WO2010116714A1 - Dalle d'écran, son procédé de fabrication et leur utilisation dans la production de dispositifs d'affichage et d'autres articles - Google Patents

Dalle d'écran, son procédé de fabrication et leur utilisation dans la production de dispositifs d'affichage et d'autres articles Download PDF

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WO2010116714A1
WO2010116714A1 PCT/JP2010/002497 JP2010002497W WO2010116714A1 WO 2010116714 A1 WO2010116714 A1 WO 2010116714A1 JP 2010002497 W JP2010002497 W JP 2010002497W WO 2010116714 A1 WO2010116714 A1 WO 2010116714A1
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group
face plate
display device
fluorine
film
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PCT/JP2010/002497
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English (en)
Japanese (ja)
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小川一文
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国立大学法人香川大学
日本電気株式会社
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Publication of WO2010116714A1 publication Critical patent/WO2010116714A1/fr

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    • C—CHEMISTRY; METALLURGY
    • C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
    • C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
    • C08J7/00—Chemical treatment or coating of shaped articles made of macromolecular substances
    • C08J7/12—Chemical modification
    • C08J7/126—Halogenation

Definitions

  • the present invention relates to a face plate for a display device, a manufacturing method thereof, and a display device and an article using the same, and more specifically, has high durability, can be manufactured at low cost, and is highly safe for human bodies and the environment.
  • the present invention relates to a face plate for a display device including an optical lens and a housing with less adhesion of fingerprints, a manufacturing method thereof, a display device and an article using the same.
  • Patent Document 1 discloses a glass plate on which a highly durable water / oil repellent / antifouling coating is formed, the water / oil repellent / antifouling coating comprising at least a fluorocarbon group and a hydrocarbon group.
  • a water / oil repellent / antifouling glass characterized in that it comprises at least one composite film containing a substance mainly containing a silyl group (for example, perfluoroalkylalkoxysilane) and a substance mainly containing a siloxane group.
  • a plate and its manufacturing method are disclosed.
  • Patent Document 2 discloses a technique for antifouling the surface of a member using fluorine gas.
  • Patent Document 1 has a drawback that the production cost is high because an expensive fluorocarbon silane compound is used.
  • the method described in Patent Document 2 does not require a solvent during the antifouling treatment, but has a problem that transparency is deteriorated due to the treatment, and a long time (several hours) is required for the reaction, so that the efficiency is poor. have.
  • the present invention has been made in view of such circumstances, and a face plate for a display device including an optical lens and a housing that has a low environmental impact at the time of processing or disposal, and that can be manufactured inexpensively and has a low adhesion of fingerprints and the like, and its manufacture. It is an object of the present invention to provide a method and a display device and an article using them.
  • the present invention solves the above-mentioned problems by providing a face plate for a display device, wherein a non-existent substance is present so as to cover at least a part of a transparent substrate exposed on the surface on the outer side.
  • the “display device” includes a device operation touch panel and a portable information terminal having both a display function and an operation function.
  • the “article” includes a mobile phone, an electronic computer, a PDA (personal digital assistant), a GPS terminal, a television receiver, a cash dispenser (CD) device, an automatic teller machine (ATM), and the like.
  • the “face plate” is a transparent member that covers the outermost surface of the display surface of the display device.
  • the touch panel has a display surface protection and input function, a camera lens of a mobile phone that is an information input member, and an input.
  • a touch panel portion of a portable information terminal that also serves as a housing and a housing is also included in the “face plate” in the present invention.
  • the “outside surface” refers to a surface that becomes the outside when the display device is assembled as a face plate, and may be abbreviated as “outside surface” hereinafter.
  • At least a part of the outer surface of the face plate for a display device including a camera lens and a housing incorporated in a cellular phone has a part or all of the hydrogen atoms in the hydrocarbon group are fluorine atoms and fluorocarbon groups.
  • the display device faceplate according to the first aspect of the present invention wherein the fluorine-containing functional group has a hydrocarbon group present so as to cover at least a part of the outer surface of the substrate.
  • water / oil / oil repellency / antifouling property water / oil / oil / oil repellency / antifouling property can be obtained at a lower cost than when an expensive fluorocarbon film compound is used.
  • a face plate for a display device having the above can be manufactured.
  • the substance having a fluorine-containing functional group includes a linear film substance having the fluorine-containing functional group, which is the outside of the substrate.
  • An organic thin film chemically bonded to the surface on the side may be formed. Since the substance having a fluorine-containing functional group present so as to cover at least a part of the surface on the outer side of the base material forms an organic thin film having a nanometer level film thickness, Water and oil repellency can be imparted without impairing optical properties and the like.
  • the fluorine-containing functional group is any one of a hydrocarbon group, a hydrocarbon group having an ester group, and a hydrocarbon group having an ether group. Or the functional group by which the several hydrogen atom was substituted by either a fluorine atom or a fluorocarbon group may be sufficient.
  • the fluorine-containing functional group is any one or more hydrogen atoms in the functional groups represented by the following formulas (I) to (V): It may be a functional group substituted with either a fluorine atom or a fluorocarbon group.
  • n and n each independently represent an integer of 0 or more and 24 or less, and m ⁇ n.
  • the fluorine-containing organic thin film may be a monomolecular film of the film substance chemically bonded to the outer surface of the substrate.
  • the fluorine-containing organic thin film is a monomolecular film, the appearance (color tone, gloss, etc.) and optical properties of the base material are not impaired, and it can be suitably applied to optical materials and housings of various devices.
  • the fluorine-containing organic thin film is chemically bonded to the surface on the outer side of the base material, it is excellent in durability and can exhibit water / oil / oil repellency / antifouling properties over a long period of time.
  • the fluorine-containing organic thin film may contain polysiloxane molecules formed of alkoxysilane and / or alkoxypolysiloxane.
  • the film substance having the fluorine-containing hydrocarbon group is bonded to the outside of the base material through a film of the polysiloxane molecule bonded and fixed to the surface on the outside side of the base material. It may be bonded and fixed to the surface on the other side.
  • the polysiloxane molecule coating is formed on the base material via a bond formed by a reaction between an alkoxysilyl group and a surface functional group present on the outer surface of the base material.
  • a part of the film substance having the fluorine-containing hydrocarbon group fixed to the outer surface is directly bonded to the outer surface of the substrate, and the rest is coated with the polysiloxane molecule. It may be bonded and fixed to the outer surface of the substrate.
  • the polysiloxane molecule coating film has a nanometer-level film thickness, so that the thermal conductivity is not impaired. Therefore, it can be suitably applied to a heat radiating member.
  • the polysiloxane molecule is an alkoxysilane and / or a formula (VII) represented by the following formula (VI): It may be formed by a condensation reaction of an alkoxypolysiloxane represented by: SiH x (OA) 4-x (VI) (AO) 3 Si (OSi (OA) 2 ) n OSi (OA) 3 (VII) In the formulas (VI) and (VII), x is 0, 1, or 2; A represents an alkyl group, n is 0, 1, or 2.
  • the substance having a fluorine-containing functional group may be a fluorine-containing organic polymer having the fluorine-containing functional group. Since the fluorine-containing organic polymer is present so as to cover at least a part of the surface on the outer side of the substrate, it has both water and oil repellency and can prevent the adhesion of dirt to the outer surface.
  • a surface roughness of the outer side surface is 10 nm or more and 400 nm or less. If the surface roughness of the outer surface of the face plate for a display device is 400 nm or less, which is the shortest wavelength of visible light, the transparency and optical characteristics of the face plate for a display device are obtained even when a transparent substrate is used. High water and oil repellency and antifouling properties can be imparted without impairing water.
  • a surface on the outer side of a transparent base material present so that the transparent substance having a hydrocarbon group covers at least a part of the surface on the outer side of the face plate.
  • step A in a gas atmosphere of a compound containing a fluorocarbon group, the surface of the substance having a hydrocarbon group on the surface of the substrate is subjected to low-pressure plasma treatment so that a part or all of the hydrogen atoms in the hydrocarbon group are fluorine.
  • a fluorocarbon group By substituting with one or both of an atom and a fluorocarbon group, water and oil repellency is imparted. Therefore, it is possible to manufacture a face plate for a display device having water repellency, oil repellency and antifouling properties at a lower cost than when an expensive fluorocarbon film compound is used.
  • the side that is outside the substrate in the mixed atmosphere of the compound gas containing the fluorocarbon group and the oxygen gas in the step A, the side that is outside the substrate in the mixed atmosphere of the compound gas containing the fluorocarbon group and the oxygen gas.
  • the surface of the substance having the hydrocarbon group on the surface may be subjected to low-pressure plasma treatment. If the substrate is subjected to low-pressure plasma treatment in a mixed atmosphere of a compound gas containing a fluorocarbon group and oxygen gas, a water- and oil-repellent and antifouling member having higher efficiency and higher durability can be provided.
  • the unevenness having a surface roughness of 10 nm or more and 400 ⁇ m or less is formed on the outer surface of the substrate before the step A. You may further have the process B to form.
  • the apparent surface energy of the surface of the water / oil repellent transparent member can be significantly reduced as compared with the case of a flat surface, and high water / oil repellent / antifouling properties can be imparted.
  • the surface roughness of the water / oil repellent transparent member is 400 nm or less which is the shortest wavelength of visible light, even when used for a transparent lens or face plate, the transparency of the lens or face plate is impaired. High water and oil repellency and antifouling properties can be imparted.
  • the coating of the substance containing a hydrocarbon group covering at least a part of the outer surface of the substrate is formed on the substrate.
  • a treatment liquid containing a film compound having a hydrocarbon group is brought into contact with the surface on the outer side of the substrate.
  • An organic thin film containing a hydrocarbon group may be formed by a reaction between the film compound and a surface functional group on the surface on the outer side of the substrate.
  • the coating of the substance having a hydrocarbon group formed on the surface on the outer side of the substrate is an organic thin film having a film thickness of nanometer level, so that the optical characteristics and the like of the substrate are impaired. Water and oil repellency can be imparted without any problem.
  • the film compound includes any one of a hydrocarbon group, a hydrocarbon group having an ester group, and a hydrocarbon group having an ether group. May be.
  • the film compound may be a film compound represented by the following formula (X).
  • Z-SiX p Y 3-p (X) Z represents a substituent containing any one of an alkyl group having 25 or less carbon atoms, an aryl group, a vinyl group, and a silicone group
  • X represents a hydrogen atom or a substituent containing any one of an alkyl group having less carbon atoms than Z, an aryl group, a vinyl group, and a silicone group
  • Y represents a halogen atom or an alkoxyl group
  • p represents 0, 1 or 2.
  • the film compound containing a hydrocarbon group is a film compound represented by any of the following formulas (XI) to (XV): May be. CH 3 (CH 2) n Si (OA) 3 (XI) [CH 3 (CH 2 ) n ] 2 Si (OA) 2 (XII) [CH 3 (CH 2 ) n ] 3 Si (OA) (XIII) CH 3 (CH 2 ) m —COO— (CH 2 ) n Si (OA) 3 (XIV) CH 3 (CH 2 ) m —O— (CH 2 ) n Si (OA) 3 (XV)
  • m and n each independently represent an integer of 0 or more and 24 or less
  • A represents an alkyl group.
  • the treatment liquid is an alkoxysilane represented by the following formula (VI) and / or an alkoxypolysiloxane represented by the formula (VII): May be included.
  • x is 0, 1, or 2
  • A represents an alkyl group
  • n is 0, 1, or 2.
  • a solution containing the alkoxysilane and / or the alkoxypolysiloxane is used on the outer side of the substrate.
  • a surface is treated to form a polysiloxane molecule film on the surface, and then the substrate on which the polysiloxane molecule film is formed is treated with the treatment liquid, and the organic layer is formed on the polysiloxane molecule film.
  • a thin film may be formed.
  • a film containing an organic polymer may be formed as the substrate in the step C.
  • a third aspect of the present invention solves the above problem by providing a display device using the face plate for a display device according to the first aspect of the present invention.
  • a fourth aspect of the present invention solves the above problem by providing an article using the display device according to the third aspect of the present invention.
  • the article according to the fourth aspect of the present invention is any of a mobile phone, an electronic computer or a display device for an electronic computer, a portable information terminal, a GPS terminal, a television receiver, a cash dispenser device, and an automatic teller machine. May be. Furthermore, the lens used for them and the housing itself may be combined. All of these articles are used for articles that often come into contact with the human body, and antifouling properties are strongly required from the viewpoint of hygiene, and the present invention can be suitably applied.
  • a face plate for a display device having a face plate that can be manufactured at a low cost at the time of processing and disposal, and a manufacturing method thereof, and a display device and an article using them. Further, according to the method of the present invention, it is possible to impart a water / oil repellent / antifouling function only on the outermost surface of the face plate having a hydrocarbon group on the outer surface at low cost, resource saving, energy saving.
  • the display device according to the present invention and an article using the display device have high antifouling properties, durability, safety for human bodies and the environment, and can exhibit antifouling properties semipermanently.
  • FIG. 3 is an explanatory diagram schematically showing an enlarged cross-sectional structure of the face plate for a display device according to the first embodiment of the present invention up to a molecular level.
  • the manufacturing method of the face plate for display apparatuses it is explanatory drawing which expanded and expanded the cross-sectional structure of the base material in which the organic thin film was formed to the molecular level typically.
  • the display device faceplate 1 As shown in FIG. 1, the display device faceplate 1 according to each embodiment of the present invention (hereinafter, the display device faceplates 10, 20, and 30 according to first to fourth embodiments which will be described individually). , 40 generic name), a transparent substance 2 having a fluorine-containing functional group in which some or all of the hydrogen atoms in the hydrocarbon group are substituted with either or both of a fluorine atom and a fluorocarbon group (hereinafter, Surfaces on the outer side of the fluorine-containing organic thin films 11, 21, 31 according to the first to third embodiments and the fluorine-containing organic polymer 41 according to the fourth embodiment, which will be described individually, At least a part of the outer surface of the transparent base material 3 exposed to the surface (hereinafter collectively referred to as base materials 12, 22, 32, and 42 according to first to fourth embodiments which will be described individually) As an example, it exists so as to cover the entire surface of the substrate 3 It is present to cover the are shown.) For engagement.
  • a face plate for a display device (hereinafter sometimes abbreviated as “face plate”) 1 is a base material 3 (covering at least a part of a surface on the outer side of a substance having a hydrocarbon group.
  • face plate Is manufactured by a method including a step A in which a low-pressure plasma treatment is performed in a gas atmosphere containing a fluorocarbon group (see FIGS. 2, 4, 7, and 8 (b)).
  • the fluorine-containing functional group is a gas atmosphere of a compound containing a fluorocarbon group on the surface on the outer side of the substrate 3 (substance having a hydrocarbon group present so as to cover at least a part thereof). It is obtained by low-pressure plasma treatment.
  • step A When plasma is generated by high frequency discharge in a gas atmosphere of a compound containing a fluorocarbon group, a fluorocarbon radical such as a fluorine radical ( ⁇ F) or a trifluoromethyl radical ( ⁇ CF 3 ) is generated. These radicals replace the hydrogen atom of the hydrocarbon group on the surface on the outside of the substrate 3 with trifluoromethyl groups 19 and 43 (an example of a fluorine atom or a fluorocarbon group) (FIGS. 2, 4, 7, 8 (b)).
  • a gas containing a compound having an unsaturated bond such as tetrafluoroethylene
  • a perfluoroalkyl group having a large carbon number can also be generated by plasma polymerization.
  • any plasma treatment apparatus that can be used for plasma surface treatment or low-temperature ashing can be used.
  • the form of the chamber include a flow tube type, a bell jar type, etc., and as a form of the electrode for discharge, a parallel plate type, a coaxial cylindrical type, a curved counter plate type such as a cylinder, a sphere, etc.
  • Examples include a hyperboloid opposed flat plate type and a plurality of fine wire opposed flat plate types.
  • the high frequency current can be applied by either a capacitive coupling method or an induction method using an external electrode.
  • the output of the high-frequency power source is appropriately adjusted depending on the material and size of the base material, the type of compound containing a fluorocarbon group used, the type and volume fraction of the added gas, the volume and pressure of the chamber, etc. For example, 10 to 250 W.
  • Examples of the compound containing a fluorocarbon group that has been confirmed to be usable include CF 4 , C 2 F 6 , C 2 F 4 , and CHF 3 .
  • CF 4 fluorocarbon group
  • C 2 F 6 C 2 F 4
  • CHF 3 CHF 3
  • even a compound that contains a CF 3 group and is liquid at normal temperature and pressure can be used as long as it can be gasified under low-pressure plasma processing conditions.
  • a trace amount (0.1 to 5% by volume) of Ar, He or the like is mixed, there is an effect of stabilizing the discharge.
  • low pressure plasma treatment may be performed in a gas atmosphere of a compound containing a fluorocarbon group after performing low pressure plasma treatment in an oxygen gas atmosphere in advance and performing oxidative etching of the outer surface.
  • Plasma treatment in an oxygen gas atmosphere has an action of cleaning the outer surface of the substrate 12 and an action of roughening the outer surface.
  • the thickness can be controlled in the range of several nanometers to several hundred microns.
  • the base material 3 used for manufacturing the face plate 1 for a display device is transparent and needs to be present so as to cover at least a part of the surface on the outer side, the substance having a hydrocarbon group, There is no restriction
  • a coating of a substance containing a hydrocarbon group covering at least a part of the outer surface is formed. It can be formed on the outer surface of the substrate 3.
  • Specific examples of the material of the substrate 3 include organic materials such as resins and inorganic materials such as glass.
  • transparent resins are polyurethane, polyester, polyethylene, polyphenylene sulfide, polyethylene terephthalate, polyethylene naphthalate, polyvinylidene chloride, polyvinyl chloride, polyolefin, polycarbonate, polyvinyl acetate, polystyrene, polysulfone, polytrimethylene terephthalate.
  • Polylactic acid Polyvinyl alcohol, polyvinyl pyrrolidone, polybutylene terephthalate, polybutylene naphthalate, polyvinylidene fluoride, polypropylene, polymer alloy, polymethylpentene, ionomer resin, acrylic resin, acetylcellulose, alkyd resin, AS resin, liquid crystal polymer, Examples include ABS resin, epoxy resin, urea resin, and other engineering plastics.
  • transparent inorganic materials include soda-lime glass, quartz glass, borosilicate glass, crystal glass, glass ceramics, and other metal oxides such as indium oxide, magnesium oxide, and ITO, sodium chloride, and fluoride. Examples thereof include inorganic salts such as single crystals, diamond, and DLC.
  • the base material 3 does not need to be a bulk material, and may be a thin film material such as a vapor deposition film or a coating, or may be a laminated material or the like.
  • the transparent thin film material include a hard coat film containing silica covering the surface of the transparent resin plate, an ITO film, or a sol-gel film of a transparent metal oxide (silica, alumina, zirconia, etc.).
  • these thin film materials may have functions of a surface protective film, a polarizing filter, a transparent conductor layer, and the like.
  • any known method such as vapor phase epitaxy (PVD and CVD), coating of a coating agent, formation of a fine particle film using nanoparticles, etc., a sol-gel method can be used.
  • the thickness of the substrate 3 may be reduced so as to have flexibility, and a transparent conductor layer such as ITO may be provided on the back side. Or what adhered these resin on the outer surface of transparent base materials, such as glass, may be used as the base material 3.
  • the surface roughness of the outer surface of the face plate 1 for display device or the substrate 3 is 10 nm or more and 400 nm or less, preferably 360 nm or less, more preferably 300 nm or less.
  • the shape of the irregularities on the outer surface of the face plate 1 for a display device is not particularly limited as long as the optical characteristics of the base material 3 are not impaired by diffraction or irregular reflection of incident light. It may be a simple shape. In general, when the surface roughness is within the above range, the surface hydrophobicity of the base material 3 can be further improved without deteriorating the surface characteristics of the base material 3, and the optical properties of visible light such as the transparency of the base material 3 can be improved. There is no loss of properties.
  • the surface roughness can be measured using any known method such as a surface roughness meter or a three-dimensional measuring instrument. Further, the size of the unevenness can be measured by image analysis using a stereoscopic microscope or an electron micrograph.
  • an decyl group (C 10 H 21 : an alkyl group that is a hydrocarbon group) is formed on the outer surface of the substrate 12.
  • a hydrogen atom of a terminal methyl group is substituted with a trifluoromethyl group 19 (a part or all of the hydrogen atoms are substituted with one or both of a fluorine atom and a fluorocarbon group)
  • a fluorine-containing organic thin film 11 including an example of a film substance having a fluorine-containing hydrocarbon group is formed.
  • the fluorine-containing organic thin film 11 is a monomolecular film made of a film substance that is covalently bonded (an example of a chemical bond) to the outer surface of the substrate 12.
  • the face plate 10 for a display device is produced by bringing a treatment liquid containing a film compound having a hydrocarbon group into contact with the outer surface of the substrate 12 and reacting the film compound with the surface functional group of the substrate 12.
  • Step C for forming an organic thin film (an example of a substance having a hydrocarbon group present so as to cover at least a part of the outer surface of the base material 12) 18 containing the obtained film material, and a fluorocarbon group
  • a part or all of the hydrogen atoms in the hydrocarbon groups contained in the organic thin film 18 are fluorine atoms by subjecting the outer surface of the base material 12 on which the organic thin film 18 has been formed in a gas atmosphere of a compound containing And a step A of forming the fluorine-containing organic thin film 11 substituted with one or both of fluorocarbon groups.
  • step B you may roughen the outer surface of the base material 12 so that it may have the surface roughness and the magnitude
  • the order in which step B is performed may be before or after step C. That is, the steps A to C include (1) Step B ⁇ Step C ⁇ Step A (the organic thin film 18 is formed after roughening the outer surface of the substrate 12), and (2) Step C ⁇ Step B. ⁇ You may carry out in any order of step A (roughening the outer surface of the substrate 12 on which the organic thin film 18 is formed).
  • the order of each step is the same for the manufacturing methods of the display device face plates 20 and 30 according to the second and third embodiments described later.
  • step B As a method for roughening the surface on the outer side of the substrate 12, the surface is roughened in advance using any known method such as sandblasting, mechanical polishing, and chemical treatment with chromic acid mixture, phosphoric acid, alkali, or the like.
  • the low pressure plasma treatment can be performed in an atmosphere containing oxygen gas and chlorine gas. Plasma treatment conditions may be adjusted as appropriate so that a surface having a desired surface roughness and unevenness can be obtained.
  • the apparatus and processing conditions used for the low-pressure plasma processing are the same as in the case of step A, and thus detailed description thereof is omitted.
  • the treatment liquid used for forming the organic thin film 18 in the step C is prepared by dispersing the film compound in a solvent.
  • “dispersion” means a state in which any one of a uniform solution, a suspension, and an emulsion is formed.
  • the membrane compound that can be used include any compound that contains a chain-like lipophilic functional group and can form a film made of the membrane substance 2 on the outer surface of the substrate 12.
  • Preferred surface functional groups include alkoxysilyl groups that react relatively rapidly with hydroxyl groups present on the surface of many materials at room temperature.
  • the lipophilic functional group is preferably a linear long-chain alkyl group having self-organization.
  • a silane compound represented by the following general formula (X) can be used as the film compound.
  • Z represents a substituent containing any one of an alkyl group having 25 or less carbon atoms, an aryl group, a vinyl group, and a silicone group
  • X represents a hydrogen atom or a substituent containing any one of an alkyl group having less carbon atoms than Z, an aryl group, a vinyl group, and a silicone group
  • Y represents a halogen atom or an alkoxyl group
  • p represents 0, 1 or 2.
  • a preferred film compound is, for example, an alkoxysilane compound represented by any of the following formulas (XI) to (XV).
  • m and n each independently represent an integer of 0 or more and 24 or less (where m ⁇ n), and A is an alkyl group, more preferably a methyl group or an ethyl group. Represents.
  • the membrane compound include compounds shown in the following (1) to (19).
  • the concentration of the membrane compound contained in the treatment liquid is preferably 0.1 mmol / L to 10 mmol / L.
  • concentration of the membrane compound is less than 0.1 mmol / L, it is difficult to form a uniform organic thin film 18, and when the concentration exceeds 10 mmol / L, gelation is likely to occur and storage stability is reduced. To do.
  • any liquid that can dissolve or stably disperse the membrane compound can be used. Since the membrane compound has high hydrophobicity, an organic solvent is used to dissolve it. However, it is preferable to use water from the viewpoint of reducing the environmental load during the manufacturing of the face plate 10 for a display device. However, it is difficult to dissolve or stably disperse the membrane compound only by using water as it is. Therefore, when water is used as a solvent, the treatment liquid contains a surfactant and / or alcohol in order to solubilize or stably disperse the membrane compound in a solvent mainly composed of water.
  • tetraalkylammonium salt which is a cationic surfactant, more specifically, a tetraalkylammonium represented by the following formula (VIII): Salt.
  • R 1 represents an alkyl group having 1 to 20 carbon atoms, more preferably 12 to 16 carbon atoms
  • R 2 , R 3 , and R 4 represent a methyl group or an ethyl group, more preferably a methyl group
  • X represents a halogen.
  • a particularly preferred tetraalkylammonium salt is hexadecyltrimethylammonium bromide CH 3 (CH 2 ) 15 N (CH 3 ) 3 Br.
  • the concentration of the tetraalkylammonium salt is preferably 0.1 mmol / L to 10 mmol / L, more preferably 0.5 mmol / L to 5 mmol / L.
  • concentration is less than 0.1 mmol / L, the membrane compound cannot be sufficiently solubilized, and when it exceeds 10 mmol / L, the pH of the treatment liquid falls outside the optimum range described later or bubbles are generated. There is a fear.
  • any alcohol that can uniformly disperse the membrane compound in water can be used.
  • ethanol, propanol (1-propanol and 2) that are compatible with water and have high volatility are used.
  • -Propanol butanol (1-butanol, 2-butanol, 2-methyl-2-propanol) and ethylene glycol are preferred.
  • These alcohols may be used alone, or any two or more kinds may be mixed and used at an arbitrary ratio.
  • the mixing ratio of water and alcohol is not particularly limited, but the volume ratio of water and alcohol is preferably 80:20 to 95: 5.
  • An acid or a base may be added to the treatment liquid in order to adjust the pH.
  • a preferred pH range is 5-12. When the pH is less than 5, the organic thin film 18 having a high density is not formed, and the storage stability of the treatment liquid is lowered. Moreover, when pH exceeds 12, there exists a possibility that the formed organic thin film 18 may be destroyed by the alkali hydrolysis of a siloxane bond.
  • the treatment liquid is prepared by a method having a step of mixing and dispersing a membrane compound and a solvent (preferably water containing a surfactant and / or alcohol). First, those components weighed so as to have a desired composition ratio are mixed. The order of adding each component is not particularly limited. Next, when the mixture is treated using an ultrasonic disperser or a homogenizer, a part of the alkoxysilyl group is converted into a silanol group by hydrolysis, and a uniform and transparent treatment liquid is obtained.
  • the treatment temperature and time are not limited, but when an ultrasonic disperser is used, for example, the treatment is performed at room temperature for 10 minutes.
  • Formation of the organic thin film 18 using the treatment liquid obtained as described above can be performed using, for example, the following method.
  • a treatment liquid is applied to the outer surface of the substrate 12 and left to stand until most of the solvent is volatilized (for example, in the atmosphere at room temperature for 1 hour).
  • the film compound is bonded to the outer surface of the base material 12 through a covalent bond (siloxane bond) formed by a condensation reaction between a hydroxyl group (not shown) on the outer surface of the base material 12 and an alkoxysilyl group.
  • a (monomolecular film) 18 is formed (see FIG. 3).
  • an extra film compound may remain on the outer surface of the substrate 12, but in such a case, it may be removed by washing with a solvent. If there is a small amount of excess membrane compound, there is a problem that even if it is left unwashed, a condensation reaction occurs due to silanol groups generated by hydrolysis of alkoxyl groups by moisture in the air, resulting in the formation of membrane materials. There is no.
  • a condensation catalyst may be added.
  • metal salts such as carboxylic acid metal salts, carboxylic acid ester metal salts, carboxylic acid metal salt polymers, carboxylic acid metal salt chelates, titanate esters and titanate ester chelates can be used.
  • the addition amount of the condensation catalyst is preferably 0.2 to 5% by mass of the alkoxysilane compound, more preferably 0.5 to 1% by mass.
  • carboxylic acid metal salts include stannous acetate, dibutyltin dilaurate, dibutyltin dioctate, dibutyltin diacetate, dioctyltin dilaurate, dioctyltin dioctate, dioctyltin diacetate, stannous dioctanoate, naphthenic acid Lead, cobalt naphthenate, iron 2-ethylhexenoate.
  • carboxylic acid ester metal salt examples include dioctyltin bisoctylthioglycolate ester salt and dioctyltin maleate ester salt.
  • carboxylic acid metal salt polymer examples include dibutyltin maleate polymer and dimethyltin mercaptopropionate polymer.
  • carboxylic acid metal salt chelate examples include dibutyltin bisacetylacetate and dioctyltin bisacetyllaurate.
  • titanate ester examples include tetrabutyl titanate and tetranonyl titanate.
  • a specific example of a titanate chelate is bis (acetylacetonyl) di-propyl titanate.
  • reaction time is further shortened. it can.
  • H3 of Japan Epoxy Resin Co. which is a ketimine compound, can be used instead of dibutyltin diacetate.
  • condensation catalyst a mixture of H3 and dibutyltin diacetate manufactured by Japan Epoxy Resin Co., Ltd. (mixing ratio is 1: 1) may be used.
  • the ketimine compound that can be used here is not particularly limited.
  • organic acid which can be used, For example, a formic acid, an acetic acid, propionic acid, a butyric acid, malonic acid etc. are mentioned.
  • a halosilane compound having a halosilyl group instead of the alkoxysilyl group may be used as the film compound.
  • a silanol condensation catalyst and a co-catalyst are not required, but halosilyl groups react quickly with water (including moisture in the air) and alcohol, so that a solvent containing water or alcohol cannot be used as a solvent.
  • the application of the treatment liquid to the outer surface of the substrate 12 and the reaction must be performed under dry conditions (relative humidity of 45% or less).
  • the fluorine-containing organic thin film 21 includes polysiloxane molecules 24 formed from alkoxysilane and / or alkoxypolysiloxane. More specifically, as shown in FIG. 4, the polysiloxane molecule 24 is fixed to the outer surface of the substrate 22 through bonding with hydroxyl groups (an example of surface functional groups) on the outer surface of the substrate 22.
  • the membrane material is formed by a reaction between an alkoxysilyl group at the end of the membrane compound (an example of a reactive group) and a hydroxyl group (an example of a surface functional group) on the outer surface of the substrate 22 or a silanol group on the polysiloxane molecule 24. It is fixed to the polysiloxane molecules 24 that coat the outer surface of the base material 22 and the outer surface of the base material 22 in a mesh form through the formed bond (Si—O— bond).
  • the face plate 20 for a display device is brought into contact with a film compound having a hydrocarbon group on the outer surface of a base material 22 and a treatment liquid in which alkoxysilane and / or alkoxypolysiloxane are mixed and dispersed in a solvent.
  • Step C see FIG.
  • a method for manufacturing the display device face plate 20 will be described.
  • the material that can be used as the base material 22 is the same as that of the base material 12 that can be used for manufacturing the face plate 10 for a display device according to the first embodiment, detailed description thereof is omitted. To do.
  • the treatment liquid used in Step C is prepared by mixing and dispersing the film compound and alkoxysilane and / or alkoxypolysiloxane in a solvent.
  • Specific examples of the compound that can be used as the film compound, the solvent and the surfactant that can be used are the same as those in the method of manufacturing the face plate 10 for a display device, and thus detailed description thereof is omitted.
  • the treatment liquid used for manufacturing the display device face plate 20 contains alkoxysilane and / or alkoxypolysiloxane in order to improve the durability of the obtained display device face plate 20.
  • the alkoxysilane is a compound represented by the formula SiH x (OA) 4-x (formula (VI)), and the alkoxypolysiloxane is represented by the formula (AO) 3 Si (OSi (OA) 2 ) n OSi (OA). 3 It is a compound represented by (Formula (VII)).
  • x is 0, 1, or 2
  • A represents an alkyl group, preferably a methyl group or an ethyl group
  • n is 0, 1, or 2.
  • alkoxysilane represented by the above formula (VI) and the alkoxypolysiloxane represented by the above formula (VII) include the following compounds (21) to (28).
  • SiH 2 (OC 2 H 5 ) 2 (28) (H 5 C 2 O) 3 SiOSi (OC 2 H 5) 3
  • the composition ratio ratio of the number of silicon atoms of the film compound and alkoxysilane and / or alkoxypolysiloxane. Is preferably from 1:10 to 1: 0, more preferably from 1: 3 to 3: 1.
  • the total concentration of the membrane compound and alkoxysilane and / or alkoxypolysiloxane is preferably 0.1 mmol / L to 50 mmol / L, more preferably 0.1 mmol / L to 10 mmol / L.
  • the total concentration is less than 0.1 mmol / L, it is difficult to form a uniform lipophilic film 17, and when the total concentration exceeds 50 mmol / L, gelation or the like is likely to occur, and storage stability is improved. descend.
  • the total concentration is 10 mmol / L to 0.1 mmol / L, gelation of the treatment liquid can be prevented, and the lifetime can be secured up to about 1 month.
  • the treatment liquid used for the production of the display device face plate 20 is a mixture comprising a film compound and alkoxysilane and / or alkoxypolysiloxane and a solvent (preferably water containing a surfactant and / or alcohol).
  • a solvent preferably water containing a surfactant and / or alcohol.
  • the film is an organic thin film 26 including a film 27a of polysiloxane molecules (24a) having unreacted silanol groups (25).
  • heat treatment may be performed in order to improve the water / oil repellency / antifouling property and the durability of the finally obtained fluorine-containing organic thin film 21.
  • the heat treatment is preferably performed at 120 ° C.
  • the hydrogen in the hydrocarbon groups contained in the organic thin film 28 is obtained by subjecting the outer surface of the base material 22 on which the organic thin film 28 is formed in the gas atmosphere of the compound containing a fluorocarbon group in the process A to low pressure plasma treatment.
  • a fluorine-containing organic thin film 21 in which some or all of the atoms are substituted with one or both of fluorine atoms and fluorocarbon groups is formed to obtain a face plate 20 for a display device. Since this is the same as the manufacturing method of the face plate 10 for a display device according to the first embodiment, detailed description is omitted. Similarly, detailed description of the process B is also omitted.
  • the display device face plate 20 thus obtained can be used in the same manner as the display device face plate 10 according to the first embodiment.
  • the fluorine-containing organic thin film 31 is a polysiloxane molecule (34) fixed on the outer surface of the substrate 32 through bonding with a hydroxyl group (an example of a surface functional group) of the substrate 32.
  • a film having a two-layer structure comprising a film of an example of a film substance having a fluorine-containing hydrocarbon group in which part or all of hydrogen atoms are substituted with either or both of a fluorine atom and a fluorocarbon group.
  • the membrane material is composed of a bond (Si—O— bond) formed by a reaction between an alkoxysilyl group (an example of a reactive group) at the end of the membrane compound and a silanol group (Si—OH) (not shown) on the polysiloxane molecule 34. ) To the coating 37 of polysiloxane molecules (34) covering the outer surface of the substrate 32 (see FIG. 7).
  • the display device face plate 30 first contacts a treatment liquid containing alkoxysilane and / or alkoxypolysiloxane with the outer surface of the substrate 32, and coats the outer surface of the substrate 32 with polysiloxane molecules. 37, and then a treatment liquid containing a film compound is brought into contact with the surface of the substrate 32 on which the polysiloxane molecule film 26 is formed on the outer surface to form a film of the film material on the polysiloxane molecule film 37.
  • the step A for obtaining the base material 32 on which the organic thin film 38 is formed and the outer surface of the base material 32 on which the organic thin film 38 is formed in a gas atmosphere of a compound containing a fluorocarbon group are subjected to low-pressure plasma treatment.
  • a face plate 40 for a display device will be described with reference to FIGS. 8 (a) and 8 (b).
  • a fluorine-containing organic polymer (of a substance having a fluorine-containing functional group) is formed so as to cover at least a part of the outer surface of the substrate 42.
  • An example 41 exists.
  • the base material 42 used for manufacturing the water / oil repellent / antifouling member 40 is covered with a hydrocarbon group 43 on the outer surface.
  • the hydrocarbon group covering the outer surface of the base material 42 before the low pressure plasma treatment is substituted with a trifluoromethyl group 44 which is an example of a fluorocarbon group.
  • the water / oil repellent / antifouling member 40 comprises a step A for subjecting the base material 42 to low-pressure plasma treatment in a gas atmosphere of a compound containing a fluorocarbon group, and an outer side of the base material 42 before the step A if necessary. And a step B of roughening the surface so as to have the surface roughness and the size of the irregularities within the above ranges.
  • a fluorocarbon radical such as a fluorine radical ( ⁇ F) or a trifluoromethyl radical ( ⁇ CF 3 ) is generated. These radicals substitute the hydrogen atom of the hydrocarbon group on the outer surface of the acrylic base material 42 with the trifluoromethyl group 43 (FIG. 8B).
  • the surface of the compound containing a fluorocarbon group is directly roughened so as to have a predetermined surface roughness and unevenness by the step B.
  • the display device face plate 40 is obtained by performing low-pressure plasma treatment in a gas atmosphere (step A).
  • the method for manufacturing a display device face plate according to the present embodiment is applied to an article made of an inorganic material or a member thereof. When doing so, the process C is implemented and the film which contains an organic polymer as the base material 42 is formed in the outer surface.
  • the organic polymer used to form the coating has a hydrocarbon group in the main chain and side chain, and in step A, part or all of the hydrogen atoms are fluorine atoms and Any organic polymer can be used as long as it can be substituted with a fluorocarbon group.
  • the film may be formed by spray coating using a solution containing an organic polymer, spin coating, dip coating, cast method, or the like, and a polymerization reaction is caused on the surface of the inorganic material by plasma polymerization or the like. To produce an organic polymer.
  • the face plate 10 for a display device For the roughening method of the outer surface of the base material 42 used in the step B and the order of performing the steps A to C, the face plate 10 for a display device according to the first to third embodiments described above, Since it is the same as the manufacturing method of 20 and 30, detailed description is abbreviate
  • Examples of the display device using the display device faceplate 1 obtained as described above include CRT (cathode ray tube, cathode ray tube), liquid crystal display device, plasma display, organic and inorganic EL display devices, and the like.
  • Articles using the display device incorporating the face plate 1 include a mobile phone, an electronic desk calculator, an electronic computer or a display for an electronic computer, a PDA (personal digital assistant), a portable game machine, a portable GPS terminal, a car navigation system, Examples include a television receiver, a portable DVD player, a digital camera, a video recording device, a cash dispenser (CD) device, an automatic teller machine (ATM), and an automatic ticket machine.
  • the molecular composition ratio means a molar ratio unless otherwise specified.
  • % means weight%.
  • Example 1 Octadecyltrimethoxysilane CH 3 (CH 2 ) 17 Si (OCH 3 ) 3 (film compound) and tetramethoxysilane Si (OCH 3 ) 4 are weighed to a molar ratio of 3: 1, and 0.1% in ethanol.
  • a well-dried glass faceplate substrate is prepared as an inorganic substrate, and the treatment liquid prepared above is applied to the outer surface in the air (relative humidity 57% to 70%), and further in the air. It was left for about 1 hour. During this time, most of the ethanol in the treatment solution evaporates into the air, and the entire surface is chemically bonded to the surface by dehydration reaction with silanol groups (Si-OH) generated by hydrolysis of alkoxysilyl groups.
  • Si-OH silanol groups
  • the unreacted excess octadecyltrimethoxysilane and tetramethoxysilane are washed away with a water-ethanol mixed solvent (this step is not always necessary if the coating amount and the liquid concentration are properly adjusted).
  • the polysiloxane molecule having a thickness of about 5 nm and the octadecylsilyl group immobilized on the outer surface of the face plate or on the polysiloxane molecule were obtained.
  • a film consisting of the above can be formed in a state of being chemically bonded to the outer surface of the faceplate substrate (FIG. 6).
  • Example 2 A face plate was produced under the same conditions as in Example 1 except that the treatment liquid did not contain tetramethoxysilane.
  • the fluorine-containing organic thin film formed on the outer surface was a monomolecular film containing no polysiloxane molecules.
  • the water droplet contact angle the same results as in Example 1 were obtained.
  • the wear resistance of the fluorine-containing organic thin film was inferior to that obtained in Example 1.
  • Example 3 First, under the conditions shown in Table 3, the surface of the glass faceplate substrate was subjected to low-pressure plasma treatment, and the surface was roughened.
  • Table 4 shows the measurement results of the water droplet contact angle of the face plate thus obtained.
  • the water droplet contact angle on the obtained face plate is greatly increased by performing the plasma surface roughening treatment. Further, in the face plate obtained in this example, a decrease in light transmittance, generation of interference fringes, haze, and the like were not observed.
  • Example 4 Production of a water / oil repellent / antifouling member based on a transparent acrylic resin substrate First, after the transparent acrylic resin substrate as a substrate was washed with ethanol, under the conditions shown in Table 5 below, Low-pressure plasma treatment (O 2 plasma treatment) in an oxygen gas atmosphere was performed. Next, plasma treatment was performed in a tetrafluoromethane (CF 4 ) atmosphere containing oxygen under the conditions shown in Table 6.
  • O 2 plasma treatment oxygen gas atmosphere
  • the water droplet contact angle of the water / oil repellent / antifouling member thus obtained was measured. Measurements were made at five different points (IV) on the same sample. The measurement results are as shown in Table 7 below.
  • the water droplet contact angle of the acrylic resin substrate before treatment was 75.0 degrees.
  • the O 2 plasma treatment has an action of cleaning the surface of the acrylic resin substrate and an action of roughening the surface of the member, and the surface roughness can be controlled by arbitrarily controlling the power of the high frequency power source and the treatment time. Can be controlled within a range of several nanometers to several hundred microns, and the final water droplet contact angle can be controlled to about 165 to 100 degrees. In particular, if the water droplet contact angle was controlled to be 150 degrees or more, a high-performance oil-repellent and antifouling member with extremely low surface energy could be produced. Further, when the surface roughness was set to be equal to or less than the wavelength of visible light (for example, 400 nm), the transparency of the acrylic resin substrate used as the base material was not impaired.
  • the wavelength of visible light for example, 400 nm
  • the materials that can be used are of any material that contains hydrocarbon groups, and in addition to artificial materials such as synthetic resin, synthetic leather, and synthetic fibers, it also applies to natural materials such as woody materials, paper, and wool. I was able to handle it.
  • the article to which the present invention can be applied may be in any form as long as it is a display device. Specifically, it can be used for a mobile phone, an electronic computer, a PDA, a GPS, a television receiver, a cash dispenser (CD) device, a display device installed in an ATM device, or a member used for them. . Furthermore, the present invention can be applied to optical lenses and casings used in these devices.

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  • Chemical & Material Sciences (AREA)
  • General Chemical & Material Sciences (AREA)
  • Health & Medical Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Medicinal Chemistry (AREA)
  • Polymers & Plastics (AREA)
  • Organic Chemistry (AREA)
  • Devices For Indicating Variable Information By Combining Individual Elements (AREA)
  • Treatments Of Macromolecular Shaped Articles (AREA)
  • Liquid Crystal (AREA)

Abstract

L'invention traite d'une dalle pour dispositifs d'affichage, qui se caractérise par sa durabilité étendue, son faible coût de production, sa haute sécurité pour la santé humaine et l'environnement et sa sensibilité moindre aux traces de doigts, etc. ; d'un procédé pour fabriquer ladite dalle ; et d'un dispositif d'affichage et d'un article fabriqués tous les deux à l'aide de ladite dalle et dudit procédé. La dalle comporte une mince couche d'enduction fluorée (11) obtenue en appliquant une substance transparente contenant des groupes hydrocarbure de façon à ce qu'elle couvre au moins une partie externe de la surface de la dalle (10) et en soumettant le revêtement à un traitement plasma à basse pression dans une atmosphère à base d'un gaz contenant des groupes fluorocarbure pour remplacer ainsi l'intégralité ou une partie des groupes hydrocarbure par des groupes fluorocarbure et/ou des atomes de fluor (19).
PCT/JP2010/002497 2009-04-10 2010-04-06 Dalle d'écran, son procédé de fabrication et leur utilisation dans la production de dispositifs d'affichage et d'autres articles WO2010116714A1 (fr)

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KR102642899B1 (ko) * 2021-07-15 2024-03-05 삼성전기주식회사 렌즈, 렌즈 어셈블리 및 휴대용 전자기기

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JPH04255345A (ja) * 1991-02-06 1992-09-10 Matsushita Electric Ind Co Ltd 防汚性光学部材およびその製造方法
JPH10292057A (ja) * 1997-02-20 1998-11-04 Matsushita Electric Ind Co Ltd 化学吸着膜およびその製造方法とそれに用いる化学吸着液
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JPH04255345A (ja) * 1991-02-06 1992-09-10 Matsushita Electric Ind Co Ltd 防汚性光学部材およびその製造方法
JPH10292057A (ja) * 1997-02-20 1998-11-04 Matsushita Electric Ind Co Ltd 化学吸着膜およびその製造方法とそれに用いる化学吸着液
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