JP2009514027A - 放射線回折着色剤 - Google Patents
放射線回折着色剤 Download PDFInfo
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Abstract
Description
本発明は、コア−シェル粒子から製造されるブラッグ回折着色剤に関する。
角度依存性(goniochromaticity)は、放射線または観察の角度の変化に応じて変化する知覚色の効果である。例えば、自動車のコーティング、装飾コーティング、プラスチック染色、印刷インク(特に安全インク)、織物及び化粧品では、角度依存性顔料が使用されている。その光学的効果は、主にシート様である粒子(従来、金属性シート様粒子であるか、または構造化された屈折率コントラストを有し、その長さスケールが光の波長に匹敵するシート様粒子)からの光の指向性反射に起因する。顔料粒子の性質によって、該顔料は、金属効果顔料(例えば、アルミニウム、亜鉛、銅またはそれらの合金)または干渉顔料(例えば、白雲母、金雲母及び黒雲母等の二酸化チタンコーティング雲母系)として知られている。
本発明は、ポリマーマトリクス中に保持される粒子の規則正しい周期的配列を含む放射線回折材料であって、前記粒子がそれぞれ、前記マトリクスとは異なる、非皮膜形成組成物のシェルに囲まれたコアを含む、放射線回折材料に関する。
基板上にコア−シェル粒子の分散物を適用する手順であって、前記コアが実質的に非膨潤性であり、前記シェルが非皮膜形成性である、手順;
前記粒子を、放射線を回折する規則正しい周期的配列に配置する手順;
前記粒子の配列にマトリクス組成物をコーティングする手順;
前記マトリクスの成分を前記シェルに分散させることによって前記シェルを膨潤させる手順;並びに
前記粒子のコーティングされた配列を固定する手順、
を含む、方法に関する。
規則正しい周期的配列を形成するコア−シェル粒子の分散物を受容する基板であって、前記シェルが膨潤性であり、実質的に非皮膜形成性である、基板;
前記配列にマトリクス組成物をコーティングするためのマトリクス供給装置;
前記コーティングされた配列を照射するための放射線源;
前記コーティングされた配列によって回折される放射線のスペクトルを測定するための放射線検出器;並びに
前記コーティングされた配列中の成分を硬化し、前記粒子の相対的な位置を固定するための硬化システム、
を備える、システムに関する。
本発明は、マトリクス内に固定されたコア−シェル粒子の規則正しい周期的配列を含み、シェル材料が非皮膜形成性であり、マトリクス材料と異なる放射線回折材料を提供する。本材料は、他の形状の中でも着色剤として粒子形状で使用するのに適している。放射線回折材料は、あらゆる波長の電磁放射線を回折する材料を指すが、本明細書で使用される「着色剤」という用語は、可視スペクトル内で放射線を回折する放射線回折材料を指す。
mλ=2ndsinθ
(式中、(m)は整数であり、(n)は配列の有効屈折率であり、(d)は粒子の層間の距離である)。有効屈折率(n)は、粒子の材料の屈折率の体積平均に近似している。一般的に球形の粒子の場合、寸法(d)は各層の粒子の中心面間の距離であり、粒子の直径に比例する。このような場合、反射する波長λも、粒子直径に比例する。
有機ポリマーマトリクス
以下の手順によって、紫外線照射硬化有機組成物を調製した。Aldrich Chemical Company, Inc.(米国ウィスコンシン州ミルウォーキー)から得た、615gのエチルアルコール中のジフェニル(2,4,6−トリメチルベンゾイル)ホスフィンオキシド/2−ヒドロキシ−2−メチル−プロピオフェノン(22.6g)の50/50配合物を、撹拌しながら、全てSartomer Company, Inc.(米国ペンシルバニア州エクストン)から得た、549gのプロポキシル化(3)グリセリルトリアシレート,105.3gのペンタエリスリトールテトラアクリレート、及び97.8gのエトキシル化(5)ペンタエリスリトールテトラアクリレートに加え、硬化性有機マトリクス組成物を調製した。
有機コア−シェル粒子
水中のポリスチレン−ジビニルベンゼンコア/スチレン−メチルメタクリレート−エチレングリコールジメタクリレート−ジビニルベンゼンシェル粒子の分散物を、以下の手順により調製した。4.9gの、Aldrich Chemical Company製の重炭酸水素ナトリウムを4090gの脱イオン水と混合し、熱電温度計、加熱マントル、攪拌機、還流冷却器及び窒素の注入口を備えた12リットルのフラスコに加えた。撹拌しながら、混合物に窒素を40分間分散させ、次いで、窒素で覆った。Cytec Industries, Inc.製の界面活性剤Aerosol MA80−I(410gの脱イオン水中に46.0g)を撹拌しながら混合物に加え、次いで、48gの脱イオン水で洗浄した。混合物を、加熱マントルを使用して約50℃まで加熱した。Aldrich Chemical Company, Inc.から入手できるスチレン単量体(832.8g)を撹拌しながら加えた。混合物を60℃に加熱した。Aldrich Chemical Company, Inc.製の過硫酸ナトリウム(144gの脱イオン水中に12.5g)を、撹拌しながら混合物に加えた。混合物の温度を40分間一定に維持した。撹拌下、Aldrich Chemical Company, Inc.製のジビニルベンゼン205.4gを混合物に加え、温度を約60℃に2.25時間維持した。Aldrich Chemical Company, Inc.製の過硫酸ナトリウム(86.4gの脱イオン水中に9.1g)を撹拌しながら混合物に加えた。全て、Aldrich Chemical Company, Inc.から入手できる、スチレン(200g)、メタクリル酸メチル(478.8g)、エチレングリコールジメタクリレート(48g)及びジビニルベンゼン(30.2g)の混合物を、撹拌しながら混合物に加えた。Rhodia, Inc.(米国ニュージャージー州クランベリー)製の界面活性剤Sipomer COPS−1(3−アリルオキシ−2−ヒドロキシ−1−プロパンスルホン酸、82.7g)を、撹拌しながら反応混合物に加えた。混合物の温度を60℃に4時間維持した。得られたポリマー分散物を5ミクロンのフィルターバッグでろ過した。次いで、ポリマー分散物を、2.41インチのフッ化ポリビニリデン膜を有する4インチの限外ろ過ハウジング(両方ともPTI Advanced Filtration, Inc.[米国カリフォルニア州オックスナード]製)を使用して限外ろ過し、蠕動ポンプを使用して、約170mL/秒の流速でろ液をくみ上げた。3000gの限外ろ過したろ液を除去した後、分散物に脱イオン水(3000g)を加えた。10023gの限外ろ過したろ液が10037gの脱イオン水と置換されるまで、この交換を数回繰り返した。次いで、混合物の固体含有量が45重量%になるまで、さらに限外ろ過したろ液を除去した。
基板上の粒子
Frontier Industrial Technology, Inc.(米国ペンシルバニア州トワンダ)製のスロットダイコーターにより、実施例2で調製された材料(1575g)を、ポリエチレンテレフタレート基板に適用し、180°Fで30秒間乾燥し、約3.5ミクロン厚さの多孔質乾燥物とした。Varian Inc.のCary500分光光度計を使用して測定した時、得られた蒸着粒子は541nmで光を回折した。粒子は、ポリエチレンテレフタレート基板に緩く蒸着し、軽く触れると容易に拭き取られた。
粒子の充填
実施例1で調製された硬化性有機マトリクス組成物(1389g)を、Frontier Industrial Technology, Inc.のスロットダイコーターを使用して、実施例3で調製したポリエチレンテレフタレート基板上の多孔性の乾燥した粒子の間質腔に適用した。適用後、120°Fのオーブン中で、表1に示す時間、サンプルを乾燥させ、次いで100Wの水銀ランプを使用して紫外線硬化させた。観察者に対して0°または平行に見た場合、得られた柔軟で透明な皮膜は赤色を有していた。観察者に対して45°以上で見た時、同じ皮膜はオレンジ色〜緑色であった。Varian, Inc.のCary500分光光度計を使用して皮膜を測定し、表2に示す光を回折した。
薄片への粉砕
実施例4で調製した材料を、50/50の脱イオン水及びイソプロピルアルコールの混合物で2回洗浄した。次いで、Exair Corporation(米国オハイオ州シンシナティ)製のエアーナイフアセンブリを使用して、ポリエチレンテレフタレート基板から材料をはがした。減圧により、材料を収集袋中に収集した。次いで、はがした材料をRetsch GmbH & Co.(ドイツ ハーン)の超遠心ミルを使用して、粉末に砕いた。Fisher Scientific International, Inc.の38ミクロン及び25ミクロンのステンレス鋼のふるいを通した。25ミクロンのふるい中の材料を粉末として集めた。
コア−シェル粒子を有する着色剤を含むコーティング組成物
実施例6の粉末を、皮膜形成結合剤及び希釈剤の最初の成分を含む容器に加えた。容器にふたをし、1分間手動で振盪させた。振盪後、容器を開け、架橋剤を加えた。容器に再びふたをし、1分間手で振盪させた。表3に示す組成物を有する、得られたコーティング組成物を、噴霧適用用に準備した。
2DT870、PPG Industries, Inc.から入手できる薄め液。
3DCX61、PPG Industries, Inc.から入手できる架橋剤。
Claims (28)
- ポリマーマトリクス中に保持される粒子の規則正しい周期的配列を含む放射線回折材料であって、
前記粒子がそれぞれ、前記マトリクスとは異なる、非皮膜形成組成物のシェルに囲まれたコアを含む、放射線回折材料。 - 前記コアの屈折率が前記シェルの屈折率と異なる、請求項1に記載の放射線回折材料。
- 前記シェルが、前記シェルの厚さ全体にわたり屈折率の勾配を有する、請求項2に記載の放射線回折材料。
- 前記マトリクスが架橋性単量体から製造され、前記単量体が、前記シェルの厚さ全体にわたる濃度勾配を有して前記シェル中に存在する、請求項3に記載の放射線回折材料。
- 前記シェルが前記マトリクスポリマーの単量体によって膨潤性であり、前記コアが実質的に非膨潤性である、請求項4に記載の放射線回折材料。
- 前記マトリクス及び前記シェルがそれぞれ、互いに異なるポリマー材料を含み、前記ポリマー材料が、ポリスチレン、ポリウレタン、アクリルポリマー、アルキドポリマー、ポリエステル、シロキサン含有ポリマー、ポリスルフィド、エポキシ含有ポリマー、及び/またはエポキシ含有ポリマー由来のポリマーを含む、請求項1に記載の放射線回折材料。
- 前記粒子コアが、ポリスチレン、ポリウレタン、アクリルポリマー、アルキドポリマー、ポリエステル、シロキサン含有ポリマー、ポリスルフィド、エポキシ含有ポリマー、エポキシ含有ポリマー由来のポリマー、金属酸化物、及び/または無機ポリマーを含むポリマー材料を含む、請求項2に記載の放射線回折材料。
- 前記コアの直径が、全粒子直径の80〜90%である、請求項1に記載の放射線回折材料。
- 前記配列が、2〜100のアスペクト比を有する粒子形状である、請求項1に記載の放射線回折材料。
- 前記放射線回折材料がシートの形状である、請求項1に記載の放射線回折材料。
- 前記放射線回折材料が粒子形状である、請求項1に記載の放射線回折材料。
- 樹脂結合剤及び請求項11に記載の放射線回折材料を含む、着色組成物。
- 着色組成物を製造する方法であって、
請求項1に記載の放射線回折材料を含む着色剤を準備する手順;
前記シェルと前記コアとの間の屈折率に差が出るように前記シェルの組成物を変質させ、それによって前記着色剤によって示される色の強度を選択する手順;及び
樹脂結合剤中に前記着色剤を分散させる手順、
を含む、方法。 - 前記シェルの前記組成物を変質させる前記手順が、ポリマーマトリクス由来の単量体が、前記シェルの前記厚さ全体にわたる勾配で分散できるようにし、それによって前記シェルを膨潤させることを含む、請求項13に記載の方法。
- 前記シェルの前記組成物を変質させる前記手順が、前記ポリマーマトリクス由来の溶媒が、前記シェルに分散できるようにし、それによって前記シェルを膨潤させる、請求項13に記載の方法。
- 前記シェルに分散した前記マトリクス単量体を架橋させ、前記シェルの直径を固定する手順も更に含む、請求項14に記載の方法。
- 放射線回折材料を製造する方法であって、
基板上にコア−シェル粒子の分散物を適用する手順であって、前記コアが実質的に非膨潤性であり、前記シェルが非皮膜形成性である、手順;
前記粒子を、放射線を回折する規則正しい周期的配列に配置する手順;
前記粒子の配列にマトリクス組成物をコーティングする手順;
前記マトリクスの成分を前記シェルに分散させることによって前記シェルを膨潤させる手順;並びに
前記粒子のコーティングされた配列を固定する手順、
を含む、方法。 - 前記分散したマトリクスが架橋性単量体を含む、請求項17に記載の方法。
- 前記分散したマトリクスが溶媒を含む、請求項17に記載の方法。
- 前記膨潤手順が、前記シェルの前記厚さ全体にわたる屈折率の勾配を形成する、請求項17に記載の方法。
- 前記膨潤手順が、前記配列の回折波長を測定し、前記シェルの膨潤度を調整して前記配列の所望の回折波長を実現することも更に含む、請求項17に記載の方法。
- 前記基板から前記固定した配列を除去し、前記固定した配列を粒子形状に微粉砕することも更に含む、請求項17に記載の方法。
- 請求項17に記載の方法に従って製造された、放射線回折材料。
- 放射線回折材料を製造するためのシステムであって、
規則正しい周期的配列を形成するコア−シェル粒子の分散物を受容する基板であって、前記シェルが膨潤性であり、実質的に非皮膜形成性である、基板;
前記配列にマトリクス組成物をコーティングするためのマトリクス供給装置;
前記コーティングされた配列を照射するための放射線源;
前記コーティングされた配列によって回折される放射線のスペクトルを測定するための放射線検出器;並びに
前記コーティングされた配列中の成分を硬化し、前記粒子の相対的な位置を固定するための硬化システム、
を備える、システム。 - 前記放射線源が可視光を照射する、請求項24に記載のシステム。
- 前記放射線検出器が分光器を含む、請求項25に記載のシステム。
- 前記コーティングされた配列によって回折される光の測定されたスペクトルと、前記硬化した配列の所望の外観とを関連付ける手段も更に備える、請求項24に記載のシステム。
- 前記基板から前記硬化した配列を除去し、前記硬化した配列を粒子形状に微粉砕する手段も更に備える、請求項24に記載のシステム。
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