JP2011203316A - Coating material for high transmissive diffusion film and high transmissive diffusion film - Google Patents
Coating material for high transmissive diffusion film and high transmissive diffusion film Download PDFInfo
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本発明は、高透過拡散膜用塗料及び高透過拡散膜に関し、特に詳しくは、ランプ等の光学部品やガラス等の透明部材に光透過性及び光拡散性を付与する際に用いて好適な高透過拡散膜用塗料及び高透過拡散膜に関するものである。 The present invention relates to a coating material for a highly permeable diffusion film and a highly permeable diffusion film, and in particular, it is suitable for use in imparting light transmittance and light diffusibility to an optical component such as a lamp or a transparent member such as glass. The present invention relates to a coating for a permeable diffusion film and a highly permeable diffusion film.
従来より、ガラス製品に光拡散性を付与した構造としては、ガラス表面にサンドブラスト加工を施し、その表面を梨地状とすることで光拡散性を持たせた構造、ガラス表面をフッ酸処理し、その表面を梨地状とすることにより、くもりガラス状とした構造等が用いられてきたが、薄いガラスでは割れが生じる虞があり、また、表面が凹凸形状のガラス製品では、部分によっては梨地状が不完全なものとなり、表面を均一に処理することが難しい等の問題点があった。そこで、ガラス表面に光拡散性を均一に付与した構造や方法として、ガラスの表面にオレイン酸等の滑性付与剤を添加した合成樹脂をコーティングすることにより滑性を付与した微細な凹凸部分を形成し、この凹凸部分の変形を防止し、透明化を防止した構造（特許文献１）、基板上に、有機系の透明樹脂と、この透明樹脂と屈折率の異なる微粒子とを含む光散乱膜用組成物をダイコート法により塗布し、光散乱膜を形成する方法（特許文献２）等が提案されている。 Conventionally, as a structure that imparts light diffusibility to glass products, sandblasting is performed on the glass surface, and the surface is given a light diffusibility by making the surface a satin finish, the glass surface is treated with hydrofluoric acid, Although the surface of the surface has a satin finish, a structure with a cloudy glass has been used, but there is a risk of cracking in thin glass. There were problems such as incompleteness and difficulty in uniformly treating the surface. Therefore, as a structure or method that uniformly imparts light diffusibility to the glass surface, the surface of the glass is coated with a synthetic resin to which a lubricity-imparting agent such as oleic acid is added. A light scattering film that is formed and has a structure in which deformation of the uneven portion is prevented and transparency is prevented (Patent Document 1), an organic transparent resin, and fine particles having a refractive index different from that of the transparent resin on the substrate A method of forming a light scattering film by applying a composition for coating by a die coating method (Patent Document 2) and the like has been proposed.
ところで、従来のガラスの表面の微細な凹凸部分に滑性を付与した構造では、オレイン酸等の滑性付与剤を添加した合成樹脂をコーティングしているので、ガラスの表面における耐熱性が不十分であるという問題点があった。
また、有機系の透明樹脂と微粒子とを含む光散乱膜用組成物を塗布した光散乱膜では、低屈折率材料である有機系の透明樹脂と、高屈折率材料である微粒子との界面効果を利用していることから、光散乱膜の光透過性が低下してしまうという問題点があった。
By the way, in the conventional structure in which the fine irregularities on the surface of the glass are provided with lubricity, since the synthetic resin to which a lubricity imparting agent such as oleic acid is added is coated, the heat resistance on the glass surface is insufficient. There was a problem that.
In addition, in a light scattering film coated with a composition for a light scattering film containing an organic transparent resin and fine particles, an interface effect between the organic transparent resin that is a low refractive index material and the fine particles that are a high refractive index material. Therefore, there is a problem that the light transmittance of the light scattering film is lowered.
本発明は、上記事情に鑑みてなされたものであって、高い光透過性、高い光拡散性及び耐熱性を同時に実現することができ、しかも、割れが生じる虞も無く、凹凸形状の表面においても面内均一性に優れた膜を形成することが可能な高透過拡散膜用塗料及び高透過拡散膜を提供することを目的とする。 The present invention has been made in view of the above circumstances, and can achieve high light transmittance, high light diffusibility, and heat resistance at the same time, and there is no risk of cracking, and on the uneven surface. Another object of the present invention is to provide a highly permeable diffusion film coating material and a highly permeable diffusion film capable of forming a film having excellent in-plane uniformity.
本発明者等は、上記課題を解決するために鋭意検討を行った結果、シリカ粒子が凝集され表面が凹凸形状かつ粒子径が１μｍ以上かつ５μｍ以下の凝集体を粉砕または破砕してなる不均一形状の凝集体片と、バインダー成分とにより塗料を構成すれば、高い光透過性、高い光拡散性及び耐熱性を有する膜を実現することができ、しかも、割れが生じる虞も無く、凹凸形状の表面においても面内均一性に優れた膜を形成することが可能であることを見出し、本発明を完成するに至った。 As a result of intensive studies to solve the above-mentioned problems, the present inventors have found that non-uniformity is obtained by pulverizing or crushing aggregates in which silica particles are aggregated and the surface is uneven and the particle diameter is 1 μm or more and 5 μm or less. If the paint is composed of the aggregate pieces in the shape and the binder component, a film having high light transmission, high light diffusibility and heat resistance can be realized, and there is no risk of cracking, and the concavo-convex shape As a result, it was found that a film excellent in in-plane uniformity can be formed even on the surface, and the present invention has been completed.
すなわち、本発明の高透過拡散膜用塗料は、シリカ粒子が凝集され表面が凹凸形状かつ粒子径が１μｍ以上かつ５μｍ以下の凝集体を粉砕または破砕してなる不均一形状の凝集体片と、バインダー成分とを含有してなることを特徴とする。 That is, the coating material for a high-permeability diffusion membrane of the present invention is a non-uniform-shaped aggregate piece formed by pulverizing or crushing an aggregate in which silica particles are aggregated and the surface is uneven and the particle diameter is 1 μm or more and 5 μm or less, And a binder component.
前記凝集体は、多孔質かつ中空の球形シリカ凝集体、多孔質かつ中実の球形シリカ凝集体、のいずれか１種からなることが好ましい。
前記バインダー成分は、エポキシ樹脂、アクリル樹脂、フッ素樹脂、フェノール樹脂、ポリエステル樹脂、ポリ塩化ビニル樹脂、ケイ素含有無機有機ハイブリッド構造体、の群から選択される１種からなることが好ましい。
The aggregate is preferably composed of any one of a porous and hollow spherical silica aggregate and a porous and solid spherical silica aggregate.
The binder component is preferably made of one selected from the group consisting of an epoxy resin, an acrylic resin, a fluororesin, a phenol resin, a polyester resin, a polyvinyl chloride resin, and a silicon-containing inorganic / organic hybrid structure.
本発明の高透過拡散膜は、本発明の高透過拡散膜用塗料を塗布してなることを特徴とする。 The highly permeable diffusion membrane of the present invention is formed by applying the coating for a highly permeable diffusion membrane of the present invention.
本発明の高透過拡散膜用塗料によれば、シリカ粒子が凝集され表面が凹凸形状かつ粒子径が１μｍ以上かつ５μｍ以下の凝集体を粉砕または破砕してなる不均一形状の凝集体片と、バインダー成分とを含有したので、この凝集体片が光の拡散性及び耐熱性に優れるとともに、凝集体を粉砕または破砕した不均一形状であることから低屈折率となり、高い光透過性、高い光拡散性及び耐熱性を同時に実現することができる。 According to the coating material for a highly permeable diffusion membrane of the present invention, a non-uniform-shaped aggregate piece formed by pulverizing or crushing an aggregate having a concavo-convex surface and a particle diameter of 1 μm or more and 5 μm or less with agglomerated silica particles; Since it contains a binder component, this aggregate piece is excellent in light diffusibility and heat resistance, and has a low refractive index due to the non-uniform shape obtained by pulverizing or crushing the aggregate, resulting in high light transmittance and high light. Diffusivity and heat resistance can be realized simultaneously.
本発明の高透過拡散膜によれば、本発明の高透過拡散膜用塗料を塗布して得られたので、割れが生じる虞も無く、凹凸形状の表面においても均一な厚みとすることができ、面内均一性に優れている。したがって、高い光透過性及び高い光拡散性を保持することができる。 According to the highly permeable diffusion membrane of the present invention, since it was obtained by applying the coating material for the highly permeable diffusion membrane of the present invention, there is no risk of cracking, and a uniform thickness can be achieved even on uneven surfaces. Excellent in-plane uniformity. Therefore, high light transmittance and high light diffusibility can be maintained.
本発明の高透過拡散膜用塗料及び高透過拡散膜を実施するための形態について説明する。
なお、この形態は、発明の趣旨をより良く理解させるために具体的に説明するものであり、特に指定のない限り、本発明を限定するものではない。
The form for implementing the coating material for highly permeable diffusion films and the highly permeable diffusion film of this invention is demonstrated.
This embodiment is specifically described for better understanding of the gist of the invention, and does not limit the present invention unless otherwise specified.
［高透過拡散膜用塗料］
本実施形態の高透過拡散膜用塗料は、シリカ粒子が凝集され表面が凹凸形状かつ粒子径が１μｍ以上かつ５μｍ以下の凝集体を粉砕または破砕してなる不均一形状の凝集体片と、バインダー成分とを含有してなる塗料である。
ここで、この凝集体としては、多孔質かつ中空の球形シリカ凝集体、多孔質かつ中実の球形シリカ凝集体、のいずれか１種からなることが好ましい。
[Coating for highly permeable diffusion membrane]
The coating material for a highly permeable diffusion film according to the present embodiment includes a non-uniformly shaped aggregate piece formed by pulverizing or crushing an aggregate having a concavo-convex surface and a particle diameter of 1 μm or more and 5 μm or less. It is the coating material containing an ingredient.
Here, the aggregate is preferably composed of any one of a porous and hollow spherical silica aggregate and a porous and solid spherical silica aggregate.
図１は、本実施形態の凝集体及び凝集体片の一例を示す模式図であり、図において、１は球形シリカ凝集体であり、例えば、粒子径が１０ｎｍ以下の球形シリカ２が多数、球形に凝集して多孔質状となっており、かつ内部には中空３が形成されている。
この球形シリカ凝集体１の２次粒子径は、１μｍ以上かつ５μｍ以下が好ましく、より好ましくは２μｍ以上かつ３μｍ以下である。
FIG. 1 is a schematic diagram illustrating an example of an aggregate and an aggregate piece of the present embodiment. In the figure, 1 is a spherical silica aggregate, for example, a large number of
The secondary particle diameter of the spherical silica aggregate 1 is preferably 1 μm or more and 5 μm or less, more preferably 2 μm or more and 3 μm or less.
この２次粒子径を１μｍ以上かつ５μｍ以下とした理由は、この凝集体１を粉砕または破砕により複数の凝集体片に分割した場合に、得られた凝集体片の高い光透過性及び高い光拡散性を両立させることができる範囲だからである。
ここで、２次粒子径が１μｍ未満の場合、複数の凝集体片に分割した場合に、得られた凝集体片の粒子径がサブミクロンあるいはナノメートルの大きさとなり、光透過性は確保されるものの光拡散性が十分に得られなくなり、ヘーズ値も低下するので好ましくなく、一方、２次粒子径が５μｍを超えると、得られた凝集体片の粒子径が５μｍ程度あるいはそれ以上のミクロンオーダーとなってしまい、光透過性が低下し、光透明性が得られなくなるので、好ましくない。
The reason why the secondary particle size is 1 μm or more and 5 μm or less is that when the aggregate 1 is divided into a plurality of aggregate pieces by pulverization or crushing, the resulting aggregate pieces have high light transmittance and high light. This is because the diffusibility is compatible.
Here, when the secondary particle diameter is less than 1 μm, when the particles are divided into a plurality of aggregate pieces, the particle diameter of the obtained aggregate pieces is submicron or nanometer, and light transmittance is ensured. However, when the secondary particle diameter exceeds 5 μm, the particle diameter of the obtained aggregate piece is about 5 μm or more microns. Since it becomes an order and light transmittance falls and optical transparency cannot be obtained, it is not preferable.
この球形シリカ凝集体１の表面の凹凸形状の評価は、例えば、細孔径、実測密度／理論密度、等の数値により評価することができる。
例えば、細孔径が１ｎｍ以上かつ１０ｎｍ以下であれば、光散乱性が優れていると評価することができる。
The evaluation of the concavo-convex shape on the surface of the spherical silica aggregate 1 can be evaluated by numerical values such as pore diameter, measured density / theoretical density, and the like.
For example, if the pore diameter is 1 nm or more and 10 nm or less, it can be evaluated that the light scattering property is excellent.
この球形シリカ凝集体１は、ボールミルやジェットミル等の粉砕手段や破砕機等の破砕手段を用いて粉砕または破砕することにより、様々な外形の凝集体片に分割され、図１（ｂ）に示す不均一形状の凝集体片１１〜１６となっている。
この凝集体片１１〜１６は、外形形状が互いに異なった不均一形状であるから、外部からの光を効果的に散乱させることができる。したがって、高い光拡散性を有している。
また、内部に中空３を有する球形シリカ凝集体１を粉砕または破砕して得られた凝集体片１１〜１６であるから、凝集体片１１〜１６における空隙部分の占める割合が高く、したがって、低屈折率を維持したものとなっている。これにより、高い光透過性を有したものとなっている。
The spherical silica aggregate 1 is divided into aggregate pieces of various outer shapes by pulverization or crushing using a crushing means such as a ball mill or a jet mill or a crushing machine, as shown in FIG. It becomes the non-uniform-shaped aggregate pieces 11-16 shown.
Since the aggregate pieces 11 to 16 are non-uniform shapes having different outer shapes, it is possible to effectively scatter light from the outside. Therefore, it has high light diffusibility.
Moreover, since it is the aggregate pieces 11-16 obtained by grind | pulverizing or crushing the spherical silica aggregate 1 which has the hollow 3 inside, the ratio for which the space | gap part accounts in the aggregate pieces 11-16 is high, Therefore low The refractive index is maintained. Thereby, it has a high light transmittance.
図２は、本実施形態の凝集体及び凝集体片の他の一例を示す模式図であり、図において、２１は球形シリカ凝集体であり、例えば、粒子径が１０ｎｍ以下の球形シリカ２が多数、球形に凝集して多孔質状となっており、かつ内部は密に詰まった中実とされている。
この球形シリカ凝集体２１の２次粒子径は、１μｍ以上かつ５μｍ以下が好ましく、より好ましくは２μｍ以上かつ３μｍ以下である。
FIG. 2 is a schematic diagram showing another example of the aggregate and aggregate pieces of the present embodiment. In the figure,
The secondary particle diameter of the
この２次粒子径を１μｍ以上かつ５μｍ以下とした理由は、この凝集体２１を粉砕または破砕により複数の凝集体片に分割した場合に、得られた凝集体片の高い光透過性及び高い光拡散性を両立させることができる範囲だからである。
ここで、２次粒子径が１μｍ未満の場合、複数の凝集体片に分割した場合に、得られた凝集体片の粒子径がサブミクロンあるいはナノメートルの大きさとなり、光透過性は確保されるものの光拡散性が十分に得られなくなり、ヘーズ値も低下するので好ましくなく、一方、２次粒子径が５μｍを超えると、得られた凝集体片の粒子径が５μｍ程度あるいはそれ以上のミクロンオーダーとなってしまい、光透過性が低下し、光透明性が得られなくなるので、好ましくない。
The reason why the secondary particle diameter is 1 μm or more and 5 μm or less is that when the
Here, when the secondary particle diameter is less than 1 μm, when the particles are divided into a plurality of aggregate pieces, the particle diameter of the obtained aggregate pieces is submicron or nanometer, and light transmittance is ensured. However, when the secondary particle diameter exceeds 5 μm, the particle diameter of the obtained aggregate piece is about 5 μm or more microns. Since it becomes an order and light transmittance falls and optical transparency cannot be obtained, it is not preferable.
この球形シリカ凝集体２１においても、上記の球形シリカ凝集体１と同様、表面の凹凸形状の評価は、例えば、細孔径、実測密度／理論密度、等の数値により評価することができる。
例えば、細孔径が１ｎｍ以上かつ１０ｎｍ以下であれば、光散乱性が優れていると評価することができる。
In the
For example, if the pore diameter is 1 nm or more and 10 nm or less, it can be evaluated that the light scattering property is excellent.
この球形シリカ凝集体２１においても、上記の球形シリカ凝集体１と同様、ボールミルやジェットミル等の粉砕手段や破砕機等の破砕手段を用いて粉砕または破砕することにより、様々な外形の凝集体片に分割され、図２（ｂ）に示す不均一形状の凝集体片３１〜３８となっている。
この凝集体片３１〜３８においても、上記の凝集体片１１〜１６と同様、外形形状が互いに異なった不均一形状であるから、外部からの光を効果的に散乱させることができる。したがって、高い光拡散性を有している。
また、中実の球形シリカ凝集体２１を粉砕または破砕して得られた凝集体片３１〜３８であるから、上記の凝集体片１１〜１６と同様、低屈折率を維持し、高い光透過性を有したものとなっている。
In the
Also in the
Moreover, since it is the aggregate pieces 31-38 obtained by grind | pulverizing or crushing the solid
バインダー成分としては、可視光線あるいは近赤外線等の所定の波長帯域の光に対して透明性を有するものであればよく、熱可塑性、熱硬化性、可視光線や紫外線や赤外線等による光（電磁波）硬化性、電子線照射による電子線硬化性等の硬化性樹脂、あるいはケイ素含有無機有機ハイブリッド構造体が好適に用いられる。
これらの樹脂としては、エポキシ樹脂、アクリル樹脂、フッ素樹脂、フェノール樹脂、ポリエステル樹脂、ポリ塩化ビニル樹脂が挙げられる。これらの樹脂の中でも、光透過性及び光拡散性に優れ、耐熱性及び機械的特性に優れている点で、エポキシ樹脂またはアクリル樹脂が好ましい。
また、ケイ素含有無機有機ハイブリッド構造体としては、アクリル・ポリシロキサンハイブリッド樹脂、エポキシ・ポリシロキサンハイブリッド樹脂、ウレタン・ポリシロキサンハイブリッド樹脂等が挙げられる。
The binder component only needs to be transparent to light in a predetermined wavelength band such as visible light or near infrared, and is thermoplastic, thermosetting, light (electromagnetic wave) by visible light, ultraviolet light, infrared light, or the like. A curable resin such as a curable resin or an electron beam curable by electron beam irradiation, or a silicon-containing inorganic / organic hybrid structure is preferably used.
Examples of these resins include epoxy resins, acrylic resins, fluororesins, phenol resins, polyester resins, and polyvinyl chloride resins. Among these resins, an epoxy resin or an acrylic resin is preferable because it is excellent in light transmittance and light diffusibility, and excellent in heat resistance and mechanical properties.
Examples of the silicon-containing inorganic / organic hybrid structure include acrylic / polysiloxane hybrid resin, epoxy / polysiloxane hybrid resin, and urethane / polysiloxane hybrid resin.
このバインダー成分の凝集体片全体量に対する割合は、３質量％以上かつ２０質量％以下が好ましい。
ここで、バインダー成分の割合が３質量％未満では、バインダー成分の量が凝集体片全体量に対して少なくなりすぎてしまい、その結果、凝集体片同士の接合が弱くなり、この塗料を塗布して得られた膜の機械的強度が低下し、膜が剥がれる等の不具合が生じる虞があり、一方、バインダー成分の割合が２０質量％を超えると、バインダー成分の量が凝集体片全体量に対して多くなりすぎてしまい、その結果、バインダー成分の過多による光拡散性の低下及び光透過性の低下の虞がある。
The ratio of the binder component to the total amount of aggregate pieces is preferably 3% by mass or more and 20% by mass or less.
Here, if the ratio of the binder component is less than 3% by mass, the amount of the binder component becomes too small with respect to the total amount of the aggregate pieces. As a result, the bonding between the aggregate pieces becomes weak, and this paint is applied. The mechanical strength of the film thus obtained is reduced, and there is a possibility that problems such as peeling off of the film may occur. On the other hand, when the ratio of the binder component exceeds 20% by mass, the amount of the binder component is the total amount of the aggregate pieces. As a result, there is a concern that the light diffusibility and light transmittance may be lowered due to excessive binder components.
この塗料に含まれる溶媒としては、水、有機溶媒、液状の樹脂モノマー、液状の樹脂オリゴマーの群から選択される１種または２種以上が好適に用いられる。
上記の有機溶媒としては、例えば、メタノール、エタノール、２−プロパノール、ブタノール、オクタノール等のアルコール類、酢酸エチル、酢酸ブチル、乳酸エチル、プロピレングリコールモノメチルエーテルアセテート、プロピレングリコールモノエチルエーテルアセテート、γ−ブチロラクトン等のエステル類、ジエチルエーテル、エチレングリコールモノメチルエーテル（メチルセロソルブ）、エチレングリコールモノエチルエーテル（エチルセロソルブ）、エチレングリコールモノブチルエーテル（ブチルセロソルブ）、ジエチレングリコールモノメチルエーテル、ジエチレングリコールモノエチルエーテル等のエーテル類、アセトン、メチルエチルケトン、メチルイソブチルケトン、アセチルアセトン、シクロヘキサノン等のケトン類、ベンゼン、トルエン、キシレン、エチルベンゼン等の芳香族炭化水素、ジメチルホルムアミド、Ｎ，Ｎ−ジメチルアセトアセトアミド、Ｎ−メチルピロリドン等のアミド類が好適に用いられ、これらの溶媒は、１種のみ単独で用いてもよく、２種以上を混合して用いてもよい。
As the solvent contained in the paint, one or more selected from the group of water, organic solvents, liquid resin monomers, and liquid resin oligomers are preferably used.
Examples of the organic solvent include alcohols such as methanol, ethanol, 2-propanol, butanol, and octanol, ethyl acetate, butyl acetate, ethyl lactate, propylene glycol monomethyl ether acetate, propylene glycol monoethyl ether acetate, and γ-butyrolactone. Esters such as diethyl ether, ethylene glycol monomethyl ether (methyl cellosolve), ethylene glycol monoethyl ether (ethyl cellosolve), ethylene glycol monobutyl ether (butyl cellosolve), ethers such as diethylene glycol monomethyl ether, diethylene glycol monoethyl ether, acetone, Methyl ethyl ketone, methyl isobutyl ketone, acetylacetone, cyclohexanone, etc. Amides, aromatic hydrocarbons such as benzene, toluene, xylene, and ethylbenzene, and amides such as dimethylformamide, N, N-dimethylacetoacetamide, and N-methylpyrrolidone are preferably used. They may be used alone or in combination of two or more.
上記の液状の樹脂モノマーとしては、アクリル酸メチル、メタクリル酸メチル等のアクリル系またはメタクリル系のモノマー、エポキシ系モノマー等が好適に用いられる。
また、上記の液状の樹脂オリゴマーとしては、ウレタンアクリレート系オリゴマー、エポキシアクリレート系オリゴマー、アクリレート系オリゴマー等が好適に用いられる。
As the liquid resin monomer, acrylic or methacrylic monomers such as methyl acrylate and methyl methacrylate, and epoxy monomers are preferably used.
Moreover, as said liquid resin oligomer, a urethane acrylate oligomer, an epoxy acrylate oligomer, an acrylate oligomer, etc. are used suitably.
この高透過拡散膜用塗料中の凝集体片の含有率は、１質量％以上かつ７０質量％以下が好ましく、より好ましくは１質量％以上かつ５０質量％以下、さらに好ましくは５質量％以上かつ３０質量％以下である。
ここで、凝集体片の含有率を１質量％以上かつ７０質量％以下と限定した理由は、この範囲が凝集体片が良好な分散状態を取りうる範囲であり、含有率が１質量％未満であると、凝集体片としての効果が低下し、高い光透過性及び高い光拡散性が得られず、また、７０質量％を超えると、凝集が激しくなり、塗料としての均一性が低下する。
The content of the aggregate pieces in the highly permeable diffusion membrane coating is preferably 1% by mass or more and 70% by mass or less, more preferably 1% by mass or more and 50% by mass or less, and further preferably 5% by mass or more and 30% by mass or less.
Here, the reason why the content rate of the aggregate pieces is limited to 1% by mass or more and 70% by mass or less is that this range is a range in which the aggregate pieces can take a good dispersion state, and the content rate is less than 1% by mass. When it is, the effect as an aggregate piece falls, high light transmittance and high light diffusibility are not acquired, and when it exceeds 70 mass%, aggregation will become intense and the uniformity as a coating will fall. .
本実施形態の高透過拡散膜用塗料によれば、シリカ粒子が凝集され表面が凹凸形状かつ粒子径が１μｍ以上かつ５μｍ以下の凝集体を粉砕または破砕してなる不均一形状の凝集体片と、バインダー成分とを含有したので、光の拡散性及び耐熱性に優れ、しかも低屈折率の凝集体片をバインダー成分中に分散させることで、高い光透過性、高い光拡散性及び耐熱性を有する膜を実現することができる。 According to the coating material for a highly permeable diffusion film of the present embodiment, the non-uniformly shaped aggregate pieces formed by pulverizing or crushing aggregates in which silica particles are aggregated and the surface is uneven and the particle diameter is 1 μm or more and 5 μm or less; Because it contains a binder component, it has excellent light diffusibility and heat resistance, and by dispersing aggregate pieces of low refractive index in the binder component, it has high light transmittance, high light diffusibility and heat resistance. The film | membrane which has can be implement | achieved.
［高透過拡散膜］
本実施形態の高透過拡散膜は、上記の高透過拡散膜用塗料を基材上に塗布して得られた膜である。
この高透過拡散膜は、上記の高透過拡散膜用塗料を基材上に塗布し、乾燥させることで、得ることができる。
このようにして得られた高透過拡散膜は、バインダー成分中にシリカ粒子が凝集され表面が凹凸形状かつ粒子径が１μｍ以上かつ５μｍ以下の凝集体を粉砕または破砕してなる不均一形状の凝集体片を分散した状態である。
[High permeability diffusion membrane]
The highly permeable diffusion film of this embodiment is a film obtained by applying the above-described coating material for a highly permeable diffusion film on a substrate.
This highly permeable diffusion film can be obtained by applying the above-described coating material for a highly permeable diffusion film on a substrate and drying it.
The thus obtained highly permeable diffusion membrane has a non-uniformly shaped aggregate formed by pulverizing or crushing aggregates in which silica particles are aggregated in a binder component and the surface is uneven and the particle diameter is 1 μm or more and 5 μm or less. It is in the state where the collected pieces are dispersed.
この高透過拡散膜では、凝集体片の含有率は、１質量％以上かつ８０質量％以下が好ましく、より好ましくは１０質量％以上かつ８０質量％以下、さらに好ましくは１０質量％以上かつ５０質量％以下である。
ここで、凝集体片の含有率を１質量％以上かつ８０質量％以下と限定した理由は、下限値の１質量％は光透過率、屈折率等の光学特性及び機械的強度等の機械的特性の向上が可能となる添加率の最小値であるからであり、一方、上限値の８０質量％は樹脂自体の特性（柔軟性、比重）を維持することができる添加率の最大値であるからである。
In this highly permeable diffusion membrane, the content of the aggregate pieces is preferably 1% by mass or more and 80% by mass or less, more preferably 10% by mass or more and 80% by mass or less, and further preferably 10% by mass or more and 50% by mass. % Or less.
Here, the reason why the content of the aggregate pieces is limited to 1% by mass or more and 80% by mass or less is that the lower limit of 1% by mass is optical characteristics such as light transmittance, refractive index, and mechanical strength such as mechanical strength. This is because it is the minimum value of the addition rate at which the characteristics can be improved, while the upper limit of 80% by mass is the maximum value of the addition rate that can maintain the properties (flexibility, specific gravity) of the resin itself. Because.
この高透過拡散膜では、凝集体片の形状や大きさ、及び含有率を調整することにより、光透過性、光拡散性、屈折率等の光学特性及び機械的強度等の機械的特性を所望の特性に調整することが可能である。 By adjusting the shape, size, and content of the aggregate pieces, this highly permeable diffusion film has desired optical characteristics such as light transmittance, light diffusivity, refractive index, and mechanical characteristics such as mechanical strength. It is possible to adjust to the characteristics.
本実施形態の高透過拡散膜によれば、上記の高透過拡散膜用塗料を基材上に塗布して得られた膜であるから、割れが生じる虞も無く、凹凸形状の表面においても均一な厚みとすることができ、面内均一性に優れている。したがって、高い光透過性及び高い光拡散性を保持することができる。 According to the highly permeable diffusion membrane of this embodiment, since it is a film obtained by applying the above-described coating material for a highly permeable diffusion film on a substrate, there is no risk of cracking, and even on uneven surfaces. Thickness, and excellent in-plane uniformity. Therefore, high light transmittance and high light diffusibility can be maintained.
以下、実施例及び比較例により本発明を具体的に説明するが、本発明はこれらの実施例によって限定されるものではない。 EXAMPLES Hereinafter, although an Example and a comparative example demonstrate this invention concretely, this invention is not limited by these Examples.
［実施例１］
多孔質状かつ内部に中空が形成された２次粒子径が２μｍの球形シリカ凝集体Ａを、分散剤を含む純水中にビーズミルを用いて粉砕・分散させ、その後ビーズを分離し、凝集体片を２０質量％、分散剤を２質量％含有する分散液を作製した。
次いで、この分散液にバインダー成分としてアクリル樹脂を、凝集体片がアクリル樹脂に対して３０質量％となるように添加して均一に混合し、実施例１の塗料を作製した。
[Example 1]
Spherical silica aggregate A having a secondary particle size of 2 μm and having a porous shape and hollow inside is pulverized and dispersed in pure water containing a dispersant using a bead mill, and then the beads are separated and aggregated. A dispersion containing 20% by mass of the piece and 2% by mass of the dispersant was prepared.
Next, an acrylic resin as a binder component was added to this dispersion so that the aggregate pieces were 30% by mass with respect to the acrylic resin and mixed uniformly to prepare the coating material of Example 1.
次いで、この塗料を、バーコート法により、ホウケイ酸ガラスからなるガラス基板（厚み×縦×横：２ｍｍ×２０ｍｍ×５０ｍｍ）上に膜厚が１．５μｍとなるように塗布し、得られた塗膜を、大気中、９０℃にて５分エアブローしながら乾燥し、実施例１の膜を得た。
次いで、ヘーズメータ ＮＤＨ−２０００（日本電色工業社製）を用いて、この膜のヘーズ値（Ｈｚ）及び全光線透過率（Ｔｔ）を測定し、光透過率の波長バラツキを算出した。また、目視により塗布ムラを評価した。
Next, this paint was applied to a glass substrate (thickness × length × width: 2 mm × 20 mm × 50 mm) made of borosilicate glass by a bar coating method so as to have a film thickness of 1.5 μm. The film was dried in air at 90 ° C. for 5 minutes while air blowing to obtain the film of Example 1.
Subsequently, using a haze meter NDH-2000 (manufactured by Nippon Denshoku Industries Co., Ltd.), the haze value (Hz) and the total light transmittance (Tt) of this film were measured, and the wavelength variation of the light transmittance was calculated. Further, the coating unevenness was evaluated visually.
ここでは、ヘーズ値（Ｈｚ）については、６０％以上を「◎」、４０％以上かつ６０％未満を「○」、２０％以上かつ４０％未満を「△」、２０％未満を「×」とした。
また、全光線透過率（Ｔｔ）については、９０％以上を「◎」、８５％以上かつ９０％未満を「○」、８０％以上かつ８５％未満を「△」、８０％未満を「×」とした。
Here, for haze values (Hz), 60% or more is “◎”, 40% or more and less than 60% is “◯”, 20% or more and less than 40% is “Δ”, and less than 20% is “×”. It was.
As for the total light transmittance (Tt), 90% or more is “「 ”, 85% or more and less than 90% is“ ◯ ”, 80% or more and less than 85% is“ Δ ”, and less than 80% is“ × ”. "
また、光透過率の波長バラツキについては、６％以下を「◎」、６％を超えかつ１０％以下を「○」、１０％を超えかつ２０％以下を「△」、２０％を超えたものを「×」とした。
また、塗布ムラについては、塗布ムラが認められなかったものを「◎」、塗布ムラが認められたものを「×」とした。
表１に測定結果を示す。
As for the wavelength variation of light transmittance, 6% or less exceeded “◎”, 6% or more exceeded 10% or less “◯”, 10% or more 20% or less “△”, or more than 20%. The thing was made into "x".
As for the coating unevenness, the case where the coating unevenness was not recognized was “◎”, and the case where the coating unevenness was recognized was “x”.
Table 1 shows the measurement results.
［実施例２］
凝集体片の含有率を３０質量％とした他は、実施例１に準じて実施例２の塗料及び膜を作製し、評価した。表１に測定結果を示す。
[Example 2]
The paint and film of Example 2 were prepared and evaluated according to Example 1 except that the content of the aggregate pieces was 30% by mass. Table 1 shows the measurement results.
［実施例３］
凝集体片の含有率を４０質量％とした他は、実施例１に準じて実施例３の塗料及び膜を作製し、評価した。表１に測定結果を示す。
[Example 3]
The paint and film of Example 3 were prepared and evaluated according to Example 1 except that the content of the aggregate pieces was 40% by mass. Table 1 shows the measurement results.
［実施例４］
球形シリカ凝集体Ａを、多孔質状かつ中実の２次粒子径が３μｍの球形シリカ凝集体Ｂに代えた他は、実施例１に準じて実施例４の塗料及び膜を作製し、評価した。表１に測定結果を示す。
[Example 4]
A coating material and a film of Example 4 were prepared and evaluated according to Example 1 except that the spherical silica aggregate A was replaced with a spherical silica aggregate B having a porous and solid secondary particle diameter of 3 μm. did. Table 1 shows the measurement results.
［実施例５］
球形シリカ凝集体Ａを、多孔質状かつ中実の２次粒子径が３μｍの球形シリカ凝集体Ｂに代え、凝集体片の含有率を３０質量％とした他は、実施例１に準じて実施例５の塗料及び膜を作製し、評価した。表１に測定結果を示す。
[Example 5]
The spherical silica aggregate A was replaced with the spherical silica aggregate B having a porous and solid secondary particle diameter of 3 μm, and the content of the aggregate pieces was 30% by mass, according to Example 1. The paint and film of Example 5 were prepared and evaluated. Table 1 shows the measurement results.
［実施例６］
球形シリカ凝集体Ａを、多孔質状かつ中実の２次粒子径が３μｍの球形シリカ凝集体Ｂに代え、凝集体片の含有率を４０質量％とした他は、実施例１に準じて実施例６の塗料及び膜を作製し、評価した。表１に測定結果を示す。
[Example 6]
The spherical silica aggregate A was replaced with the spherical silica aggregate B having a porous and solid secondary particle diameter of 3 μm, and the content of the aggregate pieces was 40% by mass, according to Example 1. The paint and film of Example 6 were prepared and evaluated. Table 1 shows the measurement results.
［実施例７］
アクリル樹脂をポリエステル樹脂に代え、凝集体片の含有率を３０質量％とした他は、実施例１に準じて実施例７の塗料及び膜を作製し、評価した。表１に測定結果を示す。
[Example 7]
The paint and film of Example 7 were prepared and evaluated according to Example 1 except that the acrylic resin was replaced with a polyester resin and the aggregate content was 30% by mass. Table 1 shows the measurement results.
［実施例８］
アクリル樹脂をフッ素樹脂に代え、凝集体片の含有率を３０質量％とした他は、実施例１に準じて実施例８の塗料及び膜を作製し、評価した。表１に測定結果を示す。
[Example 8]
The paint and film of Example 8 were prepared and evaluated according to Example 1 except that the acrylic resin was replaced with a fluororesin and the content of the aggregate pieces was 30% by mass. Table 1 shows the measurement results.
［比較例１］
凝集体片の含有率を１０質量％とした他は、実施例１に準じて比較例１の塗料及び膜を作製し、評価した。表１に測定結果を示す。
[Comparative Example 1]
The coating material and film of Comparative Example 1 were prepared and evaluated according to Example 1 except that the content of the aggregate pieces was 10% by mass. Table 1 shows the measurement results.
［比較例２］
凝集体片の含有率を５０質量％とした他は、実施例１に準じて比較例２の塗料及び膜を作製し、評価した。表１に測定結果を示す。
[Comparative Example 2]
A coating material and a film of Comparative Example 2 were prepared and evaluated according to Example 1 except that the content of the aggregate pieces was 50% by mass. Table 1 shows the measurement results.
［比較例３］
球形シリカ凝集体Ａを、多孔質状かつ中実の２次粒子径が３μｍの球形シリカ凝集体Ｂに代え、凝集体片の含有率を１０質量％とした他は、実施例１に準じて比較例３の塗料及び膜を作製し、評価した。表１に測定結果を示す。
[Comparative Example 3]
The spherical silica aggregate A was replaced with the spherical silica aggregate B having a porous and solid secondary particle diameter of 3 μm, and the content rate of the aggregate pieces was 10% by mass, according to Example 1. The paint and film of Comparative Example 3 were prepared and evaluated. Table 1 shows the measurement results.
［比較例４］
球形シリカ凝集体Ａを、多孔質状かつ中実の２次粒子径が３μｍの球形シリカ凝集体Ｂに代え、凝集体片の含有率を５０質量％とした他は、実施例１に準じて比較例３の塗料及び膜を作製し、評価した。表１に測定結果を示す。
[Comparative Example 4]
The spherical silica aggregate A was replaced with a spherical silica aggregate B having a porous and solid secondary particle diameter of 3 μm, and the content rate of the aggregate pieces was 50% by mass, according to Example 1. The paint and film of Comparative Example 3 were prepared and evaluated. Table 1 shows the measurement results.
［比較例５］
球形シリカ凝集体Ａを、２次粒子径が９μｍの球形シリカ凝集体Ｄとし、この球形シリカ凝集体Ｄの含有率を３０質量％とした他は、実施例１に準じて比較例５の塗料及び膜を作製し、評価した。表１に測定結果を示す。
[Comparative Example 5]
The coating material of Comparative Example 5 according to Example 1 except that the spherical silica aggregate A was changed to a spherical silica aggregate D having a secondary particle diameter of 9 μm and the content of the spherical silica aggregate D was 30% by mass. And films were prepared and evaluated. Table 1 shows the measurement results.
［比較例６］
球形シリカ凝集体Ａを、粒子径が０．１μｍの球状シリカ粒子Ｅに代え、この球状シリカ粒子Ｅの含有率を３０質量％とした他は、実施例１に準じて比較例６の塗料及び膜を作製し、評価した。表１に測定結果を示す。
[Comparative Example 6]
The coating material of Comparative Example 6 according to Example 1 except that the spherical silica aggregate A was replaced by spherical silica particles E having a particle diameter of 0.1 μm, and the content of the spherical silica particles E was 30% by mass. Membranes were made and evaluated. Table 1 shows the measurement results.
［比較例７］
球形シリカ凝集体Ａを、粒子径が１〜５μｍの不定形の溶融シリカの粉砕品Ｆに代え、この粉砕品Ｆの含有率を３０質量％とした他は、実施例１に準じて比較例７の塗料及び膜を作製し、評価した。表１に測定結果を示す。
[Comparative Example 7]
Comparative Example according to Example 1 except that the spherical silica aggregate A is replaced with an irregular fused silica pulverized product F having a particle size of 1 to 5 μm, and the content of the pulverized product F is 30% by mass. Seven paints and films were made and evaluated. Table 1 shows the measurement results.
［比較例８］
球形シリカ凝集体Ａを、粒子径が３μｍの球状アルミナ粒子Ｇに代え、この球状アルミナ粒子Ｇの含有率を３０質量％とした他は、実施例１に準じて比較例８の塗料及び膜を作製し、評価した。表１に測定結果を示す。
[Comparative Example 8]
The coating material and film of Comparative Example 8 were applied in the same manner as in Example 1 except that the spherical silica aggregate A was replaced with spherical alumina particles G having a particle diameter of 3 μm and the content of the spherical alumina particles G was 30% by mass. Prepared and evaluated. Table 1 shows the measurement results.
［比較例９］
球形シリカ凝集体Ａを、粒子径が０．１μｍの球状チタニア粒子Ｈに代え、この球状チタニア粒子Ｈの含有率を３０質量％とした他は、実施例１に準じて比較例９の塗料及び膜を作製し、評価した。表１に測定結果を示す。
[Comparative Example 9]
The spherical silica agglomerate A was replaced with spherical titania particles H having a particle diameter of 0.1 μm, and the content of the spherical titania particles H was 30% by mass. Membranes were made and evaluated. Table 1 shows the measurement results.
［比較例１０］
球形シリカ凝集体Ａを、粒子径が０．５μｍの多孔質の球状シリカ粒子Ｉに代え、この球状シリカ粒子Ｉの含有率を３０質量％とした他は、実施例１に準じて比較例１０の塗料及び膜を作製し、評価した。表１に測定結果を示す。
[Comparative Example 10]
Comparative Example 10 according to Example 1 except that the spherical silica aggregate A was replaced with porous spherical silica particles I having a particle diameter of 0.5 μm and the content of the spherical silica particles I was 30% by mass. A paint and film were prepared and evaluated. Table 1 shows the measurement results.
表１によれば、実施例１〜８では、塗料中の凝集体片の含有率が２０質量％〜５０質量％の範囲であることから、塗布ムラも無く、膜の表面状態も良好であり、膜のヘーズ値（Ｈｚ）、全光線透過率（Ｔｔ）及び光透過率の波長バラツキも良好であった。 According to Table 1, in Examples 1-8, since the content rate of the aggregate piece in a coating material is the range of 20 mass%-50 mass%, there is no coating nonuniformity and the surface state of a film | membrane is also favorable. Also, the haze value (Hz) of the film, the total light transmittance (Tt), and the wavelength variation of the light transmittance were good.
一方、比較例１〜４では、塗料中の凝集体片の含有率が１０質量％の場合、膜のヘーズ値（Ｈｚ）及び全光線透過率（Ｔｔ）が低く、また、含有率が５０質量％では塗布ムラが生じていた。
比較例５では、塗料中の凝集体が大き過ぎるために、全光線透過率（Ｔｔ）が低下していた。
比較例６では、塗料中の粒子の大きさが小さ過ぎるために、ヘーズ値（Ｈｚ）が低下していた。
On the other hand, in Comparative Examples 1-4, when the content rate of the aggregate piece in a coating material is 10 mass%, the haze value (Hz) and total light transmittance (Tt) of a film | membrane are low, and content rate is 50 mass. In%, coating unevenness occurred.
In Comparative Example 5, the total light transmittance (Tt) was lowered because the aggregates in the paint were too large.
In Comparative Example 6, the haze value (Hz) was lowered because the size of the particles in the paint was too small.
比較例７〜９では、球形シリカ凝集体を、溶融シリカの粉砕品、球状アルミナ粒子または球状チタニア粒子に代えたので、膜のヘーズ値（Ｈｚ）及び全光線透過率（Ｔｔ）が低く、特に球状アルミナ粒子または球状チタニア粒子を用いた場合、全ての特性が低下していた。
比較例１０では、粒子径が０．５μｍの多孔質の球状シリカ粒子を用いたので、膜のヘーズ値（Ｈｚ）及び全光線透過率（Ｔｔ）共に低下していた。
In Comparative Examples 7 to 9, since the spherical silica aggregate was replaced with a ground product of fused silica, spherical alumina particles or spherical titania particles, the haze value (Hz) and total light transmittance (Tt) of the film were low, When spherical alumina particles or spherical titania particles were used, all characteristics were deteriorated.
In Comparative Example 10, since porous spherical silica particles having a particle diameter of 0.5 μm were used, both the haze value (Hz) and the total light transmittance (Tt) of the film were reduced.
１ 球形シリカ凝集体
２ 球形シリカ
３ 中空
１１〜１６ 凝集体片
２１ 球形シリカ凝集体
３１〜３８ 凝集体片
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| JP2008291074A (en) * | 2007-05-23 | 2008-12-04 | Panasonic Corp | Light diffusible resin molded body |
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| JP2008291074A (en) * | 2007-05-23 | 2008-12-04 | Panasonic Corp | Light diffusible resin molded body |
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