JP2006003378A - Composition for light scattering film and light scattering film using same - Google Patents
Composition for light scattering film and light scattering film using same Download PDFInfo
- Publication number
- JP2006003378A JP2006003378A JP2004176450A JP2004176450A JP2006003378A JP 2006003378 A JP2006003378 A JP 2006003378A JP 2004176450 A JP2004176450 A JP 2004176450A JP 2004176450 A JP2004176450 A JP 2004176450A JP 2006003378 A JP2006003378 A JP 2006003378A
- Authority
- JP
- Japan
- Prior art keywords
- light scattering
- scattering film
- composition
- refractive index
- fine particles
- 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.)
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- 229920002050 silicone resin Polymers 0.000 description 1
- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000000758 substrate Substances 0.000 description 1
- YRHRIQCWCFGUEQ-UHFFFAOYSA-N thioxanthen-9-one Chemical compound C1=CC=C2C(=O)C3=CC=CC=C3SC2=C1 YRHRIQCWCFGUEQ-UHFFFAOYSA-N 0.000 description 1
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 1
- 229910052724 xenon Inorganic materials 0.000 description 1
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
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- Optical Elements Other Than Lenses (AREA)
- Liquid Crystal (AREA)
Abstract
Description
本発明は、反射型液晶表示装置を構成する光散乱膜の形成に用いられる光散乱膜用組成物、および光散乱膜に関する。 The present invention relates to a light scattering film composition used for forming a light scattering film constituting a reflective liquid crystal display device, and a light scattering film.
近年、液晶表示装置の普及、大型化や野外使用化に伴い、その使用条件下での耐候性、視認性、防汚性、耐熱性等が求められている。中でも、表示装置の視認性向上は表示装置の主機能に関わる重要な課題であり、視認性向上のための様々な技術が検討されている。
例えば、反射型液晶表示装置においては、視認性向上のため、基材樹脂中に基材樹脂とは異なる屈折率の微粒子を分散させてなる、反射防止膜、光拡散膜、光散乱膜等を設け、光の反射、拡散、散乱を制御することが行われている。
In recent years, with the widespread use, enlargement, and outdoor use of liquid crystal display devices, weather resistance, visibility, antifouling properties, heat resistance, and the like under the use conditions have been demanded. Above all, improvement of the visibility of the display device is an important issue related to the main function of the display device, and various techniques for improving the visibility have been studied.
For example, in a reflection type liquid crystal display device, an antireflection film, a light diffusion film, a light scattering film, etc., in which fine particles having a refractive index different from that of the base resin are dispersed in the base resin for improving visibility. It is provided to control reflection, diffusion and scattering of light.
具体的には、反射型液晶表示装置には、装置に入射した室内光や外光等の光を反射する反射板が必要であり、この反射板には光の反射機能及び光散乱機能の2つの機能が要求される。光散乱機能を持たせる部材としては、アクリル樹脂、エポキシ樹脂、ポリエステル樹脂、ポリアミド樹脂、ポリウレタン樹脂、ポリイミド樹脂等の透明樹脂中に異屈折率の微粒子を混ぜて散乱性を出す光散乱膜が用いられている。この光散乱膜には、優れた光の散乱性と光透過性が要求され、光散乱膜は、基材樹脂と微粒子の屈折率差が大きいほど優れた散乱特性を示し、更に微粒子の粒子径、及び粒度分布にも大きく影響を受ける。
しかし、従来の光散乱膜は、光の散乱特性及び表面平滑性の点で、充分に満足するものではなかった。
However, conventional light scattering films are not fully satisfactory in terms of light scattering characteristics and surface smoothness.
本発明の目的は、光散乱機能と表面平滑性に優れた光散乱膜、およびその形成に用いられる光散乱膜用組成物を提供することにある。 An object of the present invention is to provide a light scattering film excellent in light scattering function and surface smoothness, and a composition for a light scattering film used for the formation thereof.
本発明の光散乱膜用組成物は、屈折率が１．５１以上３．００以下であり、一次粒子の平均粒径が０．８〜５．０μm、変動係数が６．０〜２０．０％であり、かつ分散粒子の平均粒径が０．８〜５．０μm、変動係数が６．０〜１７．０％である微粒子と、屈折率が１．３５以上１．５１未満の透明樹脂とを含むことを特徴とする。
また、本発明の光散乱膜は、上記組成物を用いて形成され、表面粗さ（Ｒa）が３００Å以下のものである。
The composition for a light scattering film of the present invention has a refractive index of 1.51 or more and 3.00 or less, an average primary particle size of 0.8 to 5.0 μm, and a coefficient of variation of 6.0 to 20.0. %, A fine particle having an average particle diameter of 0.8 to 5.0 μm and a coefficient of variation of 6.0 to 17.0%, and a transparent resin having a refractive index of 1.35 or more and less than 1.51 It is characterized by including.
The light scattering film of the present invention is formed using the above composition and has a surface roughness (Ra) of 300 mm or less.
本発明の光散乱膜用組成物は、屈折率が１．５１以上３．００以下であり、一次粒子の平均粒径が０．８〜５．０μm、変動係数が６．０〜２０．０％であり、かつ分散粒子の平均粒径が０．８〜５．０μm、変動係数が６．０〜１７．０％である微粒子と、屈折率が１．３５以上１．５１未満の透明樹脂とを含むため、該組成物を用いることにより、光散乱機能と表面平滑性に優れた光散乱膜を形成することができる。 The composition for a light scattering film of the present invention has a refractive index of 1.51 or more and 3.00 or less, an average primary particle size of 0.8 to 5.0 μm, and a coefficient of variation of 6.0 to 20.0. %, A fine particle having an average particle diameter of 0.8 to 5.0 μm and a coefficient of variation of 6.0 to 17.0%, and a transparent resin having a refractive index of 1.35 or more and less than 1.51 Therefore, by using the composition, a light scattering film excellent in light scattering function and surface smoothness can be formed.
まず、本発明の光散乱膜用組成物について説明する。
微粒子の屈折率をn１、透明樹脂の屈折率をn２とすると、光散乱膜はn１＞n２型とn１＜n２型に分類されるが、本発明の光散乱膜用組成物は、n１＞n２型に属するものである。
本発明の光散乱膜用組成物に含有される屈折率が１．５１以上３．００以下の微粒子は、一次粒子の平均粒径が０．８〜５．０μm、好ましくは１．０〜２．７μｍ、変動係数が６．０〜２０．０％、好ましくは６．５〜１８．０％のものであり、かつ分散粒子の平均粒径が０．８〜５．０μm、好ましくは１．０〜２．７μｍ、変動係数が６．０〜１７．０％、好ましくは６．５〜１６．５％となるように透明樹脂中に分散されている。
First, the composition for light scattering films of the present invention will be described.
When the refractive index of the fine particles is n1 and the refractive index of the transparent resin is n2, the light scattering film is classified into n1> n2 type and n1 <n2 type, but the composition for light scattering film of the present invention has n1> n2. Belongs to a type.
The fine particles having a refractive index of 1.51 or more and 3.00 or less contained in the composition for light scattering film of the present invention have an average primary particle diameter of 0.8 to 5.0 μm, preferably 1.0 to 2. 0.7 μm, the coefficient of variation is 6.0 to 20.0%, preferably 6.5 to 18.0%, and the average particle size of the dispersed particles is 0.8 to 5.0 μm, preferably 1. It is dispersed in the transparent resin so that the variation coefficient is 0 to 2.7 μm, and the variation coefficient is 6.0 to 17.0%, preferably 6.5 to 16.5%.
微粒子の一次粒子及び分散粒子の変動係数が６．０％未満では光散乱膜にモアレが生じる。また、微粒子の一次粒子の変動係数が２０．０％を越える、または分散粒子の変動係数が１７．０％を超えると表面粗さが悪くなる。したがって、一次粒子の変動係数が６．０〜２０．０％の範囲内にある微粒子を選択し、さらに分散粒子の変動係数が６．０〜１７．０％になるように分散条件を適宜限定することが必要となる。 When the variation coefficient of the primary particles and the dispersed particles of the fine particles is less than 6.0%, moire occurs in the light scattering film. Further, when the variation coefficient of primary particles of fine particles exceeds 20.0% or the variation coefficient of dispersed particles exceeds 17.0%, the surface roughness is deteriorated. Therefore, fine particles having a primary particle variation coefficient in the range of 6.0 to 20.0% are selected, and the dispersion conditions are appropriately limited so that the dispersion coefficient of the dispersed particles is 6.0 to 17.0%. It is necessary to do.
微粒子の一次粒子の平均粒子径は、粒子を光学顕微鏡にて観察し、画像解析・計測ソフトウェアを用い、粒子１００個の直径を実測して算出されるものである。また、微粒子の一次粒子の変動係数は、粒子１００個の直径の標準偏差値を平均値で除した値を百分率で表したものである。また、微粒子の分散粒子の平均粒子径及び変動係数は、レーザー回折式粒度分布測定装置で測定、算出されるものである。 The average particle diameter of the primary particles of the fine particles is calculated by observing the particles with an optical microscope and measuring the diameter of 100 particles using image analysis / measurement software. The variation coefficient of the primary particles of the fine particles is a percentage obtained by dividing the standard deviation value of the diameter of 100 particles by the average value. The average particle size and variation coefficient of the dispersed particles of fine particles are measured and calculated by a laser diffraction particle size distribution measuring device.
本発明の光散乱膜用組成物に含有される屈折率が１．５１以上３．００以下の微粒子としては、メラミン樹脂（屈折率約１．５７）、スチレン樹脂（屈折率約１．５９）、ジビニルベンゼン樹脂（屈折率約１．５７）、ベンゾグアナミン樹脂（屈折率約１．５７）、アクリル−スチレン樹脂（屈折率約１．５４）、ポリカーボネート樹脂（屈折率約１．５７）、フェノール樹脂（屈折率約１．７０）、塩化ビニリデン樹脂（屈折率約１．６３）、ポリ塩化ビニル樹脂（屈折率約１．６０）等から選ばれる１種または２種以上の樹脂からなる微粒子、及び酸化セリウム（屈折率約１．６３）、ＳｉＯ2（屈折率約２．００）、ＴｉＯ2（屈折率約２．７０）、ＺrＯ2（屈折率約２．０５）、Ａｌ2Ｏ3（屈折率約１．６３）、シリカ−チタニア系粒子（屈折率約１．６７）等の無機微粒子が挙げられるが、特にこれらに限定されるものではない。また、これらの微粒子は混合して用いることができ、中空微粒子も使用できる。 The fine particles having a refractive index of 1.51 or more and 3.00 or less contained in the composition for light scattering film of the present invention include melamine resin (refractive index of about 1.57), styrene resin (refractive index of about 1.59). , Divinylbenzene resin (refractive index about 1.57), benzoguanamine resin (refractive index about 1.57), acrylic-styrene resin (refractive index about 1.54), polycarbonate resin (refractive index about 1.57), phenol resin (Refractive index of about 1.70), vinylidene chloride resin (refractive index of about 1.63), polyvinyl chloride resin (refractive index of about 1.60), etc. Cerium oxide (refractive index approximately 1.63), SiO 2 (refractive index approximately 2.00), TiO 2 (refractive index approximately 2.70), ZrO 2 (refractive index approximately 2.05), Al 2 O 3 (refractive index) 1.63), silica-titania Inorganic fine particles such as system particles (refractive index of about 1.67) can be mentioned, but the present invention is not particularly limited thereto. In addition, these fine particles can be used as a mixture, and hollow fine particles can also be used.
本発明の光散乱膜用組成物に含有される屈折率が１．３５以上１．５１未満の透明樹脂としては、アクリル樹脂(屈折率約１．５０)、フッ素含有アクリル樹脂（屈折率約１．４５）、酢酸ビニル樹脂（屈折率約１．４５）、シリコーン樹脂（屈折率約１．４５）、フッ素樹脂（屈折率約１．３５）等が挙げられるが、特にこれらに限定されるものではない。
光散乱膜用組成物中の微粒子の濃度は、組成物の全量を基準として、１〜５０重量％であることが好ましい。微粒子の濃度が５０重量％より高いと、微粒子間の距離が小さくなることから、安定な分散状態を保つことが困難となり、微粒子同士の凝集が起こり易くなる。
The transparent resin having a refractive index of 1.35 or more and less than 1.51 contained in the composition for light scattering film of the present invention includes acrylic resin (refractive index of about 1.50), fluorine-containing acrylic resin (refractive index of about 1). .45), vinyl acetate resin (refractive index of about 1.45), silicone resin (refractive index of about 1.45), fluororesin (refractive index of about 1.35), and the like. is not.
The concentration of the fine particles in the composition for light scattering film is preferably 1 to 50% by weight based on the total amount of the composition. When the concentration of the fine particles is higher than 50% by weight, the distance between the fine particles becomes small, so that it is difficult to maintain a stable dispersion state, and the fine particles tend to aggregate.
光散乱膜用組成物には、該組成物を活性エネルギー線により硬化させて光散乱膜を形成する場合、あるいは光散乱膜をリソグラフィ法によりパターニングして形成する場合には、エチレン性不飽和化合物を含有させ、さらに該組成物を紫外線により硬化させる場合には、光重合開始剤を含有させる。
また、光散乱膜用組成物をリソグラフィ法によりパターニングする際にアルカリ現像する場合には、屈折率が１．３５以上１．５１以下の透明樹脂として、アルカリ可溶性のもの、例えば、カルボキシル基を有するアクリル系樹脂等を用いることが好ましい。
The composition for a light scattering film has an ethylenically unsaturated compound when the composition is cured by active energy rays to form a light scattering film or when the light scattering film is formed by patterning by a lithography method. In the case where the composition is further cured by ultraviolet rays, a photopolymerization initiator is contained.
Further, when alkali development is performed when patterning the light scattering film composition by lithography, the transparent resin having a refractive index of 1.35 or more and 1.51 or less has an alkali-soluble one, for example, a carboxyl group. It is preferable to use an acrylic resin or the like.
エチレン性不飽和化合物は、エチレン性不飽和二重結合を1個または２個以上有する化合物であり、モノマー、オリゴマー、感光性樹脂を用いることができる。モノマーとしては、例えば、２−ヒドロキシエチル（メタ）アクリレート、２−ヒドロキシプロピル（メタ）アクリレート、シクロヘキシル（メタ）アクリレート、ポリエチレングリコールジ（メタ）アクリレート、トリメチロールプロパントリ（メタ）アクリレート、ペンタエリスリトールトリ（メタ）アクリレート、ジペンタエリスリトールヘキサ（メタ）アクリレート、ジペンタエリスリトールペンタ（メタ）アクリレート等が挙げられる。また、オリゴマーとしては、エポキシ（メタ）アクリレート、ウレタン（メタ）アクリレート、エステル（メタ）アクリレート等が挙げられ、感光性樹脂としては、ポリエステル、ポリウレタン、エポキシ樹脂、アクリル樹脂等に公知の方法でエチレン性不飽和二重結合を導入したものが挙げられる。
エチレン性不飽和化合物は、１種を単独で、あるいは２種以上を混合して用いられる。
An ethylenically unsaturated compound is a compound having one or more ethylenically unsaturated double bonds, and monomers, oligomers, and photosensitive resins can be used. Examples of the monomer include 2-hydroxyethyl (meth) acrylate, 2-hydroxypropyl (meth) acrylate, cyclohexyl (meth) acrylate, polyethylene glycol di (meth) acrylate, trimethylolpropane tri (meth) acrylate, and pentaerythritol tris. (Meth) acrylate, dipentaerythritol hexa (meth) acrylate, dipentaerythritol penta (meth) acrylate and the like. In addition, examples of the oligomer include epoxy (meth) acrylate, urethane (meth) acrylate, ester (meth) acrylate and the like, and examples of the photosensitive resin include polyester, polyurethane, epoxy resin, acrylic resin, and the like by a known method. And those having an unsaturated double bond introduced therein.
An ethylenically unsaturated compound is used individually by 1 type or in mixture of 2 or more types.
光重合開始剤としては、例えば、４−フェノキシジクロロアセトフェノン、４−ｔ−ブチル−ジクロロアセトフェノン、ジエトキシアセトフェノン、１−（４−イソプロピルフェニル）−２−ヒドロキシ−２−メチルプロパン−１オン、１−ヒドロキシシクロヘキシルフェニルケトン、２−ベンジル−２−ジメチルアミノ−１−（４−モルフォリノフェニル）−ブタン−１−オン等のアセトフェノン系光重合開始剤、ベンゾイン、ベンゾインメチルエーテル、ベンゾインエチルエーテル、ベンゾインイソプロピルエーテル、ベンジルジメチルケタール等のベンゾイン系光重合開始剤、ベンゾフェノン、ベンゾイル安息香酸、ベンゾイル安息香酸メチル、４−フェニルベンゾフェノン、ヒドロキシベンゾフェノン、アクリル化ベンゾフェノン、４−ベンゾイル−４’−メチルジフェニルサルファイド等のベンゾフェノン系光重合開始剤、チオキサンソン、２−クロルチオキサンソン、２−メチルチオキサンソン、イソプロピルチオキサンソン、２，４−ジイソプロピルチオキサンソン等のチオキサンソン系光重合開始剤、２，４，６−トリクロロ−ｓ−トリアジン、２−フェニル−４，６−ビス（トリクロロメチル）−ｓ−トリアジン、２−（ｐ−メトキシフェニル）−４，６−ビス（トリクロロメチル）−ｓ−トリアジン、２−（ｐ−トリル）−４，６−ビス（トリクロロメチル）−ｓ−トリアジン、２−ピペロニル−−４，６−ビス（トリクロロメチル）−ｓ−トリアジン、２，４−−ビス（トリクロロメチル）−６−スチリルｓ−トリアジン、２−（ナフト−１−イル）−４，６−ビス（トリクロロメチル）−ｓ−トリアジン、２−（４−メトキシ−ナフト−１−イル）−４，６−ビス（トリクロロメチル）−ｓ−トリアジン、２，４−トリクロロメチル−（ピペロニル）−６−トリアジン、２，４−トリクロロメチル（４’−メトキシスチリル）−６−トリアジン等のトリアジン系光重合開始剤、カルバゾール系光重合開始剤、イミダゾール系光重合開始剤等が挙げられる。上記光重合開始剤は、１種を単独で、あるいは２種以上を混合して用いられる。 Examples of the photopolymerization initiator include 4-phenoxydichloroacetophenone, 4-t-butyl-dichloroacetophenone, diethoxyacetophenone, 1- (4-isopropylphenyl) -2-hydroxy-2-methylpropan-1-one, 1 Acetophenone photopolymerization initiators such as -hydroxycyclohexyl phenyl ketone, 2-benzyl-2-dimethylamino-1- (4-morpholinophenyl) -butan-1-one, benzoin, benzoin methyl ether, benzoin ethyl ether, benzoin Benzoin photopolymerization initiators such as isopropyl ether and benzyl dimethyl ketal, benzophenone, benzoylbenzoic acid, methyl benzoylbenzoate, 4-phenylbenzophenone, hydroxybenzophenone, acrylated benzophenone, Benzophenone photopolymerization initiators such as benzoyl-4′-methyldiphenyl sulfide, thioxanthones such as thioxanthone, 2-chlorothioxanthone, 2-methylthioxanthone, isopropylthioxanthone, 2,4-diisopropylthioxanthone Photopolymerization initiator, 2,4,6-trichloro-s-triazine, 2-phenyl-4,6-bis (trichloromethyl) -s-triazine, 2- (p-methoxyphenyl) -4,6-bis ( Trichloromethyl) -s-triazine, 2- (p-tolyl) -4,6-bis (trichloromethyl) -s-triazine, 2-piperonyl-4,6-bis (trichloromethyl) -s-triazine, 2, , 4-Bis (trichloromethyl) -6-styryl s-triazine, 2- (naphth-1-yl) -4, -Bis (trichloromethyl) -s-triazine, 2- (4-methoxy-naphth-1-yl) -4,6-bis (trichloromethyl) -s-triazine, 2,4-trichloromethyl- (piperonyl)- Examples thereof include triazine photopolymerization initiators such as 6-triazine and 2,4-trichloromethyl (4′-methoxystyryl) -6-triazine, carbazole photopolymerization initiators, and imidazole photopolymerization initiators. The said photoinitiator is used individually by 1 type or in mixture of 2 or more types.
また、光散乱膜用組成物には、増感剤を含有させてもよい。増感剤としては、例えば、α−アシロキシエステル、アシルフォスフィンオキサイド、メチルフェニルグリオキシレート、ベンジル、９，１０−フェナンスレンキノン、カンファーキノン、エチルアンスラキノン、４，４’−ジエチルイソフタロフェノン、３，３’，４，４’−テトラ（ｔ−ブチルパーオキシカルボニル）ベンゾフェノン、４，４’−ジエチルアミノベンゾフェノン等が挙げられる。上記増感剤は、１種を単独で、あるいは２種以上を混合して用いられる。 Further, the composition for light scattering film may contain a sensitizer. Examples of the sensitizer include α-acyloxy ester, acylphosphine oxide, methylphenylglyoxylate, benzyl, 9,10-phenanthrenequinone, camphorquinone, ethylanthraquinone, 4,4′-diethyliso Examples include phthalophenone, 3,3 ′, 4,4′-tetra (t-butylperoxycarbonyl) benzophenone, 4,4′-diethylaminobenzophenone, and the like. The above sensitizers are used alone or in combination of two or more.
光散乱膜用組成物には、均一な光散乱膜を形成するため、溶剤を含有させることが好ましい。溶剤としては、例えばシクロヘキサノン、エチルセロソルブアセテート、ブチルセロソルブアセテート、１−メトキシ−２−プロピルアセテート、ジエチレングリコールジメチルエーテル、エチルベンゼン、エチレングリコールジエチルエーテル、キシレン、エチルセロソルブ、メチル−ｎアミルケトン、プロピレングリコールモノメチルエーテル、プロピレングリコールモノメチルエーテルアセテート、トルエン、メチルエチルケトン、酢酸エチル、メタノール、エタノール、イソプロピルアルコール、ブタノール、イソブチルケトン、石油系溶剤等が挙げられ、これらを単独で、もしくは混合して用いる。 The composition for a light scattering film preferably contains a solvent in order to form a uniform light scattering film. Examples of the solvent include cyclohexanone, ethyl cellosolve acetate, butyl cellosolve acetate, 1-methoxy-2-propyl acetate, diethylene glycol dimethyl ether, ethylbenzene, ethylene glycol diethyl ether, xylene, ethyl cellosolve, methyl-n amyl ketone, propylene glycol monomethyl ether, propylene glycol. Examples thereof include monomethyl ether acetate, toluene, methyl ethyl ketone, ethyl acetate, methanol, ethanol, isopropyl alcohol, butanol, isobutyl ketone, and petroleum solvents, and these are used alone or in combination.
光散乱膜用組成物には、塗工性向上、感度の向上、密着性の向上などを目的として、連鎖移動剤、界面活性剤、シランカップリング剤等の添加剤を添加しても良い。
光散乱膜用組成物は、各成分を混合し、シェーカー、ディスパー、サンドミル、アトライター、アイガー・モーターミル等の各種分散装置を用いて分散することにより製造することができる。分散粒子の変動係数を効率よく所望の範囲内にするには、メディアを用いた分散装置、例えばサンドミル、アトライター、アイガー・モーターミルで分散することが好ましい。
光散乱膜用組成物は、焼結フィルタ、メンブレンフィルタ等の手段にて、５μｍ以上の粗大粒子および混入した塵の除去を行うことが好ましい。
Additives such as a chain transfer agent, a surfactant, and a silane coupling agent may be added to the composition for a light scattering film for the purpose of improving coatability, sensitivity, and adhesion.
The composition for a light scattering film can be produced by mixing each component and dispersing them using various dispersing devices such as a shaker, a disper, a sand mill, an attritor, an Eiger motor mill and the like. In order to efficiently bring the coefficient of variation of the dispersed particles within a desired range, it is preferable to disperse with a dispersing device using a medium such as a sand mill, an attritor, or an Eiger motor mill.
It is preferable that the composition for light scattering films removes coarse particles of 5 μm or more and mixed dust by means such as a sintered filter and a membrane filter.
次に、光散乱膜について説明する。
光散乱膜は、ガラス板等の透明基板上に、スピンコート、スリットコート、ロールコート等の塗布方法により光散乱膜用組成物を塗布、乾燥し、必要に応じて活性エネルギー線を照射することにより作成される。光散乱膜をパターニングにより形成する場合には、光散乱膜用組成物を塗布、乾燥後に、フォトマスクを介して組成物塗布面側から活性エネルギー線を照射し、溶剤またはアルカリ現像液に漬浸するかスプレーなどにより現像液を噴霧して未照射部、すなわち未硬化部を除去して現像を行い、所望の形状のパターンを形成する。
Next, the light scattering film will be described.
The light scattering film is applied to a transparent substrate such as a glass plate by applying a composition for the light scattering film by a coating method such as spin coating, slit coating, roll coating, and the like, and irradiated with active energy rays as necessary. Created by. When the light scattering film is formed by patterning, after applying the composition for the light scattering film and drying, irradiate the composition application surface side with active energy rays through a photomask and immerse it in a solvent or alkaline developer. Alternatively, the developer is sprayed by spraying or the like to remove the unirradiated portion, that is, the uncured portion, and development is performed to form a pattern having a desired shape.
光散乱膜の表面粗さ（Ｒa）は、３００Å以下でなければならない。光散乱膜の表面粗さ（Ｒa）が３００Åを超えると、光散乱に乱れを生じる。
また、光散乱膜用組成物の塗布膜厚は、０．２〜５．０μｍ（乾燥時）の範囲であることが好ましく、塗工性と光散乱特性のバランスが良好なことから０．５〜３．５μｍの範囲であることがより好ましい。
The surface roughness (Ra) of the light scattering film must be 300 mm or less. When the surface roughness (Ra) of the light scattering film exceeds 300 mm, the light scattering is disturbed.
Further, the coating film thickness of the light scattering film composition is preferably in the range of 0.2 to 5.0 μm (during drying), and the balance between coating property and light scattering characteristics is 0.5. More preferably, it is in the range of ˜3.5 μm.
アルカリ現像液としては、炭酸ナトリウム、水酸化ナトリウム等の水溶液が使用され、ジメチルベンジルアミン、トリエタノールアミン等の有機アルカリを用いることもできる。また、現像液には、消泡剤や界面活性剤を添加することもできる。
なお、活性エネルギー線による露光感度を上げるために、光散乱膜用組成物を塗布乾燥後、水溶性あるいはアルカリ可溶性樹脂、例えばポリビニルアルコールや水溶性アクリル樹脂等を塗布乾燥し酸素による重合阻害を防止する膜を形成した後、組成物塗布面側から活性エネルギー線を照射することもできる。
As the alkali developer, an aqueous solution such as sodium carbonate or sodium hydroxide is used, and an organic alkali such as dimethylbenzylamine or triethanolamine can also be used. Moreover, an antifoamer and surfactant can also be added to a developing solution.
In order to increase the exposure sensitivity with active energy rays, after applying and drying the composition for light scattering film, water-soluble or alkali-soluble resin such as polyvinyl alcohol or water-soluble acrylic resin is applied and dried to prevent polymerization inhibition by oxygen. After the film to be formed is formed, active energy rays can be irradiated from the composition application surface side.
活性エネルギー線としては、電子線、紫外線、４００〜５００ｎｍの可視光を使用することができる。組成物塗布面側から照射する電子線の線源には、熱電子放射銃、電界放射銃等を使用することができる。また、紫外線および４００〜５００ｎｍの可視光の線源（光源）には、例えば、高圧水銀灯、超高圧水銀灯、メタルハライド灯、ガリウム灯、キセノン灯、カーボンアーク灯等を使用することができる。具体的には、点光源であること、輝度が安定であることから、超高圧水銀ランプ、キセノン水銀ランプが用いられることが多い。組成物塗布面側から照射する活性エネルギー線量は、５〜１０００ｍＪの範囲で適時設定できるが、工程上管理しやすい２０〜３００ｍＪの範囲であることが好ましい。 As the active energy ray, an electron beam, ultraviolet rays, or visible light of 400 to 500 nm can be used. A thermionic emission gun, a field emission gun, or the like can be used as the electron beam source irradiated from the composition application surface side. Moreover, for example, a high pressure mercury lamp, an ultrahigh pressure mercury lamp, a metal halide lamp, a gallium lamp, a xenon lamp, a carbon arc lamp, or the like can be used as a source (light source) of ultraviolet rays and visible light of 400 to 500 nm. Specifically, since it is a point light source and the luminance is stable, an ultrahigh pressure mercury lamp or a xenon mercury lamp is often used. The active energy dose irradiated from the composition application surface side can be set in a timely range of 5 to 1000 mJ, but is preferably in the range of 20 to 300 mJ that is easy to manage in the process.
以下に，実施例により本発明を説明する。なお、実施例中の「部」および「％」とは、「重量部」および「重量％」をそれぞれ表す。また、微粒子の一次粒子の平均粒子径及び変動係数は、粒子を光学顕微鏡（OLYMPUS製「BX60」）にて観察し、画像解析・計測ソフトウェア（三谷商事製「Mac Scope」）を用い、粒子100個の直径を実測して算出した。なお、変動係数は、一次粒子の直径の標準偏差値を平均値で除した値を百分率で表したものである。また、分散粒子の平均粒子径及び変動係数はレーザー回折式粒度分布測定装置 （マルバーン製「Mastersizer ２０００」）で測定した。ここで、変動係数の計算に使用した標準偏差値は、均一性（Uniformity）の値を代用した。
［実施例１］
メラミン樹脂微粒子（（株）日本触媒製「エポスターＳ12」、屈折率１．５７）３０．０部とプロピレングリコールモノメチルエーテルアセテート７０．０部を、アイガー・モーターミル（アイガージャパン（株）製「M-50 VSE-EXJ MKII」）を用い、１mmφジルコニアビーズをメディアとして、４０００rpmで２時間分散した。得られた樹脂微粒子分散液を含む下記の処方の光散乱膜用組成物をマルチシェーカー（アイラー社製「ＭＭＳ-３１０」）を用いて混合し、100mm×100mm×1.1mmのガラス板にスピンコーターで塗工し、70℃で20分乾燥後、超高圧水銀ランプを用いて、積算光量150mJで紫外線露光後、230℃1時間加熱し、約3μｍの光散乱膜を形成した。
Hereinafter, the present invention will be described by way of examples. In the examples, “parts” and “%” represent “parts by weight” and “% by weight”, respectively. In addition, the average particle size and coefficient of variation of the primary particles of fine particles can be measured by observing the particles with an optical microscope (OLYMPUS "BX60") and using image analysis / measurement software (Mitani Corporation "Mac Scope"). The diameter of each was measured and calculated. The coefficient of variation is a percentage obtained by dividing the standard deviation value of the primary particle diameter by the average value. The average particle size and coefficient of variation of the dispersed particles were measured with a laser diffraction particle size distribution analyzer (“Mastersizer 2000” manufactured by Malvern). Here, the standard deviation value used for the calculation of the coefficient of variation was a uniformity value.
[Example 1]
30.0 parts of melamine resin fine particles (Nippon Shokubai Co., Ltd. “Eposter S12”, refractive index 1.57) and 70.0 parts of propylene glycol monomethyl ether acetate were added to Eiger Motor Mill (Eiger Japan Ltd. “M” -50 VSE-EXJ MKII "), 1 mmφ zirconia beads were used as media and dispersed at 4000 rpm for 2 hours. The composition for a light scattering film having the following formulation containing the obtained resin fine particle dispersion was mixed using a multi shaker (“MMS-310” manufactured by Eiler) and spin coated on a 100 mm × 100 mm × 1.1 mm glass plate. After coating at 70 ° C. for 20 minutes, using an ultra-high pressure mercury lamp, it was exposed to ultraviolet light at an integrated light amount of 150 mJ and heated at 230 ° C. for 1 hour to form a light scattering film of about 3 μm.
（光散乱膜用組成物処方）
樹脂微粒子分散液（固形分３０％） ２０．０部
アクリル樹脂（屈折率１．５０、重量平均分子量４００００）
のシクロヘキサノン溶液（固形分２０％） ７０．０部
ジペンタエリスリトールペンタ及びヘキサアクリレート
（東亞合成製「アロニックスM-４０２」） ７．０部
光重合開始剤（チバガイギー製「イルガキュア９０７」） ２．０部
ノニオン性界面活性剤 １．０部
(Composition formulation for light scattering film)
Resin fine particle dispersion (solid content 30%) 20.0 parts Acrylic resin (refractive index 1.50, weight average molecular weight 40000)
Cyclohexanone solution (solid content 20%) 70.0 parts Dipentaerythritol penta and hexaacrylate (“Aronix M-402” manufactured by Toagosei Co., Ltd.) 7.0 parts Photopolymerization initiator (“Irgacure 907” manufactured by Ciba Geigy) 2.0 Nonionic surfactant 1.0 part
［実施例２］
メラミン樹脂微粒子をプロピレングリコールモノメチルエーテルアセテートに分散する際の分散時間を２時間から４時間に変更した以外は、実施例１と同じ操作をして約３μmの光散乱膜を得た。
［比較例１］
メラミン樹脂微粒子をプロピレングリコールモノメチルエーテルアセテートに分散する際の分散時間を２時間から３０分に変更した以外は、実施例１と同じ操作をして約３μmの光散乱膜を得た。
［比較例２］
メラミン樹脂微粒子をプロピレングリコールモノメチルエーテルアセテートに分散する際の分散装置をアイガー・モーターミルからメディアレス分散機のディスパーに変更し、分散時間を２時間から１０時間に変更した以外は、実施例１と同じ操作をして約３μmの光散乱膜を得た。
[Example 2]
A light scattering film of about 3 μm was obtained in the same manner as in Example 1 except that the dispersion time when dispersing the melamine resin fine particles in propylene glycol monomethyl ether acetate was changed from 2 hours to 4 hours.
[Comparative Example 1]
A light scattering film of about 3 μm was obtained in the same manner as in Example 1 except that the dispersion time when dispersing the melamine resin fine particles in propylene glycol monomethyl ether acetate was changed from 2 hours to 30 minutes.
[Comparative Example 2]
Example 1 except that the dispersion device for dispersing melamine resin fine particles in propylene glycol monomethyl ether acetate is changed from a Eiger motor mill to a disperser of a medialess disperser, and the dispersion time is changed from 2 hours to 10 hours. The same operation was performed to obtain a light scattering film of about 3 μm.
実施例1〜２及び比較例１〜２で得られた光散乱膜のHAZEをHAZEMETER HM-150（村上色彩技術研究所製）で測定し、膜厚及び表面粗さ(Ra)をDektak 3030（日本真空技術製）で測定した。結果を表１に示す。 The HAZE of the light scattering films obtained in Examples 1-2 and Comparative Examples 1-2 was measured with HAZEMETER HM-150 (manufactured by Murakami Color Research Laboratory), and the film thickness and surface roughness (Ra) were determined as Dektak 3030 ( (Manufactured by Nippon Vacuum Technology). The results are shown in Table 1.
実施例１〜２に示すように、微粒子の平均粒子径、屈折率及び分散条件を適宜選択することにより、高HAZEで表面粗さ３００Å以下の光散乱膜を形成できる。
比較例１〜２に示すように、メディア分散で短時間の場合及びメディアレス分散では微粒子の凝集がほぐれず、微粒子が均一に分散した表面粗さ３００Å以下の光散乱膜が得られない。
As shown in Examples 1 and 2, a light scattering film having a high HAZE and a surface roughness of 300 mm or less can be formed by appropriately selecting the average particle diameter, refractive index, and dispersion conditions of the fine particles.
As shown in Comparative Examples 1 and 2, in the case of media dispersion for a short time and medialess dispersion, the aggregation of the fine particles is not loosened, and a light scattering film having a surface roughness of 300 mm or less in which the fine particles are uniformly dispersed cannot be obtained.
Claims (3)
A light scattering film formed using the composition for a light scattering film according to claim 1 or 2 and having a surface roughness (Ra) of 300 mm or less.
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| JP2002293809A (en) * | 2001-03-30 | 2002-10-09 | Sekisui Plastics Co Ltd | Resin fine particles, method for producing the same, and resin composition containing the same |
| JP2003156606A (en) * | 2001-09-10 | 2003-05-30 | Nitto Denko Corp | Light diffusing sheet, optical element and image display device |
| JP2003156605A (en) * | 2001-11-22 | 2003-05-30 | Fuji Photo Film Co Ltd | Light scattering film, polarizing plate and liquid crystal display device using them |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2008026883A (en) * | 2006-06-19 | 2008-02-07 | Fujifilm Corp | Optical film |
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| JP4639652B2 (en) | 2011-02-23 |
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