JPH09226060A - Lid for heating container having fog resistance - Google Patents

Lid for heating container having fog resistance

Info

Publication number
JPH09226060A
JPH09226060A JP8306997A JP30699796A JPH09226060A JP H09226060 A JPH09226060 A JP H09226060A JP 8306997 A JP8306997 A JP 8306997A JP 30699796 A JP30699796 A JP 30699796A JP H09226060 A JPH09226060 A JP H09226060A
Authority
JP
Japan
Prior art keywords
surface layer
water
lid
sample
heating container
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
Application number
JP8306997A
Other languages
Japanese (ja)
Inventor
Atsushi Kitamura
厚 北村
Makoto Hayakawa
信 早川
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Toto Ltd
Original Assignee
Toto Ltd
Priority date (The priority date 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 date listed.)
Filing date
Publication date
Family has litigation
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Application filed by Toto Ltd filed Critical Toto Ltd
Priority to JP8306997A priority Critical patent/JPH09226060A/en
Publication of JPH09226060A publication Critical patent/JPH09226060A/en
Pending legal-status Critical Current

Links

Classifications

    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28HEAT EXCHANGE IN GENERAL
    • F28FDETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
    • F28F13/00Arrangements for modifying heat-transfer, e.g. increasing, decreasing
    • F28F13/18Arrangements for modifying heat-transfer, e.g. increasing, decreasing by applying coatings, e.g. radiation-absorbing, radiation-reflecting; by surface treatment, e.g. polishing
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F24HEATING; RANGES; VENTILATING
    • F24FAIR-CONDITIONING; AIR-HUMIDIFICATION; VENTILATION; USE OF AIR CURRENTS FOR SCREENING
    • F24F8/00Treatment, e.g. purification, of air supplied to human living or working spaces otherwise than by heating, cooling, humidifying or drying
    • F24F8/20Treatment, e.g. purification, of air supplied to human living or working spaces otherwise than by heating, cooling, humidifying or drying by sterilisation
    • F24F8/22Treatment, 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
    • FMECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28HEAT EXCHANGE IN GENERAL
    • F28FDETAILS OF HEAT-EXCHANGE AND HEAT-TRANSFER APPARATUS, OF GENERAL APPLICATION
    • F28F2245/00Coatings; Surface treatments
    • F28F2245/02Coatings; Surface treatments hydrophilic

Landscapes

  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • General Engineering & Computer Science (AREA)
  • Thermal Sciences (AREA)
  • Chemical & Material Sciences (AREA)
  • Combustion & Propulsion (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)
  • Pigments, Carbon Blacks, Or Wood Stains (AREA)
  • Building Environments (AREA)
  • Refuge Islands, Traffic Blockers, Or Guard Fence (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Road Signs Or Road Markings (AREA)
  • Rear-View Mirror Devices That Are Mounted On The Exterior Of The Vehicle (AREA)
  • Dental Tools And Instruments Or Auxiliary Dental Instruments (AREA)
  • Exhaust Gas Treatment By Means Of Catalyst (AREA)
  • Illuminated Signs And Luminous Advertising (AREA)
  • Detergent Compositions (AREA)
  • Compositions Of Macromolecular Compounds (AREA)
  • Joining Of Glass To Other Materials (AREA)
  • Devices For Indicating Variable Information By Combining Individual Elements (AREA)
  • Panels For Use In Building Construction (AREA)
  • Bridges Or Land Bridges (AREA)
  • Aftertreatments Of Artificial And Natural Stones (AREA)
  • Greenhouses (AREA)
  • Devices Affording Protection Of Roads Or Walls For Sound Insulation (AREA)
  • Cleaning And De-Greasing Of Metallic Materials By Chemical Methods (AREA)
  • Mirrors, Picture Frames, Photograph Stands, And Related Fastening Devices (AREA)
  • Physical Vapour Deposition (AREA)
  • Optical Radar Systems And Details Thereof (AREA)

Abstract

PROBLEM TO BE SOLVED: To obtain a lid for heating container having excellent fog resistance which prevents fog and attachment of water drops and has excellent visibility of foods to be displayed, by providing a surface layer which contains substantially transparent photocatalytic particles on at least an inside surface of a lid base material for a transparent heating container. SOLUTION: On at least an inside surface of a transparent lid base material, a surface layer which contains a substantially transparent photocatalyst is provided. Thus, the surface of the surface layer shows hydrophilic property in response to light excitation of the photocatalyst. To the surface layer, a silica and a solid acid or a silicone is added. The photocalyst means a substance wherein an excitation (light excitation) of electron in valence band is generated so as to generate conduction electron and electron hole when an energy which is larger than an energy gap between a conduction band of its crystal and the valence band, i.e., a light (excitation light) of short wavelength is applied. For example, an anatase-type titanium oxide, a rutile-type titanium oxide, a tin oxide, a zinc oxide, and a bismuth trioxide are suitably utilized.

Description

【発明の詳細な説明】Detailed Description of the Invention

【0001】[0001]

【発明の属する技術分野】本発明は、おでん等の保温状
態で売買する食品を、陳列状態で保管するための加熱容
器用の蓋に関する。
BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a lid for a heating container for storing food such as oden sold in a warm state in a display state.

【0002】[0002]

【従来の技術】おでん等の食品は保温状態で売買するた
めに、加熱容器中に保管される。その際に、水分の蒸発
を抑えるなどの目的のため、例えば、木製の蓋をする。
しかし、木製の蓋をすると、売買する食品が外から見え
ない。そこで、蓋を透明にすれば、蓋の内部の食品を陳
列状態で保管できて都合がよい。
2. Description of the Related Art Food such as oden is stored in a heating container in order to buy and sell it while keeping it warm. At that time, for example, a wooden lid is used for the purpose of suppressing evaporation of water.
But with a wooden lid, the food you buy and sell cannot be seen from the outside. Therefore, if the lid is made transparent, the food in the lid can be conveniently stored in a display state.

【0003】[0003]

【発明が解決しようとする課題】しかしながら、蓋を単
に透明にしただけでは、蓋の内側は蒸気の凝縮により曇
るので、内部の陳列食品は結局外から明瞭に視認するの
が困難である。蒸気の凝縮が更に進行し、細かい凝縮水
滴が互いに融合して大きな水滴に成長したときにも、水
滴と透明蓋との界面並びに水滴と空気との界面における
光の屈折により透視像が歪むので、やはり内部の食品が
見えにくい。本発明の目的は、曇りや水滴付着を防止す
ることが可能で、陳列された食品の視認性に優れた防曇
性を有する加熱容器用蓋を提供することにある。
However, if the lid is simply made transparent, the inside of the lid becomes cloudy due to vapor condensation, and it is difficult to visually recognize the displayed food from the outside. Even when the condensation of steam further progresses and even small condensed water droplets fuse with each other to grow into large water droplets, the perspective image is distorted by the refraction of light at the interface between the water droplet and the transparent lid and the interface between the water droplet and air. After all it is hard to see the food inside. An object of the present invention is to provide a lid for a heating container capable of preventing fogging and water droplet adhesion and having excellent anti-fogging property with excellent visibility of displayed food products.

【0004】[0004]

【課題を解決するための手段】本発明は、光触媒を含有
する表面層を形成した部材において、光触媒を光励起す
ると、部材の表面が高度に親水化されるという発見に基
づく。この現象は以下に示す機構により進行すると考え
られる。すなわち、光触媒の価電子帯上端と伝導帯下端
とのエネルギーギャップ以上のエネルギーを有する光が
光触媒に照射されると、光触媒の価電子帯中の電子が励
起されて伝導電子と正孔が生成し、そのいずれかまたは
双方の作用により、おそらく表面に極性が付与され、水
や水酸基等の極性成分が集められる。そして伝導電子と
正孔のいずれかまたは双方と、上記極性成分との協調的
な作用により、表面と前記表面に化学的に吸着した汚染
物質との化学結合を切断すると共に、表面に化学吸着水
が吸着し、さらに物理吸着水層がその上に形成されるの
である。また、一旦部材表面が高度に親水化されたなら
ば、部材を暗所に保持しても、表面の親水性はある程度
の期間持続する。
SUMMARY OF THE INVENTION The present invention is based on the discovery that, in a member having a surface layer containing a photocatalyst formed thereon, when the photocatalyst is photoexcited, the surface of the member is highly hydrophilized. This phenomenon is considered to proceed by the following mechanism. That is, when the photocatalyst is irradiated with light having an energy larger than the energy gap between the valence band upper end and the conduction band lower end of the photocatalyst, the electrons in the valence band of the photocatalyst are excited to generate conduction electrons and holes. The action of either or both of them probably imparts polarity to the surface and collects polar components such as water and hydroxyl groups. Then, one or both of conduction electrons and holes and the above-mentioned polar component cooperate with each other to cut off a chemical bond between the surface and the contaminant chemically adsorbed on the surface, and to cause a chemical adsorbed water on the surface. Is adsorbed, and a physically adsorbed water layer is formed thereon. Further, once the surface of the member is highly hydrophilized, the hydrophilicity of the surface is maintained for a certain period even if the member is kept in a dark place.

【0005】本発明では、透明な蓋基材の少なくとも内
側表面に、実質的に透明な光触媒を含有する表面層を備
えた防曇性を有する加熱容器用蓋を提供する。光触媒を
含有する表面層を備えることにより、光触媒の光励起に
応じて、表面層の表面は親水性を呈する。表面層の表面
が親水性を呈すると、蓋の内側に蒸気の凝縮により凝縮
水が付着したりしても、付着した湿分の凝縮水が前記層
の表面に一様に広がり、湿分凝縮水によって曇るのが防
止されるようになる。
According to the present invention, there is provided a lid for a heating container having an antifogging property, which comprises a transparent lid base material and a surface layer containing a substantially transparent photocatalyst on at least an inner surface thereof. By providing the surface layer containing the photocatalyst, the surface of the surface layer exhibits hydrophilicity in response to photoexcitation of the photocatalyst. When the surface of the surface layer is hydrophilic, even if condensed water adheres to the inside of the lid due to condensation of steam, the condensed water of the adhered moisture spreads evenly on the surface of the layer, and the moisture is condensed. Water will prevent it from becoming cloudy.

【0006】本発明の好ましい態様においては、表面層
には、さらにシリカが含有されているようにする。シリ
カが含有されることにより、表面が水濡れ角0゜に近い
高度の親水性を呈しやすくなると共に、暗所に保持した
ときの親水維持性が向上する。その理由はシリカは構造
中に水を蓄えることができることと関係していると思わ
れる。
In a preferred embodiment of the present invention, the surface layer further contains silica. By containing silica, the surface is likely to exhibit a high degree of hydrophilicity near a water wetting angle of 0 °, and the hydrophilicity retention when held in a dark place is improved. The reason seems to be related to the ability of silica to store water in its structure.

【0007】本発明の好ましい態様においては、表面層
には、さらに固体酸が含有されているようにする。固体
酸が含有されることにより、表面が水濡れ角0゜に近い
高度の親水性を呈しやすくなると共に、暗所に保持した
ときの親水維持性が向上する。その理由は表面層に固体
酸が含有されると、表面の極性が、光の有無にかかわら
ず大きな状態にあるために、疎水性分子よりも極性分子
である水分子を選択的に吸着させやすい。そのため安定
な物理吸着水層が形成されやすく、暗所に保持しても、
表面の親水性をかなり長期にわたり高度に維持できる。
In a preferred embodiment of the present invention, the surface layer further contains a solid acid. When the solid acid is contained, the surface is likely to exhibit a high degree of hydrophilicity near a water wetting angle of 0 °, and the hydrophilicity retention when kept in a dark place is improved. The reason is that when a solid acid is contained in the surface layer, the polarity of the surface is large regardless of the presence or absence of light, so it is easier to selectively adsorb water molecules that are polar molecules than hydrophobic molecules. . Therefore, a stable physical adsorption water layer is easily formed, and even if it is kept in a dark place,
Surface hydrophilicity can be maintained at a high level for a fairly long time.

【0008】本発明の好ましい態様においては、表面層
には、さらにシリコーンが含有されているようにする。
シリコーンが含有されることにより、光触媒の光励起に
よって、シリコーン中のシリコン原子に結合する有機基
の少なくとも一部が水酸基に置換され、さらにその上に
物理吸着水層が形成されることにより、表面が水濡れ角
0゜に近い高度の親水性を呈するようになると共に、暗
所に保持したときの親水維持性が向上する。
In a preferred embodiment of the present invention, the surface layer further contains silicone.
By containing silicone, by photoexcitation of the photocatalyst, at least a part of the organic group bonded to the silicon atom in the silicone is replaced with a hydroxyl group, and a physically adsorbed water layer is formed on the organic group, so that the surface is It exhibits a high degree of hydrophilicity close to a water wetting angle of 0 °, and improves the hydrophilicity maintaining ability when kept in a dark place.

【0009】[0009]

【発明の実施の形態】次に、本発明の具体的な構成につ
いて説明する。本発明における加熱容器用蓋基材の内側
表面には、図1又は図2に示すように、基材の表面に光
触媒を含む層が形成されている。このような表面構造を
とることで、加熱容器用蓋の内側表面は、光触媒の光励
起に応じて高度に親水化されるのである。それにより、
蓋の内側に蒸気の凝縮により凝縮水が付着したりして
も、付着した湿分の凝縮水が前記層の表面に一様に広が
り、湿分凝縮水によって曇るのが防止されるようにな
る。
BEST MODE FOR CARRYING OUT THE INVENTION Next, a specific structure of the present invention will be described. As shown in FIG. 1 or 2, on the inner surface of the heating container lid base material of the present invention, a layer containing a photocatalyst is formed on the surface of the base material. By taking such a surface structure, the inner surface of the heating container lid is highly hydrophilized in response to photoexcitation of the photocatalyst. Thereby,
Even if condensed water adheres to the inside of the lid due to the condensation of steam, the condensed water of the adhered moisture spreads evenly on the surface of the layer and prevents the condensed water of the moisture from fogging. .

【0010】図1においては、表面層が光触媒のみから
なる場合には、光触媒は酸化物であることが好ましい。
そうすることにより、酸化物は環境中の汚染物質が吸着
していない状態では親水性を示すので、光励起作用によ
りその汚染物質を排斥させ、吸着水層を形成させること
で、親水性を呈しやすく、一様な水膜が形成できる。図
2において、Mは金属元素を示す。従って、図2の場
合、最表面は一般の無機酸化物からなる。この場合も、
酸化物は環境中の汚染物質が吸着していない状態では親
水性を示すので、上記無機酸化物以外に表面層に混入す
る光触媒性酸化チタンの光励起作用によりその汚染物質
を排斥させ、吸着水層を形成させることで、一様な水膜
が形成できる。
In FIG. 1, when the surface layer comprises only a photocatalyst, the photocatalyst is preferably an oxide.
By doing so, the oxide shows hydrophilicity in the state where the pollutants in the environment are not adsorbed, so that the pollutants are rejected by the photoexcitation action and the adsorbed water layer is formed, so that the oxides easily exhibit hydrophilicity. A uniform water film can be formed. In FIG. 2, M represents a metal element. Therefore, in the case of FIG. 2, the outermost surface is made of a general inorganic oxide. Again,
Since the oxide is hydrophilic when the pollutants in the environment are not adsorbed, the photocatalytic titanium oxide mixed into the surface layer other than the inorganic oxide removes the contaminants by the photoexciting action, and the adsorbed water layer Is formed, a uniform water film can be formed.

【0011】本発明における加熱容器用蓋基材には、ガ
ラス、透明プラスチック、透明プラスチック基材の上に
透明なハードコートを設けた基材等の、透明体が好適に
利用できる。
For the lid material for the heating container in the present invention, a transparent body such as glass, transparent plastic, or a transparent plastic substrate provided with a transparent hard coat can be preferably used.

【0012】光触媒とは、その結晶の伝導帯と価電子帯
との間のエネルギーギャップよりも大きなエネルギー
(すなわち短い波長)の光(励起光)を照射したとき
に、価電子帯中の電子の励起(光励起)が生じて、伝導
電子と正孔を生成しうる物質をいい、例えば、アナター
ゼ型酸化チタン、ルチル型酸化チタン、酸化錫、酸化亜
鉛、三酸化二ビスマス、三酸化タングステン、酸化第二
鉄、チタン酸ストロンチウム等が好適に利用できる。こ
こで光触媒の光励起に用いる光源としては、太陽光、室
内照明、専用照明が利用でき、その種類としては、蛍光
灯、白熱電灯、室内照明、メタルハライドランプ、水銀
ランプ、キセノンランプ、殺菌灯等が好適に利用でき
る。光触媒の光励起により、基材表面が高度に親水化さ
れるためには、励起光の照度は、0.001mW/cm
2以上あればよいが、0.01mW/cm2以上だと好ま
しく、0.1mW/cm2以上だとより好ましい。
A photocatalyst is a photocatalyst of an electron in the valence band when it is irradiated with light (excitation light) having an energy (that is, a short wavelength) larger than the energy gap between the conduction band and the valence band of the crystal. A substance that is excited (photoexcited) to generate conduction electrons and holes. For example, anatase-type titanium oxide, rutile-type titanium oxide, tin oxide, zinc oxide, dibismuth trioxide, tungsten trioxide, oxide trioxide. Diiron, strontium titanate and the like can be preferably used. Here, as the light source used for photoexcitation of the photocatalyst, sunlight, indoor lighting, dedicated lighting can be used, and types thereof include fluorescent lamps, incandescent lamps, indoor lighting, metal halide lamps, mercury lamps, xenon lamps, germicidal lamps, etc. It can be used suitably. In order to make the surface of the base material highly hydrophilic by photoexcitation of the photocatalyst, the illuminance of the excitation light is 0.001 mW / cm.
The number is preferably 2 or more, but is preferably 0.01 mW / cm 2 or more, and more preferably 0.1 mW / cm 2 or more.

【0013】光触媒を含有する表面層の膜厚は、0.4
μm以下にするのが好ましい。そうすれば、光の乱反射
による白濁を防止することができ、表面層は実質的に透
明となる。さらに、光触媒を含有する表面層の膜厚を
0.2μm以下にすると一層好ましい。そうすれば、光
の干渉による表面層の発色を防止することができる。ま
た表面層が薄ければ薄いほどその透明度は向上する。更
に、膜厚を薄くすれば、表面層の耐摩耗性が向上する。
上記表面層の表面に、更に、親水化可能な耐摩耗性又は
耐食性の保護層や他の機能膜を設けても良い。
The thickness of the surface layer containing the photocatalyst is 0.4
It is preferable that the thickness is less than or equal to μm. Then, white turbidity due to irregular reflection of light can be prevented, and the surface layer becomes substantially transparent. More preferably, the thickness of the surface layer containing the photocatalyst is 0.2 μm or less. Then, it is possible to prevent the surface layer from being colored by light interference. Also, the thinner the surface layer, the better its transparency. Further, when the film thickness is reduced, the wear resistance of the surface layer is improved.
The surface of the surface layer may be further provided with a wear-resistant or corrosion-resistant protective layer capable of being made hydrophilic and other functional films.

【0014】上記表面層は、基材と比較して屈折率があ
まり高くないのが好ましい。好ましくは表面層の屈折率
は2以下であるのがよい。そうすれば、基材と表面層と
の界面、及び表面層と空気との界面における光の反射を
抑制できる。表面層の屈折率を2以下にするには、光触
媒に2以下の屈折率を有する物質を用いるか、或いは光
触媒が屈折率2以上の場合には、屈折率2以下の他の物
質を表面層に添加する。2以下の屈折率を有する光触媒
としては、酸化錫(屈折率1.9)等が利用できる。2
以上の屈折率を有する光触媒には、アナターゼ型酸化チ
タン(屈折率2.5やルチル型酸化チタン(屈折率2.
7)があるが、この場合には屈折率2以下の他の物質、
例えば、炭酸カルシウム(屈折率1.6)、水酸化カル
シウム(屈折率1.6)、炭酸マグネシウム(屈折率
1.5)、炭酸ストロンチウム(屈折率1.5)、ドロ
マイト(屈折率1.7)、フッ化カルシウム(屈折率
1.4)、フッ化マグネシウム(屈折率1.4)、シリ
カ(屈折率1.5)、アルミナ(屈折率1.6)、ケイ
砂(屈折率1.6)、モンモリロナイト(屈折率1.
5)、カオリン(屈折率1.6)、セリサイト(屈折率
1.6)、ゼオライト(屈折率1.5)、酸化錫(屈折
率1.9)等を表面層に添加すればよい。
The surface layer preferably has a refractive index that is not so high as that of the substrate. Preferably, the refractive index of the surface layer is 2 or less. Then, light reflection at the interface between the substrate and the surface layer and the interface between the surface layer and air can be suppressed. In order to reduce the refractive index of the surface layer to 2 or less, a substance having a refractive index of 2 or less is used for the photocatalyst, or if the photocatalyst has a refractive index of 2 or more, another substance having a refractive index of 2 or less is used for the surface layer. To be added. As a photocatalyst having a refractive index of 2 or less, tin oxide (refractive index: 1.9) or the like can be used. 2
The photocatalyst having the above refractive index includes anatase type titanium oxide (refractive index 2.5 and rutile type titanium oxide (refractive index 2.
7), but in this case, another substance with a refractive index of 2 or less,
For example, calcium carbonate (refractive index 1.6), calcium hydroxide (refractive index 1.6), magnesium carbonate (refractive index 1.5), strontium carbonate (refractive index 1.5), dolomite (refractive index 1.7). ), Calcium fluoride (refractive index 1.4), magnesium fluoride (refractive index 1.4), silica (refractive index 1.5), alumina (refractive index 1.6), silica sand (refractive index 1.6). ), Montmorillonite (refractive index 1.
5), kaolin (refractive index 1.6), sericite (refractive index 1.6), zeolite (refractive index 1.5), tin oxide (refractive index 1.9) and the like may be added to the surface layer.

【0015】上記表面層には、Ag、Cu、Znのよう
な金属を添加することができる。前記金属を添加した表
面層は、表面に付着した細菌や黴を暗所でも死滅させる
ことができる。
A metal such as Ag, Cu and Zn can be added to the surface layer. The surface layer to which the metal is added can kill bacteria and fungi attached to the surface even in a dark place.

【0016】上記表面層には、Pt、Pd、Ru、R
h、Ir、Osのような白金族金属を添加することがで
きる。前記金属を添加した表面層は、光触媒の酸化還元
活性を増強でき、脱臭浄化作用等が向上する。また、光
触媒以外に固体酸を添加した場合には、白金族金属の添
加により固体酸の酸度が向上するので、親水維持性も向
上し、付着水の水膜化がより促進されると共に、ある程
度長期間光触媒に励起光が照射されない場合の親水維持
性も向上する。上記表面層には、Moを添加することが
できる。光触媒以外に固体酸を添加した場合に、Moを
添加すると固体酸の酸度が向上するので、親水維持性も
向上し、付着水の水膜化がより促進されると共に、ある
程度長期間光触媒に励起光が照射されない場合の親水維
持性も向上する。
The surface layer includes Pt, Pd, Ru, R
A platinum group metal such as h, Ir, Os can be added. The surface layer to which the metal is added can enhance the oxidation-reduction activity of the photocatalyst and improve the deodorizing and purifying action and the like. In addition, when a solid acid is added in addition to the photocatalyst, the acidity of the solid acid is improved by the addition of a platinum group metal, so that the hydrophilicity is also improved, and the formation of a water film on the attached water is further promoted. The hydrophilicity when the excitation light is not irradiated to the photocatalyst for a long period of time is also improved. Mo can be added to the surface layer. When a solid acid is added in addition to the photocatalyst, the addition of Mo increases the acidity of the solid acid, so that the hydrophilicity is also improved, and the formation of a water film on the attached water is further promoted. The hydrophilicity when light is not irradiated is also improved.

【0017】基材がナトリウムのようなアルカリ網目修
飾イオンを含むガラス(ソーダライムガラス、並板ガラ
ス等)の場合には、基材と表面層との間にシリカ等の中
間層を形成してもよい。そうすれば、焼成中にアルカリ
網目修飾イオンが基材から表面層へ拡散するのが防止さ
れ、光触媒機能がよりよく発揮される。
When the substrate is a glass containing alkali network modifying ions such as sodium (soda lime glass, parallel plate glass, etc.), an intermediate layer such as silica may be formed between the substrate and the surface layer. Good. Then, the diffusion of the alkali network modifying ions from the base material to the surface layer during the firing is prevented, and the photocatalytic function is more effectively exhibited.

【0018】親水性とは、表面に水を滴下したときにな
じみやすい性質をいい、一般に水濡れ角が90゜未満の
状態をいう。本発明における高度の親水性とは、表面に
水を滴下したときに非常になじみやすい性質をいい、よ
り具体的には水濡れ角が10゜以下程度になる状態をい
う。特に、防曇性にはPCT/JP96/00734に
開示したように、水濡れ角が10゜以下であると好まし
く、5゜以下ではより好ましい。尚、ここで用いる“防
曇”の用語は、曇りだけでなく、凝縮水滴の成長や水滴
の付着による光学的障害を防止する技術を広く意味す
る。
The term "hydrophilic" refers to the property of being easily conformed when water is dropped on the surface, and generally refers to a state where the water wetting angle is less than 90 °. The term “high hydrophilicity” in the present invention refers to a property that is highly compatible when water is dropped on the surface, and more specifically, a state where the water wetting angle is about 10 ° or less. In particular, as disclosed in PCT / JP96 / 00734, the water wetting angle is preferably 10 ° or less, more preferably 5 ° or less, as disclosed in PCT / JP96 / 00734. The term “anti-fog” used herein broadly means not only the haze but also a technique for preventing optical obstacles due to the growth of condensed water droplets and the adhesion of water droplets.

【0019】本発明における固体酸には、硫酸担持Al
23、硫酸担持TiO2、硫酸担持ZrO2、硫酸担持S
nO2、硫酸担持Fe23、硫酸担持SiO2、硫酸担持
HfO2、TiO2/WO3、WO3/SnO2、WO3/Z
rO2、WO3/Fe23、SiO2・Al2O3、TiO
2/SiO2、TiO2/Al23、TiO2/ZrO2
が好適に利用できる。
The solid acid used in the present invention includes sulfuric acid-supported Al.
2 O 3 , sulfuric acid supported TiO 2 , sulfuric acid supported ZrO 2 , sulfuric acid supported S
nO 2 , sulfuric acid supported Fe 2 O 3 , sulfuric acid supported SiO 2 , sulfuric acid supported HfO 2 , TiO 2 / WO 3 , WO 3 / SnO 2 , WO 3 / Z
rO 2 , WO 3 / Fe 2 O 3 , SiO 2 · Al 2 O 3 , TiO
2 / SiO 2 , TiO 2 / Al 2 O 3 , TiO 2 / ZrO 2 and the like can be preferably used.

【0020】次に、表面層の形成方法について説明す
る。まず表面層が光触媒のみからなる場合の製法につい
て、光触媒がアナターゼ型酸化チタンの場合を例にとり
説明する。この場合の方法は、大別して3つの方法があ
る。1つの方法はゾル塗布焼成法であり、他の方法は有
機チタネート法であり、他の方法は電子ビーム蒸着法で
ある。 (1)ゾル塗布焼成法 アナターゼ型酸化チタンゾルを、基材表面に、スプレー
コーティング法、ディップコーティング法、フローコー
ティング法、スピンコーティング法、ロールコーティン
グ法等の方法で塗布し、焼成する。 (2)有機チタネート法 チタンアルコキシド(テトラエトキシチタン、テトラメ
トキシチタン、テトラプロポキシチタン、テトラブトキ
シチタン等)、チタンアセテート、チタンキレート等の
有機チタネートに加水分解抑制剤(塩酸、エチルアミン
等)を添加し、アルコール(エタノール、プロパノー
ル、ブタノール等)などの非水溶媒で希釈した後、部分
的に加水分解を進行させながら又は完全に加水分解を進
行させた後、混合物をスプレーコーティング法、ディッ
プコーティング法、フローコーティング法、スピンコー
ティング法、ロールコーティング法等の方法で塗布し、
乾燥させる。乾燥により、有機チタネートの加水分解が
完遂して水酸化チタンが生成し、水酸化チタンの脱水縮
重合により無定型酸化チタンの層が基材表面に形成され
る。その後、アナターゼの結晶化温度以上の温度で焼成
して、無定型酸化チタンをアナターゼ型酸化チタンに相
転移させる。 (3)電子ビーム蒸着法 酸化チタンのターゲットに電子ビームを照射することに
より、基材表面に無定型酸化チタンの層を形成する。そ
の後、アナターゼの結晶化温度以上の温度で焼成して、
無定型酸化チタンをアナターゼ型酸化チタンに相転移さ
せる。
Next, a method for forming the surface layer will be described. First, the production method in the case where the surface layer is composed only of the photocatalyst will be described by taking the case where the photocatalyst is anatase type titanium oxide as an example. In this case, there are roughly three methods. One method is a sol coating and firing method, the other method is an organic titanate method, and the other method is an electron beam evaporation method. (1) Sol-coating and firing method Anatase-type titanium oxide sol is applied to the surface of a substrate by a method such as spray coating, dip coating, flow coating, spin coating, or roll coating, and then fired. (2) Organic titanate method Titanium alkoxide (tetraethoxy titanium, tetramethoxy titanium, tetrapropoxy titanium, tetrabutoxy titanium, etc.), titanium acetate, titanium chelate, etc. are added with a hydrolysis inhibitor (hydrochloric acid, ethylamine, etc.). , After diluting with a non-aqueous solvent such as alcohol (ethanol, propanol, butanol, etc.), while partially or completely proceeding the hydrolysis, the mixture is spray-coated, dip-coated, Apply by methods such as flow coating method, spin coating method, roll coating method,
dry. By drying, the hydrolysis of the organic titanate is completed to produce titanium hydroxide, and a layer of amorphous titanium oxide is formed on the surface of the base material by dehydration-condensation polymerization of the titanium hydroxide. Thereafter, the amorphous titanium oxide is calcined at a temperature equal to or higher than the crystallization temperature of anatase to cause a phase transition from the amorphous titanium oxide to the anatase titanium oxide. (3) Electron beam evaporation method An amorphous titanium oxide layer is formed on the surface of a substrate by irradiating a titanium oxide target with an electron beam. After that, firing at a temperature higher than the crystallization temperature of anatase,
Phase transition of amorphous titanium oxide to anatase titanium oxide.

【0021】次に、表面層が光触媒とシリカからなる場
合について、光触媒がアナターゼ型酸化チタンの場合を
例にとり説明する。この場合の方法は、例えば、以下の
3つの方法がある。1つの方法はゾル塗布焼成法であ
り、他の方法は有機チタネート法であり、他の方法は4
官能性シラン法である。 (1)ゾル塗布焼成法 アナターゼ型酸化チタンゾルとシリカゾルとの混合液
を、基材表面にスプレーコーティング法、ディップコー
ティング法、フローコーティング法、スピンコーティン
グ法、ロールコーティング法等の方法で塗布し、焼成す
る。 (2)有機チタネート法 チタンアルコキシド(テトラエトキシチタン、テトラメ
トキシチタン、テトラプロポキシチタン、テトラブトキ
シチタン等)、チタンアセテート、チタンキレート等の
有機チタネートに加水分解抑制剤(塩酸、エチルアミン
等)とシリカゾルを添加し、アルコール(エタノール、
プロパノール、ブタノール等)などの非水溶媒で希釈し
た後、部分的に加水分解を進行させながら又は完全に加
水分解を進行させた後、混合物をスプレーコーティング
法、ディップコーティング法、フローコーティング法、
スピンコーティング法、ロールコーティング法等の方法
で塗布し、乾燥させる。乾燥により、有機チタネートの
加水分解が完遂して水酸化チタンが生成し、水酸化チタ
ンの脱水縮重合により無定型酸化チタンの層が基材表面
に形成される。その後、アナターゼの結晶化温度以上の
温度で焼成して、無定型酸化チタンをアナターゼ型酸化
チタンに相転移させる。 (3)4官能性シラン法 テトラアルコキシシラン(テトラエトキシシラン、テト
ラプロポキシシラン、テトラブトキシシラン、テトラメ
トキシシラン等)とアナターゼ型酸化チタンゾルとの混
合物を基材の表面にスプレーコーティング法、ディップ
コーティング法、フローコーティング法、スピンコーテ
ィング法、ロールコーティング法等の方法で塗布し、必
要に応じて加水分解させてシラノールを形成した後、加
熱等の方法でシラノールを脱水縮重合に付す。
Next, the case where the surface layer is composed of a photocatalyst and silica will be described by taking the case where the photocatalyst is anatase type titanium oxide as an example. In this case, for example, there are the following three methods. One method is the sol coating firing method, the other is the organic titanate method, the other is 4
This is a functional silane method. (1) Sol coating and baking method A mixture of anatase-type titanium oxide sol and silica sol is applied to the substrate surface by a method such as a spray coating method, a dip coating method, a flow coating method, a spin coating method, and a roll coating method, and then fired. I do. (2) Organic titanate method Titanium alkoxides (tetraethoxytitanium, tetramethoxytitanium, tetrapropoxytitanium, tetrabutoxytitanium, etc.), titanium acetate, titanium chelate, and other organic titanates are added with a hydrolysis inhibitor (hydrochloric acid, ethylamine, etc.) and silica sol. Add alcohol (ethanol,
After diluting with a non-aqueous solvent such as propanol, butanol, etc., and then allowing the hydrolysis to proceed partially or completely, the mixture is spray-coated, dip-coated, flow-coated,
It is applied by a method such as spin coating or roll coating and dried. By drying, the hydrolysis of the organic titanate is completed to produce titanium hydroxide, and a layer of amorphous titanium oxide is formed on the surface of the base material by dehydration-condensation polymerization of the titanium hydroxide. Thereafter, the amorphous titanium oxide is calcined at a temperature equal to or higher than the crystallization temperature of anatase to cause a phase transition from the amorphous titanium oxide to the anatase titanium oxide. (3) Tetrafunctional silane method A mixture of tetraalkoxysilane (tetraethoxysilane, tetrapropoxysilane, tetrabutoxysilane, tetramethoxysilane, etc.) and anatase type titanium oxide sol is spray-coated or dip-coated on the surface of a substrate. , A flow coating method, a spin coating method, a roll coating method, or the like, and if necessary, hydrolyzing to form silanol, and then silanol is subjected to dehydration condensation polymerization by a method such as heating.

【0022】次に、表面層が光触媒と固体酸からなる場
合について、光触媒がアナターゼ型酸化チタン、固体酸
がTiO2/WO3の場合を例にとり説明する。この場合
の1つの方法は、タングステン酸のアンモニア溶解液と
アナターゼ型酸化チタンゾルとを混合し、必要に応じて
希釈液(水、エタノール等)で希釈した混合物を基材の
表面にスプレーコーティング法、ディップコーティング
法、フローコーティング法、スピンコーティング法、ロ
ールコーティング法等の方法で塗布し、焼成する。他の
方法は、電子ビーム蒸着や、チタンアルコキシド、チタ
ンアセテート、チタンキレート等の有機チタネートの加
水分解及び脱水縮重合により、無定型酸化チタン被膜を
形成後、タングステン酸を塗布し、無定型酸化チタンが
結晶化し、かつTiO2/WO3複合酸化物が生成する温
度で熱処理する。
Next, the case where the surface layer is composed of a photocatalyst and a solid acid will be described by taking as an example the case where the photocatalyst is anatase type titanium oxide and the solid acid is TiO 2 / WO 3 . One method in this case is a method in which an ammonia solution of tungstic acid and an anatase type titanium oxide sol are mixed, and if necessary, a mixture diluted with a diluent (water, ethanol, etc.) is spray-coated on the surface of the base material, It is applied by a method such as a dip coating method, a flow coating method, a spin coating method or a roll coating method, and baked. Other methods include electron beam evaporation and hydrolysis and dehydration polycondensation of organic titanates such as titanium alkoxide, titanium acetate, and titanium chelate to form an amorphous titanium oxide film, and then tungstic acid is applied to the amorphous titanium oxide. Is crystallized and a heat treatment is performed at a temperature at which a TiO 2 / WO 3 composite oxide is formed.

【0023】次に、表面層が光触媒とシリコーンからな
る場合について、光触媒がアナターゼ型酸化チタンの場
合を例にとり説明する。この場合の方法は、未硬化の若
しくは部分的に硬化したシリコーン又はシリコーンの前
駆体からなる塗料とアナターゼ型酸化チタンゾルとを混
合し、シリコーンの前駆体を必要に応じて加水分解させ
た後、混合物を基材の表面にスプレーコーティング法、
ディップコーティング法、フローコーティング法、スピ
ンコーティング法、ロールコーティング法等の方法で塗
布し、加熱等の方法でシリコーンの前駆体の加水分解物
を脱水縮重合に付して、アナターゼ型酸化チタン粒子と
シリコーンからなる表面層を形成する。形成された表面
層は、紫外線を含む光の照射によりアナターゼ型酸化チ
タンが光励起されることにより、シリコーン分子中のケ
イ素原子に結合した有機基の少なくとも一部を水酸基に
置換され、さらに、その上に物理吸着水層が形成され
て、高度の親水性を呈する。ここでシリコーンの前駆体
には、メチルトリメトキシシラン、メチルトリエトキシ
シラン、メチルトリブトキシシラン、メチルトリプロポ
キシシラン、エチルトリメトキシシラン、エチルトリエ
トキシシラン、エチルトリブトキシシラン、エチルトリ
プロポキシシラン、フェニルトリメトキシシラン、フェ
ニルトリエトキシシラン、フェニルトリブトキシシラ
ン、フェニルトリプロポキシシラン、ジメチルジメトキ
シシラン、ジメチルジエトキシシラン、ジメチルジブト
キシシラン、ジメチルジプロポキシシラン、ジエチルジ
メトキシシラン、ジエチルジエトキシシラン、ジエチル
ジブトキシシラン、ジエチルジプロポキシシラン、フェ
ニルメチルジメトキシシラン、フェニルメチルジエトキ
シシラン、フェニルメチルジブトキシシラン、フェニル
メチルジプロポキシシラン、γ−グリシドキシプロピル
トリメトキシシラン、及びそれらの加水分解物、それら
の混合物が好適に利用できる。
Next, the case where the surface layer is composed of a photocatalyst and silicone will be described by taking the case where the photocatalyst is anatase type titanium oxide as an example. The method in this case is to mix a coating composed of uncured or partially cured silicone or a precursor of silicone and anatase type titanium oxide sol, and hydrolyze the precursor of silicone as needed, and then mix the mixture. Spray coating method on the surface of the substrate,
It is applied by a method such as a dip coating method, a flow coating method, a spin coating method, a roll coating method, etc., and a hydrolyzate of a silicone precursor is subjected to dehydration polycondensation by a method such as heating to obtain anatase type titanium oxide particles. A surface layer made of silicone is formed. The formed surface layer, by photoexcitation of anatase type titanium oxide by irradiation with light including ultraviolet rays, at least a part of the organic groups bonded to the silicon atom in the silicone molecule is substituted with a hydroxyl group, and further A physically adsorbed water layer is formed on the surface and exhibits a high degree of hydrophilicity. Here, the silicone precursor includes methyltrimethoxysilane, methyltriethoxysilane, methyltributoxysilane, methyltripropoxysilane, ethyltrimethoxysilane, ethyltriethoxysilane, ethyltributoxysilane, ethyltripropoxysilane, and phenyl. Trimethoxysilane, phenyltriethoxysilane, phenyltributoxysilane, phenyltripropoxysilane, dimethyldimethoxysilane, dimethyldiethoxysilane, dimethyldibutoxysilane, dimethyldipropoxysilane, diethyldimethoxysilane, diethyldiethoxysilane, diethyldibutoxy Silane, diethyldipropoxysilane, phenylmethyldimethoxysilane, phenylmethyldiethoxysilane, phenylmethyldibutoxysilane, phenol Methylpropenylmethyl dipropoxy silane, .gamma.-glycidoxypropyltrimethoxysilane, and hydrolysates thereof, mixtures thereof can be suitably used.

【0024】その他、上記コーティングを塗布したフィ
ルムを基材表面にセッケン水等の透明接着剤で貼着して
もよい。ここでフィルム基材には、ポリエチレンテレフ
タレート、ポリエステル、ポリエチレン等のプラスチッ
ク製フィルムが好適に利用できる。
In addition, the film coated with the above coating may be attached to the surface of the substrate with a transparent adhesive such as soapy water. Here, a plastic film such as polyethylene terephthalate, polyester, or polyethylene can be preferably used as the film substrate.

【0025】[0025]

【実施例】【Example】

実施例1.10cm角のポリカーボネート板上にプライ
マー塗料(信越シリコーン、PC−7A)をフローコー
ティング法にて塗布後、120℃で20分乾燥させて、
基板をプライマー樹脂層で被覆した。次に、シリコーン
系ハードコーティング剤(信越シリコーン、KP−8
5)をフローコーティング法にて塗布後、120℃で6
0分乾燥させて、ハードコート層を形成した。次に、ハ
ードコート層をコロナ放電処理した後、酸化チタン含有
塗料組成物(アナターゼ型酸化チタンゾル(日産化学、
TA−15)56重量部とシリカゾル(日本合成ゴム、
グラスカA液)33重量部を混合し、エタノール希釈
後、更にトリメトキシシラン11重量部(日本合成ゴ
ム、グラスカB液)を添加したもの)をフローコーティ
ング法にて塗布後、120℃で30分熱処理して硬化さ
せ、試料を得た。この試料を数日間暗所に放置した後、
紫外線光源(三共電気、ブラックライトブルー(BL
B)蛍光灯)を用いて試料の表面に0.5mW/cm2
の紫外線照度で約1時間紫外線を照射し、#1試料を得
た。比較のため、10cm角のポリカーボネート板を数
日間暗所に放置した#2試料も準備した。まず、#1試
料と#2試料に水滴を滴下し、滴下後の様子の観察及び
水との接触角の測定を行った。ここで水との接触角は接
触角測定器(協和界面科学、CA−X150)を用い、
滴下後30秒後の水との接触角で評価した。その結果#
1試料はマイクロシリンジから試料表面に水滴を滴下さ
れると、水滴が一様に水膜状に試料表面を拡がる様子が
観察された。また30秒後の水との接触角は約0゜まで
高度に親水化されていた。それに対し、#2試料ではマ
イクロシリンジから試料表面に水滴を滴下されると、水
滴は表面になじんでいくものの、一様に水膜状になるま
でには至らなかった。また30秒後の水との接触角は6
0゜であった。次に、#1試料と#2試料に息を吹きか
け曇り発生の有無を調べた。その結果#2試料では曇り
が生じたのに対し、#1試料では曇りは生じなかった。
さらに、#1試料を、その後2日間暗所に放置し、#3
試料を得た。そして#3試料について、同様に水との接
触角を接触角測定器により測定した。その結果、#3試
料にマイクロシリンジから試料表面に水滴を滴下される
と、#1試料と同様に、水滴が一様に水膜状に試料表面
を拡がる様子が観察された。また水との接触角は約3゜
に維持された。次に#3試料について息を吹きかけた後
の曇り発生の有無を観察した。その結果、曇りは観察さ
れなかった。
Example 1. A 10 cm square polycarbonate plate was coated with a primer coating (Shin-Etsu Silicone, PC-7A) by a flow coating method and then dried at 120 ° C. for 20 minutes,
The substrate was coated with a primer resin layer. Next, a silicone-based hard coating agent (Shin-Etsu Silicone, KP-8
After applying 5) by flow coating,
It was dried for 0 minutes to form a hard coat layer. Next, after the hard coat layer is subjected to corona discharge treatment, a titanium oxide-containing coating composition (anatase type titanium oxide sol (Nissan Chemical,
TA-15) 56 parts by weight and silica sol (Japan Synthetic Rubber,
(Grasca solution A) (33 parts by weight), diluted with ethanol, and further added with 11 parts by weight of trimethoxysilane (Nippon Synthetic Rubber, solution of Glasca solution B)) by a flow coating method, and then at 120 ° C. for 30 minutes. A sample was obtained by heat treatment and curing. After leaving this sample in the dark for several days,
UV light source (Sankyo Electric, Black Light Blue (BL
B) Using a fluorescent lamp), apply 0.5 mW / cm 2 to the surface of the sample.
The sample was irradiated with ultraviolet rays at an ultraviolet illuminance of about 1 hour to obtain a # 1 sample. For comparison, a # 2 sample in which a 10 cm square polycarbonate plate was left in the dark for several days was also prepared. First, a water drop was dropped on the # 1 sample and the # 2 sample, and the state after the drop was observed and the contact angle with water was measured. Here, the contact angle with water is measured using a contact angle measuring device (Kyowa Interface Science, CA-X150).
Evaluation was made based on the contact angle with water 30 seconds after dropping. as a result#
When a water droplet was dropped from the microsyringe on one surface of one sample, it was observed that the water droplet spreads uniformly on the surface of the sample in the form of a water film. Further, the contact angle with water after 30 seconds was highly hydrophilized to about 0 °. On the other hand, in the case of the # 2 sample, when a water drop was dropped on the sample surface from the microsyringe, the water droplet adapted to the surface but did not reach a uniform water film state. The contact angle with water after 30 seconds is 6
It was 0 °. Next, the # 1 sample and the # 2 sample were blown to examine whether or not clouding occurred. As a result, fogging occurred in the # 2 sample, but no fogging occurred in the # 1 sample.
Further, the # 1 sample was left in the dark for 2 days thereafter,
A sample was obtained. Then, for the # 3 sample, the contact angle with water was similarly measured by a contact angle measuring device. As a result, when a water drop was dropped on the sample surface from the microsyringe on the # 3 sample, it was observed that the water droplet spread uniformly on the sample surface like a # 1 sample. The contact angle with water was maintained at about 3 °. Next, the presence or absence of fogging after spraying was observed for the # 3 sample. As a result, no fogging was observed.

【0026】実施例2.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10nm)1.07gとエタ
ノール29.88gと、純水0.36gを混合し、コー
ティング液を調製した。このコーティング液をフローコ
ーティング法により、10cm角のガラス基材上に塗布
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
型シリカで結着されたコーティングをガラス板表面に形
成した。このコーティング中の、酸化チタンとシリカと
の重量比は1であった。このガラス板を数日間暗所に放
置した後、紫外線光源(三共電気、ブラックライトブル
ー(BLB)蛍光灯)を用いて試料の表面に0.5mW
/cm2の紫外線照度で約1時間紫外線を照射し、#4
試料を得た。比較のため、10cm角のガラス板を数日
間暗所に放置した#5試料も準備した。まず、#4試料
と#5試料に水滴を滴下し、滴下後の様子の観察及び水
との接触角の測定を行った。ここで水との接触角は接触
角測定器(協和界面科学、CA−X150)を用い、滴
下後30秒後の水との接触角で評価した。その結果#4
試料はマイクロシリンジから試料表面に水滴を滴下され
ると、水滴が一様に水膜状に試料表面を拡がる様子が観
察された。また30秒後の水との接触角は約0゜まで高
度に親水化されていた。それに対し、#5試料ではマイ
クロシリンジから試料表面に水滴を滴下されると、水滴
は表面になじんでいくものの、一様に水膜状になるまで
には至らなかった。また30秒後の水との接触角は30
゜であった。次に、#4試料と#5試料に息を吹きかけ
曇り発生の有無を調べた。その結果#5試料では曇りが
生じたのに対し、#1試料では曇りは生じなかった。さ
らに、#4試料を、その後2日間暗所に放置し、#6試
料を得た。そして#6試料について、同様に水との接触
角を接触角測定器により測定した。その結果、#6試料
にマイクロシリンジから試料表面に水滴を滴下される
と、#4試料と同様に、水滴が一様に水膜状に試料表面
を拡がる様子が観察された。また水との接触角は約3゜
に維持された。次に#6試料について息を吹きかけた後
の曇り発生の有無を観察した。その結果、曇りは観察さ
れなかった。
Embodiment 2 FIG. 0.69 g of tetraethoxysilane (Wako Pure Chemical Industries), 1.07 g of anatase type titanium oxide sol (TA-15, average particle size 10 nm), 29.88 g of ethanol, and 0.36 g of pure water are mixed to form a coating liquid. Was prepared. This coating liquid was applied on a 10 cm square glass substrate by a flow coating method. By holding this glass plate at a temperature of about 150 ° C. for about 20 minutes, tetraethoxysilane is subjected to hydrolysis and dehydration polycondensation, and a coating in which anatase-type titanium oxide particles are bound with amorphous silica is applied to the glass plate. Formed on the surface. The weight ratio of titanium oxide and silica in this coating was 1. After leaving this glass plate in the dark for several days, 0.5 mW was applied to the surface of the sample by using an ultraviolet light source (Sankyo Denki, black light blue (BLB) fluorescent lamp).
Irradiate with UV light for about 1 hour at UV illuminance of / cm 2 , and then # 4
A sample was obtained. For comparison, a # 5 sample in which a 10 cm square glass plate was left in the dark for several days was also prepared. First, a water drop was dropped on the # 4 sample and the # 5 sample, and the state after the drop was observed and the contact angle with water was measured. Here, the contact angle with water was evaluated using a contact angle measuring device (Kyowa Interface Science, CA-X150) based on the contact angle with water 30 seconds after dropping. As a result # 4
When a water droplet was dropped on the sample surface from the microsyringe, it was observed that the water droplet spreads uniformly on the sample surface in the form of a water film. Further, the contact angle with water after 30 seconds was highly hydrophilized to about 0 °. On the other hand, in the # 5 sample, when a water droplet was dropped from the microsyringe on the surface of the sample, the water droplet adapted to the surface, but did not reach a uniform water film shape. The contact angle with water after 30 seconds is 30
Was ゜. Next, the # 4 sample and the # 5 sample were blown to examine whether or not clouding occurred. As a result, the # 5 sample showed haze, whereas the # 1 sample did not show haze. Further, the # 4 sample was left in the dark for 2 days thereafter to obtain a # 6 sample. Then, for the # 6 sample, the contact angle with water was similarly measured with a contact angle measuring device. As a result, when water droplets were dropped on the sample surface from the microsyringe to the # 6 sample, it was observed that the water droplets spread uniformly on the sample surface in the form of a water film, similarly to the # 4 sample. The contact angle with water was maintained at about 3 °. Next, with respect to the # 6 sample, it was observed whether or not clouding had occurred after the breathing. As a result, no fogging was observed.

【0027】実施例3.10cm角のソーダライムガラ
ス板の表面に電子ビーム蒸着法により無定型酸化チタン
膜を被着し、その後500℃の温度で焼成することによ
り、無定型酸化チタンを結晶化させてアナターゼ型酸化
チタンを生成させた。アナターゼ型酸化チタン被膜の膜
厚は100nmであった。さらに、その上に25%アン
モニア水に溶解させたタングステン酸を、タングステン
酸重量に換算して0.6μg/cm2を塗布後、500
℃の温度で焼成した。 次に、このガラス板を数日間暗
所に放置した後、BLB蛍光灯を用いて試料の表面に
0.5mW/cm2の紫外線照度で約1時間紫外線を照
射し、#7試料を得た。比較のため、10cm角のガラ
ス板を数日間暗所に放置した実施例2の#5試料も準備
した。まず、#7試料と#5試料に水滴を滴下し、滴下
後の様子の観察及び水との接触角の測定を行った。ここ
で水との接触角は接触角測定器(協和界面科学、CA−
X150)を用い、滴下後30秒後の水との接触角で評
価した。その結果#7試料はマイクロシリンジから試料
表面に水滴を滴下されると、水滴が一様に水膜状に試料
表面を拡がる様子が観察された。また30秒後の水との
接触角は約0゜まで高度に親水化されていた。それに対
し、#5試料ではマイクロシリンジから試料表面に水滴
を滴下されると、水滴は表面になじんでいくものの、一
様に水膜状になるまでには至らなかった。また30秒後
の水との接触角は30゜であった。次に、#7試料と#
5試料に息を吹きかけ曇り発生の有無を調べた。その結
果#5試料では曇りが生じたのに対し、#7試料では曇
りは生じなかった。さらに、#7試料を、その後2日間
暗所に放置し、#8試料を得た。そして#8試料につい
て、同様に水との接触角を接触角測定器により測定し
た。その結果、#8試料にマイクロシリンジから試料表
面に水滴を滴下されると、#7試料と同様に、水滴が一
様に水膜状に試料表面を拡がる様子が観察された。また
水との接触角は約1゜に維持された。次に#8試料につ
いて息を吹きかけた後の曇り発生の有無を観察した。そ
の結果、曇りは観察されなかった。
Example 3 Amorphous titanium oxide was crystallized by depositing an amorphous titanium oxide film on the surface of a 10 cm square soda lime glass plate by an electron beam vapor deposition method and then firing it at a temperature of 500 ° C. Then, anatase type titanium oxide was produced. The film thickness of the anatase type titanium oxide film was 100 nm. Further, tungstic acid dissolved in 25% ammonia water was applied thereon to convert the weight of tungstic acid to 0.6 μg / cm 2, and then 500
Firing at a temperature of ° C. Next, after leaving this glass plate in the dark for several days, the surface of the sample was irradiated with ultraviolet rays at an ultraviolet illuminance of 0.5 mW / cm 2 for about 1 hour using a BLB fluorescent lamp to obtain a # 7 sample. . For comparison, a # 5 sample of Example 2 in which a 10 cm square glass plate was left in the dark for several days was also prepared. First, water drops were dropped on the # 7 sample and the # 5 sample, and the state after the drop was observed and the contact angle with water was measured. Here, the contact angle with water is measured using a contact angle measuring instrument (Kyowa Interface Science, CA-
X150) was used and the contact angle with water was evaluated 30 seconds after the dropping. As a result, it was observed that when the # 7 sample was dropped from the microsyringe on the sample surface, the water droplet spreads uniformly on the sample surface in the form of a water film. Further, the contact angle with water after 30 seconds was highly hydrophilized to about 0 °. On the other hand, in the # 5 sample, when a water droplet was dropped from the microsyringe on the surface of the sample, the water droplet adapted to the surface, but did not reach a uniform water film shape. The contact angle with water after 30 seconds was 30 °. Next, # 7 sample and #
Five samples were blown to examine the occurrence of fogging. As a result, the # 5 sample showed haze, whereas the # 7 sample did not show haze. Further, the # 7 sample was left in a dark place for two days thereafter, to obtain a # 8 sample. Then, with respect to the # 8 sample, the contact angle with water was similarly measured with a contact angle measuring device. As a result, when water droplets were dropped on the sample surface from the microsyringe to the # 8 sample, it was observed that the water droplets spread uniformly on the sample surface in the form of a water film, similarly to the # 7 sample. The contact angle with water was maintained at about 1 °. Next, with respect to the # 8 sample, it was observed whether or not clouding occurred after the breathing. As a result, no fogging was observed.

【0028】実施例4.まず、10cm角のポリエチレ
ンテレフタレート(PET)フィルムを、コロナ放電処
理後、プライマー(信越シリコーン、PC−7A)をフ
ローコーティング法で塗布し、120℃で5分熱処理す
ることにより、プライマー層を形成した。 次に、プラ
イマー層をコロナ放電処理後、シリコーン系ハードコー
ティング剤(信越シリコーン、KP−85)をフローコ
ーティング法で塗布し、120℃で5分熱処理すること
により、ハードコート層を形成した。次に、ハードコー
ト層をコロナ放電処理後、光触媒コーティング液(石原
産業のST−K01とST−K03を1:1で混合後、
アルコールで希釈することにより作製した、アナターゼ
型酸化チタンとテトラエトキシシランの部分加水分解物
を重量比13:7で含むコーティング液)をフローコー
ティング法で塗布し、常温で10分乾燥させて光触媒性
フィルムを得た。このフィルムの裏側にセッケン水を塗
布し、10cm角のガラス基材に貼着した。次に、この
ガラス板を数日間暗所に放置した後、BLB蛍光灯を用
いて試料の表面に0.5mW/cm2の紫外線照度で約
1時間紫外線を照射し、#9試料を得た。比較のため、
10cm角のガラス板を数日間暗所に放置した実施例2
の#5試料も準備した。まず、#9試料と#5試料に水
滴を滴下し、滴下後の様子の観察及び水との接触角の測
定を行った。ここで水との接触角は接触角測定器(協和
界面科学、CA−X150)を用い、滴下後30秒後の
水との接触角で評価した。その結果#9試料はマイクロ
シリンジから試料表面に水滴を滴下されると、水滴が一
様に水膜状に試料表面を拡がる様子が観察された。また
30秒後の水との接触角は約0゜まで高度に親水化され
ていた。それに対し、#5試料ではマイクロシリンジか
ら試料表面に水滴を滴下されると、水滴は表面になじん
でいくものの、一様に水膜状になるまでには至らなかっ
た。また30秒後の水との接触角は30゜であった。次
に、#9試料と#5試料に息を吹きかけ曇り発生の有無
を調べた。その結果#5試料では曇りが生じたのに対
し、#7試料では曇りは生じなかった。さらに、#9試
料を、その後2日間暗所に放置し、#10試料を得た。
そして#10試料について、同様に水との接触角を接触
角測定器により測定した。その結果、#10試料にマイ
クロシリンジから試料表面に水滴を滴下されると、#9
試料と同様に、水滴が一様に水膜状に試料表面を拡がる
様子が観察された。また水との接触角は約1゜に維持さ
れた。次に#10試料について息を吹きかけた後の曇り
発生の有無を観察した。その結果、曇りは観察されなか
った。
Embodiment 4 FIG. First, a 10-cm-square polyethylene terephthalate (PET) film was subjected to corona discharge treatment, a primer (Shin-Etsu Silicone, PC-7A) was applied by a flow coating method, and heat-treated at 120 ° C. for 5 minutes to form a primer layer. . Next, after the primer layer was subjected to corona discharge treatment, a silicone-based hard coating agent (Shin-Etsu Silicone, KP-85) was applied by a flow coating method and heat-treated at 120 ° C. for 5 minutes to form a hard coat layer. Next, after the corona discharge treatment of the hard coat layer, a photocatalyst coating liquid (ST-K01 and ST-K03 of Ishihara Sangyo were mixed at 1: 1,
A coating solution containing a partial hydrolyzate of anatase type titanium oxide and tetraethoxysilane in a weight ratio of 13: 7 prepared by diluting with alcohol is applied by a flow coating method and dried at room temperature for 10 minutes to obtain a photocatalytic property. I got a film. Soap water was applied to the back side of this film and attached to a 10 cm square glass substrate. Next, after leaving this glass plate in the dark for several days, the surface of the sample was irradiated with ultraviolet rays for about 1 hour at a UV illuminance of 0.5 mW / cm 2 using a BLB fluorescent lamp to obtain a # 9 sample. . For comparison,
Example 2 in which a 10 cm square glass plate was left in the dark for several days
# 5 sample was also prepared. First, water drops were dropped on the # 9 sample and the # 5 sample, and the state after the drop was observed and the contact angle with water was measured. Here, the contact angle with water was evaluated using a contact angle measuring device (Kyowa Interface Science, CA-X150) based on the contact angle with water 30 seconds after dropping. As a result, it was observed that when water droplets were dropped onto the sample surface of the # 9 sample from the microsyringe, the water droplets spread uniformly on the sample surface in the form of a water film. Further, the contact angle with water after 30 seconds was highly hydrophilized to about 0 °. On the other hand, in the # 5 sample, when a water droplet was dropped from the microsyringe on the surface of the sample, the water droplet adapted to the surface, but did not reach a uniform water film shape. The contact angle with water after 30 seconds was 30 °. Next, the # 9 sample and the # 5 sample were blown to examine whether or not clouding occurred. As a result, the # 5 sample showed haze, whereas the # 7 sample did not show haze. Further, the # 9 sample was left in a dark place for two days thereafter to obtain a # 10 sample.
Then, with respect to the # 10 sample, the contact angle with water was similarly measured by the contact angle measuring device. As a result, when water droplets were dropped onto the surface of the sample # 10 from the microsyringe, # 9
Similar to the sample, it was observed that the water droplets spread uniformly on the sample surface in the form of a water film. The contact angle with water was maintained at about 1 °. Next, with respect to the # 10 sample, it was observed whether or not clouding occurred after the breathing. As a result, no fogging was observed.

【0029】[0029]

【発明の効果】本発明では、透明な加熱容器用の蓋の少
なくとも内側表面に、実質的に透明な光触媒性酸化物粒
子を含有する表面層を備えることにより、光触媒の光励
起に応じて、表面層の表面は親水性を呈する。それによ
り、付着した湿分の凝縮水が前記表面層の表面に一様に
広がり、湿分凝縮水によって曇るのが防止されるように
なる。
According to the present invention, by providing a surface layer containing substantially transparent photocatalytic oxide particles on at least the inner surface of the lid for a transparent heating container, the surface is provided in response to photoexcitation of the photocatalyst. The surface of the layer exhibits hydrophilicity. As a result, the condensed water of the adhered moisture spreads evenly on the surface of the surface layer, so that the condensed water of the moisture can be prevented from becoming clouded.

【図面の簡単な説明】[Brief description of drawings]

【図1】本発明に係る透明な加熱容器用の蓋の内側の表
面構造を示す図。
FIG. 1 is a view showing a surface structure inside a lid for a transparent heating container according to the present invention.

【図2】本発明に係る透明な加熱容器用の蓋の内側の他
の表面構造を示す図。
FIG. 2 is a view showing another surface structure inside the lid for the transparent heating container according to the present invention.

Claims (9)

【特許請求の範囲】[Claims] 【請求項1】 透明な加熱容器用の蓋基材の少なくとも
内側表面に、実質的に透明な光触媒粒子を含有する表面
層を備え、前記光触媒の光励起に応じて前記層の表面が
親水性を呈するようにしたことを特徴とする防曇性を有
する加熱容器用蓋。
1. A transparent base material for a lid for a heating container is provided with a surface layer containing substantially transparent photocatalyst particles on at least an inner surface thereof, and the surface of the layer becomes hydrophilic in response to photoexcitation of the photocatalyst. A lid for a heating container having an anti-fogging property, which is characterized by being presented.
【請求項2】 前記表面層には、さらにシリカが含有さ
れていることを特徴とする請求項1に記載の防曇性を有
する加熱容器用蓋。
2. The lid for a heating container having anti-fogging property according to claim 1, wherein the surface layer further contains silica.
【請求項3】 前記表面層には、さらに固体酸が含有さ
れていることを特徴とする請求項1に記載の防曇性を有
する加熱容器用蓋。
3. The lid for a heating container having an antifogging property according to claim 1, wherein the surface layer further contains a solid acid.
【請求項4】 前記表面層には、さらにシリコーンが含
有されていることを特徴とする請求項1に記載の防曇性
を有する加熱容器用蓋。
4. The lid for a heating container having anti-fog property according to claim 1, wherein the surface layer further contains silicone.
【請求項5】 前記表面層の表面は、前記光触媒の光励
起に応じて、水との接触角に換算して10゜以下の親水
性を呈することを特徴とする請求項1〜4に記載の防曇
性を有する加熱容器用蓋。
5. The surface of the surface layer exhibits hydrophilicity of 10 ° or less in terms of contact angle with water in response to photoexcitation of the photocatalyst. Lid for heating container with anti-fog property.
【請求項6】 前記表面層の膜厚は0.4μm以下であ
ることを特徴とする請求項1〜5に記載の防曇性を有す
る加熱容器用蓋。
6. The lid for a heating container having an antifogging property according to claim 1, wherein the film thickness of the surface layer is 0.4 μm or less.
【請求項7】 前記表面層の膜厚は0.2μm以下であ
ることを特徴とする請求項1〜5に記載の防曇性を有す
る加熱容器用蓋。
7. The lid for a heating container having an antifogging property according to claim 1, wherein the film thickness of the surface layer is 0.2 μm or less.
【請求項8】 前記表面層の表面に、さらに親水化可能
な保護層が設けられていることを特徴とする請求項1〜
7に記載の防曇性を有する加熱容器用蓋。
8. A hydrophilic protective layer is further provided on the surface of the surface layer.
7. A lid for a heating container having the antifogging property according to 7.
【請求項9】 前記表面層の屈折率は2以下であること
を特徴とする請求項1〜8に記載の防曇性を有する加熱
容器用蓋。
9. The lid for a heating container having an antifogging property according to claim 1, wherein the surface layer has a refractive index of 2 or less.
JP8306997A 1995-12-22 1996-11-01 Lid for heating container having fog resistance Pending JPH09226060A (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
JP8306997A JPH09226060A (en) 1995-12-22 1996-11-01 Lid for heating container having fog resistance

Applications Claiming Priority (3)

Application Number Priority Date Filing Date Title
JP7-354649 1995-12-22
JP35464995 1995-12-22
JP8306997A JPH09226060A (en) 1995-12-22 1996-11-01 Lid for heating container having fog resistance

Publications (1)

Publication Number Publication Date
JPH09226060A true JPH09226060A (en) 1997-09-02

Family

ID=18438979

Family Applications (71)

Application Number Title Priority Date Filing Date
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Family Applications Before (51)

Application Number Title Priority Date Filing Date
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JP8281222A Pending JPH09230106A (en) 1995-12-22 1996-09-17 Anti-fogging camera filter and its anti-fogging method
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JP8281220A Expired - Lifetime JP3003593B2 (en) 1995-12-22 1996-09-17 Photocatalytic hydrophilic member
JP8282806A Pending JPH09228057A (en) 1995-12-22 1996-09-18 Wheel and its cleaning method
JP8246180A Pending JPH09230493A (en) 1995-12-22 1996-09-18 Camera
JP8282808A Pending JPH09228765A (en) 1995-12-22 1996-09-18 Blind and manufacture thereof
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Application Number Title Priority Date Filing Date
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
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JP23956899A Expired - Lifetime JP3613085B2 (en) 1995-12-22 1999-08-26 Photocatalytic hydrophilic member
JP23956799A Expired - Lifetime JP3613084B2 (en) 1995-12-22 1999-08-26 A member that exhibits hydrophilicity in response to photoexcitation of an optical semiconductor
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
JP2000181284A Pending JP2001048679A (en) 1995-12-22 2000-06-16 Photocatalytic hydrophilic tile and its production
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JP2000227056A Pending JP2001129916A (en) 1995-12-22 2000-07-27 Photocatalytic hydrophilic member
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
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
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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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* Cited by examiner, † Cited by third party
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JPH09230105A (en) * 1995-12-22 1997-09-05 Toto Ltd Antifogging method and facility applied with the method
JPH10218154A (en) * 1996-09-17 1998-08-18 Takashi Ono Object housing container

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JPH09224874A (en) 1997-09-02
JPH09227162A (en) 1997-09-02
JPH09241038A (en) 1997-09-16
JPH09228022A (en) 1997-09-02
JPH09228326A (en) 1997-09-02
JP3613084B2 (en) 2005-01-26
JP3003593B2 (en) 2000-01-31
JP2001049828A (en) 2001-02-20
JP3844182B2 (en) 2006-11-08
JPH09227160A (en) 1997-09-02
JPH09229546A (en) 1997-09-05
JPH09227178A (en) 1997-09-02
JPH09226040A (en) 1997-09-02
JPH09230118A (en) 1997-09-05
JP3385850B2 (en) 2003-03-10
JP3414365B2 (en) 2003-06-09
JP2001129916A (en) 2001-05-15
JP2001049829A (en) 2001-02-20
JP2000127289A (en) 2000-05-09
JPH09230810A (en) 1997-09-05
JP3414367B2 (en) 2003-06-09
JPH09229585A (en) 1997-09-05
JPH09230031A (en) 1997-09-05
JPH09231821A (en) 1997-09-05
JPH09227156A (en) 1997-09-02
JP2000136370A (en) 2000-05-16
JP3760509B2 (en) 2006-03-29
JP3612896B2 (en) 2005-01-19
JP3882625B2 (en) 2007-02-21
JPH09228320A (en) 1997-09-02
JPH09227169A (en) 1997-09-02
JPH09228765A (en) 1997-09-02
JP3774955B2 (en) 2006-05-17
JPH09225021A (en) 1997-09-02
JPH09231849A (en) 1997-09-05
JPH09227159A (en) 1997-09-02
JP3740736B2 (en) 2006-02-01
JPH09224793A (en) 1997-09-02
JP2001122679A (en) 2001-05-08
JP2001081948A (en) 2001-03-27
JPH09230493A (en) 1997-09-05
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JPH09229767A (en) 1997-09-05
JPH09225388A (en) 1997-09-02
JPH09228332A (en) 1997-09-02
JPH09230796A (en) 1997-09-05
JPH09231807A (en) 1997-09-05
JPH09225389A (en) 1997-09-02
JP2000141537A (en) 2000-05-23
JPH09225054A (en) 1997-09-02
JPH09224960A (en) 1997-09-02
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JPH09224800A (en) 1997-09-02
JPH09226042A (en) 1997-09-02
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JPH09230106A (en) 1997-09-05
JPH09227805A (en) 1997-09-02
JPH09225396A (en) 1997-09-02
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JPH09229724A (en) 1997-09-05
JP2002030258A (en) 2002-01-31
JPH09227832A (en) 1997-09-02
JP3588205B2 (en) 2004-11-10
JPH09228057A (en) 1997-09-02
JP2001048679A (en) 2001-02-20
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JPH09224957A (en) 1997-09-02
JPH09224490A (en) 1997-09-02
JP3003581B2 (en) 2000-01-31
JPH09225387A (en) 1997-09-02
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JP3339304B2 (en) 2002-10-28
JP2003113345A (en) 2003-04-18
JP3588202B2 (en) 2004-11-10
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JPH09230108A (en) 1997-09-05
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JPH09230107A (en) 1997-09-05
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JPH09228602A (en) 1997-09-02
JPH09225263A (en) 1997-09-02
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JP3348613B2 (en) 2002-11-20
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JPH09225276A (en) 1997-09-02
JP3075195B2 (en) 2000-08-07

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