioned and a hanging jig are integrated.

In order to form a half-mirror-like reflection film on one surface of a plate glass having a size of about 60 cm × 60 cm and a plate thickness of about 3.5 mm, two cleaned plate glasses 1 and 2 are prepared, and each has a predetermined film-forming surface. Were set at a predetermined interval so that they were on the outside (the non-film-forming surfaces faced each other), and the suction tube 6 and the tip of the tube were provided at at least one position on the peripheral edge of the glass on the interval side. A silicone rubber packing material 3 having a thickness of about 5 mm and a width of about 20 mm provided with a jig composed of a valve 5 is sandwiched, the two plate glasses 1 and 2 are pressed to form an internal space, and then the packing material is formed. The suction tube 6 provided in 3 is connected to a vacuum pump (not shown), and suction is performed until the internal pressure reaches 740 mmHg,
Immediately when the desired depressurized state is reached, the valve 5 is immediately closed, and the two plate glasses 1 and 2 are made into a depressurized closed space through the packing material 3 so that one set of double glazing 7 is formed. Hold it fixed.

Next, the two glass sheets of the multi-layer glass 7 are hung by the hanging jig 8 integrated with the hanging tool 9 with the suction port 4 side as the upper part, and then in a titania sol solution tank prepared from Ti-alkoxide. Gently soak in, then about 80m
The film was formed by slowly pulling it up at a constant speed of m / min. Furthermore, about 50 sheets of the two glass sheets like the laminated glass with the film
After being kept in a dry air flow at ° C for about 30 seconds to be sufficiently dried, the valve was opened and the two plate glasses were separated from each other by setting the atmospheric pressure between the two plate glasses. Then, each of the separated glass sheets was heat-treated at about 550 ° C. for about 30 minutes.

The obtained film-coated plate glass was a half mirror glass in which a titanium oxide film exhibiting a silvery reflection color tone was formed. In addition, the non-film-forming surface of the film-coated plate glass was clean without the liquid flowing around and causing contamination. The packing material could be used many times.

Embodiment 2 In FIGS. 2 and 3 to 4 described above, a weight adjusting weight and a buffer spacer are provided in an inner space like a double glazing in the film forming method on one side of the plate-shaped body of the present invention. It is a schematic perspective view which shows one Example of the structure.

The size is about 155 cm × 97 cm, and the plate thickness is about 2
In order to form a SiO ₂ .ZrO ₂ -based protective film having excellent chemical resistance on one surface of a base plate of a laminated glass for vehicles having a size of 2 mm, the two glass sheets 1 and 2 described above are manufactured in the same manner as in Example 1. The non-film-forming surfaces are opposed to each other at a predetermined interval, and the suction tube 6 and the attachment 11 arranged at the tip of the tube are provided at two positions on the upper side with a square in the peripheral edge along the shape of the plate glass. A square packing material 3 having a thickness of about 10 mm and a width of about 20 mm and made of an aluminum aggregate 12 with a thickness of about 5 mm covered with a silicon rubber sheet 13 is sandwiched between the jig and the jig. Of the glass sheets 1 and 2 and the packing material 3 are prevented from being inwardly dented by the decompression of the inner space, and the multi-layer glass-like 7 formed by the two glass sheets and the packing material is formed. Sometimes when immersed in the coating solution In order to prevent the double glazing 7 from rising due to the generated buoyancy, a SUS-made crossweight 14 having a thickness of 10 mm and a width of 25 mm is arranged in this internal space, and the weight 14 has a thickness at several positions on both sides. About 4-4.5 mm
The silicone rubber sheet 15 was attached and sandwiched as a buffer spacer. After that, the two suction attachments 11 provided on the packing material 3 are connected to a vacuum pump, and the suction operation is continued so that the internal pressure is maintained at about 740 to 745 mmHg. A sheet of glass sheet was hung with a tongs-like hanging jig with the suction port side as the upper part, then gently dipped in a SiO ₂ · ZrO ₂ sol solution tank, and then slowly pulled up at a constant speed of about 150 mm / min. A film was formed. Further, the two glass sheets having a double-layered glass structure with the film formed thereon were dried in a dry air stream at about 50 ° C for about 3 times.
After holding it for about 0 seconds to dry it almost completely, and carrying it in a suspended state to the inlet of the continuous firing furnace, suction by the pump was stopped, and the atmosphere was further released to separate the two glass sheets. Next, each of the separated plate glasses was placed in a furnace one by one with the film forming surface facing upward, and heat-baked at about 500 ° C. for about 20 minutes.

The obtained film-coated plate glass is colorless and transparent and
SiO with a folding rate of about 1.6₂・ ZrO ₂Protective film is formed
It was Further, as in Example 1, non-deposition of the plate glass with the film
The surface may be contaminated by the liquid and stain.
It was clean without anything.

Example 3 As shown in FIG. 5, the size is about 110 cm × 60 cm. ,
In order to form a ZnO film excellent in ultraviolet shielding performance on one surface of a vehicle bronze glass having a plate thickness of about 4 mm, two non-film-formed surfaces of the two plate glasses were formed in the same manner as in Examples 1 and 2. The suction tube 6 and the attachment 11 and the valve 5 arranged at the tip of the tube are provided in at least one place in a square shape along the plate glass shape in the gap. About 7mm, width about 40m
m packing material 3 made of fluorine-based rubber [for example, Cefral Soft (manufactured by Central Glass Co., Ltd.)] was sandwiched, and in this case, decompression was performed in the internal space formed by the two plate glasses 1 and 2 and the packing material 3. In order to prevent the two plate glasses 1 and 2 from denting inward, a buffer spacer 10 made of the same material as the packing material 3 and having the same width and thickness was held near the center of the glass. After that, the suction tube 6 provided on the packing material 3 is connected to a vacuum pump, and the internal pressure is 740 m.
Suction until reaching mHg, and when the desired depressurized state is reached, immediately close the valve and make the two plate glasses through the packing material into a depressurized closed space to form a set of double glazings 7. It is fixed and pinched.

Then, the two glass sheets like the multi-layer glass are hung by a hanging jig with the suction port side as an upper part,
Gently immerse in the ZnO sol solution bath, then 350 m
The film was formed by slowly pulling it up at a constant speed of m / min. Further, two sheets of glass sheet having a ZnO gel film-like double-layered glass formed on the outer surface of the sheet glass were kept in a dry air stream at about 50 ° C. for about 60 seconds to be almost dried, and then suspended. In this state, the sheet was conveyed to the inlet of the continuous firing furnace, and then the valve was opened to separate the two sheet glasses by setting the atmospheric pressure between the two sheet glasses. Then, each of the separated glass sheets was placed in a batch type hot air circulating furnace with the film forming surface facing upward and heat-treated at about 500 ° C. for about 30 minutes.

The obtained film-coated plate glass had a colorless and transparent film uniformly formed thereon and had a property of cutting primary blackening ultraviolet rays of 320 to 400 nm by 70% or more. Further, as in Examples 1 and 2, the liquid was clean without being contaminated by the liquid flowing into the non-film-forming surface of the film-coated plate glass.

FIG. 6 is a schematic perspective view showing one embodiment of the constitution of the packing material 3, the suspending tool 9 and the suspending jig 8 in the film forming method on one side of the plate-shaped body of the present invention. A suspending tool is provided so as to hold the packing material, and other various means such as the suspension tool may be embedded in the packing material.

Comparative Example 1 A SiO ₂ .ZrO ₂ film was formed on one surface of a laminated glass sheet for a vehicle used in Example 2 regardless of the method of the present invention. On the film formation surface,
A commercially available wide-sized (about 1.2 m wide) protective tape was evenly attached. After that, the film-forming surface that was soiled during the tape application work was wiped and washed with alcohol, and further blown with dry N ₂ gas.

The plate glass was suspended by a suspending jig, dipped in the same manner as in Example 2 to form a film, and after the coating film surface was sufficiently dried, the tape attached to the back surface was applied to the tape. The adhered solution was splashed and gently peeled off slowly so that it would not adhere to the non-film-forming glass surface and stain it. Then, the same heating operation as in Example 2 was performed to obtain a SiO ₂ .ZrO ₂ film-covered plate glass.

It is possible to prevent the above-mentioned liquid from entering the non-film-forming surface of the film-coated plate glass and causing contamination.
It wasn't always enough. Further, since the process is complicated and manual tape attachment and tape peeling operations are required, the manufacturing tact was several times as high as that of the method of the present invention such as the above-mentioned Examples, and the efficiency was inefficient. In addition, the peeled tape cannot be reused, resulting in an increase in cost.

[0027]

As described above, according to the present invention, two plate-like bodies are made of double-layer glass, and by connecting with a hanging jig and a hanging tool, dipping into a solution such as a sol-gel method, Since the film is formed by drying and heat treatment, masking, wiping, etc. are not required, and productivity, safety, quality, etc. are dramatically improved, and cost is reduced, making it easy to form a line. It has a number of effects such as labor saving, especially UV glass, privacy glass, decorative glass, glass for copier with transparent conductive film, glass for construction, related glass, vehicle glass and various optics. The present invention provides a film forming method on one surface of a plate-like body that can be used in a wide range of fields such as glass for use in glass.

[Brief description of drawings]

FIG. 1 is a view showing a method for forming a film on one surface of a plate-shaped body according to the present invention.
FIG. 3 is a schematic perspective view showing an example of a double-layer glass-like configuration composed of two sheet glasses and a packing material.

FIG. 2 is a view showing a method for forming a film on one surface of a plate-shaped body according to the present invention,
FIG. 3 is a schematic perspective view showing an example of a structure in which a double glazing and a hanging jig are integrated.

FIG. 3 is a view showing a method for forming a film on one surface of a plate-shaped body according to the present invention.
The schematic perspective view which shows one Example of the structure which arrange | positioned the weight and the buffer spacer which stuck the spacer to this weight in the internal space like double-glazed glass.

FIG. 4 is a view showing a method for forming a film on one surface of a plate-shaped body according to the present invention.
The schematic perspective view which shows one Example of a structure in a packing material.

FIG. 5 is a view showing a method for forming a film on one surface of a plate-shaped body according to the present invention.
The schematic perspective view which shows the other Example of the structure which provided the buffer spacer.

FIG. 6 is a view showing a film forming method on one surface of a plate-shaped body according to the present invention,
The schematic perspective view which shows other one Example about the structure of a packing material, a hanging tool, and a hanging jig.

[Explanation of symbols]

 1 Plate Glass 2 Plate Glass 3 Packing Material 4 Suction Port 7 Multi-Layered Glass 8 Hanging Jig 10 Buffer Spacer 12 Aggregate 13 Silicon Rubber Sheet 14 Weight 15 Silicon Rubber Sheet

─────────────────────────────────────────────────── ─── Continuation of the front page (51) Int.Cl. ⁵ Identification code Internal reference number FI Technical display location C03C 17/25 B 7003-4G G02B 1/10 Z 7820-2K // B05C 3/09 9045-4D C23C 18/31 B 8414-4K

Claims (4)

[Claims] 1. When forming a film by wet dipping on one surface of a plate-like body, two plate-like bodies are opposed to each other with a space therebetween, and the entire circumference of an end face-side edge of the plate-like body or / And, an inner space is formed by sandwiching and / or grasping a packing material having suction ports at at least one location around the entire circumferences of the end faces of the two plate-like bodies, and the inner space is degassed from the suction ports. While making it like a double-layered glass with a reduced pressure closed space, at the same time, a hanging jig is provided to integrally perform a dipping operation to coat the film, and then a drying operation and / or a heat treatment operation. A method for forming a film on one surface of a plate-like body, characterized in that the film is formed by applying the film in the state of the double glazing or in a single plate state under reduced pressure. 2. In the inner space of the double glazing,
The film forming method on one side of the plate-like body according to claim 1, wherein a buffer spacer is provided in the internal space. 3. The method for forming a film on one surface of a plate-like body according to claim 1, wherein the suction port is provided at least at one position so as to be on the upper side of the double glazing. 4. The film formation on one surface of the plate-like body according to claim 1, wherein the packing material and the hanging tool are integrated and the packing material is hung to hang the double-layered glass-like material. Law.