Method for storing vapor deposition source, and method for manufacturing spectacle lens

Abstract

The purpose of this disclosure is to provide a method for storing a vapor deposition source, with which outgas is hardly generated from the vapor deposition source when using the vapor deposition source after storage. In this method for storing a vapor deposition source, a vapor deposition source including a base material having a gap and a silane coupling agent having an amino group impregnated in the base material having a gap is stored under a condition wherein a storage temperature is 5°C or less.

Description

Method for storing evaporation sources and method for manufacturing eyeglass lenses

[0001] The present disclosure relates to a method for storing a vapor deposition source and a method for manufacturing an eyeglass lens.

[0002] Various coatings have been investigated for various lenses including spectacle lenses. For example, Patent Document 1 below discloses a method for manufacturing a mold having an optical surface with an anti-reflection coating that can be transferred to the optical surface of a lens, in which a layer of a silane coupling agent is formed by vapor deposition.

[0003] Patent No. 5987117

[0004] The present disclosure relates to a method for storing a vapor deposition source, which comprises storing a vapor deposition source including a substrate having voids and a silane coupling agent having an amino group impregnated into the substrate having voids at a storage temperature of 5° C. or less. The present disclosure also relates to a method for manufacturing an eyeglass lens.

[0005] 1 is a cross-sectional schematic view showing one embodiment of a vapor deposition source stored by a vapor deposition source storage method according to the present disclosure.

[0006] The method for storing a vapor deposition source according to the present disclosure will be described in detail below. When storing a vapor deposition source, it is desirable that outgassing from the vapor deposition source is less likely to occur when the vapor deposition source is used after storage. According to the method for storing a vapor deposition source according to the present disclosure, outgassing from the vapor deposition source is less likely to occur when the vapor deposition source is used after storage. Note that there are cases where the vapor deposition source is not used immediately after preparation, and it has been desirable that outgassing from the vapor deposition source is less likely to occur even when the vapor deposition source is not used immediately after preparation but is used after storage. In addition, the method for manufacturing eyeglass lenses according to the present disclosure will be described in detail later. Note that in this disclosure, the symbol "to" is used to mean that the numerical values ​​written before and after it are included as the lower limit and upper limit. In addition, in this disclosure, the refractive index is the refractive index at the e-line.

[0007] <Method for storing vapor deposition source> In the method for storing a vapor deposition source according to the present disclosure (hereinafter also referred to as the "storage method according to the present disclosure"), a vapor deposition source (hereinafter also simply referred to as an "impregnated vapor deposition source") including a porous substrate and a silane coupling agent having an amino group (hereinafter also referred to as an "aminosilane coupling agent") impregnated into the porous substrate is stored at a storage temperature of 5°C or less. FIG. 1 is a schematic cross-sectional view showing one embodiment of a vapor deposition source stored according to the storage method according to the present disclosure. The impregnated vapor deposition source 10 shown in FIG. 1 is a porous substrate impregnated with an aminosilane coupling agent. The impregnated vapor deposition source 10 shown in FIG. 1 is housed in a container 12.

[0008] In the storage method of the present disclosure, the impregnated evaporation source is stored under conditions where the storage temperature is 5° C. or less. The storage temperature is preferably 0° C. or less, more preferably −5° C. or less, even more preferably −10° C. or less, and particularly preferably −15° C. or less. The storage temperature is preferably −30° C. or more, more preferably −25° C. or more.

[0009] The storage atmosphere may be an inert gas atmosphere or an active gas atmosphere. Examples of the inert gas atmosphere include a nitrogen gas atmosphere and an argon gas atmosphere. Examples of the active gas atmosphere include an oxygen gas atmosphere and an air atmosphere. From the viewpoint of simplicity, it is also preferable to store the product in an air atmosphere.

[0010] In the storage method of the present disclosure, the impregnated evaporation source may be stored under conditions without any particular limitation as long as the storage temperature is 5°C or lower, but the impregnated evaporation source may be stored in a container as shown in FIG. 1 above. In addition, in the storage method of the present disclosure, the impregnated evaporation source or the container containing the impregnated evaporation source may be stored in another container. As the other container, for example, a container with a lid on top is preferred to prevent other substances from being mixed into the impregnated evaporation source. An example of the other container with a lid on top is a petri dish with a lid.

[0011] The substrate constituting the impregnation vapor deposition source is a substrate having voids. The substrate having voids is not particularly limited as long as it has voids inside and can be impregnated with an aminosilane coupling agent, and known substrates can be used. Examples of the substrate having voids include substrates selected from the group consisting of metal wool (more preferably steel wool), activated carbon, porous ceramics, and carbon fibers.

[0012] The size of the porous substrate constituting the impregnation vapor deposition source is not particularly limited and can be appropriately set depending on the purpose. For example, when the porous substrate is cylindrical, the height can be 3 to 10 mm, and the diameter of the bottom surface can be 5 to 20 mm.

[0013] The container for accommodating the deposition source is not particularly limited, and any known container can be used. The material constituting the container is not particularly limited, and examples thereof include metal, ceramic, and carbon. Examples of metals include materials containing at least one metal element selected from the group consisting of copper, molybdenum, tantalum, and tungsten. Examples of ceramics include one selected from the group consisting of magnesium oxide (magnesia), aluminum oxide (alumina), boron nitride, and silicon carbide.

[0014] An aminosilane coupling agent is a silane coupling agent having an amino group. The amino group of the aminosilane coupling agent may be any of a primary amino group, a secondary amino group, and a tertiary amino group, with a secondary amino group being preferred. The aminosilane coupling agent preferably has a hydroxyl group or a hydrolyzable group. The hydroxyl group or hydrolyzable group is preferably bonded to a silicon atom. The aminosilane coupling agent preferably has two or more amino groups. It is also preferred that the silane coupling agent has two or more secondary amino groups. The silane coupling agent preferably has four or fewer amino groups, more preferably three or fewer.

[0015] The aminosilane coupling agent is preferably a compound represented by the following formula (Y1).

[0016]

[0017] In formula (Y1), R ｙ１ and R ｙ３ each independently represents a hydroxyl group or a hydrolyzable group. Examples of the hydrolyzable group include an alkoxy group, a halogen atom, a cyano group, an acetoxy group, and an isocyanate group, with an alkoxy group or a halogen atom being preferred, and an alkoxy group being more preferred. The alkoxy group is preferably an alkoxy group having 1 to 4 carbon atoms, with a methoxy group or an ethoxy group being more preferred. Examples of the halogen atom include a fluorine atom, a chlorine atom, a bromine atom, and an iodine atom, with a chlorine atom being preferred.

[0018] In formula (Y1), R ｙ２ and R ｙ４ each independently represents a hydrocarbon group. The hydrocarbon group may be linear, branched, or cyclic. The hydrocarbon group preferably has 1 to 20 carbon atoms, more preferably 1 to 10 carbon atoms, and even more preferably 1 to 5 carbon atoms. The hydrocarbon group is preferably an alkyl group.

[0019] In formula (Y1), ny1 and ny2 each independently represent an integer of 1 to 3. ny1 and ny2 each independently represent preferably 2 or 3, and more preferably 3.

[0020] R ｙ１ If there are multiple ｙ１ R may be the same or different. ｙ２ If there are multiple ｙ２ R may be the same or different. ｙ３ If there are multiple ｙ３ R may be the same or different. ｙ４ If there are multiple ｙ４ R may be the same or different. Ｌ１ If there are multiple Ｌ１ R may be the same or different. Ｌ２ If there are multiple Ｌ２ R may be the same or different. Ｌ３ If there are multipleＬ３ R may be the same or different. Ｌ４ If there are multiple Ｌ４ R may be the same or different. Ｌ５ If there are multiple Ｌ５ They may be the same or different.

[0021] In formula (Y1), L ｙ１ is at least -NR Ｌ１ represents a divalent linking group having -, and the divalent linking group further has -NR Ｌ１ -, -C(R Ｌ２ ) (R Ｌ３ )- and -Si(R Ｌ４ ) (R Ｌ５ )-. Ｌ１ represents a hydrogen atom or an alkyl group. Ｌ２ ~R Ｌ５ R each independently represents a hydrogen atom, a fluorine atom or an alkyl group which may have a fluorine atom. Ｌ１ The alkyl group represented by R may be linear, branched, or cyclic, and is preferably linear. The number of carbon atoms in the alkyl group is preferably 1 to 5, and more preferably 1 to 3. Ｌ１ is preferably a hydrogen atom. Ｌ２ ~R Ｌ５ The alkyl group optionally having a fluorine atom represented by any one of the following is —Si(R ｓ ) ２ -R in ｓ The meaning and preferred embodiments are also the same as those of the alkyl group optionally having a fluorine atom represented by the following formula: ｙ１ is -NR Ｌ１ If the divalent linking group has -, it is -NR Ｌ１ - and -C(R Ｌ２ ) (R Ｌ３ )- and -Si(R Ｌ４ ) (R Ｌ５ )- and at least one group selected from the group consisting of ｙ１ As the Ｌ１ - and -C(R Ｌ２ ) (R Ｌ３)-, and at least two (preferably 2 to 3) -NR Ｌ１ - and at least two (preferably 2 to 9) -C(R Ｌ２ ) (R Ｌ３ )- is more preferred.

[0022] The aminosilane coupling agent is also preferably a compound represented by the following formula (Y2).

[0023]

[0024] In formula (Y2), R ｙ５ and R ｙ７ R each independently represents a hydroxyl group or a hydrolyzable group. ｙ６ and R ｙ８ each independently represents a hydrocarbon group; ny3 and ny4 each independently represents an integer of 1 to 3. R Ｌ６ and R Ｌ７ each independently represents a hydrogen atom or an alkyl group. ｙ２ ~L ｙ４ each independently represents an alkylene group which may have a fluorine atom. ｙ５ and R ｙ７ represents R in formula (Y1). ｙ１ The meaning and preferred embodiments are also the same as those of the formula (Y2). ｙ６ and R ｙ８ represents R in formula (Y1). ｙ２ The definitions and preferred embodiments of ny3 and ny4 in formula (Y2) are the same as those of ny1 and ny2 in formula (Y1), and the preferred embodiments are also the same. Ｌ６ and R Ｌ７ represents R in formula (Y1). Ｌ１ The same definition and preferred embodiments are also the same. ｙ５ If there are multiple ｙ５ R may be the same or different. ｙ６ If there are multiple ｙ６ R may be the same or different. ｙ７ If there are multiple ｙ７ R may be the same or different.ｙ８ If there are multiple ｙ８ They may be the same or different.

[0025] L ｙ２ ~L ｙ４ The alkylene group which may have a fluorine atom and is represented by any one of the following may be linear, branched, or cyclic, with linear being preferred. The number of carbon atoms in the alkylene group is preferably 1 to 30, and more preferably 1 to 10. When the alkylene group has a fluorine atom, the number of fluorine atoms in the alkylene group is preferably 1 to 10, and more preferably 1 to 5. It is also preferred that the alkylene group is an alkylene group which does not have a fluorine atom.

[0026] An example of the aminosilane coupling agent is N,N'-bis[3-(trimethoxysilyl)propyl]-1,2-ethanediamine (X-12-5263HP, manufactured by Shin-Etsu Chemical Co., Ltd.). Other examples of the aminosilane coupling agent include N-2-(aminoethyl)-3-aminopropylmethyldimethoxysilane (KBM-602, manufactured by Shin-Etsu Chemical Co., Ltd.), N-2-(aminoethyl)-3-aminopropyltrimethoxysilane (KBM-603, manufactured by Shin-Etsu Chemical Co., Ltd.), 3-aminopropyltrimethoxysilane (KBM-903, manufactured by Shin-Etsu Chemical Co., Ltd.), 3-aminopropyltriethoxysilane (KBE-903, manufactured by Shin-Etsu Chemical Co., Ltd.), and 3-triethoxysilane. Examples of suitable silyl-N-(1,3-dimethyl-butylidene)propylamine (KBE-9013P, manufactured by Shin-Etsu Chemical Co., Ltd.), X-12-1172ES (manufactured by Shin-Etsu Chemical Co., Ltd.), N-phenyl-3-aminopropyltrimethoxysilane (KBM-573, manufactured by Shin-Etsu Chemical Co., Ltd.), N-(vinylbenzyl)-2-aminoethyl-3-aminopropyltrimethoxysilane hydrochloride (KBM-6803, manufactured by Shin-Etsu Chemical Co., Ltd.), and X-12-972F (manufactured by Shin-Etsu Chemical Co., Ltd.).

[0027] The impregnation vapor deposition source may contain only one type of aminosilane coupling agent or two or more types of aminosilane coupling agents. It is also preferable that the impregnation vapor deposition source does not contain any compound other than the aminosilane coupling agent.

[0028] <Method for manufacturing eyeglass lenses> The method for manufacturing eyeglass lenses of the present disclosure includes the steps of forming a vapor deposition layer on an eyeglass lens substrate using a vapor deposition source stored according to the vapor deposition source storage method described above, and forming a water-repellent layer on the vapor deposition layer to manufacture an eyeglass lens including the eyeglass lens substrate, the vapor deposition layer, and the water-repellent layer. Note that "formed on an eyeglass lens substrate" includes cases where the vapor deposition layer is formed in direct contact with the surface of the eyeglass lens substrate, and cases where the vapor deposition layer is formed on the surface of the eyeglass lens substrate via another layer. The method for manufacturing eyeglass lenses of the present disclosure is described in detail below.

[0029] [Eyeglass Lens Substrate] In the method for manufacturing an eyeglass lens according to the present disclosure, a vapor deposition layer is formed on an eyeglass lens substrate. The eyeglass lens substrate will be described below.

[0030] The spectacle lens substrate is a member that supports the above-mentioned vapor deposition layer and other layers, including the water-repellent film layer. The type of spectacle lens substrate is not particularly limited, and examples include ordinary spectacle lens substrates composed of plastic, inorganic glass, etc., with plastic spectacle lens substrates being preferred due to their excellent handling properties. The type of plastic spectacle lens substrate is not particularly limited, and examples include finished lenses in which both the convex and concave surfaces are optically finished and molded to the desired dioptric power, semi-finished lenses in which only the convex surface is finished as an optical surface (spherical, rotationally symmetric aspherical, progressive, etc.), and lenses in which the concave surface of a semi-finished lens is processed and polished to match the wearer's prescription. The type of plastic (so-called resin) contained in the plastic spectacle lens substrate is not particularly limited, and examples include (meth)acrylic acid ester resins, thiourethane resins, allyl resins, episulfide resins, polycarbonates, urethane resins, polyesters, polystyrene, polyethersulfone, poly-4-methylpentene-1, and diethylene glycol bisallyl carbonate resin (CR-39). Among these, thiourethane resin, episulfide resin, and diethylene glycol bisallyl carbonate resin are preferably used. The thiourethane resin is obtained from a polyisocyanate compound and a polythiol compound. As the polyisocyanate compound, it is preferable to use at least one selected from m-xylylene diisocyanate, a mixture of 2,5-bis(isocyanatomethyl)-bicyclo[2,2,1]heptane and 2,6-bis(isocyanatomethyl)-bicyclo[2,2,1]heptane, isophorone diisocyanate, hexamethylene diisocyanate, and tolylene diisocyanate.As the polythiol compound, it is preferable to use at least one selected from pentaerythritol tetrakis(3-mercaptopropionate), 1,2-bis[(2-mercaptoethyl)thio]-3-mercaptopropane, and a mixture of 5,7-dimercaptomethyl-1,11-dimercapto-3,6,9-trithiaundecane, 4,7-dimercaptomethyl-1,11-dimercapto-3,6,9-trithiaundecane, and 4,8-dimercaptomethyl-1,11-dimercapto-3,6,9-trithiaundecane. The episulfide resin is obtained by ring-opening polymerization of a monomer having an episulfide group (also referred to as an epithio group) or a mixed monomer containing this monomer. As the monomer having an episulfide group, it is preferable to use at least one selected from bis(2,3-epithiopropyl) sulfide and bis(2,3-epithiopropyl) disulfide.

[0031] The thickness of the plastic eyeglass lens substrate is not particularly limited, but from the viewpoint of ease of handling, it is often about 1 to 30 mm. The refractive index of the plastic eyeglass lens substrate is not particularly limited, but it is often 1.50 or more, preferably 1.60 to 1.80, and more preferably 1.60 to 1.74.

[0032] Furthermore, the spectacle lens substrate does not have to be colorless as long as it is translucent, and may contain an ultraviolet absorber and a dye that absorbs light in a specific wavelength range from the ultraviolet to the infrared region. The spectacle lens substrate may also contain additives such as a bluing agent, a light stabilizer, and an antioxidant.

[0033] [Primer Layer] The spectacle lens obtained by the spectacle lens manufacturing method of the present disclosure may have a primer layer. That is, the spectacle lens manufacturing method of the present disclosure may include a step of forming a primer layer. The primer layer is preferably disposed between the spectacle lens substrate and the hard coat layer described below. When the primer layer is disposed between the spectacle lens substrate and the hard coat layer, it improves the adhesion of the hard coat layer to the spectacle lens substrate and improves strength against static load or impact. The material constituting the primer layer is not particularly limited, and known materials can be used, for example, resins are mainly used. The type of resin used is not particularly limited, and examples include polyurethane-based resins, epoxy-based resins, phenol-based resins, polyimide-based resins, polyester-based resins, bismaleimide-based resins, and polyolefin-based resins, with polyurethane-based resins being preferred. The primer layer may contain components other than the above resins. Examples of other components include fine particles of an oxide of at least one metal selected from Si, Al, Sn, Sb, Ta, Ce, La, Fe, Zn, W, Zr, In, and Ti, or fine particles of a composite oxide thereof, a hydrolyzable silicon compound and / or its hydrolysis condensate, a conductive filler, a specific polymer, and a surfactant.

[0034] The method for forming the primer layer is not particularly limited, and known methods can be used, such as a method in which a primer layer-forming composition containing a predetermined resin is applied to a spectacle lens substrate, and a curing treatment is performed as necessary to form a primer layer. The method for applying the primer layer-forming composition is not particularly limited, and examples thereof include a method exemplified by the method of applying a hard coat layer-forming composition described below to a spectacle lens substrate. The thickness of the primer layer is not particularly limited, but is preferably 0.3 to 2 μm.

[0035] [Hard Coat Layer] The eyeglass lens obtained by the eyeglass lens manufacturing method of the present disclosure may have a hard coat layer. That is, the eyeglass lens manufacturing method of the present disclosure may include a step of forming a hard coat layer. The hard coat layer is preferably disposed between the eyeglass lens substrate and the anti-reflection film, and is a layer that imparts scratch resistance to the eyeglass lens substrate. The hard coat layer preferably exhibits a pencil hardness of "H" or higher according to the test method defined in International Standard ISO 15184 and Japanese Industrial Standard JIS K5600, which was created based on this international standard.

[0036] As the hard coat layer, a known hard coat layer can be used, for example, an organic hard coat layer, an inorganic hard coat layer, or an organic-inorganic hybrid hard coat layer. For example, in the field of eyeglass lenses, an organic-inorganic hybrid hard coat layer is commonly used.

[0037] The hard coat layer may also contain inorganic components such as metal oxide fine particles. The type of metal oxide fine particles is not particularly limited, and examples include known metal oxide fine particles. Examples of metal oxide fine particles include fine particles of at least one metal oxide selected from Si, Al, Sn, Sb, Ta, Ce, La, Fe, Zn, W, Zr, In, and Ti. Among these, in terms of ease of handling, metal oxide fine particles are preferably fine particles of oxides containing Si (silicon oxide fine particles), oxides containing Sn (tin oxide fine particles), oxides containing Zr (zirconium oxide fine particles), or oxides containing Ti (titanium oxide fine particles). The metal oxide fine particles may contain only one of the above-mentioned metals (metal atoms) or two or more metals (metal atoms). Although Si (silicon) is sometimes classified as a semimetal, the disclosed Si is included in the metals.

[0038] A method for forming a hard coat layer using a hard coat layer-forming composition includes applying the hard coat layer-forming composition to a spectacle lens substrate (or a primer layer) to form a coating film, and then subjecting the coating film to a curing treatment such as a light irradiation treatment and a heat treatment. As the curing treatment, either one of a light irradiation treatment or a heat treatment may be performed, or both may be performed. When both are performed, the light irradiation treatment and the heat treatment may be performed simultaneously, or one may be performed first and then the other. After forming the coating film, a drying treatment such as a heat treatment may be performed, if necessary, to remove the solvent from the coating film.

[0039] The method for applying the composition for forming a hard coat layer is not particularly limited, and includes known methods (e.g., dipping coating, spin coating, spray coating, inkjet coating, and flow coating). The thickness of the coating film to be formed is not particularly limited, and a thickness that will result in a predetermined hard coat layer thickness is appropriately selected.

[0040] The conditions for the light irradiation treatment are not particularly limited, and appropriate conditions are selected depending on the type of polymerization initiator used. The type of light used for light irradiation is not particularly limited, but examples include ultraviolet light and visible light. Examples of light sources include high-pressure mercury lamps. The cumulative light amount used for light irradiation is not particularly limited, but from the viewpoints of productivity and curability of the coating film, it is preferred to use a light amount of 100 to 3000 mJ / cm. ２ is preferred, and 100 to 2000 mJ / cm ２ The conditions for the heat treatment are not particularly limited, and the optimum conditions are selected depending on the type of polymerization initiator used. The heating temperature is preferably 30 to 130°C, and the heating time is preferably 5 to 360 minutes.

[0041] The thickness of the hard coat layer is not particularly limited, but is preferably 1 μm or more, more preferably 3 μm or more. The upper limit of the thickness can be, for example, 30 μm or less. The thickness is an average thickness, and the measurement method is to measure the thickness at any five points on the hard coat layer and calculate the arithmetic average.

[0042] The hard coat layer may contain additives such as a bluing agent, a light stabilizer, and an antioxidant.

[0043] [Anti-reflection film] The eyeglass lens obtained by the eyeglass lens manufacturing method of the present disclosure may have an anti-reflection film. That is, the eyeglass lens manufacturing method of the present disclosure may include a step of forming an anti-reflection film. An anti-reflection film is a layer that has the function of preventing reflection of incident light. Specifically, it can have low reflectance characteristics (broadband low reflectance characteristics) over the entire visible range of 380 to 780 nm.

[0044] The structure of the antireflective film is not particularly limited, and may be a single-layer structure or a multilayer structure. An inorganic antireflective film is preferred as the antireflective film. An inorganic antireflective film is an antireflective film composed of an inorganic compound. In the case of a multilayer structure, a structure in which low-refractive-index layers and high-refractive-index layers are alternately stacked is preferred. Examples of materials constituting the high-refractive-index layers include oxides of titanium, zirconium, aluminum, niobium, tantalum, or lanthanum. Examples of materials constituting the low-refractive-index layers include oxides of silica. The method for producing the antireflective film is not particularly limited, and examples include dry methods such as vacuum deposition, sputtering, ion plating, ion-beam assisted deposition, and CVD.

[0045] [Vapor deposition layer] The method for manufacturing a spectacle lens according to the present disclosure includes a step of forming a vapor deposition layer on a spectacle lens substrate. When forming the vapor deposition layer, a vapor deposition source stored according to the vapor deposition source storage method of the present disclosure described above is used. The compound (aminosilane coupling agent) contained in the vapor deposition source is as described above.

[0046] The vapor deposition layer is formed by vapor deposition. A specific method for forming the vapor deposition layer includes heating a vapor deposition source under reduced pressure, vaporizing or sublimating the aminosilane coupling agent contained in the vapor deposition source, and supplying the aminosilane coupling agent onto the eyeglass lens substrate to form the vapor deposition layer. The vapor deposition layer may be formed directly on the eyeglass lens substrate, or on a surface on which a member selected from the group consisting of the primer layer, hard coat layer, and anti-reflection film is formed. When the vapor deposition layer is formed using the vapor deposition source, a vapor deposition layer containing the compound contained in the vapor deposition source is formed. The aminosilane coupling agent can improve the adhesion between the water-repellent layer and the surface of a member selected from the group consisting of the eyeglass lens substrate, primer layer, hard coat layer, and anti-reflection film, and can improve the abrasion resistance of the water-repellent layer.

[0047] The degree of vacuum when forming the vapor deposition layer is, for example, 1.0×10 －５ ~1.0 x 10 １ Pa, 1.0 × 10 －４ ~1.0 x 10 ０ Pa is preferred, and 1.0 x 10 －３ ~5.0 x 10 －１ Pa is more preferable. The degree of vacuum when forming the vapor deposition layer may be adjusted by introducing a gas. The gas to be introduced is not particularly limited, but examples thereof include nitrogen gas, oxygen gas, and argon gas, with oxygen gas being preferred. Ion-assisted vapor deposition may also be performed when forming the vapor deposition layer. Ion-assisted vapor deposition refers to a vapor deposition method in which an ion beam is irradiated onto the spectacle lens substrate during vapor deposition to increase the adhesion of the vapor deposition material.

[0048] Examples of methods for heating the evaporation source include a method of heating a container that houses the evaporation source with a heater, a method of electrically heating a container that houses the evaporation source, a method of heating the evaporation source by irradiating it with an electron beam, and a method of heating the evaporation source by irradiating it with electromagnetic waves such as infrared rays. Of these, the method of heating the evaporation source is preferably a method of irradiating it with an electron beam. In the method for manufacturing an eyeglass lens of the present disclosure, an evaporation source stored by the evaporation source storage method of the present disclosure is used, so that outgassing is less likely to occur from the evaporation source, and evaporation can be performed stably.

[0049] The thickness of the vapor-deposited layer is not particularly limited, but is preferably 1 to 1,000 nm, more preferably 3 to 100 nm, and even more preferably 10 to 50 nm. When forming the vapor-deposited layer, it is also preferable to monitor the amount of vapor deposition with a film thickness meter.

[0050] [Water-repellent layer] The method for manufacturing a spectacle lens according to the present disclosure includes forming a water-repellent layer on a vapor deposition layer to manufacture a base metal lens including a spectacle lens substrate, a vapor deposition layer, and a water-repellent layer. The water-repellent layer reduces the surface energy of the spectacle lens, improving the spectacle lens's anti-contamination function and improving the slipperiness of the spectacle lens surface, thereby improving the wear resistance of the spectacle lens. The water-repellent layer is preferably disposed as the outermost layer of the spectacle lens.

[0051] The material constituting the water-repellent layer is not particularly limited, and examples thereof include fluorine-containing compounds (compounds containing fluorine atoms) and silicon-containing compounds (compounds containing silicon atoms). Among these, the water-repellent layer preferably contains a fluorine-containing compound, and more preferably contains at least one selected from the group consisting of fluorine-substituted alkyl group-containing organosilicon compounds, their hydrolysates, and their hydrolyzed condensates. The material constituting the water-repellent layer may be used alone or in combination of two or more.

[0052] The organosilicon compound containing fluorine-substituted alkyl group is the organosilicon compound that contains alkyl group in which part or all of hydrogen atom is replaced by fluorine atom, and has hydrolyzable group.Here, the hydrolyzable group is the group that is directly bonded to silicon atom and can proceed hydrolysis reaction and condensation reaction, for example, alkoxy group, halogen atom, acyloxy group, alkenyloxy group and isocyanate group.It should be noted that when a plurality of hydrolyzable groups are directly bonded to one silicon atom, they can be the same or different.

[0053] The hydrolyzate of a fluorine-substituted alkyl group-containing organosilicon compound refers to a compound obtained by hydrolyzing the hydrolyzable groups in a fluorine-substituted alkyl group-containing organosilicon compound. The hydrolyzate may be one in which all of the hydrolyzable groups are hydrolyzed (complete hydrolyzate) or one in which only a portion of the hydrolyzable groups are hydrolyzed (partial hydrolyzate). In other words, the hydrolyzate may be a complete hydrolyzate, a partial hydrolyzate, or a mixture thereof. The hydrolyzed condensate of a fluorine-substituted alkyl group-containing organosilicon compound refers to a compound obtained by hydrolyzing the hydrolyzable groups in a fluorine-substituted alkyl group-containing organosilicon compound and condensing the resulting hydrolyzate. The hydrolyzed condensate may be one in which all of the hydrolyzable groups are hydrolyzed and the hydrolyzate is completely condensed (complete hydrolyzed condensate), or one in which only a portion of the hydrolyzable groups are hydrolyzed and a portion of the hydrolyzate is condensed (partial hydrolyzed condensate). In other words, the hydrolyzed condensate may be a complete hydrolyzed condensate, a partial hydrolyzed condensate, or a mixture thereof.

[0054] <Uses> The eyeglass lenses obtained by the eyeglass lens manufacturing method of the present disclosure are suitable for use as lenses for eyeglasses. Examples of eyeglasses include eyeglasses having a known eyeglass frame and eyeglass lenses, and examples of eyeglass frames include those having a pair of lens frames on which eyeglass lenses for the right eye and left eye are respectively attached, and temples for holding the eyeglass frame over the wearer's ears. The eyeglass lenses obtained by the eyeglass lens manufacturing method of the present disclosure have excellent abrasion resistance of the water-repellent layer due to the effect of the vapor deposition layer.

[0055] The above-mentioned embodiments will be explained in more detail below with reference to examples and comparative examples, but the present disclosure is not limited to these examples in any way.

[0056] <Reference Example> Steel wool (corresponding to a substrate having voids) was placed in a copper container, and an aminosilane coupling agent (X-12-5263HP, manufactured by Shin-Etsu Chemical Co., Ltd.) was placed in the copper container and impregnated into the steel wool to obtain a deposition source. The aminosilane coupling agent is a compound having the following structural formula:

[0057]

[0058] For the reference examples, various tests were carried out immediately after the steel wool was impregnated with the aminosilane coupling agent without storage.

[0059] <Comparative Examples 1 to 6> In Comparative Examples 1 to 6, the deposition source of the above-described Reference Example was stored in a desiccator. During storage, it was placed in a petri dish with a lid. An auto-dry type desiccator (TOSHIBA DC-87) was used, and the storage temperature was 25°C. The humidity inside the desiccator was 40%. The storage time was as shown in Table 1 below.

[0060] In Examples 1 to 6, the deposition sources of the above-described Reference Examples were stored in a freezer or refrigerator. They were stored in petri dishes with lids. The storage temperatures and storage times were as shown in Table 1 below.

[0061] <Outgassing Test 1> For a part of each example, the stored vapor deposition source was introduced into a vacuum chamber, and the amount of outgassing was evaluated. Specifically, the following procedure was performed. First, the vapor deposition source of each example, in which the impregnation amount of the aminosilane coupling agent was 165 mg, was introduced into a vapor deposition apparatus (1200-DLX-2 manufactured by Satisloh). Next, the set pressure was increased to 1.00 × 10 －２ The pressure in the chamber was set to 0.2 Pa, and oxygen gas was introduced to control the pressure in the chamber, while the output of the electron gun of the deposition device was set to 8% and the deposition source was heated. When pressure control was performed while heating the deposition source, if the pressure could be controlled until the material in the deposition source was used up, this is recorded as "normal" in Table 1, and if an error occurred in the deposition device during the pressure control, this is recorded as "abnormal." If the error was "abnormal," the pressure in the chamber at the time the error was issued is recorded in Table 1.

[0062] <Outgassing Test 2> For some of the examples, the stored vapor deposition source was introduced into a vacuum chamber, and the amount of outgassing was evaluated. Specifically, the following procedure was performed. First, the vapor deposition source of each example, in which the impregnation amount of the aminosilane coupling agent was 190 mg, was introduced into a vapor deposition apparatus (1200-DLX-2 manufactured by Satisloh). After introduction, the pressure inside the chamber was reduced to 1.00 × 10 －３ The vacuum was drawn for about 30 minutes until the pressure reached Pa. Thereafter, without pressure control, the output of the electron gun of the deposition apparatus was set to 8%, and heating was continued for about 1 minute until the deposition source was exhausted (i.e., until the deposition rate reached 0), and the maximum pressure observed during this time (maximum pressure) was recorded. The value obtained by subtracting the maximum pressure when the storage time was 0 hours from the maximum pressure is shown in Table 1 below as the maximum pressure change.

[0063] <Water-repellent performance> For some of the examples, a vapor deposition layer was formed on a spectacle lens substrate using the vapor deposition source of each example, and a water-repellent layer was then formed on the vapor deposition layer to obtain spectacle lenses. The water-repellent performance of the obtained spectacle lenses was evaluated. Specifically, spectacle lenses were obtained by the following procedure, and the water-repellent performance was evaluated. First, an NL3-SP (size 75 mmφ, center thickness 1.1 mm) manufactured by Nikon-Essilor was prepared as a plastic spectacle lens substrate. A coating liquid was applied to the surface of the plastic spectacle lens substrate by the immersion method, and the resulting solution was cured by heating to form a primer layer (urethane-based impact resistance improving coating layer) with a thickness of approximately 1 μm. A silicone-based hard coating layer (scratch resistance improving layer) with a thickness of approximately 2 μm was formed on the primer layer. Next, a low refractive index layer (SiO ２ layer) and a high refractive index layer (ZrO ２ The layer furthest from the plastic eyeglass lens substrate side of the formed anti-reflection film was a SiO ２ It was a layer.

[0064] Next, using the evaporation source of each example, an aminosilane coupling agent was evaporated onto the anti-reflection film to form an evaporated layer. The evaporation time was adjusted so that the thickness of the evaporated layer would be 15 to 35 nm. The evaporation source used had an impregnation amount of the aminosilane coupling agent of 165 mg. The evaporation of the aminosilane coupling agent using the evaporation source was performed by irradiating the evaporation source with an electron beam to heat it. The conditions were as follows: Evaporation apparatus: 1200-DLX-2 manufactured by Satisloh Electronics Co., Ltd. Electron gun output: 8% Pressure during evaporation: 1.00 x 10 －２ Pa Pressure control gas: oxygen gas It was confirmed that control at the above pressure was performed normally when an aminosilane coupling agent was deposited on an anti-reflective film using the deposition source of each example shown in Table 1 below.

[0065] Next, SURFCLEAR EW (Canon Optron Inc.) was vacuum-deposited on the vapor-deposited layer to form a water-repellent layer. The vacuum deposition of the water-repellent layer was performed in the vapor deposition apparatus described above, following the deposition of the aminosilane coupling agent, by heating the vapor deposition source of the water-repellent layer without controlling the pressure. Through the above procedure, a spectacle lens having, in this order, a spectacle lens substrate, a vapor-deposited layer, and a water-repellent layer was obtained.

[0066] [Initial Contact Angle and Initial Sliding Angle] A 1 μL water droplet was placed on the surface of the water-repellent layer side of the eyeglass lens, and the water contact angle (initial contact angle) was measured by the sessile drop method using a contact angle measuring device (DM-500 / DM-SA, manufactured by Kyowa Interface Science Co., Ltd.). The analysis method was the ellipse fitting method. A 20 μL water droplet was placed on the surface of the water-repellent layer side of the eyeglass lens, and the water sliding angle (initial sliding angle) was measured by the sliding method using the contact angle measuring device. The analysis methods were as follows: Analysis method: perfect circle fitting method Tilt method: continuous tilt Sliding detection: before sliding Movement judgment: forward and backward Sliding judgment distance: 10 dots

[0067] [Contact angle after test and sliding angle after test] A rubbing abrasion resistance test was conducted on the surface of the water-repellent layer side of the eyeglass lens. Specifically, a 16-ply paper cloth (Kimwipe (registered trademark) Wiper S-200, manufactured by Nippon Paper Crecia Co., Ltd.) was attached to a 15 mm square elastic body (plastic eraser, 1156SMTR00, manufactured by Maped Co., Ltd.), and the rubbing abrasion resistance test was conducted so that the cloth came into contact with the surface of the water-repellent layer side of the eyeglass lens. The conditions for the rubbing abrasion resistance test were as follows: Load: 200 g Stroke: 30 mm Speed: 90 reciprocations / min Number of times: 20,000 times

[0068] After the above-mentioned rubbing abrasion resistance test was conducted, the contact angle after the rubbing abrasion resistance test (post-test contact angle) and the sliding angle after the rubbing abrasion resistance test (post-test sliding angle) were measured in the same manner as the above-mentioned initial contact angle and initial sliding angle. Note that, from a practical standpoint, the contact angle after the rubbing abrasion resistance test (post-test contact angle) is preferably 110° or more. Furthermore, from a practical standpoint, the sliding angle after the rubbing abrasion resistance test (post-test sliding angle) is preferably 30° or less.

[0069] <Results> The storage conditions and test results for each of the above examples are shown in Table 1. In Table 1, for example, the notation "2.32E-02" means 2.32 x 10 －２ Represents.

[0070]

[0071] The results in Table 1 confirmed that outgassing was suppressed when the vapor deposition source was stored at a storage temperature of 5°C or less (Examples 1 to 6). On the other hand, when the vapor deposition source was stored at a storage temperature above 5°C, outgassing increased, and pressure control during vapor deposition was sometimes impossible (Comparative Examples 1 to 6). A comparison between Example 3 and Example 6 confirmed that outgassing was suppressed when the storage temperature was 0°C or less (more preferably, −5°C or less, −10°C or less, and −15°C or less, in that order). Furthermore, a comparison between the Reference Example and Examples 4 and 5 confirmed that a water-repellent layer exhibiting properties equivalent to those obtained when the vapor deposition source was used before storage was formed, even when the vapor deposition source was stored at a storage temperature of 5°C or less and then used for vapor deposition.

[0072] 10 Impregnation deposition source 12 Container

Claims

1. A method for storing a vapor deposition source, comprising storing the vapor deposition source, which comprises a substrate having voids and a silane coupling agent having an amino group impregnated into the substrate having voids, at a storage temperature of 5°C or less.

2. The method for storing an evaporation source according to claim 1, wherein the porous substrate is selected from the group consisting of metal wool, activated carbon, porous ceramics, and carbon fiber.

3. The method for storing an evaporation source according to claim 1 or 2, wherein the amino group is a secondary amino group.

4. The method for storing a vapor deposition source according to any one of claims 1 to 3, wherein the silane coupling agent is a compound represented by the following formula (Y1): In formula (Y1), R ｙ１ and R ｙ３ R each independently represents a hydroxyl group or a hydrolyzable group. ｙ２ and R ｙ４ each independently represents a hydrocarbon group; ny1 and ny2 each independently represents an integer of 1 to 3; L ｙ１ is at least -NR Ｌ１ represents a divalent linking group having -, and the divalent linking group further has -NR Ｌ１ -, -C(R Ｌ２ ) (R Ｌ３ )- and -Si(R Ｌ４ ) (R Ｌ５ )-. Ｌ１ represents a hydrogen atom or an alkyl group. Ｌ２ ~R Ｌ５ each independently represents a hydrogen atom, a fluorine atom or an alkyl group which may have a fluorine atom.

5. The method for storing an evaporation source according to any one of claims 1 to 4, wherein the storage temperature is -20 to -5°C.

6. The method for storing an evaporation source according to any one of claims 1 to 5, wherein the storage atmosphere is an air atmosphere.

7. A method for manufacturing eyeglass lenses, comprising the steps of: forming a vapor deposition layer on an eyeglass lens substrate using the vapor deposition source stored by the method for storing a vapor deposition source according to any one of claims 1 to 6; and forming a water-repellent layer on the vapor deposition layer, thereby manufacturing an eyeglass lens comprising the eyeglass lens substrate, the vapor deposition layer, and the water-repellent layer.

Images