JPH10193489A - Thin film forming material and forming method for thin film - Google Patents

Abstract

PROBLEM TO BE SOLVED: To form a homogeneous thin film for effectively and stably realizing desired characteristics on a base material in simple steps by holding thin film forming substance on a porous material made of normal temperature curable substance. SOLUTION: After water is added to gypsum and agitated, it is cast in a plastic casting mold 1 and dried at ambient temperature. The gypsum 2 in the mold 1 is impregnated with water-repellent treating solution containing perfluoroalkyl group-containing compound. Further, the gypsum 2 is dried, for example, at 70 deg.C, then removed from the mold 1, and installed in a vacuum tank 4 of a vacuum deposition unit. Then, a synthetic resin lens 7 to become base material to be deposited is set in the tank 4. An electron beam 11 is emitted to a sample by an electron beam depositing method by using an electron gun 8 and ZrO2 , 9, SiO2 10 provided oppositely, an SiO2 thin film and ZrO2 thin film are alternately laminated to obtain a lens with an antireflection film.

Description

DETAILED DESCRIPTION OF THE INVENTION

[0001]

BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a material used for surface treatment of a base material or a coat film on the base material, and a method of forming a thin film as the surface treatment.

[0002]

2. Description of the Related Art In performing a surface treatment for imparting functions such as antifouling, waterproofing, and dustproofing to the surface of various substrates, the surface of the substrate is made of an organic material having the above-described functions such as antifouling and waterproofing. It is widely practiced to provide a thin film. As a method for forming such a thin film, for example, a method in which a water-repellent substance diluted in an organic solvent is directly applied to a base layer formed on a substrate (Japanese Patent Application Laid-Open No. 60-40254), Method of immersing a substrate (lens)
30902) are known. Also, a method of evaporating an organic substance impregnated in porous ceramics in a vacuum chamber to form a protective film on a substrate (Japanese Patent Laid-Open No. 4-72055), a method of depositing an organic substance impregnated in a fibrous metal lump in a vacuum chamber A method of forming an organic coating film on an inorganic coating film by evaporating the coating film in an atmosphere (Japanese Patent Laid-Open No. 6-340966) is known.

[0003]

However, each of the above-mentioned various thin film forming methods has the following disadvantages.

In the method of directly applying a water-repellent substance to a substrate, the uniformity of the obtained coating film may not always be sufficient. In particular, when the coating is performed on an inorganic thin film formed by a vacuum process such as vacuum deposition, a vacuum process (a deposition process)
The substrate on which the inorganic thin film has been formed is once taken out of the vacuum chamber and then applied again in another step, so that the process is complicated and the coating film tends to be uneven, and it is difficult to obtain a uniform water-repellent thin film.

[0005] The immersion method also requires a similar complicated process, especially when coating is performed on an inorganic thin film formed in a vacuum process, and requires a dilute solution many times the required amount. Waste liquid treatment facilities and treatment costs for not discharging to the environment are required.

In the method of evaporating an organic substance impregnated in ceramics, steps such as pressing and high-temperature sintering are required to form the ceramics, and the porosity of the ceramics is reduced to control the amount of the organic substances impregnated. Needs to be adjusted. Therefore, it is required to precisely control the particle size, sintering temperature, purity, and the like of the ceramics, which leads to complicated material preparation steps and increased costs.
In addition, an organic binder is often used for preparing the ceramic itself. In this case, when an organic substance (an organic binder or a decomposition product thereof) remains, a film-forming material (for example, an organic silicone or a perfluoroalkyl group) impregnated in the ceramic is used. Or the like, and reacts with or evaporates together and adheres to the substrate to be treated, thereby deteriorating the properties of the obtained thin film, such as a decrease in contact angle, and making it impossible to obtain desired antifouling and waterproofing effects.

The method of evaporating an organic substance impregnated in a fibrous metal lump is simpler than the other methods described above. However, particularly when copper, aluminum, or the like is used as the metal material, the melting point of these metals is 600 ° C. to 800 ° C., and depending on the adjustment of the heating conditions, the metal lump melts or the dissolved metal itself evaporates. It may adhere to the substrate, and may rarely adversely affect the properties of the obtained thin film, such as coloring and lowering the contact angle. Further, since the metal has a high thermal conductivity, the temperature rise during heating is very fast, and it may be necessary to adjust the evaporation amount of the impregnated organic substance with high accuracy.

[0008] The present invention has been made in view of the above-mentioned problems, and it is an object of the present invention to provide desired properties, particularly, antifouling, dustproof, water repellent, and oil repellent on a substrate by a simple process. It is an object of the present invention to provide a thin film forming material and a thin film forming method capable of forming a homogeneous thin film capable of effectively and stably realizing such functions.

[0009]

Means for Solving the Problems The thin film forming material of the present invention comprises:
It is characterized in that a thin film forming substance is held on a porous material made of a room temperature curable substance.

The thin film forming method of the present invention is characterized in that a thin film forming substance impregnated in a porous material made of a room temperature curable substance is evaporated to form a thin film on a substrate.

[0011]

BEST MODE FOR CARRYING OUT THE INVENTION The thin film forming material of the present invention is a porous material in which a thin film forming material is held, and the thin film forming material is preferably used to be deposited on a substrate by evaporation or the like. The thin film forming material of the present invention is characterized in that a room temperature curable substance is used as the material of the porous material.

In the present invention, the term "room temperature curable substance" refers to, for example, a powdery substance, which is cured by adding water or an alcohol containing water and treating (eg, heating) in a temperature range of room temperature to about 100 ° C. Substance. However, especially due to the heat generated by the substance itself during the curing reaction during the curing process, 100
It also includes substances having a temperature exceeding ℃.

As the cold-curable substance, a porous substance that is preferably cured by water (or alcohol containing water) is used as described above. Specifically, for example, inorganic glue substances such as Portland cement and alumina cement, and inorganic porous substances such as gypsum (calcium sulfate), lime (calcium oxide or calcium hydroxide), and zinc oxide can be used. In particular, considering the ease of preparing a porous material such as a short curing time, a simple component configuration, and easy control of the particle size affecting the porosity of the porous material after curing, gypsum, It is desirable to use gypsum having a particle size distribution of about 1 to 100 μm as measured by a centrifugal sedimentation method.

The above-mentioned cold-setting substance is cured with water and then impregnated with a thin-film forming substance. When the thin-film forming substance is water-soluble and can be diluted with water, the cold-setting substance is directly added to the aqueous solution. It is also possible to solidify and dry the room-temperature-curable substance and simultaneously prepare a thin-film forming material impregnated with the thin-film forming substance. Further, when the substrate on which the thin film is formed (substrate to be treated) is made of a material which dislikes moisture in particular, a room temperature curable substance is used in order to reduce the incorporation of moisture into the thin film formed on the substrate. After solidifying with water, the film may be dried at 150 ° C. to 700 ° C. to evaporate the water, and then impregnated with a thin film forming substance to prepare a thin film forming material with a reduced amount of water.

Further, in the porous material made of the above-mentioned cold-setting material, 70% by weight or less of another material which is not hardened at normal temperature is adjusted so as to adjust the void so that the thin-film forming material is contained in the void. May be mixed with powder of an inorganic substance such as quartz having a particle size of 0.5 mm or less in an amount of about 70% by weight or less.

In the case where gypsum is used as a cold-setting material, in order to form voids so as to contain a necessary amount of a thin film-forming substance, water is mixed with ca. It is desirable to prepare.

The thin film forming substance used in the thin film forming material of the present invention is selected according to the function required for the thin film to be formed. For example, in a thin film forming material used for performing a surface treatment that imparts functions such as water repellency, oil repellency, and dust resistance to a base material, a material capable of imparting these functions in a thin film state is formed into a thin film. Apply substance.

In particular, as the thin film forming substance imparting water repellency, for example, a water repellent organic material such as an organosiloxane compound or a perfluoroalkyl group-containing compound can be suitably used. Specific examples of such organosiloxane compounds include diethoxydimethylsilane,
Other than triethoxymethylsilane, etc., JP-A-61-130
902. Further, specific examples of the perfluoroalkyl group-containing compound include 2- (perfluorooctyl) ethyltriaminosilane and 2- (perfluorohexyl) ethyltriaminosilane, and are described in JP-A-63-296002. A perfluoroalkyl group-containing compound is exemplified. In addition, a silane compound such as chlorotriethylsilane can be used. These compounds may be used alone or in combination of two or more.

The above-mentioned thin film-forming substance, in particular, an organic silicone compound or a compound containing a perfluoroalkyl group, is generally supplied in the form of a stock solution or a solution diluted with a solvent. Then, a stock solution or solution containing these substances is directly immersed in a porous material made of a hardened room-temperature-curable material as described above, or a method of dropping and impregnating the stock solution or solution in a required amount with a pipette, or A method of solidifying a cold-setting material directly in the form of a solution, particularly an aqueous solution (when the thin-film forming material is water-soluble). Prepare.

In the present invention, the thin film forming substance held in the above thin film forming material is evaporated and deposited on a predetermined substrate to form a thin film, and a desired function is imparted to the surface of the substrate. .

As a specific example, a thin film forming material using a water repellent material as the above thin film forming material is used.
The water-repellent substance is heated and evaporated in a vacuum, and the water-repellent substance is deposited directly on the surface of the substrate or on a coating such as an inorganic coat film formed on the substrate to form a water-repellent thin film. Provides water repellency to the surface.

Here, as a method for evaporating the thin film-forming substance, a method using halogen lamp heater heating or resistance heating in air or under reduced pressure is applied. Preferably, a method of heating the thin film forming material in a closed system such as in a vacuum chamber is used.

The conditions for evaporating the thin film forming substance in a vacuum are preferably determined as appropriate according to the type and state of the thin film forming substance and the base material. For example, an inorganic coated thin film such as SiO ₂ on a plastic base material is preferable. When a thin film is formed by heating and evaporating and depositing a water-repellent substance on the optical lens on which is formed, it is more preferable to perform the process at a degree of vacuum of 10 ^-6 to 10 ^-3 Torr.

In the present invention, the substrate on which the thin film is formed is not particularly limited. For example, in the case of forming a water-repellent thin film using a water-repellent thin film-forming substance, there is no particular limitation as long as the outermost surface is a coat film made of an inorganic substance. And a glass lens, a plastic lens, an optical filter, an automobile windshield, and a display panel on which an inorganic antireflection film is formed.

[0025]

DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Hereinafter, the present invention will be described in more detail with reference to the drawings and embodiments, but the present invention is not limited to the following.

(Example 1) Gypsum (manufactured by San-Esu Gypsum Co., Ltd.
Trade name: calcined gypsum / particle size distribution 5-50 μm) 50 g in water 2
After adding 5 g and stirring well for 1 minute, this was mixed with a plastic mold 1 having a diameter of 18 mm and a depth of 10 mm as shown in FIG.
And dried for 1 hour at room temperature. The gypsum 2 in the mold 1 has the chemical formula nC ₈ F ₁₇ CH ₂ CH ₂ Si (N
A perfluoroalkyl group-containing compound represented by H ₂ ) ₃ was diluted with meta-xylene hexafluoride to 3% and impregnated with 1 ml of a water-repellent solution using a pipette. Further, after the gypsum 2 was dried at 70 ° C. for 20 minutes, it was taken out of the mold 1 and placed in a vacuum tank of a vacuum evaporation apparatus (Sincron VE800 / Sincron). That is, as shown in FIG. 2, the resistance heating boat 6 is installed on the resistance heating boat 6 in the structure where the resistance heating board 6 is installed between the resistance heating electrodes 5 provided in the vacuum chamber 4 of the vacuum evaporation apparatus 3. Plaster 2 was installed.

Next, in the vacuum chamber 4, a synthetic resin lens 7 made of diethylene glycol bisallyl carbonate resin as a base material to be deposited was set. Then, the electron gun 8 provided opposite thereto and ZrO as a vapor deposition sample are used.
₂ 9, a SiO ₂ 10 using, by an electron beam evaporation method (by irradiating an electron beam 11 on the sample) Si on the lens 7
The O ₂ thin film and the ZrO ₂ thin film are alternately formed from the substrate side with a SiO ₂ film of about 3 μm, a ZrO ₂ film of about 0.015 μm,
O ₂ film about 0.02 μm, ZrO ₂ film about 0.1 μm, SiO
_Two films were laminated so as to have a thickness of about 0.08 μm to obtain a lens with an antireflection film.

Subsequently, after forming the anti-reflection film, the synthetic resin lens 7 is not taken out of the vacuum chamber 4 but is previously set on the resistance heating boat 6 to form a thin film forming material (gypsum holding the thin film forming substance). 2 was heated at about 500 ° C. for 3 minutes to evaporate the perfluoroalkyl group-containing compound, and a water-repellent thin film was formed on the antireflection film of the lens by vapor deposition.

After the vapor deposition, the synthetic resin lens 7 was taken out, the state of the surface was observed, and the contact angle of the surface with water was measured using a CA-Z type contact angle meter manufactured by Kyowa Interface Science. After the measurement, a weight of about 1 kg was applied to the lens paper containing acetone and rubbed 50 times back and forth, and then the contact angle was measured again to observe the change. After the synthetic resin lens 7 was left in the air for one week, the surface was observed and the contact angle was measured in the same manner as described above. The results are shown in Table 1 below.
Shown in

Example 2 Gypsum (manufactured by San-Esu Gypsum Co., Ltd.)
Trade name: calcined gypsum / particle size distribution 5-50 μm) 50 g in water 2
After adding 5 g and stirring well for 1 minute, this was mixed with a plastic mold 1 having a diameter of 18 mm and a depth of 10 mm as shown in FIG.
And dried at room temperature for 1 hour, and further heated at 200 ° C. for 1 hour in an oven to evaporate water. The gypsum in the mold 1 has a chemical formula of nC ₈ F ₁₇ CH ₂ CH ₂ Si
A perfluoroalkyl group-containing compound represented by (NH ₂ ) ₃ was diluted to 3% with meta-xylene hexafluoride and impregnated with 1 ml of a water-repellent solution using a pipette.
Further, the gypsum 2 was dried at 70 ° C. for 20 minutes, taken out of the mold, and set on the resistance heating board 6 in the vacuum chamber 4 of the vacuum evaporation apparatus (Sincron VE800) 3 shown in FIG.

Subsequently, according to the same procedure as in Example 1, the anti-reflection film ((Si
After forming a laminated film of O ₂ and ZrO ₂ ), a water-repellent thin film was further formed by a vacuum evaporation method using the thin film forming material (2) provided on the resistance heating board (6). About the surface on the side where the thin film of the lens thus obtained was formed, Example 1
Observation and the contact angle with water were measured and evaluated in the same manner as in (1) immediately after the formation of the water-repellent film and after standing in the air for one week. The results are shown in Table 1 below.

(Example 3) Gypsum (manufactured by San-Esu Gypsum Co., Ltd.
Trade name: calcined gypsum / particle size distribution 5 to 50 μm) 50 g of CF
25 g of a 3% aqueous solution of ₃ (CH ₂ ) ₂ SiCl ₃ was added and stirred well for 1 minute.
After pouring into a plastic mold 1 having a depth of 10 mm and drying at room temperature for 1 hour, it was taken out of the mold and
Similarly to FIG. 2, the vacuum deposition apparatus 3 (Sincron VE) shown in FIG.
800) in a vacuum chamber 4 (FIG. 2).
Reference).

Subsequently, according to the same procedure as in Example 1, the anti-reflection film (SiO 2) was formed on the synthetic resin lens (7) by vacuum evaporation.
After forming a laminated film of ZrO ₂ and ZrO ₂ ), a water-repellent thin film was formed by vacuum evaporation using the thin film forming material (2) provided on the above-mentioned resistance heating board (6). Observation and the contact angle with water were measured and evaluated on the surface of the lens thus obtained on which the thin film was formed in the same manner as in Example 1 (immediately after the formation of the water-repellent film and after leaving it in the air for one week). The results are shown in Table 1 below.

Example 4 Gypsum (manufactured by San-Esu Gypsum Co., Ltd.
Trade name: calcined gypsum / particle size distribution 5-50 μm) 50 g in water 2
After adding 5 g and stirring well for 1 minute, this was mixed with a plastic mold 1 having a diameter of 18 mm and a depth of 10 mm as shown in FIG.
And dried at room temperature for 1 hour, and further heated in an oven at 200 ° C. for 1 hour to evaporate water. The gypsum in the mold 1 has a chemical formula of nC ₈ F ₁₇ CH ₂ CH ₂ Si
A perfluoroalkyl group-containing compound represented by (OCH ₃ ) ₃ (not diluted) was impregnated with 0.5 ml using a pipette. Further, the gypsum was taken out of the mold, dried at 70 ° C. for 20 minutes, and then placed on the resistance heating board 6 in the vacuum chamber 4 of the vacuum evaporation apparatus (Sincron VE800) 3 shown in FIG.

Subsequently, according to the same procedure as in Example 1, the anti-reflection film (SiO 2) was formed on the synthetic resin lens (7) by vacuum evaporation.
After forming a laminated film of ZrO ₂ and ZrO ₂ ), a water-repellent thin film was formed by vacuum evaporation using the thin film forming material (2) provided on the above-mentioned resistance heating board (6). Observation and the contact angle with water were measured and evaluated for the surface of the lens thus obtained on which the thin film was formed in the same manner as in Example 1 (immediately after the formation of the water-repellent film and after leaving it in the air for one week). The results are shown in Table 1 below.

(Example 5) In accordance with the same procedure as in Example 1, an antireflection film (SiO 2) was formed on the synthetic resin lens (7) by vacuum evaporation.
₂ and a layered film of ZrO ₂ ), taken out of the vacuum chamber, and added to the chemical formula nC ₈ F ₁₇ CH ₂ CH ₂ Si (NH ₂ ).
Perfluoroalkyl group-containing compound solution for water repellent treatment was diluted to 3% metaxylene hexafluoride represented by ₃ was coated directly with a brush. Observation and the contact angle with water were measured and evaluated for the surface of the lens thus obtained on which the thin film was formed in the same manner as in Example 1 (immediately after the formation of the water-repellent film and after leaving it in the air for one week). The results are shown in Table 1 below.

After leaving the lens of this example for one week, cloudiness occurred on a part of the surface, and the lens could not be used as a spectacle lens or the like. This is considered to be because the water-repellent substance was applied to the lens, so that the substance adhered excessively thickly, and the functional groups in the substance reacted with moisture in the atmosphere to produce cloudiness.

(Example 6) In accordance with the same procedure as in Example 1, an anti-reflection film (SiO 2) was formed on the synthetic resin lens (7) by vacuum evaporation.
₂ and ZrO ₂ ) are formed, taken out of the vacuum chamber, and taken out of the chemical formula nC ₂ F ₁₇ CH ₂ CH ₂ Si (NH ₂ ).
_The perfluoroalkyl group-containing compound represented by 3 was directly immersed in a solution for water-repellent treatment diluted to 3% with meta-xylene hexafluoride. Observation and the contact angle with water were measured and evaluated for the surface of the lens thus obtained on which the thin film was formed in the same manner as in Example 1 (immediately after the formation of the water-repellent film and after leaving it in the air for one week). The results are shown in Table 1 below.

After leaving for one week, the surface of the lens of this example became cloudy on a part of the surface, and was unusable as a spectacle lens or the like. This is because the lens was directly immersed in the solution of the water-repellent substance, so that the water-repellent substance adhered to the lens excessively thickly, and the functional groups in the substance reacted with atmospheric moisture to produce white turbidity. Conceivable.

(Example 7) A copper container having a diameter of 18 mm and a depth of 10 mm was filled with steel wool, and this was filled with the chemical formula nC.
_A perfluoroalkyl group-containing compound represented by ₈ F ₁₇ CH ₂ CH ₂ Si (NH ₂ ) ₃ was diluted to 3% with meta-xylene hexafluoride and impregnated with 1 ml of a solution for water-repellent treatment using a pipette. . Furthermore, after drying this at 70 ° C. for 20 minutes, the vacuum evaporation apparatus (SYNCHRON VE80) used in Example 1 was used.
0) It was set on the resistance heating board 6 (see FIG. 2) in the vacuum chamber 4 of 3.

Subsequently, according to the same procedure as in Example 1, an antireflection film (SiO ₂ and Z
After forming the rO ₂ laminated film), the thin film forming material (2) provided on the resistance heating board (6) described above is further used,
A water-repellent thin film was formed by a vacuum deposition method. Observation and a contact angle with respect to water were measured and evaluated for the surface of the lens thus obtained on which the thin film was formed in the same manner as in Example 1 (immediately after forming the water-repellent film and after leaving it in the air for one week). The results are shown in Table 1 below.

After the formation of the water-repellent thin film by vacuum evaporation, a very small amount of copper used as the thin film forming material adhered to the resistance heating board. This is presumably due to the very small amount of melting of the copper container.

(Example 8) A copper container having a diameter of 18 mm and a depth of 10 mm was filled with steel wool, and this was filled with the chemical formula nC.
_A perfluoroalkyl group-containing compound represented by ₈ F ₁₇ CH ₂ CH ₂ Si (NH ₂ ) ₃ was diluted to 3% with meta-xylene hexafluoride and impregnated with 1 ml of a solution for water-repellent treatment using a pipette. . After drying at 70 ° C. for 20 minutes, the steel wool was taken out of the copper container and placed on the resistance heating board 6 (see FIG. 2) in the vacuum chamber 4 of the vacuum evaporation apparatus (Sincron VE800) 3 used in Example 1. installed.

Subsequently, according to the same procedure as in Example 1, an anti-reflection film (SiO ₂ and Z
After forming the rO ₂ laminated film), the thin film forming material (2) provided on the resistance heating board (6) described above is further used,
A water-repellent film was formed by a vacuum deposition method. Observation and the contact angle with water were measured and evaluated on the surface of the obtained lens on which the film was formed in the same manner as in Example 1 (immediately after the formation of the water-repellent film and after leaving it in the air for one week). In the example, in the process of forming the water-repellent thin film, the steel wool moves on the resistance heating board due to the flow of the air exhausted during the vacuum evacuation, and it is difficult to stably hold the steel wool. It could not be obtained uniformly.

Example 9 Commercially available Portland cement (deer)
Portland cement made of island concrete, trade name: particle size
(Distribution is 1 to 30 μm) Add 20 g of water to 50 g and 1 minute
After stirring well, 18mm in diameter as shown in Fig. 1
Pour into a 10 mm plastic mold and add
Dried at 200 ° C for 1 hour in an oven.
Heat to evaporate water. Cement in such a mold 1
Has the chemical formula nC₈F₁₇CH_TwoCH _TwoSi (NH_Two)_ThreeIn table
Perfluoroalkyl group-containing compound
Solution for water repellent treatment diluted to 3% with hexafluorofluoride
Was impregnated with 1 ml using a pipette. Furthermore, cement
(2) is dried at 70 ° C. for 20 minutes, taken out of the mold, and
1, the vacuum evaporation apparatus (Sincron VE) shown in FIG.
800) installed on the resistance heating boat 6 in the vacuum chamber 4
did.

Subsequently, according to the same procedure as in Example 1, an antireflection film (SiO 2) was formed on the synthetic resin lens (7) by vacuum evaporation.
₂ and ZrO ₂ ), and then a water-repellent thin film is formed by a vacuum evaporation method using the thin film forming material (2) provided on the resistance heating boat (6). The surface on the formed side was evaluated in the same manner as in Example 1. The results are shown in Table 1 below.

(Example 10) 50 g of gypsum (manufactured by San-Esu Gypsum Co., Ltd., trade name: calcined gypsum / particle size distribution of 5 to 50 μm) and silicon dioxide powder (manufactured by Kishida Chemical, trade name: Siliconoxide: particle size of about 35 μm or less) ) After adding 25g of water to 10g and stirring well for 1 minute,
A part thereof is 18 mm in diameter and 10 m in depth as shown in FIG.
m, poured into a plastic mold, dried at room temperature for 1 hour, and further heated in an oven at 200 ° C. for 1 hour.
The water was evaporated. The gypsum in the mold 1 has a chemical formula n
The solution was 1ml impregnated with a pipette to the _{-C 8 F 17 CH 2 CH 2} Si (NH 2) 3 perfluoroalkyl group-containing compound represented by the diluted metaxylene hexafluoride 3% was for water repellent treatment Was. Further, the gypsum 2 was dried at 70 ° C. for 20 minutes, taken out of the mold, and set on the resistance heating boat 6 in the vacuum tank 4 of the vacuum evaporation apparatus (Sincron VE800) shown in FIG.

Subsequently, according to the same procedure as in Example 1, the anti-reflection film (SiO 2) was formed on the synthetic resin lens (7) by vacuum evaporation.
₂ and ZrO ₂ ), and then a water-repellent thin film is formed by a vacuum evaporation method using the thin film forming material (2) provided on the resistance heating boat (6). The surface on the formed side was evaluated in the same manner as in Example 1. The results are shown in Table 1 below.

[0049]

[Table 1]

According to the results shown in Table 1, the thin-film forming material in which the water-repellent substance is held by gypsum (Examples 1 to 4), the thin-film forming material in which the water-repellent substance is held by portland cement (Example 9), Alternatively, using a thin film forming material (Example 10) in which a water-repellent substance is held in gypsum containing fine powder (silicon dioxide),
The water-repellent thin film formed on the surface of the synthetic resin lens (with an anti-reflection film) by the vacuum evaporation method reduces the change in the contact angle to water due to the influence from the outside, that is, the change in the water repellency, and obtains stable characteristics. Have been.

Further, in the thin film forming materials as in Examples 1 to 4, 9, and 10, the porous material made of the room temperature curable material stably holds the thin film forming material supplied in all forms, and Also in the vapor deposition process, it can be easily installed and used in the apparatus.

[0052]

As described in detail above, according to the present invention,
A thin film forming material is provided in which a thin film forming material is held on a porous material made of a room temperature curable substance. Using such a thin film forming material, on a predetermined base material, by a simple operation at low cost,
High quality thin films can be obtained.

[Brief description of the drawings]

FIG. 1 is a cross-sectional view schematically showing a state in which gypsum is filled in a plastic mold during preparation of a thin film-forming material according to an embodiment of the present invention.

FIG. 2 is a diagram showing a structure of a vacuum evaporation apparatus used in an embodiment of the present invention.

[Description of Signs] 1 Plastic mold 2 Gypsum, cement (thin film forming material) 3 Vacuum deposition device 4 Vacuum tank 5 Resistance heating electrode 6 Resistance heating board 7 Lens 8 Electron gun 9 ZrO ₂ 10 SiO ₂ 11 Electron beam

──────────────────────────────────────────────────の Continued on the front page (51) Int.Cl. ⁶ Identification code FI G09F 9/30 312 G02B 1/10 Z

Claims (14)

[Claims] 1. A thin film forming material in which a thin film forming material is held on a porous material made of a room temperature curable substance. 2. The thin film forming material according to claim 1, wherein the thin film forming material is a water-repellent organic material. 3. The thin film forming material according to claim 2, wherein the water-repellent organic substance is an organic silicone compound or a perfluoroalkyl group-containing compound. 4. The thin film forming material according to claim 1, wherein the room temperature curable substance is a substance that is cured by water. 5. The thin film-forming material according to claim 1, wherein the cold-setting material comprises cement. 6. The thin film-forming material according to claim 1, wherein the room temperature curable substance comprises gypsum. 7. The thin film-forming material according to claim 6, wherein the gypsum has a particle size distribution of 5 to 50 μm. 8. The thin film forming material according to claim 1, wherein the porous material made of the room temperature curable substance is mixed with a substance which does not cure at room temperature of 70% by weight or less. 9. The thin film forming material according to claim 1, wherein the porous material made of the room temperature curable substance is cured in a state containing water or a water-soluble water repellent substance. 10. A thin film forming method for forming a thin film on a substrate by evaporating a thin film forming substance held in a porous material made of a room temperature curable substance. 11. The thin film forming method according to claim 10, wherein the thin film forming material is made of a water repellent organic substance, and a water repellent thin film is formed on a substrate. 12. The thin film forming method according to claim 10, wherein a thin film is formed on a layer made of an inorganic substance formed on a base material. 13. The method according to claim 10, wherein the thin film is formed in a vacuum chamber. 14. The thin film forming method according to claim 12, wherein a layer made of the inorganic material is formed on the substrate in a vacuum chamber, and a water-repellent thin film is formed on the inorganic material layer in the same vacuum chamber. .