JPH11269432A - Microparticle-dispersed coating fluid - Google Patents
Microparticle-dispersed coating fluidInfo
- Publication number
- JPH11269432A JPH11269432A JP7377498A JP7377498A JPH11269432A JP H11269432 A JPH11269432 A JP H11269432A JP 7377498 A JP7377498 A JP 7377498A JP 7377498 A JP7377498 A JP 7377498A JP H11269432 A JPH11269432 A JP H11269432A
- Authority
- JP
- Japan
- Prior art keywords
- dispersion
- resin
- fine particles
- film
- vehicle
- 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
Abstract
Description
【０００１】[0001]
【発明の属する技術分野】本発明は、ビヒクル中に微粒
子を均一に分散させる、基板表面成膜用の微粒子分散液
に関する。BACKGROUND OF THE INVENTION 1. Field of the Invention The present invention relates to a fine particle dispersion for forming a film on a substrate surface, which uniformly disperses fine particles in a vehicle.
【０００２】[0002]
【従来技術とその解決する課題】従来、塗料、印刷イン
キ、接着剤などの分野では、例えば、樹脂液に顔料を分
散させた液をガラス表面に塗布して種々の色調の着色ガ
ラスを得るもの、或いはガラス粉末と導電性金属粉との
混合体をセラッミック基板表面に塗布して回路素子等を
得るもの等、各種の機能性を付与するために種々の微粒
子、すなわち機能性微粒子をビヒクル中に分散させるこ
とが、盛んに行われている。2. Description of the Related Art Conventionally, in the fields of paints, printing inks, adhesives, etc., for example, a method in which a liquid in which a pigment is dispersed in a resin liquid is applied to a glass surface to obtain colored glass of various colors. Alternatively, various fine particles, such as those obtained by applying a mixture of glass powder and conductive metal powder to the surface of a ceramic substrate to obtain various circuit elements, etc. Dispersing is a popular activity.
【０００３】しかし、ビヒクルと微粒子との比重差等か
ら、微粒子は常に沈降しようとする状態にあり、貯蔵中
に微粒子が凝集して、容器の底部に沈殿を生じて分散液
が不均一となり、安定化せず、塗膜の色ムラ、光沢の差
異、塗膜の強度物性に影響を与え、品質上問題となるこ
とがある。However, due to the difference in specific gravity between the vehicle and the fine particles, the fine particles are always in a state of sedimentation, and the fine particles agglomerate during storage and precipitate at the bottom of the container, resulting in an uneven dispersion. Without stabilization, it may affect the color unevenness of the coating film, the difference in gloss, and the strength physical properties of the coating film, resulting in quality problems.
【０００４】これらの微粒子の沈降を防止するための一
つの方法として、沈降防止剤を分散液中に添加する方法
が広く採用されており、例えば非極性溶媒中に膨潤・微
細に分散させたペースト状で一般に用いられる酸化ポリ
エチレン系、微粒子等とともに緩いフローキュレーショ
ン構造を形成したり、あるいは両性的性質を持ち微粒子
に吸着して吸着層を厚くすることにより分散安定性を向
上する等の界面活性剤系等がある。As one method for preventing the sedimentation of these fine particles, a method of adding an antisettling agent to a dispersion is widely adopted. For example, a paste which is swollen and finely dispersed in a nonpolar solvent is used. Surface activity, such as forming a loose flow curation structure with commonly used polyethylene oxide, fine particles, etc. in the form of particles, or improving the dispersion stability by thickening the adsorption layer by adsorbing on the fine particles with amphoteric properties Agent system.
【０００５】しかしながら、例えばポリシラザン溶液等
のビヒクルにおいては、汎用のアルコール系あるいは水
系が主溶剤である沈降防止剤を用いるとポリシラザンと
沈降防止剤が反応してゲル化し、使用することが出来な
いなどの問題があった。また、機能性微粒子が有機顔料
の場合には、塗布液の非水溶媒中で結晶が成長したり、
粒子が凝集したりして、着色力が低下したりするため、
沈降防止剤を使用したとしても、分散後約１０分程度以
内に塗布しなければ微粒子が凝集をし始め、安定化せ
ず、結果色ムラ、ヘーズ値（曇度値）等が増加し透明性
を失う等の欠点を有していた。However, in a vehicle such as a polysilazane solution, if a general-purpose alcohol-based or water-based anti-settling agent is used, the polysilazane and the anti-settling agent react to form a gel and cannot be used. There was a problem. When the functional fine particles are organic pigments, crystals grow in the non-aqueous solvent of the coating solution,
Because the particles are agglomerated and the coloring power is reduced,
Even if an anti-settling agent is used, if it is not applied within about 10 minutes after dispersion, the fine particles begin to agglomerate and do not stabilize, resulting in increased color unevenness, haze value (cloudiness value), etc., and transparency. Disadvantages such as loss of
【０００６】[0006]
【課題を解決するための手段】本発明は、ビヒクル中に
機能性微粒子を混合分散させた後の分散液に、超音波を
印加することにより、液の安定性が増大し、超音波印加
後、少なくとも１０数時間後にこの分散液を成膜・焼成
しても色ムラのない、ヘーズ値の小さい、均一で高品質
の透光性塗膜を形成することができる基板成膜用の微粒
子分散液を提供するものである。According to the present invention, the stability of a liquid is increased by applying ultrasonic waves to a dispersion liquid obtained by mixing and dispersing functional fine particles in a vehicle. Even when the dispersion is formed and baked after at least ten and several hours, there is no color unevenness, a small haze value, and a uniform fine particle dispersion for film formation on a substrate capable of forming a high-quality translucent coating film. A liquid is provided.
【０００７】すなわち本発明は、ビヒクル中に機能性微
粒子を混合分散させた分散液を透光性基材上に塗布成膜
し、透光性膜付き基材を製造する分散液において、混合
分散後の分散液に超音波を印加した後または印加しなが
ら透光性基材表面に成膜する微粒子分散塗布液に関す
る。That is, according to the present invention, a dispersion in which functional fine particles are mixed and dispersed in a vehicle is coated on a light-transmitting substrate to form a film, and the dispersion is mixed and dispersed. The present invention relates to a fine particle-dispersed coating liquid that forms a film on the surface of a light-transmitting substrate after or while applying ultrasonic waves to the subsequent dispersion liquid.
【０００８】また、ポリシラザン樹脂と有機顔料を溶液
中に分散させた分散液において、該分散液中のポリシラ
ザン樹脂の含有量は固形分で４５〜９９重量％であるこ
とが好ましく、さらに混合分散後の分散液中の微粒子の
粒径は１００ｎｍ以下であることが好ましい。さらに、
分散液は沈降防止剤を含有しないことが適当である。Further, in a dispersion in which a polysilazane resin and an organic pigment are dispersed in a solution, the content of the polysilazane resin in the dispersion is preferably 45 to 99% by weight in terms of solid content. The particle diameter of the fine particles in the dispersion liquid is preferably 100 nm or less. further,
Suitably, the dispersion does not contain an antisettling agent.
【０００９】[0009]
【発明の実施の形態】以下、本発明の詳細を説明する。
分散液は、ビヒクル中に機能性微粒子を分散させたもの
より構成される。ビヒクルとしては、主なものとして有
機系としてポリシラザン樹脂、アクリル樹脂、エポキシ
樹脂、ポロウレタン樹脂、弗素樹脂、フェノール樹脂、
アルキド樹脂、等を用いることが出来る。なお、ポリシ
ラザン樹脂の場合分散液中の固形分としてのポリシラザ
ン樹脂を４５〜９９重量％含有させることができ、４５
重量％以下であると成膜された膜の強度が弱くなり好ま
しくない。DESCRIPTION OF THE PREFERRED EMBODIMENTS The details of the present invention will be described below.
The dispersion is composed of a dispersion of functional fine particles in a vehicle. As the vehicle, polysilazane resin, acrylic resin, epoxy resin, polyurethane resin, fluorine resin, phenol resin, and the like are mainly used as organic materials.
Alkyd resin and the like can be used. In the case of the polysilazane resin, 45 to 99% by weight of the polysilazane resin as a solid content in the dispersion can be contained.
If the content is less than 10% by weight, the strength of the formed film becomes weak, which is not preferable.
【００１０】機能性微粒子としては、顔料としては無機
系顔料として、例えば酸化物系（酸化チタン、酸化鉄、
べんがら）、複合酸化物系等が、また有機系顔料として
はアゾ系、縮合多環系顔料（キナクリドン系、イソイン
ドリノ系、イソインドリン系、スレン系、ペリレン系、
チオインジゴ系、ジオキサジン系、キノフタロン系、ジ
ケトピロロピロール系）、フタロシアニン系等、その他
カーボンブラック等を使用することが出来る。As the functional fine particles, pigments such as inorganic pigments such as oxides (titanium oxide, iron oxide,
Benga), complex oxides, etc., and organic pigments such as azo pigments, condensed polycyclic pigments (quinacridone pigments, isoindolino pigments, isoindoline pigments, sulene pigments, perylene pigments,
Thioindigo, dioxazine, quinophthalone, diketopyrrolopyrrole), phthalocyanine, and other carbon blacks.
【００１１】ビヒクルと微粒子の混合溶液を混合分散す
る方法としては、水平に設置された円筒状の容器とその
中に適量のボールまたはペブル分散媒体とから構成され
たボールミル法或いはペブルミル法、強力な撹拌が生じ
ている砂粒の詰まった円筒容器中にて混合分散させるサ
ンドグラインダー法、ロールとロール間で混合分散させ
るロールミル法、その他高速インペラー法、高速度スト
ーンミル法等を使用することが出来る。なお、そのうち
のボールミル法は、ビヒクルと微粒子と予混合を必要と
せず、蒸発による溶剤の消失・外部からの汚染等がない
ので、特に好ましい方法であり、微粒子が充分に解離す
るまで混合粉砕し、基材がガラスなどの透光性であり且
つ透光性被膜を成膜する場合には、混合分散後の解離下
微粒子の大きさを１００ｎｍ以下にすると、成膜された
膜はヘイズ値（濁度）も２％以下と小さく、透光性が大
きくなり、より好ましい。As a method of mixing and dispersing a mixed solution of a vehicle and fine particles, a ball mill method or a pebble mill method comprising a horizontally disposed cylindrical container and an appropriate amount of a ball or pebble dispersion medium therein, A sand grinder method of mixing and dispersing in a cylindrical container filled with sand particles with stirring, a roll mill method of mixing and dispersing between rolls, a high-speed impeller method, a high-speed stone mill method, and the like can be used. The ball mill method does not require pre-mixing of the vehicle and the fine particles, and it is a particularly preferable method because the solvent does not disappear due to evaporation or contamination from the outside.Therefore, mixing and grinding are performed until the fine particles are sufficiently dissociated. When the base material is a light-transmitting film such as glass and a light-transmitting film is formed, if the size of the fine particles under dissociation after mixing and dispersion is set to 100 nm or less, the formed film has a haze value ( (Turbidity) is as small as 2% or less, and the translucency is increased, which is more preferable.
【００１２】本発明に用いられる基材は、透光性を有す
るガラス、セラミックス、樹脂等に用いることが可能で
あり、その形状は板状が好ましいがこれに限定されるも
のではない。例えば、ガラス基板としては、建築用窓ガ
ラスや自動車用窓ガラス等に通常使用されているフロ−
トガラス（無色または着色）、ならびにその種類あるい
は色調、他の機能性膜との組み合わせ、形状等に特に限
定されるものではなく、さらに曲げ板ガラスとしてはも
ちろん各種強化ガラスや強度アップガラスであり、平板
や単板で使用できるとともに、複層ガラスあるいは合せ
ガラスとしても使用できる。また、樹脂製の基材として
は、アクリル樹脂、塩ビ樹脂、ポリウレタン樹脂、ポリ
カーボネート樹脂、ポリプロピレン樹脂等特に限定され
るものではない。The substrate used in the present invention can be used for a glass, a ceramic, a resin or the like having a light transmitting property, and the shape thereof is preferably a plate shape, but is not limited thereto. For example, as a glass substrate, a flow glass commonly used for architectural window glass, automobile window glass, and the like is used.
Glass (colorless or colored), its type or color tone, combination with other functional films, shape, etc. are not particularly limited. In addition to being able to be used as a single plate or a single plate, it can also be used as a double glazing or a laminated glass. The resin substrate is not particularly limited, such as an acrylic resin, a PVC resin, a polyurethane resin, a polycarbonate resin, and a polypropylene resin.
【００１３】分散液に印加される超音波は、１０〜５０
ＫＨｚの範囲で、通常５時間以内印加することが好まし
く、特に５分間〜６０分間、さらに好ましくは１０分間
〜３０分間印加するのが良い。なお、基板表面に成膜す
る際に超音波を印加していても差し支えない。成膜され
た膜は、通常室温〜４００℃（有機顔料の場合、３００
℃以下）の範囲で焼成し、該膜を硬化させる。The ultrasonic wave applied to the dispersion is 10 to 50.
In the range of KHz, it is usually preferable to apply within 5 hours, especially 5 to 60 minutes, more preferably 10 to 30 minutes. Note that ultrasonic waves may be applied when forming a film on the substrate surface. The formed film is usually at room temperature to 400 ° C. (in the case of an organic pigment, 300 ° C.
(° C. or lower) to cure the film.
【００１４】[0014]
【作用】本発明は、ビヒクルと機能性微粒子をボールミ
ル等で混合分散して微粒子を充分に解離後、超音波を印
加することにより液の安定性を増大させ、超音波印加後
少なくとも１０数時間放置後にこの分散液を塗布しても
得られる透光性塗膜付き基材は、色ムラのない、ヘーズ
値の小さな、微粒子の凝集によるムラの発生がない、均
一且つ高品質の透光性膜付き基材が得られる。超音波を
印加することにより微粒子が凝集しなくなる理由につい
てははっきりしないが、超音波を印加することによりゼ
ータ電位が上昇し、微粒子の凝集を抑制し安定化するも
のと考えられる。According to the present invention, the vehicle and the functional fine particles are mixed and dispersed by a ball mill or the like to sufficiently dissociate the fine particles, and then the ultrasonic wave is applied to increase the stability of the liquid. A substrate with a light-transmitting coating film obtained by applying this dispersion after standing has no color unevenness, a small haze value, no unevenness due to aggregation of fine particles, uniform and high-quality light-transmitting properties. A substrate with a film is obtained. Although the reason why the application of the ultrasonic wave does not cause the aggregation of the fine particles is not clear, it is considered that the application of the ultrasonic wave increases the zeta potential and suppresses and stabilizes the aggregation of the fine particles.
【００１５】実施例１ ビヒクルとしての珪素−窒素結合を有する化合物である
ポリシラザン樹脂の溶液（東燃（株）製、ポリシラザン
樹脂の固形分２０ｗｔ％：キシレン溶媒８０ｗｔ％）１
００ｇと有機顔料であるキナクリドン（大日精化工業
（株）製、c.i.ピグメントレッド１２２）０.２ｇをボ
ールミルに投入し、１２時間混合分散する。次いで該分
散液をディピング槽（サイズ；３００×３００×４０ｍ
ｍ）に移し替えたのち、超音波（神明台工業（株）製、
２６ＫＨｚ−出力６００Ｗ）を３０分間印加させる。分
散液をディピング槽中に２時間放置後、片面にマスキン
グを施したガラス基板（サイズ；２５０×３００×３.
５ｍｍ）をこの槽に浸漬させたのち、５ｍｍ／ｓの引き
上げ速度で該基板を垂直に該槽より引き上げたのち、２
００℃に保持された乾燥炉で３０分間乾燥することによ
り、被膜を硬化させた。Example 1 A solution of a polysilazane resin which is a compound having a silicon-nitrogen bond as a vehicle (manufactured by Tonen Co., Ltd., solid content of polysilazane resin: 20 wt%: xylene solvent: 80 wt%) 1
0.2 g of quinacridone (ci Pigment Red 122, manufactured by Dainichi Seika Kogyo Co., Ltd.) as an organic pigment is put into a ball mill, and mixed and dispersed for 12 hours. Next, the dispersion is placed in a dipping tank (size: 300 × 300 × 40 m).
m) and then transferred to ultrasonic (Shinmeidai Kogyo Co., Ltd.
26 KHz-output 600 W) is applied for 30 minutes. After leaving the dispersion in a dipping tank for 2 hours, a glass substrate (size: 250 × 300 × 3.
5 mm) is immersed in this bath, and the substrate is vertically pulled out of the bath at a pulling speed of 5 mm / s.
The coating was cured by drying in a drying oven maintained at 00 ° C. for 30 minutes.
【００１６】得られた機能性膜は、膜厚１．５μｍの桃
色の着色膜であり、この膜のヘーズ値は０.５％、可視
光線透過率７７％と非常に透明性のよい着色膜付きガラ
スが得られた。このガラスは建築用装飾ガラス或いは車
両用のフロントドアの窓ガラス等として使用可能であ
る。The obtained functional film is a pink colored film having a film thickness of 1.5 μm, and has a haze value of 0.5% and a visible light transmittance of 77%, which is very transparent. A coated glass was obtained. This glass can be used as decorative glass for buildings or window glass of front doors for vehicles.
【００１７】なお、得られた機能性被膜付きガラス基板
の膜厚、ヘーズ値、可視光透過率の測定は、次の装置を
用いて行った。 （膜厚測定） 測定機器；日本真空技術（株）製、型式Ｄｅｋｔａｋ３
０３０ サンプルサイズ；１００×５０×３.５ｍｍ（測定サイ
ズに切断） （ヘーズ値測定） 測定機器；日本電色工業（株）製、型式ＮＤＨ２０Ｄ サンプルサイズ；１００×５０×３.５ｍｍ （可視光透過率） 測定機器；日立（株）製、型式Ｕ−４０００ サンプルサイズ；１００×５０×３.５ｍｍ 実施例２ 実施例１と同様のビヒクル及び顔料を用い、実施例１と
同一の条件で混合分散する。次いで実施例１と同様な方
法で分散液に同じ超音波を１５分間印加させる。分散液
をディピング槽中に１０時間放置後 実施例１と同一の
ガラス基板をこの槽に浸漬させたのち、５ｍｍ／ｓの引
き上げ速度で該基板を垂直に該槽より引き上げたのち、
２００℃に保持された乾燥炉で６０分間乾燥する。The thickness, haze value and visible light transmittance of the obtained glass substrate with a functional film were measured using the following apparatus. (Film thickness measurement) Measuring equipment: Model Dektak3, manufactured by Japan Vacuum Engineering Co., Ltd.
030 Sample size; 100 × 50 × 3.5 mm (cut to measurement size) (Haze value measurement) Measuring equipment: Model NDH20D manufactured by Nippon Denshoku Industries Co., Ltd. Sample size: 100 × 50 × 3.5 mm (Visible light transmission Ratio) Measuring instrument: Model U-4000, manufactured by Hitachi, Ltd. Sample size: 100 × 50 × 3.5 mm Example 2 Using the same vehicle and pigment as in Example 1, mixed and dispersed under the same conditions as in Example 1. I do. Next, the same ultrasonic wave is applied to the dispersion for 15 minutes in the same manner as in Example 1. After leaving the dispersion liquid in the dipping tank for 10 hours, the same glass substrate as in Example 1 was immersed in this tank, and then the substrate was vertically pulled up from the tank at a lifting speed of 5 mm / s.
Dry in a drying oven maintained at 200 ° C. for 60 minutes.
【００１８】得られた機能性膜は、実施例１と同様に、
膜厚１.５μｍの桃色の着色膜であり、この膜のヘーズ
値は０.５％、可視光線透過率７７％と非常に透明性の
よい着色膜付きガラスが得られた。このガラスは建築用
装飾ガラス或いは車両用のフロントドアの窓ガラス等と
して使用可能である。The obtained functional film was prepared in the same manner as in Example 1.
The film was a pink colored film having a thickness of 1.5 μm. The haze value of this film was 0.5%, and the visible light transmittance was 77%. As a result, a glass with a highly transparent colored film was obtained. This glass can be used as decorative glass for buildings or window glass of front doors for vehicles.
【００１９】実施例３ ビヒクルとしてのポリシラザン樹脂の溶液（東燃（株）
製、ポリシラザン樹脂の固形分２０ｗｔ％：キシレン溶
媒８０ｗｔ％）１００ｇと無機顔料である複合酸化物
（大日精化工業製、９５５０（黒色顔料）６.３ｇをボ
ールミルに投入し、１２時間混合分散する。次いで該分
散液をディピング槽（サイズ；３００×３００×４０ｍ
ｍ）に移し替えたのち、超音波（神明台工業（株）製、
２６ＫＨｚ−出力６００Ｗ）を３０分間印加させる。分
散液をディピング槽中に１時間放置後、片面にマスキン
グを施したガラス基板（サイズ；２５０×３００×３.
５ｍｍ）をこの槽に浸漬させたのち、６ｍｍ／ｓの引き
上げ速度で該基板を垂直に該槽より引き上げたのち、２
５０℃に保持された乾燥炉で３０分間乾燥することによ
り、被膜を硬化させた。Example 3 A solution of a polysilazane resin as a vehicle (Tonen Co., Ltd.)
G of polysilazane resin (solid content: 20 wt%: xylene solvent: 80 wt%) and 6.3 g of a composite oxide as inorganic pigment (manufactured by Dainichi Seika Kogyo Co., Ltd., 9550 (black pigment)) are charged into a ball mill and mixed and dispersed for 12 hours. Next, the dispersion was placed in a dipping tank (size: 300 × 300 × 40 m).
m) and then transferred to ultrasonic (Shinmeidai Kogyo Co., Ltd.
26 KHz-output 600 W) is applied for 30 minutes. After the dispersion was left in a dipping tank for 1 hour, a glass substrate (size: 250 × 300 × 3.
5 mm) is immersed in this bath, and the substrate is vertically pulled out of the bath at a pulling speed of 6 mm / s.
The coating was cured by drying in a drying furnace maintained at 50 ° C. for 30 minutes.
【００２０】得られた機能性膜は、膜厚２．０μｍのグ
レーの着色膜であり、この膜のヘーズ値は０.６％、可
視光線透過率３０％と非常に透明性のよい着色膜付きガ
ラスが得られた。このガラスは建築用装飾ガラス或いは
車両用のリアドアの窓ガラス等として使用可能である。The obtained functional film is a gray colored film having a thickness of 2.0 μm, and has a haze value of 0.6% and a visible light transmittance of 30%, which is very transparent. A coated glass was obtained. This glass can be used as decorative glass for buildings or window glass of rear doors for vehicles.
【００２１】実施例４ ビヒクルとしてのポリシラザン樹脂溶液（東燃（株）
製、ポリシラザン樹脂の固形分１０ｗｔ％：キシレン溶
媒８０ｗｔ％）１００ｇと無機顔料である複合酸化物
（大日精化工業（株）製、９４１０（青色顔料）１０ｇ
をボールミルに投入し、２４時間混合分散する。次いで
該分散液をディピング槽（サイズ；３００×３００×４
０ｍｍ）に移し替えたのち、超音波（神明台工業（株）
製、２６ＫＨｚ−出力６００Ｗ）を３０分間印加させ
る。分散液をディピング槽中に１時間放置後、片面にマ
スキングを施したガラス基板（サイズ；２５０×３００
×３.５ｍｍ）をこの槽に浸漬させたのち、８ｍｍ／ｓ
の引き上げ速度で該基板を垂直に該槽より引き上げたの
ち、２５０℃に保持された乾燥炉で３０分間乾燥するこ
とにより、被膜を硬化させた。Example 4 Polysilazane resin solution as vehicle (Tonen Corp.)
G of polysilazane resin: 10 g of polysilazane resin: 80 g of xylene solvent) and 10 g of composite oxide as inorganic pigment (manufactured by Dainichi Seika Kogyo Co., Ltd., 9410 (blue pigment))
Into a ball mill and mixed and dispersed for 24 hours. Next, the dispersion is placed in a dipping tank (size: 300 × 300 × 4
0mm) and then ultrasonic (Shinmeidai Industry Co., Ltd.)
, 26 KHz-600 W output) for 30 minutes. After leaving the dispersion in a dipping tank for 1 hour, a glass substrate (size: 250 × 300
× 3.5 mm) was immersed in this tank, and then 8 mm / s
The substrate was vertically lifted from the bath at a lifting speed of, and then dried in a drying furnace maintained at 250 ° C. for 30 minutes to cure the coating.
【００２２】得られた機能性膜は、膜厚１．５μｍの青
色の着色膜であり、この膜のヘーズ値は０.４％、可視
光線透過率４６％と非常に透明性のよい着色膜付きガラ
スが得られた。このガラスは建築用装飾ガラス或いは車
両用のリアドアの窓ガラス等として使用可能である。The obtained functional film is a blue colored film having a thickness of 1.5 μm, and has a haze value of 0.4% and a visible light transmittance of 46%, which is very transparent. A coated glass was obtained. This glass can be used as decorative glass for buildings or window glass of rear doors for vehicles.
【００２３】比較例１ 実施例１と同様のビヒクル及び顔料を用い、実施例１と
同一の条件で混合分散する。その後、超音波を印加させ
ることなく、混合分散後３０分後に、実施例１と同一の
条件でガラス基板表面に成膜し、乾燥する。Comparative Example 1 Using the same vehicle and pigment as in Example 1, mixed and dispersed under the same conditions as in Example 1. Thereafter, a film is formed on the surface of the glass substrate under the same conditions as in Example 1 and dried after 30 minutes from the mixing and dispersion without applying ultrasonic waves.
【００２４】得られた膜は、可視光線透過率は７７％で
あったが、ヘーズ値が３.５と非常に高く、ガラスに濁
り感が生じており、建築用、車のフロントドアの窓ガラ
スとしては使用不可能であった。The resulting film had a visible light transmittance of 77%, but had a very high haze value of 3.5, causing a turbidity in the glass, and was used for architectural and car front door windows. It could not be used as glass.
【００２５】[0025]
【発明の効果】本発明の方法によれば、ビヒクル中に添
加した機能性微粒子を混合分散後、少なくとも１０数時
間以上放置しても該微粒子が凝集することがなく、安定
化し、均一且つヘイズの小さな透光性の高品質の被膜が
得られる。さらに、沈降防止剤が使用出来ないような液
においても適用出来、また、沈降防止剤を用いた液であ
っても微粒子が沈降する傾向が極めて小さいので、作業
効率が図れる等、簡単な方法で高品質の透明塗膜が得ら
れる効果を有する。According to the method of the present invention, even if the functional fine particles added to the vehicle are mixed and dispersed, the fine particles are not aggregated even when left for at least 10 hours or more, and are stabilized, uniform and haze-free. And a light-transmitting, high-quality film having a small particle size is obtained. Furthermore, the method can be applied to a liquid in which an anti-settling agent cannot be used.Also, even in a liquid using an anti-settling agent, the tendency of fine particles to settle down is extremely small, so that a simple method such as working efficiency can be achieved. It has the effect of obtaining a high quality transparent coating film.
───────────────────────────────────────────────────── フロントページの続き (51)Int.Cl.6 識別記号 ＦＩ Ｃ０９Ｄ 183/16 Ｃ０９Ｄ 183/16 ──────────────────────────────────────────────────続 き Continued on the front page (51) Int.Cl. 6 Identification code FI C09D 183/16 C09D 183/16
Claims (4)
た分散液を透光性基材上に塗布成膜し、透光性膜付き基
材を製造する分散液において、該分散液は、ビヒクル中
に微粒子を混合分散後の分散液に超音波を印加されて微
粒子の凝集を抑制し、安定化されたものであることを特
徴とする微粒子分散塗布液。1. A dispersion in which functional fine particles are mixed and dispersed in a vehicle, and the dispersion is coated and formed on a light-transmitting substrate to produce a substrate with a light-transmitting film. Ultrasonic waves are applied to the dispersion liquid after mixing and dispersing the fine particles in the vehicle to suppress aggregation of the fine particles and to stabilize the dispersion liquid.
散させた分散液において、分散液中のポリシラザン樹脂
の含有量は固形分で４５〜９９重量％であることを特徴
とする請求項１記載の微粒子分散塗布液。2. A dispersion in which a polysilazane resin and an organic pigment are dispersed in a solution, wherein the content of the polysilazane resin in the dispersion is 45 to 99% by weight in solid content. Fine particle dispersion coating liquid.
であることを特徴とする請求項１乃至２記載の微粒子分
散塗布液。3. The fine particle-dispersed coating liquid according to claim 1, wherein the particle diameter of the fine particles in the dispersion is 100 nm or less.
徴とする請求項１乃至３記載の微粒子分散塗布液。4. The fine particle-dispersed coating liquid according to claim 1, wherein the dispersion liquid does not contain an antisettling agent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7377498A JPH11269432A (en) | 1998-03-23 | 1998-03-23 | Microparticle-dispersed coating fluid |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| JP7377498A JPH11269432A (en) | 1998-03-23 | 1998-03-23 | Microparticle-dispersed coating fluid |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| JPH11269432A true JPH11269432A (en) | 1999-10-05 |
Family
ID=13527904
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| JP7377498A Pending JPH11269432A (en) | 1998-03-23 | 1998-03-23 | Microparticle-dispersed coating fluid |
Country Status (1)
| Country | Link |
|---|---|
| JP (1) | JPH11269432A (en) |
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000068330A1 (en) * | 1999-05-10 | 2000-11-16 | Shunichi Haruyama | Inorganic-organic film and starting liquid composition therefor and method for preparation thereof, and applications and method for preparing them |
| EP1178021A1 (en) * | 2000-08-04 | 2002-02-06 | Ishizuka Glass Co., Ltd. | Resin film-coated recyclable glass bottles and method for producing the same |
| EP1325944A2 (en) | 2001-12-18 | 2003-07-09 | Toda Kogyo Corporation | Fine organic pigment particles, dispersion containing said fine particles and process for producing the fine organic pigment particles |
| JP2004532925A (en) * | 2001-06-18 | 2004-10-28 | ピーピージー インダストリーズ オハイオ， インコーポレイテッド | Use of nanoparticulate organic pigments in paints and coatings |
| JP2005177596A (en) * | 2003-12-18 | 2005-07-07 | Hamamatsu Photonics Kk | Particulate, and method and apparatus for manufacturing the same |
| JP2006272937A (en) * | 2005-03-30 | 2006-10-12 | Dainippon Printing Co Ltd | Decorative sheet |
| DE102007023094A1 (en) | 2007-05-16 | 2008-11-20 | Clariant International Ltd. | Color pigmented coating composition with high hiding power, increased scratch resistance and easy to clean properties |
| CN101857744A (en) * | 2009-04-07 | 2010-10-13 | 精工爱普生株式会社 | The manufacture method of water resistant aluminum pigment dispersion, water resistant aluminum pigment and contain its aqueous ink composition |
| US8283395B2 (en) | 2005-05-09 | 2012-10-09 | Fujifilm Corporation | Method of producing organic-particles-dispersion liquid |
| US8679341B2 (en) | 2005-05-06 | 2014-03-25 | Fujifilm Corporation | Method of concentrating nanoparticles and method of deaggregating aggregated nanoparticles |
| CN107902916A (en) * | 2017-11-11 | 2018-04-13 | 蚌埠承永玻璃制品有限公司 | A kind of preparation method of self-cleaning glass |
| KR102265267B1 (en) * | 2021-01-13 | 2021-06-17 | (주)에스케이솔라에너지 | Color Photovoltaic Module For Building |
-
1998
- 1998-03-23 JP JP7377498A patent/JPH11269432A/en active Pending
Cited By (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2000068330A1 (en) * | 1999-05-10 | 2000-11-16 | Shunichi Haruyama | Inorganic-organic film and starting liquid composition therefor and method for preparation thereof, and applications and method for preparing them |
| EP1178021A1 (en) * | 2000-08-04 | 2002-02-06 | Ishizuka Glass Co., Ltd. | Resin film-coated recyclable glass bottles and method for producing the same |
| JP2004532925A (en) * | 2001-06-18 | 2004-10-28 | ピーピージー インダストリーズ オハイオ， インコーポレイテッド | Use of nanoparticulate organic pigments in paints and coatings |
| JP2006219674A (en) * | 2001-06-18 | 2006-08-24 | Ppg Ind Ohio Inc | Use of nanoparticulate organic pigment in paint and coating |
| EP1325944A2 (en) | 2001-12-18 | 2003-07-09 | Toda Kogyo Corporation | Fine organic pigment particles, dispersion containing said fine particles and process for producing the fine organic pigment particles |
| EP1325944A3 (en) * | 2001-12-18 | 2003-07-23 | Toda Kogyo Corporation | Fine organic pigment particles, dispersion containing said fine particles and process for producing the fine organic pigment particles |
| US7432314B2 (en) | 2001-12-18 | 2008-10-07 | Toda Kogyo Corporation | Functional material, dispersion containing the functional material, and process for producing the functional material |
| US7597277B2 (en) | 2003-12-18 | 2009-10-06 | Hamamatsu Photonics K.K. | Microparticles, microparticle production method, and microparticle production apparatus |
| JP2005177596A (en) * | 2003-12-18 | 2005-07-07 | Hamamatsu Photonics Kk | Particulate, and method and apparatus for manufacturing the same |
| WO2005058480A3 (en) * | 2003-12-18 | 2005-09-01 | Hamamatsu Photonics Kk | Particle and particle manufacturing method and apparatus |
| JP2006272937A (en) * | 2005-03-30 | 2006-10-12 | Dainippon Printing Co Ltd | Decorative sheet |
| US8679341B2 (en) | 2005-05-06 | 2014-03-25 | Fujifilm Corporation | Method of concentrating nanoparticles and method of deaggregating aggregated nanoparticles |
| US8283395B2 (en) | 2005-05-09 | 2012-10-09 | Fujifilm Corporation | Method of producing organic-particles-dispersion liquid |
| DE102007023094A1 (en) | 2007-05-16 | 2008-11-20 | Clariant International Ltd. | Color pigmented coating composition with high hiding power, increased scratch resistance and easy to clean properties |
| JP2010526925A (en) * | 2007-05-16 | 2010-08-05 | クラリアント・インターナシヨナル・リミテツド | Color pigmented coating composition with high hiding power, increased scratch resistance, and ease of cleaning |
| US8470924B2 (en) | 2007-05-16 | 2013-06-25 | Az Electronic Materials Usa Corp. | Color-pigmented paint composition having high covering powder, increased scratch resistance, and easy-to clean properties |
| CN101857744A (en) * | 2009-04-07 | 2010-10-13 | 精工爱普生株式会社 | The manufacture method of water resistant aluminum pigment dispersion, water resistant aluminum pigment and contain its aqueous ink composition |
| CN107902916A (en) * | 2017-11-11 | 2018-04-13 | 蚌埠承永玻璃制品有限公司 | A kind of preparation method of self-cleaning glass |
| KR102265267B1 (en) * | 2021-01-13 | 2021-06-17 | (주)에스케이솔라에너지 | Color Photovoltaic Module For Building |
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