JP2015127810A - 光学用部材及びその製造方法 - Google Patents
光学用部材及びその製造方法 Download PDFInfo
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- JP2015127810A JP2015127810A JP2014239239A JP2014239239A JP2015127810A JP 2015127810 A JP2015127810 A JP 2015127810A JP 2014239239 A JP2014239239 A JP 2014239239A JP 2014239239 A JP2014239239 A JP 2014239239A JP 2015127810 A JP2015127810 A JP 2015127810A
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- MYWQGROTKMBNKN-UHFFFAOYSA-N tributoxyalumane Chemical compound [Al+3].CCCC[O-].CCCC[O-].CCCC[O-] MYWQGROTKMBNKN-UHFFFAOYSA-N 0.000 description 1
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- MDDPTCUZZASZIQ-UHFFFAOYSA-N tris[(2-methylpropan-2-yl)oxy]alumane Chemical compound [Al+3].CC(C)(C)[O-].CC(C)(C)[O-].CC(C)(C)[O-] MDDPTCUZZASZIQ-UHFFFAOYSA-N 0.000 description 1
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- 238000009849 vacuum degassing Methods 0.000 description 1
- 229940070710 valerate Drugs 0.000 description 1
- NQPDZGIKBAWPEJ-UHFFFAOYSA-N valeric acid Chemical compound CCCCC(O)=O NQPDZGIKBAWPEJ-UHFFFAOYSA-N 0.000 description 1
- 239000012808 vapor phase Substances 0.000 description 1
- 239000003643 water by type Substances 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- 150000003752 zinc compounds Chemical class 0.000 description 1
- XOOUIPVCVHRTMJ-UHFFFAOYSA-L zinc stearate Chemical compound [Zn+2].CCCCCCCCCCCCCCCCCC([O-])=O.CCCCCCCCCCCCCCCCCC([O-])=O XOOUIPVCVHRTMJ-UHFFFAOYSA-L 0.000 description 1
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Abstract
【解決手段】基材1の表面に積層体が形成された光学用部材であって、積層体は、表面層に多孔質層又は凹凸構造6を有する層5を有し、かつ、積層体は、基材1から表面層に向かって、主鎖中に芳香環及び/又はイミド環を有するポリマーを主成分とする第一の有機樹脂層2と、ポリマレイミドまたはその共重合体を主成分とする第二の有機樹脂層3とを有する光学用部材である。
【選択図】図2
Description
前記積層体は、表面層に多孔質層又は凹凸構造を有する層を有し、前記積層体は、前記基材から前記表面層に向かって主鎖中に芳香環及び/又はイミド環を有するポリマーを主成分とする第一の有機樹脂層と、
下記一般式(1)で表される繰り返し構造を含むポリマレイミドまたはその共重合体を主成分とする第二の有機樹脂層と、を有することを特徴とする光学用部材に関する。
主鎖中に芳香環及び/又はイミド環を有するポリマーの溶液を基材上に塗布した後、20〜150℃で乾燥させ第一の有機樹脂層を形成する工程と、
前記第一の有機樹脂層上に、下記一般式(1)で表される繰り返し構造を含むポリマレイミドまたはその共重合体の溶液を塗布した後、20〜150℃で乾燥させ第二の有機樹脂層を形成する工程と、
前記第二の有機樹脂層上に、酸化ケイ素粒子ゾルまたは酸化アルミニウム前駆体ゾルを用いて多孔質層又は凹凸構造を有する層を形成する工程と、
を含むことを特徴とする光学用部材の製造方法に関する。
本発明の光学部材は、光学レンズ、光学プリズム、光学ファインダーに用いることができる。なかでも、光学レンズに好適に用いることができる。
S0:測定面が理想的にフラットであるとした時の面積、|XR−XL|×|YT−YB|、F(X,Y):測定点(X,Y)における高さ、XはX座標、YはY座標、XLからXR:測定面のX座標の範囲、
YBからYT:測定面のY座標の範囲、
Z0:測定面内の平均の高さ
本発明の光学用部材の製造方法は、主鎖中に芳香環及び/又はイミド環を有するポリマーの溶液を基材上に塗布した後、20〜150℃で乾燥させ第一の有機樹脂層を形成する工程を有する。その後、前記ポリマレイミドまたはその共重合体の溶液を第一の層上に塗布した後、20〜150℃で乾燥させ第二の有機樹脂層を形成する工程を有する。さらに、酸化ケイ素粒子ゾルまたは酸化アルミニウム前駆体ゾルを用いて多孔質層又は凹凸構造を有する層を形成する工程を有する。
メチルメタクリレート、エチルメタクリレート、ビニルメタクリレート、アリルメタクリレート、ブチルメタクリレート、tert−ブチルメタクリレート、イソブチルメタクリレート、イソアミルメタクリレート、ヘキシルメタクリレート、シクロヘキシルメタクリレート、ヒドロキシエチルメタクリレート、2−ヒドロキシプロピルメタクリレート、4−ヒドロキシブチルメタクリレート、2−メトキシエチルメタクリレート、2−アセトキシエチルメタクリレート、2−メトキシプロピルメタクリレート、テトラヒドロフルフリルメタクリレート、グリシジルメタクリレート、2,2,2−トリフルオロエチルメタクリレート、1,1,1,3,3,3−ヘキサフルオロプロピルメタクリレート、2,2,3,3−テトラフルオロプロピルメタクリレート、3−(メタクリロイルオキシ)プロピルトリメトキシシラン、3−(メタクリロイルオキシ)プロピルトリエトキシシランなどのメタクリレート類、
アクリルアミド、N−メチロールアクリルアミド、N−メトキシメチルアクリルアミド、N−ブトキシメチルアクリルアミドなどのアクリルアミド類、
メチルビニルエーテル、エチルビニルエーテル、n−プロピルビニルエーテル、イソプロピルビニルエーテル、n−ブチルビニルエーテル、tert−ブチルビニルエーテル、イソブチルビニルエーテル、n−ペンチルビニルエーテル、n−ヘキシルビニルエーテル、n−オクチルビニルエーテル、シクロヘキシルビニルエーテル、2−ヒドロキシエチルビニルエーテル、3−ヒドロキシプロピルビニルエーテルなどのビニルエーテル類、
エチレン、イソブテン、1−ペンテン、1−ヘキセン、1−オクテン、ジイソブチレン、2−メチル−1−ブテン、2−メチル−1−ペンテン、2−メチル−1−ヘキセン、1−メチル−1−ヘプテン、1−イソオクテン、2−メチル−1−オクテン、2−エチル−1−ペンテン、2−メチル−2−ブテン、2−メチル−2−ペンテン、2−メチル−2−ヘキセン等のオレフィン類、などである。
アゾビスイソブチロニトリル、アゾビスイソバレロニトリル、2,2−アゾビス(4−メトキシ−2,4−ジメチルバレロニトリル)、2,2−アゾビス(2,4−ジメチルバレロニトリル)、2,2−アゾビス(2−メチルブチロニトリル)、1,1’−アゾビス(シクロヘキサン−1−カルボニトリル)、2−(カルボモイルアゾ)イソブチロニトリル、2,2−アゾビス〔2−メチル−N−[1、1ビス(ヒドロキシルメチル)−2−ヒドロキシルエチル]プロピオンアミド〕、2,2−アゾビス〔2−メチル−N−(2−ヒドロキシルエチル)プロピオンアミド〕、2,2−アゾビス〔N−(2−プロペニル)2−メチルプロピオンアミド〕、2,2−アゾビス(N−ブチル−2−メチルプロピオンアミド)、2,2−アゾビス(N−シクロヘキシル−2−メチルプロピオンアミド)、2,2−アゾビ〔2−(5−メチル−2−イミダゾリン−2−イル)プロパン〕ジハイドロクロライド、2,2−アゾビス〔2−(2−イミダゾリン−2−イル)プロパン〕ジハイドロクロライド、2,2−アゾビス〔2−(2−イミダゾリン−2−イル)プロパン〕ジサルフェート・ジハイドレート、2,2−アゾビス〔2−(3,4,5,6−テトラヒドロピリミジン−2−イル)プロパン〕ジハイドロクロライド、2,2−アゾビス〔2−[1−(2−ヒドロキシエチル)2−イミダゾリン−2−イル]プロパン〕ジハイドロクロライド、2,2−アゾビス〔2−(2−イミダゾリン−2−イル)プロパン〕、2,2−アゾビス(2−メチルプロピオンアミジン)ジハイドロクロライド、2,2−アゾビス〔N−(2−カルボキシエチル)2−メチルプロピオンアミジン〕、2,2−アゾビス(2−メチルプロピオンアミドキシム)、ジメチル−2,2’−アゾビスブチレ−ト、4,4’−アゾビス(4−シアノペンタノイックアシッド)、2,2−アゾビス(2,4,4−トリメチルペンタン)などのアゾビス系ラジカル重合開始剤などである。
16.6gの4,4’−ビス(4−アミノフェノキシ)ビフェニルおよび1.3gの1,3−ビス(3−アミノプロピル)テトラメチルジシロキサンを146.4gのN,N−ジメチルアセトアミド(以下、DMAcと略す)に溶解した。このジアミン溶液を水冷攪拌しながら13.0gの4−(2,5−ジオキソテトラヒドロフラン−3−イル)−1,2,3,4−テトラヒドロナフタレン−1,2−ジカルボン酸無水物をゆっくり加えた。この溶液を15時間室温で攪拌し、重合反応を行った。さらに、223.2gのDMAcで希釈してから7.4mlのピリジンと3.8mlの無水酢酸を加え、室温で1時間攪拌した。さらに、オイルバスで60〜70℃に加熱しながら4時間攪拌した。強攪拌したメタノール中にゆっくりと重合溶液を投入し析出させたポリマーを濾別してから、メタノール中で数回攪拌洗浄した。濾別回収したポリマーを80〜90℃で真空乾燥を行った。白色の粉末状の脂肪族ポリイミドを28.5g(収率:94%)得た。数平均分子量は25,100であり、1H−NMRスペクトルからイミド化率99%であった。得られたポリイミド粉末は1−アセトキシ−2−メトキシプロパンや酢酸ブチルに不溶であった。
下記一般式(4)で表させる繰り返し構造を有する分岐メラミンポリマーの光硬化塗料(製品名:ハイパーテックUR101、日産化学製)をシクロペンタノン/シクロヘキサノン混合溶媒で濃度2.9質量%まで希釈し、分岐メラミンポリマー溶液2とした。
50gの分岐型メラミンポリマー溶液2と54.2gのポリイミド溶液1を室温で攪拌混合して、分岐型メラミンポリマーとポリイミドのブレンド比が0.56/0.44(質量比)のブレンドポリマー溶液3を調製した。
1.5gのポリスチレン粉末(1モル%ジビニルベンゼン架橋、東京化成製)を97.5gのシクロヘキサノン溶液に溶解してから5.0gの20%ナノジルコニアMEK分散液(平均粒子径7nm、住友大阪セメント製)を添加した。エバポレーターでMEKを留去してナノジルコニア分散液5を調製した。
6.74gのN−ベンジルマレイミド(以下、BzMIと略す)、4.30gのN−シクロヘキシルマレイミド、および0.08gの2,2’−アゾビス(イソブチロニトリル)(以下、AIBNと略す)を25.8gのトルエンに攪拌溶解した。この溶液を氷水冷しながら脱気と窒素置換を繰り返し行った後、窒素フローしながら60〜70℃で7時間攪拌した。強攪拌したメタノール中にゆっくりと重合溶液を投入し析出させたポリマーを濾別してから、メタノール中で数回攪拌洗浄した。濾別回収したポリマーを80〜90℃で真空乾燥を行った。白色粉末状の下記式(5)のポリマレイミドを10.2g(収率92%)得た。GPC測定により数平均分子量が18,200であった。表1に各ポリマーの合成結果を示した。IRスペクトルから1700cm−1にイミド環のC=O伸縮振動による吸収が、1750cm−1にメタクリレート単位のC=O伸縮振動による吸収がそれぞれ確認された。得られたポリマレイミド粉末は1−メトキシ−2−プロパノールや1−ペンタノールに不溶であった。
9.55gのBzMI、0.90gのメチルメタクリレート、0.08gのAIBN、および24.4gのトルエンを用いてポリマレイミドと同様の方法で重合、取り出しを行った。白色粉末状で下記式(6)のポリ(マレイミド−CO−メタクリレート)を9.5g(収率90%)得た。数平均分子量は14,200であった。IRスペクトルから1690cm−1にイミド環のC=O伸縮振動による吸収が、1750cm−1にメタクリレート単位のC=O伸縮振動による吸収がそれぞれ確認された。得られたポリ(マレイミド−CO−メタクリレート)粉末は1−メトキシ−2−プロパノールや1−ペンタノールに不溶であった。
2.5gの市販のポリスチレン粉末(重量平均分子量20,000、フルカ製)を97.5gの1−アセトキシ−2−メトキシプロパンに溶解してポリスチレン溶液9を調製した。
14.8gのアルミニウム−sec−ブトキシド(ASBD、川研ファインケミカル製)と、3.42gの3−メチル−2,4−ペンタンジオンと、2−エチルブタノールとを均一になるまで混合攪拌した。1.94gの0.01M希塩酸を2−エチルブタノール/1−エトキシ−2−プロパノールの混合溶媒に溶解してから、前記アルミニウム−sec−ブトキシドの溶液にゆっくり加え、暫く攪拌した。溶媒は最終的に36.9gの2−エチルブタノールと15.8gの1−エトキシ−2−プロパノールの混合溶媒になるように調製した。さらに120℃のオイルバス中で2から3時間以上攪拌することによって酸化アルミニウム前駆体ゾル11を調製した。動的光散乱法で測定した平均粒子径は10nmであった。
19.0gの20%酸化ケイ素中空微粒子のIPAゾル(スルーリア1011、日揮日本触媒製)に96.2gの2−メトキシプロパノールを加えてからエバポレーターでIPAを留去して酸化ケイ素微粒子ゾル13を調製した。
ゲルパーミエションクロマトグラフィー(Gel Permeation Chromatography、GPC)装置(ウォーターズ(WATERS)社製)で、Shodex LF−804 カラム(昭和電工株式会社製)を2本直列に配置し、40℃、展開溶媒としてTHFを用い、RI(Refractive Index、示差屈折率)検出器により測定した。得られた数平均分子量は標準ポリスチレン換算値である。
赤外分光スペクトル測定装置(Spectrum One、パーキンエルマー製)と付属のユニバーサルATRを用いて650cm−1から4000cm−1の範囲の赤外透過スペクトルを測定した。
粒度分布計(ゼータサイザーナノS、マルバーン製)を用い、ガラス製セルに約1mlの酸化アルミニウム前駆体ゾルを入れて25℃で測定した。屈折率を1.5、吸収を0.01とし、予め測定したゾルの粘度測定値を用いて解析を行ない、粒度分布曲線(粒子径−散乱強度)の極大値から平均粒子径を求めた。解析に用いた粘度は標準ローター(1°34’、R24)を装備した回転式粘度計(東機産業社、RE80型粘度計)を用いて25℃で測定した。
両面を研磨した大きさ約φ30mm、厚さ約5mmのガラス基板をアルカリ洗剤中で超音波洗浄し、純水でリンスした後、クリーンオーブン中で60℃/30分乾燥した。
絶対反射率測定装置(USPM−RU、オリンパス製)を用い、400nmから700nmの範囲の入射角0°時の反射率測定を行った。最小値は0.05%未満を○、0.05%以上を×と判定した。平均値は0.1%未満を○、0.1%以上0.2%未満を△、0.2%以上を×と判定した。
スライドプロジェクターの光を透過させ、膜にクモリなどが無いか目視観察した。クモリが見られない場合を○、クモリが見られる場合を×と判定した。
分光エリプソメータ(VASE、ジェー・エー・ウーラム・ジャパン製)を用い、波長380nmから800nmまで測定し、解析から膜厚を求めた。
分光エリプソメータ(VASE、ジェー・エー・ウーラム・ジャパン製)を用い、波長380nmから800nmまで測定した。屈折率は波長550nmの屈折率とした。
基板表面をPd/Pt処理を行い、FE−SEM(S−4800、日立ハイテク製)を用いて加速電圧2kVで表面観察を行った。
洗浄したLa2O3を主成分とするnd=1.72、νd=50のガラス基板上にポリイミド溶液1を適量滴下し、さらに4500rpmで20秒スピンコートを行った。この基板を100℃で20分間加熱し、膜厚25nmで波長550nmの屈折率が1.671のポリイミド膜の付いた基板を作製した。
絶対反射率の最大値は◎0.1%以下、○0.2%以下、△0.5%以下、×0.5%超
絶対反射率の平均値は◎0.05%以下、○0.1%以下、△0.2%以下、×0.2%超
高温高湿下絶対反射率変化は○0.05%以下、△0.1%以下、×0.1%超
洗浄したLa2O3を主成分とするnd=1.83、νd=43のガラス基板上にブレンドポリマー溶液3を適量滴下し、さらに4500rpmで20秒スピンコートを行った。この基板を100℃で20分間加熱し、膜厚45nmで波長550nmの屈折率が1.756のブレンドポリマー膜の付いた基板を作製した。
ポリマレイミド溶液をポリ(マレイミド−co−メタクリレート)溶液8に変えた以外は実施例2と同様の方法で反射防止膜付き基板を作製した。ポリ(マレイミド−co−メタクリレート)膜の膜厚は22nmで波長550nmの屈折率は1.563であった。
ガラス基板をTiO2を主成分とするnd=1.85、νd=24のガラス基板に変えた以外は実施例2と同様の方法で反射防止膜付き基板を作製した。
ガラス基板をLa2O3を主成分とするnd=2.00、νd=28のガラス基板に変え、ブレンドポリマー溶液3に変えて分岐型メラミンポリマー溶液2を適量滴下し、さらに2500rpmで20秒スピンコートを行った。この基板を100℃で20分間加熱し、膜厚60nmで波長550nmの屈折率が1.815のブレンドポリマー膜の付いた基板を作製した。
洗浄したLa2O3を主成分とするnd=1.83、νd=43のガラス基板上にブレンドポリマー溶液3を適量滴下し、さらに4500rpmで20秒スピンコートを行った。この基板を100℃で20分間加熱し、膜厚45nmで波長550nmの屈折率が1.756のブレンドポリマー膜の付いた基板を作製した。
ポリマレイミド溶液6をポリスチレン溶液9に変えた以外は実施例2と同様の方法で反射防止膜付き基板を作製した。ポリスチレン膜の膜厚は22nmで波長550nmの屈折率は1.595であったが、酸化アルミニウム前駆体ゾル11を塗布時にポリスチレン膜の一部が溶けて約10nmまで薄膜化した。
ブレンドポリマー溶液3をナノジルコニア分散液5に変えた以外は実施例2と同様の方法で反射防止膜付き基板を作製した。ナノジルコニア分散膜の膜厚は46nmで波長550nmの屈折率は1.745であったが、ポリマレイミド溶液6を塗布時にナノジルコニア分散膜の一部が溶けて約20nmまで薄膜化した。
洗浄したLa2O3を主成分とするnd=1.83、νd=43のガラス基板上にポリマレイミド溶液6を適量滴下し、さらに2000rpmで20秒スピンコートを行った。この基板を100℃で20分間加熱し、膜厚35nmで波長550nmの屈折率が1.570のポリマレイミド膜の付いた基板を作製した。
洗浄したLa2O3を主成分とするnd=1.83、νd=43のガラス基板上にブレンドポリマー溶液4を適量滴下し、さらに6000rpmで20秒スピンコートを行った。この基板を100℃で20分間加熱し、膜厚26nmで波長550nmの屈折率が1.750のブレンドポリマー膜の付いた基板を作製した。
ポリマレイミド溶液7をポリスチレン溶液10に変えた以外は実施例2と同様の方法で反射防止膜付き基板を作製した。ポリスチレン膜の膜厚は70nmで波長550nmの屈折率は1.600であったが、酸化ケイ素微粒子ゾル13を塗布時にポリスチレン膜の一部が溶けて約45nmまで薄膜化した。
洗浄したLa2O3を主成分とするnd=1.83、νd=43のガラス基板上にポリマレイミド溶液7を適量滴下し、さらに4500rpmで20秒スピンコートを行った。この基板を100℃で20分間加熱し、膜厚70nmで波長550nmの屈折率が1.580のポリマレイミド膜の付いた基板を作製した。それ以外は実施例6と同様の方法でポリマレイミド膜上に酸化ケイ素微粒子が堆積した膜を作製した。
La2O3を主成分とするnd=1.83、νd=43のガラスからなるレンズの凹面(直径45mm、曲率半径27mm)上に実施例2と同様の方法で、表面に酸化アルミニウムを主成分とする微細な突起状組織を形成した。
2 第一の有機樹脂層
3 第二の有機樹脂層
4 多孔質層
5 凹凸(突起)を有する層
6 凹凸(突起)
7 突起の傾斜方向
8 突起の傾斜方向
9 基材表面の接線
Claims (14)
- 基材表面に積層体が形成された光学用部材であって、
前記積層体は、表面層に多孔質層又は凹凸構造を有する層を有し、前記積層体は、前記基材から前記表面層に向かって、主鎖中に芳香環及び/又はイミド環を有するポリマーを主成分とする第一の有機樹脂層と、
下記一般式(1)で表される繰り返し構造を含むポリマレイミドまたはその共重合体を主成分とする第二の有機樹脂層と、を有することを特徴とする光学用部材。
(1)
(式(1)中、R1は、無置換若しくはフェニル基、水酸基、アルコキシル基、アセトキシル基、環状エーテル基、アミノ基、アルコキシシリル基、ハロゲン原子が置換した炭素数1〜8の線状、分岐状、環状いずれかのアルキル基、アルケニル基、又は無置換若しくはアルキル基、アルケニル基、アルコキシル基、アセトキシル基、アルコキシシリル基、ニトロ基、ハロゲン原子が置換したフェニル基、ビフェニル基、ナフチル基である。mは、1以上の整数である。) - 前記第一の有機樹脂層の前記主鎖中に芳香環及び/又はイミド環を有するポリマーは、シクロヘキサノン、シクロペンタノン、γーブチロラクトンの中から少なくとも1種類の溶媒に可溶で、酢酸エステル類または乳酸エステル類のうち少なくとも1種類の溶媒に不溶であることを特徴とする請求項1に記載の光学用部材。
- 前記第二の有機樹脂層の前記ポリマレイミドまたはその共重合体は、酢酸エステル類または乳酸エステル類の内少なくとも1種類の溶媒に可溶で、炭素数3以上7以下のアルコール類の内少なくとも1種類の溶媒に不溶であることを特徴とする請求項1又は2に記載の光学用部材。
- 前記第一の有機樹脂層の前記主鎖中に芳香環及び/又はイミド環を有するポリマーは、分岐型メラミンポリマーであることを特徴とする請求項1乃至3のいずれか一項に記載の光学用部材。
- 前記第一の有機樹脂層の屈折率n1と、前記第二の有機樹脂層の屈折率n2と、前記多孔質又は前記凹凸構造を有する層の屈折率n3が、n1>n2>n3であることを特徴とする請求項1乃至5のいずれか一項に記載の光学用部材。
- 前記凹凸構造は、酸化アルミニウムを主成分とする板状結晶であることを特徴とする請求項1乃至6のいずれか一項に記載の光学用部材。
- 前記多孔質層が酸化ケイ素の微粒子を有していることを特徴とする請求項1乃至6のいずれか一項に記載の光学用部材。
- 前記基材が無機ガラスであることを特徴とする請求項1乃至7のいずれか一項に記載の光学用部材。
- レンズの表面に積層体が形成された光学レンズであって、
前記積層体は、表面層に多孔質層又は凹凸構造を有する層を有し、前記積層体は、前記レンズから前記表面層に向かって主鎖中に芳香環及び/又はイミド環を有するポリマーを主成分とする第一の有機樹脂層と、
下記一般式(1)で表される繰り返し構造を含むポリマレイミドまたはその共重合体を主成分とする第二の有機樹脂層と、を有することを特徴とする光学レンズ。
(1)
(式(1)中、R1は、無置換若しくはフェニル基、水酸基、アルコキシル基、アセトキシル基、環状エーテル基、アミノ基、アルコキシシリル基、ハロゲン原子が置換した炭素数1〜8の線状、分岐状、環状いずれかのアルキル基、アルケニル基、又は無置換若しくはアルキル基、アルケニル基、アルコキシル基、アセトキシル基、アルコキシシリル基、ニトロ基、ハロゲン原子が置換したフェニル基、ビフェニル基、ナフチル基である。mは、1以上の整数である。) - 基材表面に積層体が形成された光学用部材の製造方法において、
主鎖中に芳香環及び/又はイミド環を有するポリマーの溶液を基材上に塗布した後、20〜150℃で乾燥させ第一の有機樹脂層を形成する工程と、
前記第一の有機樹脂層上に、下記一般式(1)で表される繰り返し構造を含むポリマレイミドまたはその共重合体の溶液を塗布した後、20〜150℃で乾燥させ第二の有機樹脂層を形成する工程と、
前記第二の有機樹脂層上に、酸化ケイ素粒子ゾルまたは酸化アルミニウム前駆体ゾルを用いて多孔質層又は凹凸構造を有する層を形成する工程と、
を含むことを特徴とする光学用部材の製造方法。
(1)
(式(1)中、R1は、無置換若しくはフェニル基、水酸基、アルコキシル基、アセトキシル基、環状エーテル基、アミノ基、アルコキシシリル基、ハロゲン原子が置換した炭素数1〜8の線状、分岐状、環状いずれかのアルキル基、アルケニル基、又は無置換若しくはアルキル基、アルケニル基、アルコキシル基、アセトキシル基、アルコキシシリル基、ニトロ基、ハロゲン原子が置換したフェニル基、ビフェニル基、ナフチル基である。mは、1以上の整数である。) - 前記第一の有機樹脂層を形成する工程で用いた前記主鎖中に芳香環及び/又はイミド環を有するポリマーの溶液は、シクロヘキサノン、シクロペンタノン、γーブチロラクトンを合計で50質量%以上100質量%以下含有し、
前記第二の有機樹脂層を形成する工程で用いた前記ポリマレイミドまたはその共重合体の溶液は、酢酸エステル類、ギ酸エステル類、乳酸エステル類を合計で50質量%以上100質量%以下含有し、シクロヘキサノン、シクロペンタノン、γーブチロラクトンを合計で0質量%以上10質量%未満含有する前記酸化アルミニウム前駆体ゾルまたは酸化ケイ素粒子ゾルは、炭素数3以上7以下のアルコール類を溶媒全体に対して80質量%以上100質量%以下含有することを特徴とする請求項11記載の光学用部材の製造方法。 - 前記凹凸構造を有する層を形成する工程は、
酸化アルミニウム前駆体ゾルを塗布する工程と、
前記塗布した酸化アルミニウム前駆体ゾルを50℃以上250℃以下で乾燥および/又は焼成して酸化アルミニウム膜を形成する工程と、
前記酸化アルミニウム膜を温水に浸漬することで酸化アルミニウムを主成分とする結晶からなる凹凸構造を有する層を形成する工程と、
を有する請求項11又は12に記載の光学用部材の製造方法。 - 前記多孔質層を形成する工程は、
酸化ケイ素粒子ゾルを塗布する工程と、
前記塗布した酸化ケイ素粒子ゾルを50℃以上250℃以下で乾燥および/又は焼成して酸化ケイ素の微粒子からなる層を形成する工程と、
を有する請求項11又は12に記載の光学用部材の製造方法。
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