JP4696098B2 - Black material, black material dispersion, black light shielding film, and substrate with black light shielding film - Google Patents
Black material, black material dispersion, black light shielding film, and substrate with black light shielding film Download PDFInfo
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- JP4696098B2 JP4696098B2 JP2007194383A JP2007194383A JP4696098B2 JP 4696098 B2 JP4696098 B2 JP 4696098B2 JP 2007194383 A JP2007194383 A JP 2007194383A JP 2007194383 A JP2007194383 A JP 2007194383A JP 4696098 B2 JP4696098 B2 JP 4696098B2
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- Manufacture Of Metal Powder And Suspensions Thereof (AREA)
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Description
本発明は、黒色材料と黒色材料分散液および黒色遮光膜並びに黒色遮光膜付基材に関し、さらに詳しくは、黒色度および光遮蔽性に優れ、しかも安価な黒色材料、この黒色材料を分散媒中に分散させた黒色材料分散液、この黒色材料分散液を用いて作製された黒色遮光膜、および、この黒色遮光膜を備えた黒色遮光膜付基材に関するものである。 The present invention relates to a black material, a black material dispersion, a black light-shielding film, and a substrate with a black light-shielding film. More specifically, the black material is excellent in blackness and light shielding properties and inexpensive, and the black material is dispersed in a dispersion medium. The present invention relates to a black material dispersion liquid dispersed in a black light shielding film, a black light shielding film produced using the black material dispersion liquid, and a substrate with a black light shielding film provided with the black light shielding film.
従来、黒色材料は、黒色光遮蔽性フィルム、黒色光遮蔽性ガラス、プラズマディスプレイ（ＰＤＰ）や液晶ディスプレイ（ＬＣＤ）などのフラットパネルディスプレイ（ＦＰＤ）のブラックマトリックス材料、ブラックシール材、ブラックマスク材などに黒色や光遮蔽性を付与する材料として利用されている。
このような黒色材料として、本発明者等は、先に、銀錫合金微粒子からなる黒色材料を提案している（例えば、特許文献１、２参照）。
この銀錫合金微粒子からなる黒色材料は、可視光線の反射率が低く、黒色度に優れているから、光遮蔽性に優れた黒色遮光膜を形成することができる。
As such a black material, the present inventors have previously proposed a black material made of silver tin alloy fine particles (see, for example, Patent Documents 1 and 2).
Since the black material composed of the silver-tin alloy fine particles has a low visible light reflectivity and excellent blackness, it is possible to form a black light-shielding film having excellent light shielding properties.
しかしながら、上記の銀錫合金微粒子からなる黒色材料にあっても、更なる光遮蔽性の改善が求められていた。 However, even in the case of a black material made of the above-described silver-tin alloy fine particles, further improvement in light shielding properties has been demanded.
本発明は、上記の課題を解決するためになされたものであって、可視光線の反射率が低く、黒色度が高く、かつ、光遮蔽性に優れた黒色材料、この黒色材料を分散媒中に分散させた黒色材料分散液、この黒色材料分散液を用いて作製された黒色遮光膜、および、この黒色遮光膜を備えた黒色遮光膜付基材を提供することを目的とする。 The present invention has been made to solve the above-described problems, and has a low visible light reflectance, a high blackness, and a light shielding property, and a black material in a dispersion medium. It is an object of the present invention to provide a black material dispersion liquid dispersed in a black light shielding film, a black light shielding film produced using the black material dispersion liquid, and a substrate with a black light shielding film provided with the black light shielding film.
本発明者等は、上記の課題を解決するために鋭意研究を行った結果、銀錫合金微粒子と銀微粒子の含有率を調整すれば、黒色度および光遮蔽性に優れた黒色材料が得られることを見出し、本発明を完成するに至った。 As a result of intensive studies to solve the above problems, the present inventors can obtain a black material having excellent blackness and light shielding properties by adjusting the content of silver tin alloy fine particles and silver fine particles. As a result, the present invention has been completed.
すなわち、本発明の黒色材料は、銀錫合金微粒子と銀微粒子からなり、前記銀微粒子の含有率は３０重量％以上かつ９０重量％以下であることを特徴とする。 That is, the black material of the present invention comprises silver tin alloy fine particles and silver fine particles, and the content of the silver fine particles is 30 wt% or more and 90 wt% or less.
本発明の黒色材料では、前記銀微粒子の含有率は５０重量％以上かつ７５重量％以下であることが好ましい。 In the black material of the present invention, the silver fine particle content is preferably 50 wt% or more and 75 wt% or less.
本発明の黒色材料分散液は、本発明の黒色材料を分散媒中に分散してなることを特徴とする。 The black material dispersion of the present invention is characterized in that the black material of the present invention is dispersed in a dispersion medium.
本発明の黒色遮光膜は、本発明の黒色材料分散液を基材の一主面に塗布してなることを特徴とする。 The black light-shielding film of the present invention is characterized in that the black material dispersion of the present invention is applied to one main surface of a substrate.
本発明の黒色遮光膜付基材は、基材の一主面に、請求項４に記載の黒色遮光膜を備えてなることを特徴とする。 The base material with a black light shielding film of the present invention is characterized in that the black light shielding film according to claim 4 is provided on one main surface of the base material.
本発明の黒色材料によれば、銀錫合金微粒子と銀微粒子からなり、前記銀微粒子の含有率は３０重量％以上かつ９０重量％以下であるので、黒色度および光遮蔽性に優れたものとなる。 According to the black material of the present invention, it is composed of silver tin alloy fine particles and silver fine particles, and the content of the silver fine particles is 30% by weight or more and 90% by weight or less. Therefore, the black material has excellent blackness and light shielding properties. Become.
本発明の黒色材料と黒色材料分散液および黒色遮光膜並びに黒色遮光膜付基材の最良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 best mode of the black material, the black material dispersion, the black light shielding film, and the substrate with the black light shielding film of the present invention will be described.
This embodiment is specifically described for better understanding of the gist of the invention, and does not limit the present invention unless otherwise specified.
「黒色材料」
本実施形態の黒色材料は、銀錫合金微粒子と銀微粒子からなり、前記銀微粒子の含有率が３０重量％以上かつ９０重量％以下の材料である。
ここで、銀微粒子の含有率（重量％）は、粉末Ｘ線回折チャートのリートベルト解析を利用して求めたものである。粉末X線回折チャートのリートベルト解析は、黒色材料中の銀錫合金、銀などの理論プロファイルを、粉末Ｘ線回折により得られた実測プロファイルにフィティングすることにより行うものである。この粉末X線回折チャートのリートベルト解析は、市販されている解析ソフトを利用して行うことができる。
"Black material"
The black material of the present embodiment is made of silver tin alloy fine particles and silver fine particles, and the content of the silver fine particles is 30 wt% or more and 90 wt% or less.
Here, the content (% by weight) of the silver fine particles is obtained by using a Rietveld analysis of a powder X-ray diffraction chart. Rietveld analysis of a powder X-ray diffraction chart is performed by fitting a theoretical profile of silver tin alloy, silver, etc. in a black material to an actual measurement profile obtained by powder X-ray diffraction. Rietveld analysis of this powder X-ray diffraction chart can be performed using commercially available analysis software.
銀錫合金微粒子としては、化学式ＡｇｘＳｎにて表した場合、化学的に安定した銀錫合金が得られるｘの範囲は１≦ｘ≦１０であり、さらに、化学的安定性と黒色度が同時に得られるｘの範囲は３≦ｘ≦４である。
この黒色材料では、ｘの範囲は１≦ｘ≦１０の範囲であればよいが、化学的安定性と黒色度を同時に得るためには、ｘの範囲は３≦ｘ≦４であることが好ましい。
As the silver tin alloy fine particles, when expressed by the chemical formula Ag x Sn, the range of x in which a chemically stable silver tin alloy can be obtained is 1 ≦ x ≦ 10, and further, the chemical stability and blackness are The range of x obtained simultaneously is 3 ≦ x ≦ 4.
In this black material, the range of x may be in the range of 1 ≦ x ≦ 10, but in order to obtain chemical stability and blackness at the same time, the range of x is preferably 3 ≦ x ≦ 4. .
また、この黒色材料における銀微粒子の含有率は、３０重量％以上かつ９０重量％以下であり、好ましくは４０重量％以上かつ８０重量％以下であり、より好ましくは５０重量％以上かつ７５重量％以下である。
ここで、銀微粒子の含有率を上記の範囲に限定した理由は、銀微粒子の含有率が３０重量％未満では、十分な光遮蔽性を得ることができないからであり、一方、銀微粒子の含有率が９０重量％を超えると、黒色材料の主成分が実質的に銀微粒子からなり、光の反射率が高くなってしまい、十分な黒色度を有する黒色遮光膜を得ることができないからである。
The content of the silver fine particles in the black material is 30% by weight or more and 90% by weight or less, preferably 40% by weight or more and 80% by weight or less, more preferably 50% by weight or more and 75% by weight. It is as follows.
Here, the reason why the content of the silver fine particles is limited to the above range is that when the content of the silver fine particles is less than 30% by weight, sufficient light shielding properties cannot be obtained. If the ratio exceeds 90% by weight, the main component of the black material is substantially composed of silver fine particles, the light reflectance is increased, and a black light-shielding film having sufficient blackness cannot be obtained. .
また、この黒色材料は、実質的に錫微粒子を含有していない。ここで、実質的に錫微粒子を含有していないとは、Ｘ線回析法により錫の存在が確認されないことを意味する。黒色材料が錫微粒子を含有していると、この黒色材料を用いて形成した黒色遮光膜の光遮蔽性が大幅に低下する。 Further, this black material does not substantially contain tin fine particles. Here, substantially not containing tin fine particles means that the presence of tin is not confirmed by the X-ray diffraction method. When the black material contains tin fine particles, the light shielding property of the black light shielding film formed using the black material is significantly lowered.
この黒色材料の平均一次粒子径は、１ｎｍ以上かつ２００ｎｍ以下が好ましく、より好ましくは１０ｎｍ以上かつ１００ｎｍ以下である。
ここで、平均一次粒子径を上記の範囲に限定した理由は、平均一次粒子径を上記の範囲内とすることで所望の黒色遮光膜を容易に形成することができるからである。すなわち、平均一次粒子径が１ｎｍ未満では、可視光線の波長と比較して小さ過ぎるために透過光量が増加し、所望の黒色度が得られなくなるおそれがあるからであり、一方、平均一次粒子径が２００ｎｍを超えると、黒色遮光膜にて所望の黒色度を得ることが困難になるおそれがあるからである。
The average primary particle diameter of the black material is preferably 1 nm or more and 200 nm or less, more preferably 10 nm or more and 100 nm or less.
Here, the reason why the average primary particle size is limited to the above range is that a desired black light-shielding film can be easily formed by setting the average primary particle size within the above range. That is, if the average primary particle size is less than 1 nm, the amount of transmitted light increases because it is too small compared to the wavelength of visible light, and the desired blackness may not be obtained. If the thickness exceeds 200 nm, it may be difficult to obtain a desired blackness with the black light-shielding film.
この黒色材料の製造方法としては、銀錫合金微粒子と銀微粒子からなり、銀微粒子の含有率が３０重量％以上かつ９０重量％以下の黒色材料が得られる方法であれば特に制限はなく、気相反応法、噴霧熱分解法、アトマイズ法、液相反応法、凍結乾燥法、水熱合成法など、通常の微粒子合成法を用いて作製することができ、これらの方法のなかでも、上記の黒色材料が容易に得られる液相反応法を用いることが好ましい。 The method for producing this black material is not particularly limited as long as it is a method comprising a silver-tin alloy fine particle and a silver fine particle, and a black material having a silver fine particle content of 30 wt% or more and 90 wt% or less. It can be prepared by using usual fine particle synthesis methods such as phase reaction method, spray pyrolysis method, atomization method, liquid phase reaction method, freeze-drying method, hydrothermal synthesis method, and among these methods, It is preferable to use a liquid phase reaction method by which a black material can be easily obtained.
液相反応法の一例としては、例えば、錫コロイド分散液中に銀化合物溶液を滴下し、錫と銀とを合金化させ、銀錫合金微粒子と銀微粒子を生成する方法を例示することができる。
この製造方法にあっては、反応条件（例えば、錫と銀との比率、反応液のｐＨ、反応温度、反応時間など）を適宜調整することにより、銀錫合金微粒子の生成量、銀微粒子の生成量を任意に制御することができる。
As an example of the liquid phase reaction method, for example, a method in which a silver compound solution is dropped into a tin colloid dispersion liquid and tin and silver are alloyed to produce silver tin alloy fine particles and silver fine particles can be exemplified. .
In this production method, by appropriately adjusting the reaction conditions (for example, the ratio of tin and silver, the pH of the reaction solution, the reaction temperature, the reaction time, etc.), the production amount of silver tin alloy fine particles, The production amount can be arbitrarily controlled.
この液相反応法は、液相中での反応により合成が完結するので、黒色材料を回収する必要はなく、容易に黒色材料分散液とすることが可能である。
また、この黒色材料を用いて黒色遮光膜を作製する場合、感光性樹脂との分散性を考慮して、水分散系から有機溶媒分散系に変更してもよい。有機溶媒分散系に変更する場合、液相から回収したケーキ状の凝集物を一旦機械的に粉砕して粉末とし、その後、ボールミル、ビーズミルなどの湿式混合機を用いて有機溶媒中にて分散処理する方法が採られる。
In this liquid phase reaction method, the synthesis is completed by a reaction in the liquid phase, so that it is not necessary to recover the black material, and the black material dispersion can be easily obtained.
Moreover, when producing a black light shielding film using this black material, in consideration of dispersibility with the photosensitive resin, the water dispersion system may be changed to an organic solvent dispersion system. When changing to an organic solvent dispersion system, cake-like agglomerates collected from the liquid phase are temporarily pulverized into powder, and then dispersed in an organic solvent using a wet mixer such as a ball mill or bead mill. The method to do is taken.
「黒色材料分散液」
本実施形態の黒色材料分散液は、本実施形態の黒色材料を分散媒中に分散した分散液である。
この分散液における黒色材料の含有率は、１重量％以上かつ８０重量％以下が好ましく、より好ましくは５重量％以上かつ５０重量％以下、さらに好ましくは１０重量％以上かつ４０重量％以下である。
ここで、黒色材料の含有率を１重量％以上かつ８０重量％以下と限定した理由は、この範囲は黒色材料が良好な分散状態を取りうる範囲であるからである。また、黒色材料の含有率が１重量％未満では、黒色材料としての効果が低下し、一方、８０重量％を超えると、黒色材料の濃度が高くなり過ぎてペースト状態となり、分散液としての特徴を消失するからである。
"Black material dispersion"
The black material dispersion of this embodiment is a dispersion in which the black material of this embodiment is dispersed in a dispersion medium.
The content of the black material in this dispersion is preferably 1% by weight or more and 80% by weight or less, more preferably 5% by weight or more and 50% by weight or less, and further preferably 10% by weight or more and 40% by weight or less. .
Here, the reason why the content of the black material is limited to 1 wt% or more and 80 wt% or less is that this range is a range in which the black material can take a good dispersion state. Further, when the content of the black material is less than 1% by weight, the effect as the black material is reduced. On the other hand, when the content exceeds 80% by weight, the concentration of the black material becomes too high to be in a paste state, and the characteristics as a dispersion liquid Because it disappears.
分散媒は、基本的には、水、有機溶媒、樹脂成分のうち少なくとも１種以上を含有したものである。
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、オクタノールなどのアルコール類；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−ブチロラクトンなどのエステル類；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などのエーテル類；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、シクロヘキサノンなどのケトン類；ベンゼン、トルエン、キシレン、エチルベンゼンなどの芳香族炭化水素；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−メチルピロリドンなどのアミド類が好適に用いられ、これらの溶媒のうち１種または２種以上を用いることができる。
The dispersion medium basically contains at least one of water, an organic solvent, and a resin component.
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 Any ketones; aromatic hydrocarbons such as benzene, toluene, xylene, and ethylbenzene; amides such as dimethylformamide, N, N-dimethylacetoacetamide, and N-methylpyrrolidone are preferably used, and one of these solvents Or 2 or more types can be used.
上記の樹脂成分としては、電離放射線硬化型樹脂が用いられ、例えば、アクリル酸メチル、メタクリル酸メチルなど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などの紫外線硬化型モノマー；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などの紫外線硬化型樹脂オリゴマーが好適に用いられる。
また、樹脂成分としては、フェノール樹脂、エポキシ樹脂、メラミン樹脂、尿素樹脂、ポリエステル樹脂、アルキド樹脂、ポリウレタンなどの熱硬化型樹脂；ポリビニルピロリドン、ポリビニルアルコールなどのバインダー樹脂が好適に用いられる。
As the above resin component, ionizing radiation curable resins are used, for example, acrylic or methacrylic monomers such as methyl acrylate and methyl methacrylate, ultraviolet curable monomers such as epoxy monomers; urethane acrylate oligomers, UV curable resin oligomers such as epoxy acrylate oligomers and acrylate oligomers are preferably used.
As the resin component, thermosetting resins such as phenol resin, epoxy resin, melamine resin, urea resin, polyester resin, alkyd resin, and polyurethane; binder resin such as polyvinyl pyrrolidone and polyvinyl alcohol are preferably used.
「黒色遮光膜および黒色遮光膜付き基材」
本実施形態の黒色遮光膜は、本実施形態の黒色材料分散液を基材の一主面上に塗布してなる黒色の膜である。
本実施形態の黒色遮光膜付基材は、基材の表面（一主面）に、本実施形態の黒色遮光膜を備えたものである。
"Black light shielding film and base material with black light shielding film"
The black light-shielding film of this embodiment is a black film formed by applying the black material dispersion liquid of this embodiment on one main surface of the substrate.
The base material with a black light shielding film of the present embodiment is provided with the black light shielding film of the present embodiment on the surface (one main surface) of the base material.
本実施形態の黒色遮光膜は、上記の黒色材料分散液を基材の一主面上に、各種塗布法により塗布して塗膜を形成し、例えば、この塗膜を硬化処理することにより、容易に得ることができる。
この硬化処理としては、上記の分散媒として電離放射線硬化型樹脂を用いる場合、紫外線、電子線、Ｘ線などの放射線の照射（放射線の照射後、必要に応じて熱処理を施してもよい。）が挙げられ、上記の分散媒として熱硬化型樹脂やバインダー樹脂を用いる場合、熱処理が挙げられる。
放射線の照射量は、電離放射線硬化型樹脂が十分に硬化するために十分な量とするが、通常、２０ｍＪ／ｃｍ２〜１０００ｍＪ／ｃｍ２とする。
熱処理の温度としては、基材が耐え得る温度であれば特に制限されず、例えば、大気雰囲気中、８０℃〜３００℃の範囲の温度にて３分〜１２０分程度の熱処理を例示することができる。
The black light-shielding film of this embodiment is formed by applying the above black material dispersion on one main surface of the substrate by various application methods to form a coating film, for example, by curing the coating film, Can be easily obtained.
In this curing treatment, when an ionizing radiation curable resin is used as the dispersion medium, irradiation with radiation such as ultraviolet rays, electron beams, and X-rays (heat treatment may be performed as necessary after radiation irradiation). In the case where a thermosetting resin or a binder resin is used as the dispersion medium, a heat treatment may be mentioned.
The dose of radiation is an amount sufficient to ionizing radiation curable resin is cured sufficiently, usually with 20mJ / cm 2 ~1000mJ / cm 2 .
The temperature of the heat treatment is not particularly limited as long as the substrate can withstand the temperature. For example, the heat treatment may be performed in an air atmosphere at a temperature in the range of 80 ° C. to 300 ° C. for about 3 minutes to 120 minutes. it can.
この黒色遮光膜は、銀錫合金微粒子と銀微粒子からなり、銀微粒子の含有率は３０重量％以上かつ９０重量％以下である黒色材料を含む分散液を塗布したものであるので、黒色度および光遮蔽性に優れたものとなる。
この黒色遮光膜をガラス基板などの基材上に形成することにより、容易に黒色遮光膜付基板を得ることができる。
This black light-shielding film is composed of silver tin alloy fine particles and silver fine particles, and a dispersion containing a black material having a silver fine particle content of 30 wt% or more and 90 wt% or less is applied. Excellent light shielding properties.
By forming this black light-shielding film on a substrate such as a glass substrate, a substrate with a black light-shielding film can be easily obtained.
以下、実施例および比較例により本発明をさらに具体的に説明するが、本発明はこれらの実施例に限定されるものではない。 EXAMPLES Hereinafter, although an Example and a comparative example demonstrate this invention further more concretely, this invention is not limited to these Examples.
「実施例１」
錫コロイド分散液（平均一次粒子径２０ｎｍ、固形分１０重量％、住友大阪セメント製）を１０．０ｇ分取し、これに純水を加えて３００ｍｌのＡ液を作製した。
また、純水に、ぶどう糖２３．０ｇと、酒石酸２．０ｇと、エタノール４０．０ｇとを加え、全重量が５００ｇのＢ液を作製した。
さらに、純水に、硝酸銀１５．０ｇと、濃アンモニア水（ＮＨ３濃度：２８重量％）を５０．０ｍｌ加え、全重量が５００ｇのＣ液を作製した。
"Example 1"
10.0 g of a tin colloid dispersion (average primary particle size 20 nm, solid content 10% by weight, manufactured by Sumitomo Osaka Cement) was collected, and pure water was added thereto to prepare 300 ml of Liquid A.
In addition, 23.0 g of glucose, 2.0 g of tartaric acid, and 40.0 g of ethanol were added to pure water to prepare a liquid B having a total weight of 500 g.
Further, 15.0 g of silver nitrate and 50.0 ml of concentrated aqueous ammonia (NH 3 concentration: 28% by weight) were added to pure water to prepare a liquid C having a total weight of 500 g.
次いで、Ｂ液とＣ液を混合してＤ液とし、このＤ液より５０．０ｇを分取し、これをＡ液に加え、この混合溶液を攪拌しながら、この混合溶液に０．０５Ｎの水酸化ナトリウム水溶液１０ｇをゆっくり滴下し、さらに、１０重量％の酒石酸水溶液６０．０ｇ加えた。
次いで、この混合溶液を、マグネチックスターラーを用いて１時間攪拌し、その後、遠心分離により洗浄を行い、粒子（固形分）濃度が１５重量％の分散液を得た。
Next, liquid B and liquid C are mixed to form liquid D, and 50.0 g is taken from liquid D, added to liquid A, and the mixed solution is stirred to add 0.05 N. Sodium hydroxide aqueous solution 10g was dripped slowly, and also 60.0g of 10 weight% tartaric acid aqueous solution was added.
Next, this mixed solution was stirred for 1 hour using a magnetic stirrer, and then washed by centrifugation to obtain a dispersion having a particle (solid content) concentration of 15% by weight.
また、この分散液を濾過して粒子を分離し、この粒子を乾燥させて粉末試料を作製し、この粉末試料中の生成相を粉末Ｘ線回折法により同定したところ、銀錫合金（Ａｇ３Ｓｎ、Ａｇ４Ｓｎ）、銀の存在が確認された。
さらに、この粉末試料中の銀錫合金、銀の含有率（重量％）を、リートベルト解析法により求めた。
これらの結果を表１に示す。
Further, the dispersion was filtered to separate particles, and the particles were dried to produce a powder sample. When the produced phase in the powder sample was identified by a powder X-ray diffraction method, a silver tin alloy (Ag 3 Sn, Ag 4 Sn), and the presence of silver were confirmed.
Furthermore, the silver tin alloy and silver content (% by weight) in the powder sample were determined by Rietveld analysis.
These results are shown in Table 1.
次いで、この分散液に、粒子（固形分）とポリビニルピロドリン（ＰＶＰ）の体積比が２５：７５となるようにポリビニルピロドリン（ＰＶＰ）水溶液を添加し、超音波分散機（ソニファイアー４５０、ＢＲＡＮＳＯＮ ＵＬＴＲＡＳＯＮＩＣ社製）により分散処理し、１時間放置して実施例１の分散液（塗布液）を得た。 Next, an aqueous polyvinyl pyrodrine (PVP) solution was added to this dispersion so that the volume ratio of particles (solid content) to polyvinyl pyrodrine (PVP) was 25:75, and an ultrasonic disperser (Sonifier 450, A dispersion (coating solution) of Example 1 was obtained by dispersing with BRANSON ULTRASONIC and leaving it for 1 hour.
次いで、この実施例１の分散液（塗布液）を用いて、厚み１．１ｍｍの大きさのガラス基板上にスピンコート法により塗膜を形成した。
次いで、乾燥機を用いて、２４０℃にて１時間熱処理し、実施例１の黒色遮光膜付基材を作製した。
Next, a coating film was formed by spin coating on a glass substrate having a thickness of 1.1 mm using the dispersion liquid (coating liquid) of Example 1.
Subsequently, it heat-processed at 240 degreeC for 1 hour using the dryer, and produced the base material with a black light shielding film of Example 1. FIG.
次いで、この黒色遮蔽膜の光遮蔽性を評価した。
まず、黒色遮光膜の光学濃度（ＯＤ値）を、反射透過濃度計（マクベス濃度計）を用いて測定した。
また、黒色遮光膜の膜厚を、膜厚測定器テンコール（テンコール社製）により測定し、５００ｎｍの波長の光に対する黒色遮光膜自体の反射率を分光スペクトロメーターにより測定した。
これらの測定結果を表１に示す。
Subsequently, the light shielding property of this black shielding film was evaluated.
First, the optical density (OD value) of the black light shielding film was measured using a reflection transmission densitometer (Macbeth densitometer).
Moreover, the film thickness of the black light-shielding film was measured with a film thickness meter Tencor (manufactured by Tencor), and the reflectance of the black light-shielding film itself with respect to light having a wavelength of 500 nm was measured with a spectrophotometer.
These measurement results are shown in Table 1.
「実施例２」
錫コロイド分散液（平均一次粒子径３０ｎｍ、固形分１０重量％、住友大阪セメント製）を用いた以外は、実施例１と同様にして分散液を作製した。
また、この分散液を濾過して粒子を分離し、この粒子を乾燥させて粉末試料を作製し、実施例１と同様にして、この粉末試料中の生成相を粉末Ｘ線回折法により同定したところ、銀錫合金（Ａｇ３Ｓｎ、Ａｇ４Ｓｎ）、銀の存在が確認された。
さらに、この粉末試料中の銀錫合金、銀の含有率（重量％）を、リートベルト解析法により求めた。
これらの結果を表１に示す。
"Example 2"
A dispersion was prepared in the same manner as in Example 1 except that a tin colloid dispersion (average primary particle size 30 nm, solid content 10% by weight, manufactured by Sumitomo Osaka Cement) was used.
The dispersion was filtered to separate the particles, and the particles were dried to prepare a powder sample. In the same manner as in Example 1, the product phase in the powder sample was identified by the powder X-ray diffraction method. However, the presence of silver tin alloys (Ag 3 Sn, Ag 4 Sn) and silver was confirmed.
Furthermore, the silver tin alloy and silver content (% by weight) in the powder sample were determined by Rietveld analysis.
These results are shown in Table 1.
次いで、この分散液を用い、実施例１と同様にして、ポリビニルピロドリン（ＰＶＰ）を添加して実施例２の分散液（塗布液）を得た。
また、この実施例２の分散液（塗布液）を用いた以外は、実施例１と同様にして黒色遮光膜を作製し、この黒色遮光膜について、実施例１と同様にして評価した。
これらの結果を表１に示す。
Next, using this dispersion, polyvinyl pyrodrine (PVP) was added in the same manner as in Example 1 to obtain a dispersion (coating liquid) of Example 2.
Further, a black light-shielding film was produced in the same manner as in Example 1 except that the dispersion liquid (coating liquid) of Example 2 was used, and this black light-shielding film was evaluated in the same manner as in Example 1.
These results are shown in Table 1.
「比較例１」
錫コロイド分散液（平均一次粒子径３０ｎｍ、固形分１０重量％、住友大阪セメント製）を１０．０ｇ分取し、これに純水を加えて３００ｍｌのＦ液を作製した。
次いで、実施例１で作製したＢ液とＣ液を混合しＤ液とし、このＤ液より５０．０ｇを分取し、これをＦ液に加え、この混合溶液を攪拌しながら、０．０５Nの水酸化ナトリウム水溶液１０ｇをゆっくり滴下した。
次いで、この混合溶液を、マグネチックスターラーを用いて１時間攪拌し、その後遠心分離により洗浄を行い、粒子（固形分）濃度が１５重量％の分散液を得た。
"Comparative Example 1"
10.0 g of a tin colloid dispersion (average primary particle size 30 nm, solid content 10% by weight, manufactured by Sumitomo Osaka Cement) was taken, and pure water was added thereto to prepare 300 ml of F solution.
Next, the B liquid and the C liquid prepared in Example 1 were mixed to obtain a D liquid, and 50.0 g was separated from the D liquid, and this was added to the F liquid. Of sodium hydroxide was slowly added dropwise.
Subsequently, this mixed solution was stirred for 1 hour using a magnetic stirrer, and then washed by centrifugation to obtain a dispersion having a particle (solid content) concentration of 15% by weight.
また、この分散液を濾過して粒子を分離し、この粒子を乾燥させて粉末試料を作製し、実施例１と同様にして、この粉末試料中の生成相を粉末Ｘ線回折法により同定したところ、銀錫合金（Ａｇ３Ｓｎ、Ａｇ４Ｓｎ）、銀、錫の存在が確認された。
さらに、この粉末試料中の銀錫合金、銀の含有率（重量％）を、リートベルト解析法により求めた。
これらの結果を表１に示す。
The dispersion was filtered to separate the particles, and the particles were dried to prepare a powder sample. In the same manner as in Example 1, the product phase in the powder sample was identified by the powder X-ray diffraction method. However, the presence of silver tin alloy (Ag 3 Sn, Ag 4 Sn), silver and tin was confirmed.
Furthermore, the silver tin alloy and silver content (% by weight) in the powder sample were determined by Rietveld analysis.
These results are shown in Table 1.
次いで、この分散液を用い、実施例１と同様にして、ポリビニルピロドリン（ＰＶＰ）を添加して比較例１の分散液（塗布液）を得た。
また、この比較例１の分散液（塗布液）を用いた以外は、実施例１と同様にして黒色遮光膜を作製し、この黒色遮光膜について、実施例１と同様にして評価した。
これらの結果を表１に示す。
Next, using this dispersion, polyvinyl pyrodrine (PVP) was added in the same manner as in Example 1 to obtain a dispersion (coating solution) of Comparative Example 1.
Further, a black light-shielding film was produced in the same manner as in Example 1 except that the dispersion liquid (coating liquid) of Comparative Example 1 was used, and this black light-shielding film was evaluated in the same manner as in Example 1.
These results are shown in Table 1.
「比較例２」
６０℃に保温した純水３００ｍｌに、錫コロイド分散液（平均一次粒子径：５０ｎｍ、固形分：２０重量％、住友大阪セメント製）１５ｇと、銀コロイド分散液（平均一次粒子径：１０ｎｍ、固形分：２０重量％、住友大阪セメント製）６０ｇを加え、このコロイド分散液を６０℃に保持して６０分間攪拌した後、超音波を５分間照射した。
次いで、このコロイド分散液を遠心分離により濃縮し、固形分濃度が１５重量％の分散液を得た。
"Comparative Example 2"
In 300 ml of pure water kept at 60 ° C., 15 g of a tin colloid dispersion (average primary particle size: 50 nm, solid content: 20 wt%, manufactured by Sumitomo Osaka Cement) and a silver colloid dispersion (average primary particle size: 10 nm, solid) (Min: 20% by weight, manufactured by Sumitomo Osaka Cement) 60 g was added, and the colloidal dispersion was kept at 60 ° C. and stirred for 60 minutes, followed by irradiation with ultrasonic waves for 5 minutes.
Next, the colloidal dispersion was concentrated by centrifugation to obtain a dispersion having a solid concentration of 15% by weight.
また、この分散液を濾過して粒子を分離し、この粒子を乾燥させて粉末試料を作製し、実施例１と同様にして、この粉末試料中の生成相を粉末Ｘ線回折法により同定したところ銀錫合金（Ａｇ３Ｓｎ、Ａｇ４Ｓｎ）、銀の存在が確認された。
さらに、この粉末試料中の銀錫合金、銀の含有率（重量％）を、リートベルト解析法により求めた。
これらの結果を表１に示す。
The dispersion was filtered to separate the particles, and the particles were dried to prepare a powder sample. In the same manner as in Example 1, the product phase in the powder sample was identified by the powder X-ray diffraction method. However, the presence of silver tin alloys (Ag 3 Sn, Ag 4 Sn) and silver was confirmed.
Furthermore, the silver tin alloy and silver content (% by weight) in the powder sample were determined by Rietveld analysis.
These results are shown in Table 1.
次いで、この分散液を用い、実施例１と同様にして、ポリビニルピロドリン（ＰＶＰ）を添加して比較例２の分散液（塗布液）を得た。
また、この比較例２の分散液（塗布液）を用いた以外は、実施例１と同様にして黒色遮光膜を作製し、この黒色遮光膜について、実施例１と同様にして評価した。
これらの結果を表１に示す。
Subsequently, using this dispersion, polyvinyl pyrodrine (PVP) was added in the same manner as in Example 1 to obtain a dispersion (coating solution) of Comparative Example 2.
Further, a black light-shielding film was produced in the same manner as in Example 1 except that the dispersion liquid (coating liquid) of Comparative Example 2 was used, and this black light-shielding film was evaluated in the same manner as in Example 1.
These results are shown in Table 1.
表１の結果から、実施例１、２の黒色遮光膜は、反射率が小さいことから黒色度に優れ、また、光学濃度（ＯＤ）が大きいことから光遮蔽性に優れることが分かった。
一方、比較例１、２の黒色遮光膜は、実施例１、２の黒色遮光膜に比較して、光学濃度（ＯＤ）が小さいことから光遮蔽性に劣ることが分かった。
From the results in Table 1, it was found that the black light-shielding films of Examples 1 and 2 were excellent in blackness due to their low reflectance, and excellent in light shielding properties because of their high optical density (OD).
On the other hand, it was found that the black light-shielding films of Comparative Examples 1 and 2 were inferior in light shielding properties because the optical density (OD) was small compared to the black light-shielding films of Examples 1 and 2.
本発明の黒色材料は、可視光線の反射率が低く、黒色度が高く、光遮蔽性に優れているので、黒色光遮蔽性フィルム、黒色光遮蔽性ガラス、プラズマディスプレイ（ＰＤＰ）や液晶ディスプレイ（ＬＣＤ）などのフラットパネルディスプレイ（ＦＰＤ）向けのブラックマトリックス材料、ブラックシール材、ブラックマスク材などに、黒色や光遮蔽性を付与する材料として好適に利用することができるので、産業上の利用可能性は極めて大きい。
The black material of the present invention has low visible light reflectance, high blackness, and excellent light shielding properties. Therefore, a black light shielding film, black light shielding glass, a plasma display (PDP) and a liquid crystal display ( It can be used as a black matrix material, black seal material, black mask material, etc. for flat panel displays (FPD) such as LCDs, as a material that imparts black color and light shielding properties. The nature is extremely large.
Claims (5)
A base material with a black light-shielding film, comprising the black light-shielding film according to claim 4 on one main surface of the base material.
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| JP2012167194A (en) * | 2011-02-15 | 2012-09-06 | Sumitomo Osaka Cement Co Ltd | Black material, black material dispersed liquid, black resin composition, black film, and base material coated with the black film |
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