JPH09227178A - Laminated glass and its production - Google Patents
Laminated glass and its productionInfo
- Publication number
- JPH09227178A JPH09227178A JP8136777A JP13677796A JPH09227178A JP H09227178 A JPH09227178 A JP H09227178A JP 8136777 A JP8136777 A JP 8136777A JP 13677796 A JP13677796 A JP 13677796A JP H09227178 A JPH09227178 A JP H09227178A
- Authority
- JP
- Japan
- Prior art keywords
- laminated glass
- photocatalyst
- glass
- producing
- water
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Pending
Links
- 239000005340 laminated glass Substances 0.000 title claims abstract description 72
- 238000004519 manufacturing process Methods 0.000 title claims abstract description 48
- 239000011941 photocatalyst Substances 0.000 claims abstract description 56
- 239000011521 glass Substances 0.000 claims abstract description 55
- 238000000576 coating method Methods 0.000 claims abstract description 31
- 239000011248 coating agent Substances 0.000 claims abstract description 28
- 239000002985 plastic film Substances 0.000 claims abstract description 25
- 229920006255 plastic film Polymers 0.000 claims abstract description 23
- 230000001443 photoexcitation Effects 0.000 claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 13
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 48
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical group O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims description 31
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 26
- 238000000034 method Methods 0.000 claims description 20
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 claims description 9
- 229920001296 polysiloxane Polymers 0.000 claims description 6
- 125000002887 hydroxy group Chemical group [H]O* 0.000 claims description 5
- 229910052814 silicon oxide Inorganic materials 0.000 claims description 5
- 230000002238 attenuated effect Effects 0.000 claims 1
- 239000010410 layer Substances 0.000 abstract description 31
- 239000011229 interlayer Substances 0.000 abstract description 8
- 230000005660 hydrophilic surface Effects 0.000 abstract description 2
- 239000003054 catalyst Substances 0.000 abstract 1
- 239000010408 film Substances 0.000 description 23
- 238000005187 foaming Methods 0.000 description 10
- 230000001699 photocatalysis Effects 0.000 description 9
- 239000000243 solution Substances 0.000 description 8
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 7
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 6
- 239000005357 flat glass Substances 0.000 description 6
- BOTDANWDWHJENH-UHFFFAOYSA-N Tetraethyl orthosilicate Chemical compound CCO[Si](OCC)(OCC)OCC BOTDANWDWHJENH-UHFFFAOYSA-N 0.000 description 5
- 230000007062 hydrolysis Effects 0.000 description 5
- 238000006460 hydrolysis reaction Methods 0.000 description 5
- 229920003023 plastic Polymers 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 4
- 229910021417 amorphous silicon Inorganic materials 0.000 description 4
- XGZNHFPFJRZBBT-UHFFFAOYSA-N ethanol;titanium Chemical compound [Ti].CCO.CCO.CCO.CCO XGZNHFPFJRZBBT-UHFFFAOYSA-N 0.000 description 4
- 238000007539 photo-oxidation reaction Methods 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 230000018044 dehydration Effects 0.000 description 3
- 238000006297 dehydration reaction Methods 0.000 description 3
- 230000007774 longterm Effects 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 230000035515 penetration Effects 0.000 description 3
- 238000006068 polycondensation reaction Methods 0.000 description 3
- 239000000758 substrate Substances 0.000 description 3
- 239000010936 titanium Substances 0.000 description 3
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical group [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000002518 antifoaming agent Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- 230000000295 complement effect Effects 0.000 description 2
- 230000007423 decrease Effects 0.000 description 2
- 230000001747 exhibiting effect Effects 0.000 description 2
- 239000012634 fragment Substances 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 239000003112 inhibitor Substances 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 125000000962 organic group Chemical group 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 230000002093 peripheral effect Effects 0.000 description 2
- 239000004033 plastic Substances 0.000 description 2
- 239000005336 safety glass Substances 0.000 description 2
- SCPYDCQAZCOKTP-UHFFFAOYSA-N silanol Chemical compound [SiH3]O SCPYDCQAZCOKTP-UHFFFAOYSA-N 0.000 description 2
- 229910052710 silicon Inorganic materials 0.000 description 2
- 239000004447 silicone coating Substances 0.000 description 2
- 239000005361 soda-lime glass Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000010409 thin film Substances 0.000 description 2
- LLZRNZOLAXHGLL-UHFFFAOYSA-J titanic acid Chemical compound O[Ti](O)(O)O LLZRNZOLAXHGLL-UHFFFAOYSA-J 0.000 description 2
- 229910052719 titanium Inorganic materials 0.000 description 2
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- 239000003513 alkali Substances 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- WMWLMWRWZQELOS-UHFFFAOYSA-N bismuth(iii) oxide Chemical compound O=[Bi]O[Bi]=O WMWLMWRWZQELOS-UHFFFAOYSA-N 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000000694 effects Effects 0.000 description 1
- 238000001704 evaporation Methods 0.000 description 1
- 230000008020 evaporation Effects 0.000 description 1
- 238000010304 firing Methods 0.000 description 1
- 239000003779 heat-resistant material Substances 0.000 description 1
- 230000002209 hydrophobic effect Effects 0.000 description 1
- 125000001165 hydrophobic group Chemical group 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 1
- 229910052753 mercury Inorganic materials 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910001507 metal halide Inorganic materials 0.000 description 1
- 150000005309 metal halides Chemical class 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 239000011259 mixed solution Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- QGLKJKCYBOYXKC-UHFFFAOYSA-N nonaoxidotritungsten Chemical compound O=[W]1(=O)O[W](=O)(=O)O[W](=O)(=O)O1 QGLKJKCYBOYXKC-UHFFFAOYSA-N 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000003825 pressing Methods 0.000 description 1
- 230000002265 prevention Effects 0.000 description 1
- 238000009877 rendering Methods 0.000 description 1
- 239000003566 sealing material Substances 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 description 1
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 description 1
- 229910001887 tin oxide Inorganic materials 0.000 description 1
- 239000005341 toughened glass Substances 0.000 description 1
- 229910001930 tungsten oxide Inorganic materials 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
Classifications
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
- F28F13/00—Arrangements for modifying heat-transfer, e.g. increasing, decreasing
- F28F13/18—Arrangements for modifying heat-transfer, e.g. increasing, decreasing by applying coatings, e.g. radiation-absorbing, radiation-reflecting; by surface treatment, e.g. polishing
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F24—HEATING; RANGES; VENTILATING
- F24F—AIR-CONDITIONING; AIR-HUMIDIFICATION; VENTILATION; USE OF AIR CURRENTS FOR SCREENING
- F24F8/00—Treatment, e.g. purification, of air supplied to human living or working spaces otherwise than by heating, cooling, humidifying or drying
- F24F8/20—Treatment, e.g. purification, of air supplied to human living or working spaces otherwise than by heating, cooling, humidifying or drying by sterilisation
- F24F8/22—Treatment, e.g. purification, of air supplied to human living or working spaces otherwise than by heating, cooling, humidifying or drying by sterilisation using UV light
-
- F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
- F28—HEAT EXCHANGE IN GENERAL
- F28F—DETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
- F28F2245/00—Coatings; Surface treatments
- F28F2245/02—Coatings; Surface treatments hydrophilic
Landscapes
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- General Engineering & Computer Science (AREA)
- Combustion & Propulsion (AREA)
- Thermal Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Physics & Mathematics (AREA)
- Catalysts (AREA)
- Paints Or Removers (AREA)
- Surface Treatment Of Glass (AREA)
- Laminated Bodies (AREA)
- Surface Treatment Of Optical Elements (AREA)
- Finishing Walls (AREA)
- Application Of Or Painting With Fluid Materials (AREA)
- Coating Of Shaped Articles Made Of Macromolecular Substances (AREA)
- Materials Applied To Surfaces To Minimize Adherence Of Mist Or Water (AREA)
- Prevention Of Fouling (AREA)
- Optical Elements Other Than Lenses (AREA)
- Building Environments (AREA)
- Pigments, Carbon Blacks, Or Wood Stains (AREA)
- Refuge Islands, Traffic Blockers, Or Guard Fence (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
- Road Signs Or Road Markings (AREA)
- Dental Tools And Instruments Or Auxiliary Dental Instruments (AREA)
- Exhaust Gas Treatment By Means Of Catalyst (AREA)
- Rear-View Mirror Devices That Are Mounted On The Exterior Of The Vehicle (AREA)
- Aftertreatments Of Artificial And Natural Stones (AREA)
- Mirrors, Picture Frames, Photograph Stands, And Related Fastening Devices (AREA)
- Compositions Of Macromolecular Compounds (AREA)
- Detergent Compositions (AREA)
- Bridges Or Land Bridges (AREA)
- Devices For Indicating Variable Information By Combining Individual Elements (AREA)
- Panels For Use In Building Construction (AREA)
- Joining Of Glass To Other Materials (AREA)
- Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
- Illuminated Signs And Luminous Advertising (AREA)
- Greenhouses (AREA)
- Devices Affording Protection Of Roads Or Walls For Sound Insulation (AREA)
- Respiratory Apparatuses And Protective Means (AREA)
- Fire-Detection Mechanisms (AREA)
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は合わせガラス及びそ
の製造方法に係わるもので、特に合わせガラスの製造時
及び使用時に中間層において発泡が起こらない合わせガ
ラス及びその製造方法に関するものである。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a laminated glass and a method for producing the same, and more particularly to a laminated glass which does not cause foaming in an intermediate layer during production and use of the laminated glass and a method for producing the same.
【０００２】[0002]
【従来の技術】合わせガラスや強化ガラスとは、割れに
くく、また万一割れても破片が丸みを持つように、ある
いは飛散しにくいように作られた安全ガラスの一つであ
る。安全ガラスは自動車用風防ガラスや鉄道車両の窓ガ
ラス、航空機の窓ガラス、舷窓のガラス、家屋の窓ガラ
ス、防弾及び防犯ガラス、水槽などに多く用いられてい
る。2. Description of the Related Art Laminated glass and tempered glass are one of safety glasses made so that they are hard to break, and even if they break, the fragments have a rounded shape or are hard to scatter. Safety glass is widely used for windshields for automobiles, window glass for railroad cars, window glass for aircraft, glass for portholes, window glass for houses, bulletproof and crime prevention glass, and aquariums.
【０００３】合わせガラスは２枚又は数枚のガラス板を
透明なプラスチックの中間膜で接着したものである。通
常この中間膜にはポリビニルブチラールのフィルムが使
われており、ポリビニルブチラールは強靭性と接着性を
兼備しているため、合わせガラスの他に金属用の接着剤
としても多用されている。この中間膜のため、前記した
ように万一合わせガラスが割れてもほとんど破片が飛散
しない。合わせガラスは通常ガラス板を使用して製造さ
れるが、複数のプラスチック板の使用又はガラス板とプ
ラスチック板の同時使用が可能である。Laminated glass is made by bonding two or several glass plates with a transparent plastic interlayer film. Usually, a polyvinyl butyral film is used for this interlayer film, and since polyvinyl butyral has both toughness and adhesiveness, it is widely used as an adhesive for metals as well as laminated glass. Due to this intermediate film, as described above, even if the laminated glass is broken, almost no fragments are scattered. Laminated glass is usually manufactured by using glass plates, but it is possible to use a plurality of plastic plates or use both glass plates and plastic plates at the same time.
【０００４】合わせガラスは、ガラス板にポリビニルブ
チラールなどの中間膜を挿入して予備圧着した後、さら
にオートクレーブ中において加温しながら最終的に圧着
して製造する。ガラス板とプラスチックフィルムの接着
に当たって遭遇する最も大きな難点は、両者の接着界面
に気泡が生成し、これを除去すること又はその生成を防
止することが極めて困難なことである。Laminated glass is manufactured by inserting an interlayer film such as polyvinyl butyral into a glass plate, preliminarily press-bonding it, and finally pressure-bonding it while heating it in an autoclave. The greatest difficulty encountered in adhering the glass plate and the plastic film is that bubbles are formed at the adhesive interface between them and it is extremely difficult to remove or prevent the formation of bubbles.
【０００５】また、合わせガラスは自動車の風防ガラス
等に多用されており、夏期には太陽熱等により風防ガラ
ス自体が高温となることがしばしばある。これにより製
造直後には目視により確認できなかった気泡が、実際に
は残存していた極めて小さな気泡の膨張あるいは残存水
分の蒸発により出現することがある。それゆえ製造工程
において中間層の水分管理は非常に重要となる。しかし
ながら、製造時に可能な限り水分を除去したとしても、
中間膜のポリビニルブチラールが水分及び湿分に耐性が
低いため、長期間の使用により吸水し同様な現象が起こ
る可能性がある。水分の含有量が多いと耐貫通性は向上
するが、使用時特に７０℃以上の高温時に中間層で気泡
が生じ商品価値を低下したり、接着力が失われ剥離した
りする。また、水分が少ないとガラス板と中間膜の接着
度は増大するが耐貫通性が低下し、合わせガラスの安全
性が低下する。Laminated glass is often used in windshields of automobiles and the like, and the windshield itself often becomes hot due to solar heat in summer. As a result, bubbles that could not be visually confirmed immediately after production may appear due to expansion of extremely small bubbles that actually remained or evaporation of residual moisture. Therefore, water management of the intermediate layer is very important in the manufacturing process. However, even if water is removed as much as possible during manufacturing,
Since polyvinyl butyral of the interlayer film has low resistance to moisture and moisture, there is a possibility that water may be absorbed by the long-term use and a similar phenomenon may occur. When the content of water is large, the penetration resistance is improved, but during use, especially at a high temperature of 70 ° C. or higher, air bubbles are generated in the intermediate layer to lower the commercial value, or the adhesive strength is lost and peeling occurs. Further, when the water content is low, the degree of adhesion between the glass plate and the interlayer film increases, but the penetration resistance decreases, and the safety of the laminated glass decreases.
【０００６】製造時及び使用時に発泡を生じない合わせ
ガラスの製造方法には、これまで種々のものが提案され
ている。例えば特開昭５８−１９０８４６号公報に記載
された技術では、合わせガラス中間層の発泡は周縁部に
特に生じやすいので、ガラス板より若干小さいプラスチ
ックフィルム中間膜をはさみ、プラスチックフィルム中
間膜で覆われていない部分には不透湿性シール材を設け
て、圧着製造している。この技術により断面部から水分
が吸収される作用を防いでいる。Various methods have been proposed so far for producing a laminated glass that does not cause foaming during production and use. For example, in the technique disclosed in Japanese Patent Laid-Open No. 58-190846, since foaming of the laminated glass intermediate layer is particularly likely to occur in the peripheral portion, a plastic film intermediate film slightly smaller than the glass plate is sandwiched and covered with the plastic film intermediate film. A non-moisture impermeable sealing material is provided on the unfilled portion, and pressure bonding is performed. This technique prevents the action of absorbing water from the cross section.
【０００７】また残存する気泡を排出するためにプラス
チックフィルムとガラス板を圧着する際、接着面に液状
脱泡剤を存在させ、圧着工程で生成する気泡を液状脱泡
剤とともに接着面からしごき出して排出する技術が特開
昭６１−５２０９２号公報に開示されている。When the plastic film and the glass plate are pressure-bonded to discharge the remaining air bubbles, a liquid defoaming agent is allowed to exist on the bonding surface, and the air bubbles generated in the pressure bonding process are squeezed out together with the liquid defoaming agent from the bonding surface. A technique for discharging the ink is disclosed in JP-A-61-52092.
【０００８】[0008]
【発明が解決しようとする課題】しかしながら前述した
従来の合わせガラスの製造方法には、それぞれ以下のよ
うな問題点が存在する。まず特開昭５８−１９０８４６
号公報に記載された技術では、ガラス板中央部の発泡を
防止することができない。目に見えない程度の気泡が残
存していると、高温条件下では中央部に発泡するおそれ
がある。However, the above-mentioned conventional methods for producing laminated glass have the following problems, respectively. First, JP-A-58-190846
The technique described in the publication cannot prevent foaming in the central portion of the glass plate. If invisible bubbles remain, there is a risk of foaming in the central portion under high temperature conditions.
【０００９】また、特開昭６１−５２０９２号公報に記
載された技術では、合わせガラス製造時段階の気泡は取
り除くことができ、ある程度の期間発泡を防ぐことはで
きるが、長期間使用後に周辺部からの水分や湿分が吸水
されることによる気泡の発生は防止できない。Further, according to the technique disclosed in Japanese Patent Laid-Open No. 61-52092, bubbles can be removed at the stage of manufacturing laminated glass and foaming can be prevented for a certain period of time, but the peripheral portion after long-term use It is not possible to prevent the generation of bubbles due to the absorption of water and moisture from water.
【００１０】２枚のガラス板の間に水分が存在する場
合、ガラス板と水との接触角が小さいときには気泡が生
じにくいことがこれまでにわかっている。つまりガラス
板表面が親水性であるならば水との接触角が小さくなり
気泡が生じにくい。この水との接触角は１０°以下であ
ることが望まれる。通常ガラス板はコンタミネーション
のない本来の性質としては約５〜２０°であるが、しか
しながら時間の経過とともに低級カルボン酸等の親水
基、疎水基の双方を含む成分がガラス表面に徐々に吸着
し、表面が疎水化されてしまう。したがって、発泡を防
ぐための十分な親水性を継続的に備えているとはいえな
い。It has been known so far that when water is present between two glass plates, bubbles are unlikely to be generated when the contact angle between the glass plates and water is small. That is, if the surface of the glass plate is hydrophilic, the contact angle with water becomes small and bubbles are less likely to occur. The contact angle with water is desired to be 10 ° or less. Normally, a glass plate has a natural property of about 5 to 20 ° without contamination, but over time, components containing both a hydrophilic group and a hydrophobic group such as a lower carboxylic acid are gradually adsorbed on the glass surface. , The surface becomes hydrophobic. Therefore, it cannot be said that it continuously has sufficient hydrophilicity to prevent foaming.
【００１１】本発明が解決しようとする課題は、合わせ
ガラスの製造時及び高温下等での使用時において中間層
に気泡が生じない合わせガラス及びその製造方法を提供
することにある。The problem to be solved by the present invention is to provide a laminated glass in which no bubbles are generated in the intermediate layer during the production of the laminated glass and during use under high temperature and the like, and a method for producing the same.
【００１２】[0012]
【課題を解決するための手段】本発明者は、以上の課題
を達成するために種々検討し、光触媒を光励起すると光
触媒の表面が高度に親水化されることを知見し、本発明
に想到した。すなわち、光触媒を光励起すると光触媒の
表面が高度に親水化されることを世界で初めて発見し
た。光触媒性酸化チタンを紫外線で光励起したところ、
水との接触角が１０°以下、より詳しくは５°以下、特
に約０°になる程度に表面が高度に親水化されることが
発見された。Means for Solving the Problems The present inventor has conducted various studies to achieve the above-mentioned object, and found that photoexcitation of the photocatalyst causes the surface of the photocatalyst to be highly hydrophilic, and has arrived at the present invention. . That is, it was discovered for the first time in the world that the photocatalyst surface is highly hydrophilized when it is photoexcited. When photocatalytic titanium oxide was photoexcited with ultraviolet light,
It has been discovered that the surface is highly hydrophilized to such an extent that the contact angle with water is 10 ° or less, more specifically 5 ° or less, and especially about 0 °.
【００１３】本発明はこの新発見に基づくもので、光触
媒を含有させたコーティングをガラス部材表面に施し、
光励起によって高度に親水化した表面を有するガラス部
材面をプラスチックフィルムと接着させて合わせガラス
を製造した場合、合わせガラスの製造時及び高温下での
使用時に、中間層に気泡が発生するのを防止することが
できる。The present invention is based on this new discovery, in which a coating containing a photocatalyst is applied to the surface of a glass member,
When a laminated glass is manufactured by adhering the glass member surface, which has a highly hydrophilic surface by photoexcitation, to a plastic film, it prevents the generation of bubbles in the intermediate layer during the manufacturing of the laminated glass and the use at high temperature. can do.
【００１４】前記課題を解決するため、請求項１に記載
の合わせガラスは、プラスチックフィルムと接触するガ
ラス部材の二つの接触面のうち、少なくとも一方のガラ
ス部材面に光触媒含有膜を有することを特徴とする。し
たがって、中間層に水分が残存していた場合や外部から
水分を吸水した場合に、光励起することにより光触媒含
有膜が超親水化され、水との接触角が小さくなるため、
高温下で使用しても気泡を発生しない。In order to solve the above problems, the laminated glass according to claim 1 has a photocatalyst-containing film on at least one of the two contact surfaces of the glass member that contacts the plastic film. And Therefore, when water remains in the intermediate layer or when water is absorbed from the outside, the photocatalyst-containing film is superhydrophilized by photoexcitation, and the contact angle with water becomes small,
No bubbles are generated even when used at high temperatures.
【００１５】請求項２記載の合わせガラスの製造方法
は、複数のガラス部材を準備する工程と、プラスチック
フィルムと接触させるガラス部材の二つの接触面のうち
少なくとも１面の表面に光触媒材料をコーティングする
工程と、紫外線照射により光触媒含有膜を光励起する工
程と、プラスチックフィルムがガラス部材にコーティン
グした光触媒含有膜面と少なくとも一方の面で接触する
ように挟み圧着して合わせガラスを作製する工程を有す
ることを特徴とする。したがって、プラスチックフィル
ムとガラス部材を圧着する製造工程で、中間層に水が残
存していたとしても、光励起により超親水化された光触
媒材料を含有する膜の作用により一様な水膜を形成する
ため、気泡が生じにくい。According to a second aspect of the present invention, in the method for producing a laminated glass, a step of preparing a plurality of glass members, and at least one surface of the two contact surfaces of the glass member to be brought into contact with the plastic film is coated with a photocatalytic material. Having a step, a step of photoexciting the photocatalyst-containing film by ultraviolet irradiation, and a step of producing a laminated glass by sandwiching and pressing so that the plastic film is in contact with the photocatalyst-containing film surface coated on the glass member on at least one surface Is characterized by. Therefore, in the manufacturing process in which the plastic film and the glass member are pressure-bonded, even if water remains in the intermediate layer, a uniform water film is formed by the action of the film containing the photocatalytic material superhydrophilized by photoexcitation. Therefore, bubbles are unlikely to occur.
【００１６】請求項３記載の合わせガラス及びその製造
方法は、請求項１もしくは２のいずれか一に記載の合わ
せガラス及びその製造方法において、プラスチックフィ
ルムが紫外線波長領域の光を減衰することなく透過させ
る材料で構成されていることを特徴とする。したがっ
て、一方からのみ紫外線が照射される場合、特に紫外線
が透過する側の光触媒材料をコーティングを施した面が
光励起されるに十分な量の紫外線を到達させることでき
る。The laminated glass and the manufacturing method thereof according to claim 3 are the laminated glass and the manufacturing method according to any one of claims 1 and 2, wherein the plastic film transmits light in the ultraviolet wavelength region without attenuating. It is characterized in that it is made of a material. Therefore, when ultraviolet rays are irradiated from only one side, a sufficient amount of ultraviolet rays can reach particularly the surface coated with the photocatalytic material on the side through which the ultraviolet rays are transmitted to be photoexcited.
【００１７】請求項４記載の合わせガラス及びその製造
方法は、請求項１もしくは２のいずれか一に記載の合わ
せガラス及びその製造方法において、ガラス部材が紫外
線波長領域の光を減衰することなく透過させることを特
徴とする。したがって、一方からのみ紫外線が照射され
る場合、特に紫外線が透過する側の光触媒材料をコーテ
ィングを施した面が光励起されるに十分な量の紫外線を
到達させることできる。The laminated glass according to claim 4 and the method for manufacturing the same are the laminated glass according to claim 1 and the method for manufacturing the same, wherein the glass member transmits light in the ultraviolet wavelength region without attenuating it. It is characterized by Therefore, when ultraviolet rays are irradiated from only one side, a sufficient amount of ultraviolet rays can reach particularly the surface coated with the photocatalytic material on the side through which the ultraviolet rays are transmitted to be photoexcited.
【００１８】請求項５記載の合わせガラス及びその製造
方法は、請求項１もしくは２のいずれか一に記載の合わ
せガラス及びその製造方法において、光触媒が酸化チタ
ンであることを特徴とする。したがって、酸化チタンは
無害であり、化学的に安定であり、かつ安価に入手可能
であるという利点がある。さらに、酸化チタンはバンド
ギャップエネルギーが高く、したがって光励起するに必
要な光は紫外線であるため、光励起の過程で可視光を吸
収せず補色成分による発色が起こらない。The laminated glass according to claim 5 and the method for producing the same are the laminated glass according to claim 1 and the method for producing the same, wherein the photocatalyst is titanium oxide. Therefore, titanium oxide has the advantages of being harmless, chemically stable, and inexpensively available. Furthermore, since titanium oxide has a high band gap energy and therefore the light necessary for photoexcitation is ultraviolet light, visible light is not absorbed in the process of photoexcitation and color development by the complementary color component does not occur.
【００１９】請求項６記載の合わせガラス及びその製造
方法は、請求項１もしくは２のいずれか一に記載の合わ
せガラス及びその製造方法において、光触媒が酸化チタ
ンと酸化シリコンからなることを特徴とする。したがっ
て、蛍光灯などに含まれる微弱な紫外線でも容易に親水
化することができる。A laminated glass according to claim 6 and a method for producing the same are the laminated glass according to claim 1 and the method for producing the same, wherein the photocatalyst is composed of titanium oxide and silicon oxide. . Therefore, even weak UV light contained in a fluorescent lamp or the like can be easily made hydrophilic.
【００２０】請求項７記載の合わせガラス及びその製造
方法は、請求項１もしくは２のいずれか一に記載の合わ
せガラス及びその製造方法において、光触媒が酸化チタ
ンと一部水酸置換したシリコーンであることを特徴とす
る。したがって、酸化チタンと、耐光酸化性塗料用組成
物である一部水酸置換したシリコーンを組み合わせ塗布
した場合には、常温又は低温でコーティングを形成する
ことが可能であり、基材に塗布することが容易であり、
太陽光などで容易に光励起でき、その超親水性は長時間
維持し、蛍光灯のような室内照明灯の光でも超親水性を
回復することができ、シリコーン分子のケイ素原子に結
合した有機基が光励起により水酸基に置換される速度を
速めることができる。The laminated glass according to claim 7 and the method for producing the same are the laminated glass according to claim 1 and the method for producing the same, wherein the photocatalyst is a titanium oxide partially substituted with hydroxy. It is characterized by Therefore, when a combination of titanium oxide and a partially hydroxy-substituted silicone that is a composition for photo-oxidation resistant coating is applied in combination, it is possible to form a coating at room temperature or at a low temperature. Is easy and
It can be easily photoexcited by sunlight, maintains its superhydrophilicity for a long time, and can recover superhydrophilicity even under the light of indoor lighting such as fluorescent lamps. It is possible to accelerate the rate at which is substituted with a hydroxyl group by photoexcitation.
【００２１】請求項８記載の合わせガラス及びその製造
方法は、請求項１もしくは２のいずれか一に記載の合わ
せガラス及びその製造方法において、光触媒含有層の表
面が、光励起時に水との接触角に換算して約１０°以下
の水漏れ性を呈することを特徴とする。したがって、中
間層に水分が残存していた場合や外部から水分を吸水し
た場合に、高温下で使用しても気泡を発生しない。ま
た、プラスチックフィルムとガラス部材を圧着する製造
工程で、中間層に水が残存していたとしても、光励起に
より超親水化された光触媒含有膜の作用により一様な水
膜を形成するため、気泡が生じにくい。The laminated glass according to claim 8 and the method for producing the same are the laminated glass according to claim 1 and the method for producing the same, wherein the surface of the photocatalyst-containing layer has a contact angle with water upon photoexcitation. It is characterized by exhibiting water leakage of about 10 ° or less. Therefore, when water remains in the intermediate layer or when water is absorbed from the outside, no bubbles are generated even when used at high temperature. In addition, even if water remains in the intermediate layer in the manufacturing process in which the plastic film and the glass member are pressure-bonded, a uniform water film is formed by the action of the photocatalyst-containing film that is superhydrophilized by photoexcitation, Is less likely to occur.
【００２２】請求項９記載の合わせガラス及びその製造
方法は、請求項１もしくは２のいずれか一に記載の合わ
せガラス及びその製造方法において、光触媒含有層の表
面が、光励起時に水との接触角に換算して約５°以下の
水漏れ性を呈することを特徴とする。したがって、中間
層に水分が残存していた場合や外部から水分を吸水した
場合に、高温下で使用しても気泡を発生しない。また、
プラスチックフィルムとガラス部材を圧着する製造工程
で、中間層に水が残存していたとしても、光励起により
超親水化された光触媒含有膜の作用により一様な水膜を
形成するため、気泡が生じにくい。The laminated glass according to claim 9 and the method for producing the same are the laminated glass according to claim 1 and the method for producing the same, wherein the surface of the photocatalyst-containing layer has a contact angle with water upon photoexcitation. It is characterized by exhibiting water leakage of about 5 ° or less. Therefore, when water remains in the intermediate layer or when water is absorbed from the outside, no bubbles are generated even when used at high temperature. Also,
In the manufacturing process where the plastic film and glass member are pressure bonded, even if water remains in the intermediate layer, bubbles are generated because a uniform water film is formed by the action of the photocatalyst-containing film that is superhydrophilized by photoexcitation. Hateful.
【００２３】[0023]
【発明の実施の形態】本発明による合わせガラス及びそ
の製造方法の一実施の形態について説明する。光触媒の
バンドギャップエネルギーより高いエネルギーの波長を
もった光を、充分な照度及び時間照射すると、光触媒含
有コーティングの表面は超親水性を呈する。ここで用い
る“超親水性”又は“超親水性の”の用語は、水との接
触角に換算して約１０°以下、好ましくは約５°以下の
高度の親水性を意味する。同様に、“超親水化”又は
“超親水化する”の用語は、表面を水との接触角に換算
して約１０°以下、好ましくは約５°以下の高度の親水
性にすることを意味する。BEST MODE FOR CARRYING OUT THE INVENTION An embodiment of the laminated glass and the method for producing the same according to the present invention will be described. When light having a wavelength of energy higher than the band gap energy of the photocatalyst is irradiated with sufficient illuminance and time, the surface of the photocatalyst-containing coating exhibits superhydrophilicity. As used herein, the term "superhydrophilic" or "superhydrophilic" means a high degree of hydrophilicity of about 10 ° or less, preferably about 5 ° or less in terms of a contact angle with water. Similarly, the term "superhydrophilizing" or "superhydrophilizing" refers to rendering a surface highly hydrophilic at about 10 ° or less, preferably about 5 ° or less, in terms of contact angle with water. means.
【００２４】本発明で製作する合わせガラスでは、図１
に示すように、ガラス１とガラス２を合わせる面にこの
光触媒含有層３及び４が形成されているようにすること
により、光触媒のバンドギャップエネルギーより高いエ
ネルギーの波長をもった光の照射によって超親水性層が
形成される。その光触媒含有層の表面に、すなわち中間
層に透明なポリビニルブチラールなどのプラスチックフ
ィルム５を挟み、合わせガラスとしている。これによ
り、プラスチックフィルムとガラス部材を圧着する製造
工程において、中間層に水が残存していたとしても、光
励起により超親水化された光触媒含有膜の作用により一
様な水膜を形成するため、気泡が生じにくすることがで
きる。また、中間膜のポリビニルブチラールは吸水性が
高く、たとえ製造段階で可能な限り水分を排除したとし
ても、長期間の使用により吸水し、それにより水分を含
有した合わせガラスを高温下で使用すると、発泡が起こ
ることがある。しかし、合わせガラス中間層に含まれる
水分はその超親水性層の作用で一様に広がるため、高温
下で使用しても発泡が起こらない。The laminated glass produced by the present invention has the structure shown in FIG.
As shown in FIG. 3, by forming the photocatalyst-containing layers 3 and 4 on the surface where the glass 1 and the glass 2 are joined together, it is possible to irradiate with light having a wavelength higher than the bandgap energy of the photocatalyst. A hydrophilic layer is formed. On the surface of the photocatalyst containing layer, that is, in the intermediate layer, a transparent plastic film 5 such as polyvinyl butyral is sandwiched to form a laminated glass. Thereby, in the manufacturing process of pressure-bonding the plastic film and the glass member, even if water remains in the intermediate layer, a uniform water film is formed by the action of the photocatalyst-containing film superhydrophilized by photoexcitation. Bubbles can be made less likely to occur. Further, polyvinyl butyral of the interlayer film has a high water absorption, even if water is removed as much as possible in the manufacturing stage, it absorbs water by long-term use, thereby using a laminated glass containing water at a high temperature, Foaming may occur. However, since the water contained in the laminated glass intermediate layer spreads uniformly by the action of the superhydrophilic layer, foaming does not occur even when used at high temperature.
【００２５】光励起するための光源としては、蛍光灯、
白熱電灯、メタルハライドランプ、水銀ランプのような
室内照明灯を使用することができる。合わせガラスは室
内では水槽などに利用されている。これらの照明に含ま
れる紫外線に曝され、光励起により合わせガラスの中間
層のプラスチックフィルムに接している光触媒含有コー
ティング表面が超親水化される。また合わせガラスは自
動車用風防ガラスや鉄道車両の窓ガラス、航空機の窓ガ
ラス、舷窓のガラス、家屋の窓ガラス、防弾及び防犯ガ
ラスなどに用いられている。これらは主に屋外で使用さ
れるため、有利なことに太陽光に含まれる紫外線により
光触媒は自然に光励起される。As a light source for photoexcitation, a fluorescent lamp,
Interior lighting such as incandescent lamps, metal halide lamps and mercury lamps can be used. Laminated glass is used in water tanks and the like indoors. When exposed to the ultraviolet rays contained in these illuminations, the photocatalyst-containing coating surface in contact with the plastic film of the intermediate layer of the laminated glass is made superhydrophilic by photoexcitation. Laminated glass is also used for windshields for automobiles, window glass for railroad cars, window glass for aircraft, glass for portholes, window glass for houses, bulletproof and security glass. Since these are mainly used outdoors, the photocatalyst is naturally photoexcited by the ultraviolet rays contained in the sunlight.
【００２６】光励起は、表面の水との接触角が約１０°
以下、好ましくは約５°以下、特に約０°になるまで行
い、あるいは行わせることができる。一般には、０．０
０１ｍＷ／ｍｃ2 の紫外線照度で光励起すれば、数日で
水との接触角が約０°になるまで超親水化することがで
きる。地表に降り注ぐ太陽光に含まれる紫外線の照度は
約０．１〜１ｍＷ／ｃｍ2 であるから、太陽光に曝せば
より短時間で表面を超親水化することができる。表面が
一旦高度に親水化された後は、親水性は夜間でも持続す
る。再び太陽光に曝される度に親水性は回復され、維持
る。Photoexcitation has a contact angle with water on the surface of about 10 °.
The following can be performed or can be performed until the temperature is preferably about 5 ° or less, particularly about 0 °. Generally 0.0
When photoexcited with an ultraviolet illuminance of 01 mW / mc 2 , superhydrophilicity can be achieved until the contact angle with water becomes about 0 ° in a few days. Since the illuminance of ultraviolet rays contained in sunlight falling on the surface of the earth is about 0.1 to 1 mW / cm 2 , the surface can be made superhydrophilic in a shorter time by exposure to sunlight. Once the surface has been highly hydrophilized, the hydrophilicity persists at night. Each time it is exposed to sunlight again the hydrophilicity is restored and maintained.
【００２７】光触媒含有コーティングに使用可能な光触
媒としては、酸化チタン（アナターゼ型及びルチル
型）、酸化亜鉛、酸化錫、チタン酸ストロンチウム、酸
化タングステン、三酸化二ビスマス、酸化鉄のような金
属酸化物がある。中でも酸化チタンは無害であり、化学
的に安定であり、かつ安価に入手可能である。さらに、
酸化チタンはバンドギャップエネルギーが高く、したが
って光励起には紫外線を必要とし、光励起の過程で可視
光を吸収しないので、補色成分による発色が起こらな
い。酸化チタンはまた、酸化シリコンと組み合わせるこ
とで、蛍光灯などに含まれる微弱な紫外線でも容易に親
水化することができる。Photocatalysts usable in the photocatalyst-containing coating include metal oxides such as titanium oxide (anatase type and rutile type), zinc oxide, tin oxide, strontium titanate, tungsten oxide, dibismuth trioxide, iron oxide. There is. Among them, titanium oxide is harmless, chemically stable, and inexpensively available. further,
Titanium oxide has a high band gap energy and therefore requires ultraviolet light for photoexcitation and does not absorb visible light in the process of photoexcitation, so that coloration due to a complementary color component does not occur. By combining titanium oxide with silicon oxide, it is possible to easily make hydrophilic even weak UV light contained in a fluorescent lamp or the like.
【００２８】光触媒性材料の層を形成する方法には、焼
結させて結晶性酸化チタンなどの光触媒性材料層を形成
する方法、無定形の光触媒の前駆体の薄膜を表面に固定
し加熱結晶化させる方法、光触媒を含有する耐光酸化性
塗料を表面に塗布し硬化させる方法などがある。酸化チ
タンと、耐光酸化性塗料用組成物である一部水酸置換し
たシリコーンを組み合わせ塗布する方法では、塗膜形成
要素を硬化させた後、光触媒を光励起すると、シリコー
ン分子のケイ素原子に結合した有機基は光触媒の光触媒
作用により水酸基に置換され、光触媒性コーティングの
表面は超親水化される。この光触媒含有シリコーン塗料
は常温又は比較的低温で硬化させることができるので、
非耐熱性の材料で形成されている基材にも適用すること
ができる。また、この光触媒含有シリコーン塗料はシロ
キサン結合を有するので、光触媒の光酸化作用に対する
充分な対抗性を有する。さらに、表面が一旦超親水化さ
れた後には、暗所に保持しても長期間超親水性を維持
し、かつ、蛍光灯のような室内照明灯の光でも超親水性
を回復することができる。その上、少なくとも一部水酸
置換したシリコーンを使用すると、シリコーン分子のケ
イ素原子に結合した有機基が光励起により水酸基に置換
される速度を速めることができる。The method of forming the layer of the photocatalytic material includes a method of forming a layer of the photocatalytic material such as crystalline titanium oxide by sintering, a method of fixing a thin film of an amorphous photocatalyst precursor on the surface, and heating crystal. And a method of applying a photooxidation-resistant coating material containing a photocatalyst to the surface and curing it. In the method of applying a combination of titanium oxide and a partially hydroxy-substituted silicone which is a composition for a photo-oxidation resistant coating, after curing the film-forming element, when the photocatalyst was photoexcited, it was bonded to the silicon atom of the silicone molecule. The organic groups are replaced with hydroxyl groups by the photocatalytic action of the photocatalyst, and the surface of the photocatalytic coating is made superhydrophilic. Since this photocatalyst-containing silicone coating can be cured at room temperature or a relatively low temperature,
It can also be applied to a substrate formed of a non-heat resistant material. Further, since this photocatalyst-containing silicone coating has a siloxane bond, it has sufficient resistance to the photooxidation action of the photocatalyst. Furthermore, once the surface has been made superhydrophilic, it can maintain superhydrophilicity for a long time even if kept in a dark place, and can recover superhydrophilicity even with the light of indoor lighting such as fluorescent lamps. it can. In addition, the use of at least partially hydroxy-substituted silicone can accelerate the rate at which the organic group bonded to the silicon atom of the silicone molecule is replaced by the hydroxyl group by photoexcitation.
【００２９】自動車の風防ガラスに用いる合わせガラス
などにコーティングする場合、光触媒含有コーティング
の膜厚は０．２μｍ以下にするのが好ましい。そうすれ
ば、光の干渉による光触媒含有コーティングの発色を防
止することができるため、視界を妨げることがなく運転
にも支障を来さない。また、光触媒含有コーティングが
薄ければ薄いほど基材の透明度を確保することができ
る。When coating laminated glass used for windshields of automobiles, the film thickness of the photocatalyst-containing coating is preferably 0.2 μm or less. By doing so, the color formation of the photocatalyst-containing coating due to the interference of light can be prevented, so that the visibility is not hindered and the driving is not hindered. Also, the thinner the photocatalyst-containing coating, the more transparent the substrate can be ensured.
【００３０】[0030]
【実施例】ガラス板に光触媒含有コーティングを施し、
施した面に接触するようにプラスチックフィルムを挟
み、合わせガラスを作製した。光触媒含有コーティング
は２種類の方法で行った。１番目の製法は、テトラエト
キシシラン（和光純薬）０．６９ｇとアナターゼ型酸化
チタンゾル（日産化学、ＴＡ−１５、平均粒径０．０１
μｍ）１．０７ｇとエタノール２９．８８ｇと純水０．
３６ｇを混合し、コーティング溶液を調整した。なお溶
液中の固形分は１重量％となるようにした。このコーテ
ィング溶液をフローコーティング法により、厚さ３ｍｍ
のソーダライムガラス板の片面に塗布した。このガラス
板を約２０分間約１５０℃の温度に保持することによ
り、テトラエトキシシランを加水分解と脱水縮重合に付
し、アナターゼ型酸化チタン粒子が無定形酸化シリコン
のバインダーで結着されたコーティングをガラス板の表
面に形成した。酸化チタンと酸化シリコンの重量比は１
であった。こうして光触媒含有コーティングを施したガ
ラス板＃１を得た。Example: A glass plate is coated with a photocatalyst containing coating,
A plastic film was sandwiched so as to come into contact with the surface on which the laminated glass was produced. The photocatalyst-containing coating was performed by two methods. The first manufacturing method is tetraethoxysilane (Wako Pure Chemical Industries, Ltd.) 0.69 g and anatase type titanium oxide sol (Nissan Kagaku, TA-15, average particle size 0.01).
μm) 1.07 g, ethanol 29.88 g, and pure water 0.1.
36 g was mixed to prepare a coating solution. The solid content in the solution was adjusted to 1% by weight. This coating solution was applied by flow coating to a thickness of 3 mm.
It was applied to one surface of a soda lime glass plate. By holding this glass plate at a temperature of about 150 ° C. for about 20 minutes, the tetraethoxysilane is subjected to hydrolysis and dehydration polycondensation, and the anatase-type titanium oxide particles are bound by an amorphous silicon oxide binder. Was formed on the surface of the glass plate. The weight ratio of titanium oxide and silicon oxide is 1
Met. Thus, a glass plate # 1 coated with a photocatalyst-containing coating was obtained.
【００３１】２番目の製法は、エタノールの溶媒８６重
量部に、テトラエトキシシランＳｉ（ＯＣ2 Ｈ5 ）
4（和光純薬、大阪）６重量部と純水６重量部とテトラ
エトキシシランの加水分解抑制剤として３６％塩酸２重
量部を加えて混合し、酸化シリコンコーティング溶液を
調整した。混合により溶液は発熱するので、混合液を約
１時間放置冷却した。この溶液をフローコーティング法
により１０ｃｍ四角のソーダライムガラス板の表面に塗
布し、８０℃の温度で乾燥させた。乾燥に伴い、テトラ
エトキシシランは加水分解を受けてまずシラノールＳｉ
（ＯＨ）4 になり、続いてシラノールの脱水縮重合によ
り無定形酸化シリコンの薄膜がガラス板の表面に形成さ
れた。The second method is to add tetraethoxysilane Si (OC 2 H 5 ) to 86 parts by weight of ethanol solvent.
4 (Wako Pure Chemical Industries, Osaka) 6 parts by weight, 6 parts by weight of pure water and 2 parts by weight of 36% hydrochloric acid as a hydrolysis inhibitor of tetraethoxysilane were added and mixed to prepare a silicon oxide coating solution. Since the solution generated heat by mixing, the mixed solution was left to cool for about 1 hour. This solution was applied to the surface of a 10 cm square soda lime glass plate by a flow coating method, and dried at a temperature of 80 ° C. As it was dried, tetraethoxysilane was hydrolyzed and silanol
It became (OH) 4 , and then a dehydration polycondensation of silanol formed a thin film of amorphous silicon oxide on the surface of the glass plate.
【００３２】次に、テトラエトキシチタンＴｉ（ＯＣ2
Ｈ5 ）4 （Ｍｅｒｃｋ）１重量部とエタノール９重量部
との混合物に加水分解抑制剤として３６％塩酸を０．１
重量部添加して酸化チタンコーティング溶液を調整し、
この溶液を前記ガラス板の表面に乾燥空気中でフローコ
ーティング法により塗布した。塗布量は酸化チタンに換
算して４５μｇ／ｃｍ2 とした。テトラエトキシチタン
の加水分解速度は極めて早いので、塗布の段階でテトラ
エトキシチタンの一部は加水分解され、水酸化チタンＴ
ｉ（ＯＨ）4 が生成し始めた。Next, tetraethoxy titanium Ti (OC 2
To a mixture of 1 part by weight of H 5 ) 4 (Merck) and 9 parts by weight of ethanol, 0.1% of 36% hydrochloric acid was added as a hydrolysis inhibitor.
A titanium oxide coating solution is prepared by adding parts by weight,
This solution was applied to the surface of the glass plate in dry air by a flow coating method. The coating amount was 45 μg / cm 2 in terms of titanium oxide. Since the rate of hydrolysis of tetraethoxytitanium is extremely fast, part of tetraethoxytitanium is hydrolyzed at the coating stage, and titanium hydroxide T
i (OH) 4 started to form.
【００３３】次に、このガラス板を１〜１０分間約１５
０℃の温度に保持することにより、テトラエトキシチタ
ンの加水分解を完了させると共に、生成した水酸化チタ
ンを脱水縮重合に付し、無定形チタンを生成させた。こ
うして、無定形酸化シリコンの上に無定形酸化チタンが
コーティングされたガラス板を得た。Next, the glass plate is exposed to about 15 minutes for about 15 minutes.
By maintaining the temperature at 0 ° C., the hydrolysis of tetraethoxytitanium was completed, and the produced titanium hydroxide was subjected to dehydration polycondensation to produce amorphous titanium. Thus, a glass plate in which amorphous titanium oxide was coated on amorphous silicon oxide was obtained.
【００３４】この試料を５００℃の温度で焼成して、無
定形酸化チタンをアナターゼ型酸化チタンに変換させガ
ラス板＃２を得た。無定形酸化チタンコーティングの下
層には無定形酸化シリコンのコーティングが施されてい
るので、焼成の最中にガラス板中のナトリウムなどのア
ルカリ網目修飾イオンはガラス基材から酸化チタンコー
ティング中に拡散していないと考えられる。This sample was fired at a temperature of 500 ° C. to convert amorphous titanium oxide into anatase type titanium oxide to obtain glass plate # 2. Since the amorphous silicon oxide coating is applied to the lower layer of the amorphous titanium oxide coating, alkali network modifying ions such as sodium in the glass plate diffuse from the glass substrate into the titanium oxide coating during firing. It is considered not to.
【００３５】また、比較のため表面に光触媒含有コーテ
ィングを施していない通常のガラス板＃３も準備した。For comparison, an ordinary glass plate # 3 having no surface coated with a photocatalyst was also prepared.
【００３６】次に、２枚のガラス板の光触媒含有コーテ
ィングを向かい合わせた間にポリビニルブチラールを挟
み、合わせガラスを製作し試料＃１〜３を得た。Then, polyvinyl butyral was sandwiched between the photocatalyst-containing coatings of two glass plates facing each other to manufacture laminated glass, and samples # 1 to 3 were obtained.
【００３７】＃１〜３の試料を数日間暗所に放置した
後、２０Ｗのブルーライトブラック（ＢＬＢ）蛍光灯
（三共電気、ＦＬ２０ＢＬＢ）を用いて試料の表面に
０．５ｍＷ／ｃｍ2 の紫外線照度（アナターゼ型酸化チ
タンのバンドギャップエネルギーより高いエネルギーの
紫外線−３８７ｎｍより短い波長の紫外線−の照度）で
約１時間紫外線を照射した。After the samples # 1 to # 3 were left in the dark for several days, a 20 W blue light black (BLB) fluorescent lamp (Sankyo Denki, FL20BLB) was used to apply 0.5 mW / cm 2 of ultraviolet rays to the surface of the samples. Ultraviolet rays were irradiated for about 1 hour at an illuminance (ultraviolet rays having an energy higher than the band gap energy of anatase type titanium oxide-ultraviolet rays having a wavelength shorter than 387 nm).
【００３８】＃１〜３試料の耐貫通性を調べたところ、
通常の合わせガラスと同等であった。またこれらを１０
０℃の条件下に７２時間放置し、中間層の発泡を視認し
たところ、通常の合わせガラス＃３では気泡が確認され
たのに対し、光触媒をコーティングした合わせガラス＃
１及び２では気泡の発生は確認できなかった。When the penetration resistance of # 1 to 3 samples was examined,
It was equivalent to ordinary laminated glass. Also these 10
When left for 72 hours at 0 ° C. and visually observed the foaming of the intermediate layer, air bubbles were observed in the ordinary laminated glass # 3, whereas the laminated glass coated with the photocatalyst #
In 1 and 2, generation of bubbles could not be confirmed.
【００３９】[0039]
【発明の効果】本発明は以上説明したように構成されて
いるので、以下に記載するような優れた効果を奏する。
合わせガラスの中間層の透明なプラスチックフィルムに
接するガラス表面に、光励起により超親水化される光触
媒含有コーティングを施しているため、製造工程もしく
は使用時において高温に曝されても中間層に気泡を発生
しない。Since the present invention is configured as described above, it has the following excellent effects.
Since the glass surface in contact with the transparent plastic film of the intermediate layer of laminated glass is coated with a photocatalyst that is made superhydrophilic by photoexcitation, bubbles are generated in the intermediate layer even when exposed to high temperatures during the manufacturing process or use. do not do.
【図１】本発明の一実施の形態の合わせガラス及びその
製造方法を説明するための合わせガラスの断面図であ
る。FIG. 1 is a cross-sectional view of a laminated glass for explaining a laminated glass and a manufacturing method thereof according to an embodiment of the present invention.
１，２ ガラス板 ３，４ 光触媒含有層 ５ プラスチックフィルム 1, 2 glass plate 3, 4 photocatalyst containing layer 5 plastic film
Claims (9)
を介装し圧着してなる合わせガラスにおいて、プラスチ
ックフィルムと接触するガラス部材の二つの接触面のう
ち、少なくとも一方の接触面に光触媒含有膜を有する合
わせガラス。1. A laminated glass comprising a plurality of glass members with a plastic film interposed and pressure bonded, wherein at least one of the two contact surfaces of the glass member which comes into contact with the plastic film has a photocatalyst-containing film. Laminated glass.
スチックフィルムと接触させるガラス部材の少なくとも
一方の表面に光触媒材料をコーティングする工程と、紫
外線照射により光触媒材料を光励起する工程と、少なく
とも一方のガラス部材の光触媒材料コーティング面とプ
ラスチックフィルムとが接触するようにプラスチックフ
ィルムを複数のガラス部材に挟み圧着して合わせガラス
を作製する工程を有する合わせガラスの製造方法。2. A step of preparing a plurality of glass members, a step of coating a photocatalyst material on at least one surface of a glass member to be brought into contact with a plastic film, a step of photoexciting a photocatalyst material by ultraviolet irradiation, and at least one of: 1. A method for producing a laminated glass, comprising a step of producing a laminated glass by sandwiching a plastic film between a plurality of glass members so that the surface of the glass member coated with the photocatalyst material and the plastic film are in contact with each other and press-bonding.
光を減衰することなく透過させる材料で構成されている
請求項１もしくは２のいずれか一に記載の合わせガラス
及びその製造方法。3. The laminated glass according to claim 1, wherein the plastic film is made of a material that allows light in the ultraviolet wavelength region to pass through without being attenuated, and the method for producing the same.
ることなく透過させる請求項１もしくは２のいずれか一
に記載の合わせガラス及びその製造方法。4. The laminated glass according to claim 1 or 2, and the method for producing the same, wherein the glass member allows light in the ultraviolet wavelength region to pass through without attenuation.
は２のいずれか一に記載の合わせガラス及びその製造方
法。5. The laminated glass according to claim 1, wherein the photocatalyst is titanium oxide, and the method for producing the same.
る請求項１もしくは２のいずれか一に記載の合わせガラ
ス及びその製造方法。6. The laminated glass according to claim 1, wherein the photocatalyst is composed of titanium oxide and silicon oxide, and the method for producing the same.
リコーンである請求項１もしくは２のいずれか一に記載
の合わせガラス及びその製造方法。7. The laminated glass according to claim 1, wherein the photocatalyst is a silicone partially substituted with titanium oxide for hydroxy, and a method for producing the same.
接触角に換算して約１０°以下の水漏れ性を呈する請求
項１もしくは２のいずれか一に記載の合わせガラス及び
その製造方法。8. The laminated glass and the production thereof according to claim 1, wherein the surface of the photocatalyst-containing layer exhibits a water leak property of about 10 ° or less in terms of a contact angle with water upon photoexcitation. Method.
接触角に換算して約５°以下の水漏れ性を呈する請求項
１もしくは２のいずれか一に記載の合わせガラス及びそ
の製造方法。9. The laminated glass according to claim 1, wherein the surface of the photocatalyst-containing layer has a water leakage property of about 5 ° or less in terms of a contact angle with water upon photoexcitation, and the production thereof. Method.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP8136777A JPH09227178A (en) | 1995-12-22 | 1996-05-30 | Laminated glass and its production |
Applications Claiming Priority (3)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7-354649 | 1995-12-22 | ||
| JP35464995 | 1995-12-22 | ||
| JP8136777A JPH09227178A (en) | 1995-12-22 | 1996-05-30 | Laminated glass and its production |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH09227178A true JPH09227178A (en) | 1997-09-02 |
Family
ID=18438979
Family Applications (71)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP8083499A Pending JPH09231821A (en) | 1995-12-22 | 1996-04-05 | Luminaire and method for maintaining illuminance |
| JP13408196A Expired - Lifetime JP3385850B2 (en) | 1995-12-22 | 1996-04-19 | Composite material with hydrophilicity |
| JP10079496A Expired - Lifetime JP3740736B2 (en) | 1995-12-22 | 1996-04-23 | HEAT EXCHANGER AND HEAT EXCHANGER OPERATION METHOD |
| JP15017196A Expired - Lifetime JP3760509B2 (en) | 1995-12-22 | 1996-05-22 | Greenhouse ceiling and its condensation prevention method |
| JP8150410A Pending JPH09225263A (en) | 1995-12-22 | 1996-05-23 | Air pollutant removing filter, air pollutant removing fan and ventilator using the fan |
| JP8156383A Pending JPH09231849A (en) | 1995-12-22 | 1996-05-29 | Insulator and dirt preventing method therefore |
| JP8136777A Pending JPH09227178A (en) | 1995-12-22 | 1996-05-30 | Laminated glass and its production |
| JP13653596A Expired - Lifetime JP3339304B2 (en) | 1995-12-22 | 1996-05-30 | Painted object and painting method |
| JP13782996A Ceased JP3189682B2 (en) | 1995-12-22 | 1996-05-31 | Antifouling material |
| JP8168643A Pending JPH09232096A (en) | 1995-12-22 | 1996-06-06 | Electrification preventing method, and electrification preventive composite material |
| JP8145265A Pending JPH09225276A (en) | 1995-12-22 | 1996-06-07 | Separating membrane and formation of surface layer to separating membrane |
| JP8168662A Pending JPH09225389A (en) | 1995-12-22 | 1996-06-10 | Method for making member hydrophilic and preventing deterioration by ultraviolet ray, hydrophilic ultraviolet resistant member and its manufacture |
| JP8158518A Pending JPH09225021A (en) | 1995-12-22 | 1996-06-19 | Medical material |
| JP8195184A Expired - Lifetime JP3003581B2 (en) | 1995-12-22 | 1996-06-20 | A member that exhibits hydrophilicity in response to optical excitation of an optical semiconductor |
| JP8272814A Pending JPH09226041A (en) | 1995-12-22 | 1996-09-06 | Member for preventing attachment of condensation water drop and method for preventing attachment of condensation water drop of the member |
| JP8272815A Pending JPH09224957A (en) | 1995-12-22 | 1996-09-06 | Laser beam focusing lens, dentistry and oral surgery treatment device using the same, and preventing device of laser beam irregular reflection due to stuck waterdrop |
| JP8272808A Pending JPH09229724A (en) | 1995-12-22 | 1996-09-07 | Non-fogging cover for instrument panel of motorcycle, motorcycle equipped with the cover, and fogging-preventing method for the cover |
| JP27280996A Expired - Fee Related JP3588202B2 (en) | 1995-12-22 | 1996-09-07 | Anti-fog road mirror and its anti-fog method |
| JP8238927A Pending JPH09227159A (en) | 1995-12-22 | 1996-09-10 | Front and rear window glass of vehicle |
| JP8275189A Pending JPH09231807A (en) | 1995-12-22 | 1996-09-10 | Vehicle headlight cover, vehicle with it, and its defogging method |
| JP27519096A Expired - Lifetime JP3277983B2 (en) | 1995-12-22 | 1996-09-10 | Outdoor display panel and its cleaning method |
| JP8281220A Expired - Lifetime JP3003593B2 (en) | 1995-12-22 | 1996-09-17 | Photocatalytic hydrophilic member |
| JP8281222A Pending JPH09230106A (en) | 1995-12-22 | 1996-09-17 | Anti-fogging camera filter and its anti-fogging method |
| JP8281224A Pending JPH09228134A (en) | 1995-12-22 | 1996-09-17 | Antifogging helmet shield and antifogging method |
| JP8281223A Expired - Lifetime JP3063968B2 (en) | 1995-12-22 | 1996-09-17 | Anti-fog vehicle mirror, automobile equipped with the same, anti-fog film for vehicle mirror and anti-fog method for vehicle mirror |
| JP8281225A Pending JPH09230107A (en) | 1995-12-22 | 1996-09-17 | Anti-fogging glass lens and its anti-fogging method |
| JP28122196A Expired - Lifetime JP3743075B2 (en) | 1995-12-22 | 1996-09-17 | Antifogging dental mirror and antifogging method |
| JP8246180A Pending JPH09230493A (en) | 1995-12-22 | 1996-09-18 | Camera |
| JP8282807A Pending JPH09224874A (en) | 1995-12-22 | 1996-09-18 | Water-closet bowl made of resin |
| JP8282810A Pending JPH09228545A (en) | 1995-12-22 | 1996-09-18 | Glass block and its cleaning method |
| JP28281296A Expired - Lifetime JP3612896B2 (en) | 1995-12-22 | 1996-09-18 | Exterior wall building materials and methods for cleaning them |
| JP8282805A Pending JPH09231499A (en) | 1995-12-22 | 1996-09-18 | Light source cover for traffic signal, traffic signal with it, and cleaning method for light source cover for traffic signal |
| JP8282809A Pending JPH09230108A (en) | 1995-12-22 | 1996-09-18 | Anti-fogging plastic lens and its anti-fogging method |
| JP8282806A Pending JPH09228057A (en) | 1995-12-22 | 1996-09-18 | Wheel and its cleaning method |
| JP08282811A Expired - Fee Related JP3075195B2 (en) | 1995-12-22 | 1996-09-18 | Anti-fog wash mirror, vanity table provided with the same, anti-fog film for wash mirror and anti-fog method for wash mirror |
| JP8282808A Pending JPH09228765A (en) | 1995-12-22 | 1996-09-18 | Blind and manufacture thereof |
| JP8284532A Pending JPH09227805A (en) | 1995-12-22 | 1996-09-19 | Photocatalytic hydrophilic coating composition |
| JP8284533A Pending JPH09227161A (en) | 1995-12-22 | 1996-09-19 | Pane, film for applying thereto and antifogging and cleaning thereof |
| JP28453496A Expired - Lifetime JP3173391B2 (en) | 1995-12-22 | 1996-09-19 | Hydrophilic film, and method for producing and using the same |
| JP28579796A Expired - Lifetime JP3697795B2 (en) | 1995-12-22 | 1996-09-20 | Display and cleaning method thereof |
| JP28895596A Expired - Lifetime JP3774955B2 (en) | 1995-12-22 | 1996-09-25 | Self-cleaning handrail and handrail cleaning method |
| JP28895496A Expired - Fee Related JP3588205B2 (en) | 1995-12-22 | 1996-09-25 | Self-cleaning guard fence and method of cleaning guard fence |
| JP28895696A Expired - Fee Related JP3588206B2 (en) | 1995-12-22 | 1996-09-25 | Self-cleaning road decorative panel, and method of cleaning road decorative panel |
| JP8291007A Pending JPH09225054A (en) | 1995-12-22 | 1996-09-26 | Gas mask and storing device for gas mask |
| JP8291005A Pending JPH09230031A (en) | 1995-12-22 | 1996-09-26 | Inter-vehicle distance detecting device and automobile having it |
| JP8291006A Pending JPH09229767A (en) | 1995-12-22 | 1996-09-26 | Pyroelectric infrared detector |
| JP8297248A Pending JPH09227169A (en) | 1995-12-22 | 1996-10-18 | Transfer sheet, and transferring of photocatalytic and hydrophilic thin film |
| JP8298237A Pending JPH09229546A (en) | 1995-12-22 | 1996-10-22 | Door for refrigerated showcase having see-through ensuring property |
| JP8298236A Pending JPH09227162A (en) | 1995-12-22 | 1996-10-22 | Vehicle pane for securing rainy weather view, and automobile mounted therewith |
| JP8298235A Pending JPH09230119A (en) | 1995-12-22 | 1996-10-22 | Road mirror for assuring visual field in rainy weather |
| JP8298234A Pending JPH09226531A (en) | 1995-12-22 | 1996-10-22 | Rainy weather visibility securable vehicular mirror, automobile and two wheeler having it |
| JP8306997A Pending JPH09226060A (en) | 1995-12-22 | 1996-11-01 | Lid for heating container having fog resistance |
| JP8307000A Pending JPH09224800A (en) | 1995-12-22 | 1996-11-01 | Glassware and water-washing method |
| JP8323516A Pending JPH09241038A (en) | 1995-12-22 | 1996-11-19 | Photocatalytic hydrophilic member and its production |
| JP8340470A Pending JPH09225387A (en) | 1995-12-22 | 1996-12-05 | Hydrophilic member and method to make surface of member hydrophilic |
| JP34047296A Expired - Fee Related JP3348613B2 (en) | 1995-12-22 | 1996-12-05 | Photocatalytic hydrophilic coating composition |
| JP34047196A Expired - Lifetime JP3303696B2 (en) | 1995-12-22 | 1996-12-05 | Photocatalytic hydrophilic coating composition |
| JP08344585A Expired - Lifetime JP3141802B2 (en) | 1995-12-22 | 1996-12-09 | Hydrophilic member and method for maintaining hydrophilicity |
| JP23956799A Expired - Lifetime JP3613084B2 (en) | 1995-12-22 | 1999-08-26 | A member that exhibits hydrophilicity in response to photoexcitation of an optical semiconductor |
| JP23956899A Expired - Lifetime JP3613085B2 (en) | 1995-12-22 | 1999-08-26 | Photocatalytic hydrophilic member |
| JP34300999A Expired - Fee Related JP3844182B2 (en) | 1995-12-22 | 1999-12-02 | Hydrophilic film and method for producing and using the same |
| JP2000180301A Expired - Lifetime JP3414365B2 (en) | 1995-12-22 | 2000-06-15 | Building materials for exterior walls |
| JP2000181287A Expired - Fee Related JP3465664B2 (en) | 1995-12-22 | 2000-06-16 | Building materials for exterior walls |
| JP2000181286A Expired - Lifetime JP3414367B2 (en) | 1995-12-22 | 2000-06-16 | Building materials for exterior walls |
| JP2000181284A Pending JP2001048679A (en) | 1995-12-22 | 2000-06-16 | Photocatalytic hydrophilic tile and its production |
| JP2000227055A Withdrawn JP2001089752A (en) | 1995-12-22 | 2000-07-27 | Member capable of obtaining hydrophilic nature in accordance with photoexcitation of optical semiconductor and manufacturing method thereof |
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| JP2002244772A Pending JP2003113345A (en) | 1995-12-22 | 2002-08-26 | Antistatic coating composition |
Family Applications Before (6)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP8083499A Pending JPH09231821A (en) | 1995-12-22 | 1996-04-05 | Luminaire and method for maintaining illuminance |
| JP13408196A Expired - Lifetime JP3385850B2 (en) | 1995-12-22 | 1996-04-19 | Composite material with hydrophilicity |
| JP10079496A Expired - Lifetime JP3740736B2 (en) | 1995-12-22 | 1996-04-23 | HEAT EXCHANGER AND HEAT EXCHANGER OPERATION METHOD |
| JP15017196A Expired - Lifetime JP3760509B2 (en) | 1995-12-22 | 1996-05-22 | Greenhouse ceiling and its condensation prevention method |
| JP8150410A Pending JPH09225263A (en) | 1995-12-22 | 1996-05-23 | Air pollutant removing filter, air pollutant removing fan and ventilator using the fan |
| JP8156383A Pending JPH09231849A (en) | 1995-12-22 | 1996-05-29 | Insulator and dirt preventing method therefore |
Family Applications After (64)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP13653596A Expired - Lifetime JP3339304B2 (en) | 1995-12-22 | 1996-05-30 | Painted object and painting method |
| JP13782996A Ceased JP3189682B2 (en) | 1995-12-22 | 1996-05-31 | Antifouling material |
| JP8168643A Pending JPH09232096A (en) | 1995-12-22 | 1996-06-06 | Electrification preventing method, and electrification preventive composite material |
| JP8145265A Pending JPH09225276A (en) | 1995-12-22 | 1996-06-07 | Separating membrane and formation of surface layer to separating membrane |
| JP8168662A Pending JPH09225389A (en) | 1995-12-22 | 1996-06-10 | Method for making member hydrophilic and preventing deterioration by ultraviolet ray, hydrophilic ultraviolet resistant member and its manufacture |
| JP8158518A Pending JPH09225021A (en) | 1995-12-22 | 1996-06-19 | Medical material |
| JP8195184A Expired - Lifetime JP3003581B2 (en) | 1995-12-22 | 1996-06-20 | A member that exhibits hydrophilicity in response to optical excitation of an optical semiconductor |
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| JP8282810A Pending JPH09228545A (en) | 1995-12-22 | 1996-09-18 | Glass block and its cleaning method |
| JP28281296A Expired - Lifetime JP3612896B2 (en) | 1995-12-22 | 1996-09-18 | Exterior wall building materials and methods for cleaning them |
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| JP8282806A Pending JPH09228057A (en) | 1995-12-22 | 1996-09-18 | Wheel and its cleaning method |
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| JP8284532A Pending JPH09227805A (en) | 1995-12-22 | 1996-09-19 | Photocatalytic hydrophilic coating composition |
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| JP28453496A Expired - Lifetime JP3173391B2 (en) | 1995-12-22 | 1996-09-19 | Hydrophilic film, and method for producing and using the same |
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| JP28895696A Expired - Fee Related JP3588206B2 (en) | 1995-12-22 | 1996-09-25 | Self-cleaning road decorative panel, and method of cleaning road decorative panel |
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| JP8298235A Pending JPH09230119A (en) | 1995-12-22 | 1996-10-22 | Road mirror for assuring visual field in rainy weather |
| JP8298234A Pending JPH09226531A (en) | 1995-12-22 | 1996-10-22 | Rainy weather visibility securable vehicular mirror, automobile and two wheeler having it |
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| JP8323516A Pending JPH09241038A (en) | 1995-12-22 | 1996-11-19 | Photocatalytic hydrophilic member and its production |
| JP8340470A Pending JPH09225387A (en) | 1995-12-22 | 1996-12-05 | Hydrophilic member and method to make surface of member hydrophilic |
| JP34047296A Expired - Fee Related JP3348613B2 (en) | 1995-12-22 | 1996-12-05 | Photocatalytic hydrophilic coating composition |
| JP34047196A Expired - Lifetime JP3303696B2 (en) | 1995-12-22 | 1996-12-05 | Photocatalytic hydrophilic coating composition |
| JP08344585A Expired - Lifetime JP3141802B2 (en) | 1995-12-22 | 1996-12-09 | Hydrophilic member and method for maintaining hydrophilicity |
| JP23956799A Expired - Lifetime JP3613084B2 (en) | 1995-12-22 | 1999-08-26 | A member that exhibits hydrophilicity in response to photoexcitation of an optical semiconductor |
| JP23956899A Expired - Lifetime JP3613085B2 (en) | 1995-12-22 | 1999-08-26 | Photocatalytic hydrophilic member |
| JP34300999A Expired - Fee Related JP3844182B2 (en) | 1995-12-22 | 1999-12-02 | Hydrophilic film and method for producing and using the same |
| JP2000180301A Expired - Lifetime JP3414365B2 (en) | 1995-12-22 | 2000-06-15 | Building materials for exterior walls |
| JP2000181287A Expired - Fee Related JP3465664B2 (en) | 1995-12-22 | 2000-06-16 | Building materials for exterior walls |
| JP2000181286A Expired - Lifetime JP3414367B2 (en) | 1995-12-22 | 2000-06-16 | Building materials for exterior walls |
| JP2000181284A Pending JP2001048679A (en) | 1995-12-22 | 2000-06-16 | Photocatalytic hydrophilic tile and its production |
| JP2000227055A Withdrawn JP2001089752A (en) | 1995-12-22 | 2000-07-27 | Member capable of obtaining hydrophilic nature in accordance with photoexcitation of optical semiconductor and manufacturing method thereof |
| JP2000227056A Pending JP2001129916A (en) | 1995-12-22 | 2000-07-27 | Photocatalytic hydrophilic member |
| JP2000247609A Pending JP2001122679A (en) | 1995-12-22 | 2000-08-17 | Antifouling tile |
| JP2001140242A Pending JP2002030258A (en) | 1995-12-22 | 2001-05-10 | Coated material and method for coating |
| JP2002020533A Expired - Fee Related JP3882625B2 (en) | 1995-12-22 | 2002-01-29 | Sound insulation wall and cleaning method for sound insulation wall |
| JP2002244772A Pending JP2003113345A (en) | 1995-12-22 | 2002-08-26 | Antistatic coating composition |
Country Status (1)
| Country | Link |
|---|---|
| JP (71) | JPH09231821A (en) |
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| JPH0810576A (en) * | 1994-07-05 | 1996-01-16 | Ebara Res Co Ltd | Removing method of harmful gas and device therefor |
| JPH08119673A (en) * | 1994-10-21 | 1996-05-14 | Kansai Paint Co Ltd | Hydrophilization treatment of glass |
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| JPH08277147A (en) * | 1995-03-31 | 1996-10-22 | Nippon Muki Co Ltd | Plate glass |
| JP3101537B2 (en) * | 1995-05-10 | 2000-10-23 | ワイケイケイ株式会社 | Antifouling building material and exterior building material unit |
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1996
- 1996-04-05 JP JP8083499A patent/JPH09231821A/en active Pending
- 1996-04-19 JP JP13408196A patent/JP3385850B2/en not_active Expired - Lifetime
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- 1996-09-18 JP JP8246180A patent/JPH09230493A/en active Pending
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1999
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2000
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2001
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2002
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2001080974A (en) * | 1999-09-08 | 2001-03-27 | Fuji Photo Film Co Ltd | Composite base plate material and method for producing the same |
| JP2016104681A (en) * | 2014-12-01 | 2016-06-09 | 大日本印刷株式会社 | Method for producing laminated glass, and laminated glass |
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