Vapor deposition source and method for manufacturing vapor deposition source

Abstract

The present invention addresses the problem of providing a vapor deposition source with which it is possible, in cases where a vapor deposition source used in a film formation process for performing coating by vacuum vapor deposition contains a liquid that contains a non-fluorine organic compound, to form a high-quality film by preventing outflow of the liquid from the vapor deposition source due to vibration during physical distribution and inclination during storage and maintaining an appropriate content. In order to solve the problem, the present invention provides vapor deposition source which includes a container, and a fibrous material and a liquid in the container, wherein: the liquid contains a non-fluorine organic compound and has a kinematic viscosity a at 25°C that satisfies formula (i); and the fibrous material has a fiber diameter x (mm) and a density y (g / cm3) that satisfy formulae (ii) to (iv).

Description

Evaporation source and method for manufacturing the same

[0001] The present invention relates to an evaporation source used in a film-forming process for coating by vacuum evaporation, and a method for manufacturing the evaporation source. It also relates to an evaporation method, an article, and an optical component.

[0002] Coating a thin film that improves functionality, such as an antifouling material or a scratch-resistant material, on the surface of an optical substrate such as glass or plastic is performed in various fields. In applications where coating a thin film, particularly when light transmittance is emphasized, strict control of the film thickness is required, so the vacuum evaporation method is used. The vacuum evaporation method is known to be excellent in film thickness uniformity during thin film formation.

[0003] Recently, it has been proposed to use organic compounds as coating materials for improving the functionality of the surface by the vacuum evaporation method. As an evaporation source when coating an organic compound by the vacuum evaporation method, the evaporation sources shown in Patent Document 1 and Patent Document 2 have been proposed.

[0004] Patent Document 1 discloses an evaporation material in which a fluorine-containing aminosilane compound as an organic film-forming substance is attached to a mass of fibrous conductive substances. Further, Patent Document 2 proposes using a thin film-forming substance impregnated in a fibrous substance in a container as an evaporation source, and discloses that a high-quality antifouling film can be formed.

[0005] As a coating material for improving the functionality of the surface, organic fluorine compounds that are excellent in antifouling properties and scratch resistance are often used. However, organic fluorine compounds are hardly decomposable, and there are concerns such as bioaccumulation and mobility. Particularly for items that people touch, a surface coating that improves functionality with an organic compound that does not contain fluorine atoms (hereinafter, non-fluorinated organic compound) is desired.

[0006] Japanese Patent Laid-Open No. 6-340966 Japanese Patent Laid-Open No. 2016-11460

[0007] The present invention provides a vapor deposition source used in a film forming process for coating by vacuum evaporation. When the vapor deposition source contains a liquid containing a non-fluorinated organic compound, it prevents the outflow of the liquid in the vapor deposition source due to vibration during logistics or inclination during storage, and can form a high-quality film by maintaining an appropriate content. Another object of the present invention is to provide a method for manufacturing the above vapor deposition source.

[0008] The present invention relates to a vapor deposition source including a container and a fibrous substance and a liquid in the container. The liquid contains a non-fluorinated organic compound, and the kinematic viscosity a at 25 °C satisfies the following formula (i). The fiber diameter x [mm] and density y [g / cm ３ of the fibrous substance satisfy the following formulas (ii) to (iv). It is a vapor deposition source. 0.57 ≤ a ≤ 14000 (i) 0.01 ≤ x ≤ 0.30 (ii) 0.04 ≤ y ≤ 1.54 (iii) x / y ≤ 0.31 (iv)

[0009] The present invention also includes an arrangement step of arranging a fibrous substance in a container, and an impregnation step of impregnating the fibrous substance with a liquid of a non-fluorinated organic compound or an impregnating liquid containing a liquid containing a non-fluorinated organic compound. The liquid and the impregnating liquid have a kinematic viscosity a at 25 °C that satisfies the following formula (i). The fiber diameter x [mm] and density y [g / cm ３ of the fibrous substance satisfy the following formulas (ii) to (iv). It is a method for manufacturing a vapor deposition source. 0.57 ≤ a ≤ 14000 (i) 0.01 ≤ x ≤ 0.30 (ii) 0.04 ≤ y ≤ 1.54 (iii) x / y ≤ 0.31 (iv)

[0010] According to the present invention, it is possible to provide a vapor deposition source for vacuum evaporation coating that can prevent the outflow of the liquid containing a non-fluorinated organic compound in the vapor deposition source due to vibration during logistics or inclination during storage, and can form a high-quality film by maintaining an appropriate content. Further, according to the present invention, the above vapor deposition source can be manufactured.

[0011] Schematic diagram of the vapor deposition source

[0012] The following describes embodiments of the evaporation source and method for manufacturing the evaporation source according to the present invention, with reference to preferred embodiments. However, the present invention is not limited to the embodiments described below. In the present invention, unless otherwise specified, the descriptions of numerical ranges such as "XX or more and YY or less" or "XX to YY" mean a numerical range that includes the lower and upper limits which are the endpoints. Furthermore, when a numerical range is described in steps, the upper and lower limits of each numerical range can be arbitrarily combined. In addition, in this disclosure, for example, a description such as "at least one selected from the group consisting of XX, YY, and ZZ" means any of XX, YY, ZZ, a combination of XX and YY, a combination of XX and ZZ, a combination of YY and ZZ, or a combination of XX, YY, and ZZ. Note that if XX is a group, multiple selections may be made from XX, and the same applies to YY and ZZ.

[0013] (Container) The shape of the container in this invention is arbitrary as long as it is suitable for the vacuum deposition process, but it is preferable that at least one side is open in order to enclose the fibrous material. Furthermore, it is preferable that the open area is close to the outer diameter of the container in order to prevent unevenness in the thickness of the film after deposition. The container may also be tapered toward the open side.

[0014] The material used to form the above-mentioned container can be any material suitable for the vacuum deposition process, but it is preferably a metal, carbon, or ceramic from the viewpoint of thermal conductivity and moldability. More preferably, the material used to form the container is a metal. The metal may be a single metal such as copper, iron, aluminum, tungsten, molybdenum, or tantalum, or an alloy. Furthermore, the single metals and alloys may be plated.

[0015] The size, height, depth, and volume of the above-mentioned container can be arbitrarily determined by the chamber volume of the vacuum deposition apparatus, the size of the hearth and hearth liner that constitute the evaporation source by the resistance heating device or electron gun installed inside the vacuum deposition apparatus, and the amount of liquid containing the non-fluorine organic compound.

[0016] The thickness of the material forming the above container can be arbitrarily determined as long as it is a thickness suitable for the vacuum deposition process. Preferably, the thickness of the material forming the above container is 3 mm or less. Furthermore, it is preferable that the thickness is 1 mm or less. Preferably, the outer diameter of the above container is 100 mmΦ or less. Furthermore, it is preferable that the outer diameter is 35 mmΦ or less. Furthermore, it is preferable that the outer diameter is 26 mmΦ or less. Also, preferably, the outer diameter of the above container is 4 mmΦ or more. That is, preferably, the outer diameter of the above container is 4 mmΦ or more and 100 mmΦ or less. Furthermore, preferably, the outer diameter is 4 mmΦ or more and 35 mmΦ or less. Furthermore, preferably, the outer diameter is 4 mmΦ or more and 26 mmΦ or less. Preferably, the inner diameter of the above container is 94 mmΦ or less. Furthermore, preferably, the inner diameter is 29 mmΦ or less. Furthermore, preferably, the inner diameter is 20 mmΦ or less. Also, preferably, the inner diameter of the above container is 3 mmΦ or more. That is, preferably, the inner diameter of the above container is 3 mmΦ or more and 94 mmΦ or less. Furthermore, it is preferable that the inner diameter is 3 mmΦ or more and 29 mmΦ or less. Furthermore, it is preferable that the inner diameter is 3 mmΦ or more and 20 mmΦ or less. The height of the above container is preferably 50 mm or less. Furthermore, it is preferable that the height is 20 mm or less. Also, it is preferable that the height of the above container is 3 mm or more. That is, it is preferable that the height of the above container is 3 mm or more and 50 mm or less. Furthermore, it is preferable that the height is 3 mm or more and 20 mm or less. The depth of the above container is preferably 47 mm or less. Furthermore, it is preferable that it is 17 mm or less. Also, it is preferable that the depth of the above container is 2 mm or more and 47 mm or less. Furthermore, it is preferable that it is 2 mm or more and 17 mm or less.

[0017] (Fibrous material) The fibrous material in this invention has a fiber diameter (x [mm]) of 0.01 mm or more and 0.30 mm or less, and a density (y [g / cm³]). ３ ]) is 0.04 g / cm³ ３ Above, 1.54g / cm ３The following conditions apply, and the ratio of fiber diameter to density (x / y) is 0.31 or less. The material forming the fibrous substance is preferably a metal or carbon. More preferably, the material forming the fibrous substance is a metal. Examples of metals include elemental metals such as iron, stainless steel, aluminum, and copper. Fibers made of alloys may also be used.

[0018] The fiber diameter of a fibrous material can be determined by measuring the length of the fiber portion in an image observed using an optical microscope or electron microscope. The fiber diameter of the fibrous material is preferably 0.01 mm or more and 0.30 mm or less, and more preferably 0.012 mm or more and 0.30 mm or less. Furthermore, it is preferable that it be 0.012 mm or more and 0.20 mm or less. The density of the fibrous material can be determined from the weight of the fibrous material placed in the container and the volume of the fibrous material placed in the container. The volume of the fibrous material can be determined from the height of the fibrous material when it is placed in the container and the area of ​​the fibrous material when it is placed in the container.

[0019] The height of the fibrous material when it is placed in the above container can be arbitrarily determined as long as it does not exceed the height of the container. Preferably, the height of the fibrous material is 45 mm or less. More preferably, it is 13 mm or less. The area of ​​the fibrous material when it is placed in the above container can be arbitrarily determined as long as the fibrous material does not move around too much within the container. Specifically, it is preferable that the area of ​​the fibrous material is 90% or more of the bottom area of ​​the container. More preferably, the area of ​​the fibrous material is 95% or more of the bottom area of ​​the container. Furthermore, it is preferable that the area of ​​the fibrous material and the bottom area of ​​the container are equal. If the area of ​​the fibrous material is less than 90% of the bottom area of ​​the container, the fibrous material will move around inside the container and will come out of the container during transport. In this state, the purpose of holding the liquid containing non-fluorinated organic compounds inside the container cannot be achieved. When a fibrous material is placed in the above-mentioned container, the occupancy rate of the fibrous material relative to the volume of the container is preferably 30 vol% to 100 vol%, more preferably 40 vol% to 80 vol%, and even more preferably 50 vol% to 70 vol%.

[0020] The density of the fibrous material is 0.04 g / cm ３ or more and 1.54 g / cm ３ or less, and more preferably 0.20 g / cm ３ or more and 1.30 g / cm ３ or less. Even more preferably, it is 0.40 g / cm ３ or more and 1.00 g / cm ３ or less. When the density of the fibrous material exceeds 1.54 g / cm ３ , the liquid containing the non-fluorinated organic compound does not penetrate into the interior of the fibrous material in the container and remains on the surface of the fibrous material. In this state, the purpose of holding the liquid containing the non-fluorinated organic compound in the container cannot be achieved.

[0021] Also, when the density of the fibrous material is less than 0.04 g / cm ３ , the liquid containing the non-fluorinated organic compound cannot be retained in the fibrous material in the container, and when the container is tilted 90° and left standing for 24 hours, the liquid containing the non-fluorinated organic compound leaks out from the fibrous material. Similar to the above state, in this state, the purpose of holding the liquid containing the non-fluorinated organic compound in the container cannot be achieved. The density of the fibrous material is adjusted to 0.04 g / cm ３ or more and 1.54 g / cm ３ or less through a process of adjusting the density after adding the fibrous material into the container constituting the evaporation source. The adjustment method can be adjusted by processes such as pressurizing the fibrous material in the container or vibrating the fibrous material in the container, but any method can be used as long as the density can be adjusted within the density range of the present invention.

[0022] Furthermore, whether a fibrous material can hold a liquid containing a non-fluorinated organic compound is determined by a parameter consisting of the fiber diameter and density of the fibrous material, where the fiber diameter of the fibrous material is the numerator and the density of the fibrous material is the denominator. If the parameter consisting of the ratio of the fiber diameter to density of the fibrous material is greater than 0.31, the fibrous material in the container cannot retain the liquid containing the non-fluorinated organic compound, and the liquid will seep out from the fibrous material when the container is tilted. In the same state as described above, the purpose of holding the liquid containing the non-fluorinated organic compound in the container cannot be achieved. If the parameter consisting of the ratio of the fiber diameter to density of the fibrous material is 0.31 or less, the fibrous material in the container can retain the liquid containing the non-fluorinated organic compound, and the liquid will not seep out even when the container is tilted. Moreover, it is preferable that the parameter consisting of the ratio of the fiber diameter to density of the fibrous material is 0.20 or less.

[0023] (Liquid containing a non-fluorinated organic compound) The liquid containing a non-fluorinated organic compound in this invention has a kinematic viscosity of 0.57 mm at a temperature of 25°C. ２ / s or more, 14000mm ２ The density is less than or equal to / s. The fiber diameter in the container is 0.01 mm or more and 0.3 mm or less, and the density is 0.04 g / cm³. ３ Above, 1.54g / cm ３ A fibrous material having the following characteristics, and a fiber diameter-to-density ratio of 0.31 or less, and a kinematic viscosity of 0.57 mm at a temperature of 25°C. ２ / s or more, 14000mm ２ The effects of the present invention can be obtained by having a viscosity of 0.57 mm² or less. In other words, it is possible to provide a vapor deposition source for vacuum deposition coating that can prevent the leakage of liquid containing non-fluorine organic compounds from the deposition source due to vibration during logistics or tilting during storage, and maintain an appropriate content, thereby forming a high-quality film. The kinematic viscosity of the above-mentioned liquid containing non-fluorine organic compounds at 25°C is 0.57 mm². ２ / s or more, 14000mm ２ The kinematic viscosity is less than or equal to 0.57 mm². ２If the kinematic viscosity is lower than / s, it is difficult to obtain the outflow prevention effect of the present invention even if the fiber diameter and density of the fibrous material are modified. The kinematic viscosity is 4.0 mm ２ Preferably, it should be 7.0 mm or more. ２ It is more preferable that the kinematic viscosity is 14,000 mm² or higher. ２ If the kinematic viscosity is higher than / s, the vapor deposition source will not be able to penetrate the gaps in the fibrous material during manufacturing, and the effect of the present invention, which is to prevent leakage of the liquid containing non-fluorine organic compounds in the vapor deposition source due to vibration during logistics or tilting during storage, will not be achieved. The above kinematic viscosity is 9040 mm². ２ Preferably, it should be less than or equal to 6730 mm. ２ It is more preferable that the value be less than or equal to / s, and 6530 mm ２ It is particularly preferable that the kinematic viscosity be less than or equal to / s. A more preferable range for the above kinematic viscosity is 0.57 mm ２ / s or more 14000mm ２ / s or less, 4.0mm ２ / s or more 14000mm ２ / s or less, 7.0mm ２ / s or more 14000mm ２ It is less than or equal to / s, and more preferably 0.57 mm ２ / s or more 9040mm ２ / s or less, 4.0mm ２ / s or more 9040mm ２ / s or less, 7.0mm ２ / s or more 9040mm ２ It is less than or equal to / s, and more preferably 0.57 mm ２ / s or more 6730mm ２ / s or less, 4.0mm ２ / s or more 6730mm ２ / s or less, 7.0mm ２ / s or more 6730mm ２ It is less than or equal to / s, and more preferably 0.57 mm ２ / s or more 6530mm ２ / s or less, 4.0mm ２ / s or more 6530mm ２ / s or less, 7.0mm ２ / s or more 6530mm ２ It is less than or equal to / s.

[0024] There are no limitations on the method for measuring the kinematic viscosity of a liquid containing a non-fluorinated organic compound at a temperature of 25°C; measurement using a viscometer or the like is possible. In the following examples, the measurement was performed using an A&D Corporation tuning fork vibration viscometer SV-100. The non-fluorinated organic compound contained in the above liquid is an organic compound that, after being coated by vacuum deposition, has functions such as water repellency, oil repellency, scratch resistance, abrasion resistance, slipperiness, and insulation. A non-fluorinated organic compound is essentially a compound that does not contain fluorine atoms. Examples of non-fluorinated organic compounds having the above functions include non-fluorinated organic compounds having a long-chain alkyl moiety and non-fluorinated organic compounds having a siloxane moiety. Each of these will be described below.

[0025] (Non-fluorinated organic compounds having long-chain alkyl moieties) Non-fluorinated organic compounds having long-chain alkyl moieties have at least one long-chain alkyl moiety in the chemical structure constituting the compound. The non-fluorinated organic compounds having long-chain alkyl moieties in the present invention include polyolefins composed of long-chain alkyl groups. Furthermore, it is preferable that the non-fluorinated organic compounds having long-chain alkyl moieties are non-fluorinated organic compounds having both a long-chain alkyl moiety and a reactive moiety. The non-fluorinated organic compounds having long-chain alkyl moieties are preferably non-fluorinated organic compounds having an organic moiety having at least one bond selected from the group consisting of saturated hydrocarbon bonds, unsaturated hydrocarbon bonds, ether bonds, carbon-oxygen double bonds, carbon-nitrogen bonds, and carbon-nitrogen double bonds, and a reactive moiety. For use as an evaporation source for coating by vacuum deposition, it is preferable that the long-chain alkyl moiety has a total carbon number of 16 or more and 200 or less. Furthermore, it is preferable that it has a carbon number of 30 or more and 100 or less. The above-mentioned reactive sites are optional as long as they can be used for coating purposes, but are preferably hydroxyl groups, alkenyl groups, carboxyl groups, amino groups, epoxy groups, acryloyl groups, methacryloyl groups, polyether groups, mercapto groups, diol groups, and alkoxysilyl groups. Examples of alkoxysilyl groups include monoalkoxysilyl groups, dialkoxysilyl groups, and trialkoxysilyl groups. Among these, alkoxysilyl groups are preferred, preferably dialkoxysilyl groups and trialkoxysilyl groups, and even more preferably trialkoxysilyl groups.

[0026] The following are specific examples of non-fluorinated organic compounds having long-chain alkyl moieties, but the examples are not limited to these. Specifically, non-fluorinated organic compounds are, for example, compounds represented by general formula (1). １ -X-R ２(1) Here, “an organic site having at least one bond selected from the group consisting of saturated hydrocarbon bonds, unsaturated hydrocarbon bonds, ether bonds, carbon-oxygen double bonds, carbon-nitrogen bonds, and carbon-nitrogen double bonds” is the site represented by X in the general formula (1) above. The site represented by X in the general formula (1) above includes one or more sites having at least one bond selected from the group consisting of saturated hydrocarbon bonds, unsaturated hydrocarbon bonds, ether bonds, carbon-oxygen double bonds, carbon-nitrogen bonds, and carbon-nitrogen double bonds. Furthermore, an organic site having at least one bond selected from the group consisting of saturated hydrocarbon bonds, unsaturated hydrocarbon bonds, ether bonds, carbon-oxygen double bonds, carbon-nitrogen bonds, and carbon-nitrogen double bonds may have only one type of bond in one or more cases, or it may have a combination of two or more types of bonds.

[0027] Furthermore, the region indicated by X may branch during the combination and have a side chain that includes the region of the above group. R in the general formula (1) above １ and R ２ Each of these may independently be a hydrolyzable group, a silanol group, a hydroxyl group, a reactive organic group, an organic group containing a hydrolyzable group-containing silyl group, an alkylsilyl group, or a hydrogen atom. Preferably, it is an organic group containing a hydrolyzable group-containing silyl group, a hydroxyl group, and a hydrogen atom. More preferably, it is a hydroxyl group or a hydrogen atom. Examples of hydrolyzable groups include alkoxy groups having 1 to 10 carbon atoms such as methoxy, ethoxy, propoxy, and butoxy groups; alkoxyalkoxy groups having 2 to 10 carbon atoms such as methoxymethoxy and methoxyethoxy groups; acyloxy groups having 1 to 10 carbon atoms such as acetoxy groups; alkenyloxy groups having 2 to 10 carbon atoms such as isopropenoxy groups; halogen groups such as chloro, bromo, and iodo groups; and amino groups. Among these, methoxy, ethoxy, isopropenoxy, and chloro groups are preferred. Examples of reactive organic groups include methacryloyl, carboxyl, epoxy, and diol groups. Among these, methacryloyl groups and carboxyl groups are preferred.

[0028] An organic group containing a hydrolyzable group-containing silyl group is, for example, an organic group in which the hydrolyzable group is directly or indirectly bonded to a silicon atom. Examples of hydrolyzable groups include alkoxy groups having 1 to 10 carbon atoms such as methoxy, ethoxy, propoxy, and butoxy groups; alkoxyalkoxy groups having 2 to 10 carbon atoms such as methoxymethoxy and methoxyethoxy groups; acyloxy groups having 1 to 10 carbon atoms such as acetoxy groups; alkenyloxy groups having 2 to 10 carbon atoms such as isopropenoxy groups; halogen groups such as chloro, bromo, and iodo groups; and amino groups. The number of hydrolyzable groups in an organic group containing a hydrolyzable group-containing silyl group is preferably 1 to 3, more preferably 2 to 3, and even more preferably 3. An organic group containing a hydrolyzable group-containing silyl group may also have an alkylsilyl group as described later. In other words, examples of organic groups containing hydrolyzable silyl groups include trimethoxysilyl group, dimethoxymethylsilyl group, ethyldimethoxysilyl group, methoxydimethylsilyl group, diethylmethoxysilyl group, ethylmethoxymethylsilyl group, triethoxysilyl group, diethoxyethylsilyl group, diethoxymethylsilyl group, ethoxydiethylsilyl group, and ethoxyethylmethylsilyl group.

[0029] Examples of alkylsilyl groups include alkylsilyl groups having 1 to 10 carbon atoms, where the number of carbon atoms is preferably 1 to 5, more preferably 1 to 3, and particularly preferably 1. The number of alkyl groups is preferably 1 to 3, more preferably 2 to 3, and even more preferably 3. Specifically, examples of alkylsilyl groups include trimethylsilyl, triethylsilyl, ethyldimethylsilyl, and diethylmethylsilyl groups.

[0030] Specific examples of non-fluorinated organic compounds having long-chain alkyl moieties, or liquids containing non-fluorinated organic compounds, include the compounds shown in Table 1, but are not limited to these.

[0031]

[0032] (Non-fluorinated organic compounds having a siloxane bond-containing moiety) Non-fluorinated organic compounds having a siloxane bond-containing moiety have at least one siloxane moiety in the structure constituting the compound. The siloxane moiety is a moiety composed of a silicon atom and an oxygen atom, and in chemical formula it is a moiety having a structure in which -(Si-O)- is repeated. Preferably the above Si has at least one methyl group, a phenyl group, or a hydrogen atom. In addition, the moiety represented by X in the above general formula (1) may be bonded to the above Si. Specifically, in chemical formula it is -(Si(CH ３ ) ２ It is preferable that the moiety has a structure in which -O)- is repeated. The siloxane moiety is -(Si-(CH ３ ) ２ The number of repetitions of O)- is preferably 4 to 140, and more preferably 10 to 70. Furthermore, non-fluorinated organic compounds having a siloxane moiety preferably have a siloxane moiety and a reactive moiety in the chemical composition constituting the compound. The reactive moiety can be any as long as it can be used for coating applications, but is preferably a hydroxyl group, alkenyl group, carboxylic acid group, amino group, epoxy group, acrylic group, methacryloyl group, monoalkoxysilyl group, dialkoxysilyl group, or trialkoxysilyl group. Among these, dialkoxysilyl groups and trialkoxysilyl groups are preferred, and is even more preferably a trialkoxysilyl group. Specific examples of non-fluorinated organic compounds having a siloxane moiety are shown below, but are not limited to these.

[0033] Specifically, non-fluorinated organic compounds are, for example, non-fluorinated organic compounds having a siloxane bond site represented by general formula (2). ３ -Y-R ４(2) Specifically, preferably at least one selected from the group consisting of dimethylsiloxane compounds, diphenylsiloxane compounds, methylphenylsiloxane compounds, methylhydrogensiloxane compounds and phenylhydrogensiloxane compounds, and more preferably at least one selected from the group consisting of dimethylsiloxane compounds, diphenylsiloxane compounds and methylphenylsiloxane compounds.

[0034] In formula (2), the moiety represented by Y may have a portion of its side chain substituted with an organic group such as an amino group, epoxy group, mercapto group, carboxyl group, polyether group, or long-chain alkyl group. Furthermore, the moiety represented by Y may branch during the combination process and have a side chain containing the moieties from the above group.

[0035] R in general formula (2) ３ and R ４ Each of these is preferably independently a hydrolyzable group, a silanol group, a hydroxyl group, a reactive organic group, an organic group containing a hydrolyzable group-containing silyl group, an alkylsilyl group, or a hydrogen atom. Examples of hydrolyzable groups include alkoxy groups having 1 to 10 carbon atoms such as methoxy, ethoxy, propoxy, and butoxy groups; alkoxyalkoxy groups having 2 to 10 carbon atoms such as methoxymethoxy and methoxyethoxy groups; acyloxy groups having 1 to 10 carbon atoms such as acetoxy groups; alkenyloxy groups having 2 to 10 carbon atoms such as isopropenoxy groups; halogen groups such as chloro, bromo, and iodo groups; and amino groups. Among these, methoxy, ethoxy, isopropenoxy, and chloro groups are preferred. Examples of reactive organic groups include methacryloyl, carboxyl, epoxy, and diol groups. Among these, methacryloyl and carboxyl groups are preferred.

[0036] An organic group containing a hydrolyzable group-containing silyl group is, for example, an organic group in which the hydrolyzable group is directly or indirectly bonded to a silicon atom. Examples of hydrolyzable groups include alkoxy groups having 1 to 10 carbon atoms such as methoxy, ethoxy, propoxy, and butoxy groups; alkoxyalkoxy groups having 2 to 10 carbon atoms such as methoxymethoxy and methoxyethoxy groups; acyloxy groups having 1 to 10 carbon atoms such as acetoxy groups; alkenyloxy groups having 2 to 10 carbon atoms such as isopropenoxy groups; halogen groups such as chloro, bromo, and iodo groups; and amino groups. The number of hydrolyzable groups in an organic group containing a hydrolyzable group-containing silyl group is preferably 1 to 3, more preferably 2 to 3, and even more preferably 3. An organic group containing a hydrolyzable group-containing silyl group may also have an alkylsilyl group as described later. In other words, examples of organic groups containing hydrolyzable silyl groups include trimethoxysilyl group, dimethoxymethylsilyl group, ethyldimethoxysilyl group, methoxydimethylsilyl group, diethylmethoxysilyl group, ethylmethoxymethylsilyl group, triethoxysilyl group, diethoxyethylsilyl group, diethoxymethylsilyl group, ethoxydiethylsilyl group, and ethoxyethylmethylsilyl group.

[0037] Examples of alkylsilyl groups include alkylsilyl groups having 1 to 10 carbon atoms, where the number of carbon atoms is preferably 1 to 5, more preferably 1 to 3, and particularly preferably 1. The number of alkyl groups is preferably 1 to 3, more preferably 2 to 3, and even more preferably 3. Specifically, examples of alkylsilyl groups include trimethylsilyl, triethylsilyl, ethyldimethylsilyl, and diethylmethylsilyl groups.

[0038] Specific examples of non-fluorinated organic compounds having a siloxane bond-containing site include the compounds shown in Table 2, but the compound is not limited to these.

[0039]

[0040] (Method of deposition, article) The deposition source of the present invention, as described above, can be used to deposit a material onto a target by heating it by resistance heating or irradiation with an electron beam and causing it to evaporate. Specifically, any known method, such as a method using a vacuum deposition apparatus, can be used. In this way, by heating the deposition source by resistance heating or irradiation with an electron beam and causing it to evaporate, an article with a surface layer formed on the target can be obtained. The article can be any article, but examples include optical components such as eyeglass lenses, touch panels, and the like.

[0041] (Method for manufacturing a vapor deposition source) The present invention also includes a placement step of arranging a fibrous material in a container, and an impregnation step of impregnating the fibrous material with a liquid containing a non-fluorine organic compound or an impregnation solution containing a liquid containing a non-fluorine organic compound, wherein the liquid and the impregnation solution satisfy the above formula (i) at 25°C, and the fiber diameter x [mm] and density y [g / cm] of the fibrous material. ３ The invention provides a method for manufacturing a vapor deposition source that satisfies the above formulas (ii) to (iv).

[0042] The process of placing fibrous material into a container involves placing fibrous material, which has been processed to fit inside the container and be of an appropriate size, into the container. The method of placing the fibrous material into the container may be by hand using tweezers or the like, or by machine; any method that allows it to be placed in the appropriate position is acceptable.

[0043] The density of the fibrous material is 0.04 g / cm³. ３ Above, 1.54g / cm ３ To achieve this, a method such as pressurizing the container from the opening can be used.

[0044] By adding a liquid containing a non-fluorinated organic compound, or an impregnation solution containing a liquid containing a non-fluorinated organic compound and a solvent, to a container containing a fibrous material and then removing the solvent, the kinematic viscosity of the liquid containing the non-fluorinated organic compound at 25°C is reduced to 0.57 mm². ２ / s or more, 14000mm ２Let / s. If a liquid containing a non-fluorinated organic compound can be added to a container without adding a solvent, use a liquid containing a non-fluorinated organic compound whose kinematic viscosity at 25°C after being added to the container satisfies the range of the present invention. If the liquid containing a non-fluorinated organic compound needs to be made into a solution using a solvent, add an impregnation solution containing the liquid containing the non-fluorinated organic compound and the solvent to the container, remove the solvent, and then use a liquid containing a non-fluorinated organic compound whose kinematic viscosity at 25°C satisfies the range of the present invention. The method of adding the liquid containing the non-fluorinated organic compound or the impregnation solution containing the liquid containing the non-fluorinated organic compound and the solvent to the container is arbitrary as long as it is a method that can measure an appropriate amount for the deposition process. A dispenser or a dispenser may be used. Methods for removing the solvent from the solution containing the liquid containing the non-fluorinated organic compound and the solvent include forced air drying, vacuum drying, and heat drying. An appropriate removal method can be taken depending on the solvent.

[0045] The present disclosure will be described in more detail below with reference to examples, but the present disclosure is not limited to the following examples.

[0046] Hereinafter, one embodiment of the present invention will be described with reference to the drawings. Figure 1 is a diagram showing an example of the configuration of an evaporation source according to this embodiment. As shown in Figure 1, the evaporation source 10 of this embodiment has a configuration in which a fibrous material 2 is placed in, for example, a metal container 1, and a non-fluorine organic compound 3 is impregnated into the fibrous material 2.

[0047] [Example 1] (Container preparation) A container made by processing a 1 mm thick copper plate was placed inside a container containing fibrous material consisting of iron fibers (steel wool) with a fiber diameter of 0.012 mm, with a density of 0.04 g / cm³ inside the container. ３ The container was filled in such a manner to create a container with fibrous material installed. (Impregnation) 300 μl of compound h shown in Table 2 was weighed out using a micropipette and dropped into the above container to impregnate the steel wool with the non-fluorine organic compound h, thereby creating an evaporation source.

[0048] (Evaluation of impregnation feasibility) To determine whether a non-fluorine organic compound has impregnated the fibrous material in a container, 300 μl of the compounds shown in Tables 1 and 2 was weighed using a micropipette and visually checked whether the entire amount was impregnated into the fibrous material when dropped into the container. If the entire amount was impregnated, it was marked as "acceptable," and if the entire amount was not impregnated, it was marked as "unacceptable."

[0049] (Evaluation of leakage of non-fluorinated organic compounds from containers) To determine whether non-fluorinated organic compounds leak from containers containing fibrous material, 300 μl of the compounds shown in Tables 1 and 2 were weighed using a micropipette, dropped into the container, and allowed to completely impregnate the fibrous material. The container was then tilted 90° and left to stand for 24 hours, and the presence of leakage of the compound from the fibrous material was visually confirmed. Leakage was indicated as "yes," and no leakage as "no." Furthermore, containers where the entire amount of the above non-fluorinated organic compound could not be impregnated were not evaluated for leakage and were indicated as "-."

[0050] (Evaluation Results) The evaluation results are shown in Table 3-1.

[0051] [Examples 2-106] Fibrous materials having the fiber diameters described in Tables 3-1, 3-2, and 3-3 were filled into containers to the densities described in Tables 3-1, 3-2, and 3-3, respectively. Then, the compounds described in Tables 1 and 2 were weighed using a micropipette in the same manner as in Example 1 and dropped into the containers to prepare evaporation sources impregnated with non-fluorine organic compounds. The evaluation results are shown in Tables 3-1, 3-2, and 3-3.

[0052] [Examples 107-109] After filling containers with fibrous materials having the fiber diameters described in Table 3-3, respectively, to the density described in Table 3-3, C ６ H １４ A non-fluorine organic compound impregnation solution g was prepared by using as a solvent and non-fluorine organic compound e as a solute to make up 20 wt% of the total. Similar to Example 1, the non-fluorine organic compound impregnation solution g was weighed using a micropipette and dropped into a container, and then dried under reduced pressure to form C ６ H １４The components were removed, and an evaporation source impregnated with a non-fluorine organic compound was prepared. The evaluation results are shown in Table 3-3.

[0053] [Comparative Example 1] (Container Preparation) A container made by processing a 1 mm thick copper plate was filled with iron fibers (hereinafter referred to as steel wool) with a fiber diameter of 0.012 mm, so that the density inside the container was 0.03 g / cm³. ３ The container was filled in this manner to create a container with fibrous material installed. (Impregnation with non-fluorine organic compound) 300 μl of compound h shown in Table 2 was weighed out using a micropipette and dropped into the above container to create an evaporation source impregnated with non-fluorine organic compound h. The evaluation results are shown in Table 3-3.

[0054] [Comparative Examples 2-40] Fibrous materials having the fiber diameters described in Table 3-3 were each filled into containers to the density described in Table 3-3. Then, the non-fluorine organic compounds described in Tables 1 and 2 were weighed using a micropipette in the same manner as in Example 1 and dropped into the containers to prepare evaporation sources impregnated with the non-fluorine organic compounds. The evaluation results are shown in Table 3-3.

[0055]

[0056]

[0057] The present invention includes the following: (1) A container and a vapor deposition source comprising a fibrous material and a liquid in the container, wherein the liquid contains a non-fluorine organic compound, and its kinematic viscosity a at 25°C satisfies the following formula (i), and the fiber diameter x [mm] and density y [g / cm³] of the fibrous material. ３ ] is a vapor deposition source that satisfies the following formulas (ii) to (iv): 0.57 ≤ a ≤ 14000 (i) 0.01 ≤ x ≤ 0.30 (ii) 0.04 ≤ y ≤ 1.54 (iii) x / y ≤ 0.31 (iv) (2) The non-fluorine organic compound is a long-chain alkyl moiety having 16 or more carbon atoms and 200 or less, or -(Si-(CH ３ ) ２(1) The vapor deposition source according to (1), having any or both of the siloxane moieties having a siloxane bond with a repeating number of 4 to 140 O)-. (3) The vapor deposition source according to (1) or (2), wherein the nonfluorine organic compound has one or more selected from the group consisting of a hydroxyl group, an alkenyl group, a carboxyl group, an amino group, an epoxy group, an acryloyl group, a methacryloyl group, a polyether group, a mercapto group, a diol group, and an alkoxysilyl group. (4) The fiber diameter x [mm] and density y [g / cm] of the fibrous material. ３ (v) (5) A vapor deposition method comprising the step of heating and evaporating the vapor deposition source described in any one of (1) to (4) by resistance heating or electron beam irradiation. (6) An article having a surface layer formed by heating and evaporating the vapor deposition source described in any one of (1) to (5) by resistance heating or electron beam irradiation. (7) An optical component having a surface layer formed by heating and evaporating the vapor deposition source described in any one of (1) to (6) by resistance heating or electron beam irradiation. (8) A method comprising the placement step of arranging a fibrous material in a container, and the impregnation step of impregnating the fibrous material with an impregnation liquid containing a non-fluorine organic compound liquid or a liquid containing a non-fluorine organic compound, wherein the kinematic viscosity a at 25°C of the liquid and the impregnation liquid satisfies the following formula (i), and the fiber diameter x [mm] and density y [g / cm] of the fibrous material. ３ (i) 0.01 ≤ x ≤ 0.30 (ii) 0.04 ≤ y ≤ 1.54 (iii) x / y ≤ 0.31 (iv) (9) The method for manufacturing a vapor deposition source according to (8), wherein the impregnation liquid contains a solvent, and the method includes a solvent removal step after the impregnation step in which the solvent is removed.

[0058] 10 Evaporation source 1 Container 2 Fibrous material 3 Non-fluorinated organic compound

Claims

1. A container and a vapor deposition source containing a fibrous material and a liquid, wherein the liquid contains a non-fluorine organic compound, its kinematic viscosity a at 25°C satisfies the following formula (i), and the fiber diameter x [mm] and density y [g / cm³] of the fibrous material. ３ The vapor deposition source satisfies the following equations (ii) to (iv): 0.57 ≤ a ≤ 14000 (i) 0.01 ≤ x ≤ 0.30 (ii) 0.04 ≤ y ≤ 1.54 (iii) x / y ≤ 0.31 (iv) 2. The non-fluorinated organic compound is a long-chain alkyl moiety having 16 to 200 carbon atoms, or -(Si-(CH ３ ) ２ The vapor deposition source according to claim 1, comprising any or both of the siloxane moieties having a siloxane bond with a number of repeating O)- symbols of 4 to 140.

3. The vapor deposition source according to claim 1 or 2, wherein the nonfluorine organic compound has one or more selected from the group consisting of a hydroxyl group, an alkenyl group, a carboxyl group, an amino group, an epoxy group, an acryloyl group, a methacryloyl group, a polyether group, a mercapto group, a diol group, and an alkoxysilyl group.

4. Fiber diameter x [mm] and density y [g / cm³] of the fibrous material. ３ The vapor deposition source according to any one of claims 1 to 3, wherein the following formula (v) is satisfied: x / y ≤ 0.20 (v) 5. A vapor deposition method comprising the step of heating and evaporating the vapor deposition source described in any one of claims 1 to 4 by resistance heating or irradiation with an electron beam.

6. An article having a surface layer formed by heating and evaporating the deposition source according to any one of claims 1 to 5 by resistance heating or electron beam irradiation.

7. An optical component having a surface layer formed by heating and evaporating the deposition source according to any one of claims 1 to 6 by resistance heating or electron beam irradiation.

8. The process includes a placement step of arranging a fibrous material in a container, and an impregnation step of impregnating the fibrous material with a liquid containing a non-fluorine organic compound or an impregnation solution containing a liquid containing a non-fluorine organic compound, wherein the liquid and the impregnation solution satisfy the following formula (i) at 25°C, and the fiber diameter x [mm] and density y [g / cm³] of the fibrous material. ３ The following is a method for manufacturing a vapor deposition source that satisfies equations (ii) to (iv): 0.57 ≤ a ≤ 14000 (i) 0.01 ≤ x ≤ 0.30 (ii) 0.04 ≤ y ≤ 1.54 (iii) x / y ≤ 0.31 (iv) 9. The method for producing a vapor deposition source according to claim 8, wherein the impregnation liquid contains a solvent, and the method includes a solvent removal step after the impregnation step to remove the solvent.

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