JP4488764B2 - 透明反射防止膜、その製造方法および光学部材 - Google Patents
透明反射防止膜、その製造方法および光学部材 Download PDFInfo
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- JP4488764B2 JP4488764B2 JP2004046256A JP2004046256A JP4488764B2 JP 4488764 B2 JP4488764 B2 JP 4488764B2 JP 2004046256 A JP2004046256 A JP 2004046256A JP 2004046256 A JP2004046256 A JP 2004046256A JP 4488764 B2 JP4488764 B2 JP 4488764B2
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- XPGAWFIWCWKDDL-UHFFFAOYSA-N propan-1-olate;zirconium(4+) Chemical compound [Zr+4].CCC[O-].CCC[O-].CCC[O-].CCC[O-] XPGAWFIWCWKDDL-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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Description
前記微細な凹凸を有する膜の中心線平均粗さを面拡張した平均面粗さRa’値が5nm以上、かつ表面積比Sr=S/S0(但し、S0は測定面が理想的にフラットであるときの面積、Sは実際の測定面の表面積を示す。)が1.1以上であることを特徴とする。
前記微細な凹凸を有する膜に含有されるアルミナ、シリカ、チタニア、ジルコニアから選ばれた少なくとも1種の含有量が、膜重量に対して重量比で0.01以上1.0未満であることを特徴とする。
また、本発明は、上記の透明反射防止膜を有する光学部材である。
亜鉛化合物としては、例えば酢酸亜鉛、塩化亜鉛、硝酸亜鉛、ステアリン酸亜鉛、オレイン酸亜鉛、サリチル酸亜鉛などが挙げられ、特に酢酸亜鉛、塩化亜鉛が好ましい。
S0 :測定面が理想的にフラットであるとした時の面積、|X R−X L|×|Y T−Y B|、
F(X,Y):測定点(X,Y)における高さ、XはX座標、YはY座標、
X L〜X R:測定面のX座標の範囲、
Y B〜Y T:測定面のY座標の範囲、
Z0 :測定面内の平均の高さ
また、表面積比(Sr)は、Sr=S/S0 〔S0 :測定面が理想的にフラットであるときの面積。S:実際の測定面の表面積。〕で求められる。なお、実際の測定面の表面積は次のようにして求める。先ず、最も近接した3つのデータ点(A,B,C)より成る微小三角形に分割し、次いで各微小三角形の面積△Sを、ベクトル積を用いて求める。△S(△ABC)=|AB×AC|/2〔但し、ABおよびACは各辺の長さ〕となり、この△Sの総和が求める表面積Sになる。
Ra’が5nm以上で、Srが1.1以上であると、前記の理由で微細な凹凸による効果が低下する恐れが無くなる。
各実施例、比較例で得られた、表面に微細な凹凸を有する透明膜について、下記の方法で評価を行った。
(1)被膜形状観察
走査型電子顕微鏡(FE−SEM、日立製作所製S5000)を用いて被膜の表層表面の写真観察(加速電圧;5.0kV、倍率;3万倍(表面))を行った。
走査型プローブ顕微鏡(SPM、DFMモード、セイコ−電子工業製SPI3800)を用いて、JISB0601で定義されている中心線平均粗さを面拡張した平均面粗さRa’値と表面積比Srを求めた。
X線回折装置(理学電気製RINT2100)を用い、CuKα線を用いて測定した。
(3)透過率測定
自動光学素子測定装置(ART−25GD、日本分光製)を用いた。円盤状ガラス板を使用した。透過率測定における光の入射角は0°であった。
大きさ約100mm×100mm、厚さ約2mmのクリア・フロートガラス基板(組成はソーダライムシリケート系)をイソプロピルアルコールで超音波洗浄し乾燥した後、コーティング用ガラス基板とした。
実施例1で得られた、表面に微細な凹凸をもつ膜の透過率は約96%であり、表面に形成された微細な凹凸により優れた反射防止性能を示した。ここで、透過率は、表面に微細な凹凸を有する膜を形成させたガラス基板の透過率を表す。
実施例1と同様の亜鉛化合物含有溶液である塗布液を用い、実施例1と同様の洗浄を行った同様のガラス基板を、該塗布液中に浸漬した後、ディッピング法(2mm/秒の引き上げ速度、20℃、56%R.H.下)で、ガラス基板の表面に塗布膜を形成した。乾燥後、100℃で1時間熱処理し、透明な皮膜を得た。次に、60℃の純水とエタノールの混合液(50/50wt%)中に5分間浸漬したのち、100℃で10分間乾燥させた。
実施例2で得られた、表面に微細な凹凸をもつ膜の透過率は約95%であり、優れた反射防止性能を示した。
酢酸亜鉛2水和物〔Zn(CH3 COO)2 ・2H2 O〕を2−メトキシエタノール〔2ME〕中に溶解させ、安定化剤として、モノエタノールアミン〔MEA〕を添加し、約3時間室温で攪拌した。ここで溶液の重量比は、Zn(CH3 COO)2 ・2H2 O:2ME:MEA=14:80:4の割合とした。以上のようにして、亜鉛化合物含有溶液である塗布液を調製した。
また、X線分析測定から前記微細な凹凸は酸化亜鉛の結晶であることがわかった。
実施例3で得られた、表面に微細な凹凸をもつ膜の透過率は約96%であり、優れた反射防止性能を示した。
亜鉛化合物含有溶液にアルミニウム化合物およびジルコニウム化合物を添加した溶液を調製した。亜鉛化合物含有溶液は実施例3と同様の方法で調製した。
実施例4で得られた、表面に微細な凹凸をもつ膜の透過率は約97%であり、優れた反射防止性能を示した。
亜鉛化合物含有溶液に、アルミニウム化合物、ケイ素化合物およびチタン化合物を添加した溶液を調製した。亜鉛化合物含有溶液は実施例3と同様の方法で調製した。
実施例5で得られた、表面に微細な凹凸をもつ膜の透過率は約96%であり、優れた反射防止性能を示した。
Claims (8)
- 酸化亜鉛を主成分とし、アルミナ、シリカ、チタニア、ジルコニアから選ばれた少なくとも一種を含有する皮膜を有する透明反射防止膜であって、前記皮膜の表面には、前記酸化亜鉛を主成分とする結晶からなる微細な凹凸が形成されていることを特徴とする透明反射防止膜。
- 前記微細な凹凸の高さが0.005〜1μmであることを特徴とする請求項1記載の透明反射防止膜。
- 前記微細な凹凸を有する膜の中心線平均粗さを面拡張した平均面粗さRa’値が5nm以上、かつ表面積比Sr=S/S0(但し、S0は測定面が理想的にフラットであるときの面積、Sは実際の測定面の表面積を示す。)が1.1以上であることを特徴とする請求項1または2記載の透明反射防止膜。
- 前記皮膜に含有されるアルミナ、シリカ、チタニア、ジルコニアから選ばれた少なくとも1種の含有量が、前記皮膜重量に対して重量比で0.01以上1.0未満であることを特徴とする請求項1記載の透明反射防止膜。
- 前記透明反射防止膜は基材上に形成されていることを特徴とする請求項1乃至4のいずれかに記載の透明反射防止膜。
- 請求項1乃至5のいずれかに記載の透明反射防止膜を有する光学部材。
- 基材上に、亜鉛化合物を主成分とし、アルミニウム化合物、ケイ素化合物、チタン化合物、ジルコニウム化合物から選ばれた少なくとも一種を含有する溶液を塗布して皮膜を形成させる工程と、前記皮膜を20℃以上の含水液に浸漬して前記皮膜表面に微細な凹凸を形成させる工程とを有することを特徴とする透明反射防止膜の製造方法。
- 前記皮膜を形成させる工程は、前記溶液を塗布した後、乾燥あるいは熱処理を行なうことを特徴とする請求項7記載の透明反射防止膜の製造方法。
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JP2007183366A (ja) | 2006-01-05 | 2007-07-19 | Pentax Corp | 防塵性光透過性部材及びその用途、並びにその部材を具備する撮像装置 |
JP2007213780A (ja) * | 2006-01-11 | 2007-08-23 | Pentax Corp | 反射防止膜を有する光学素子 |
TW200746123A (en) | 2006-01-11 | 2007-12-16 | Pentax Corp | Optical element having anti-reflection coating |
KR101419869B1 (ko) | 2006-05-31 | 2014-07-16 | 가부시키가이샤 한도오따이 에네루기 켄큐쇼 | 표시장치 |
US20080198457A1 (en) | 2007-02-20 | 2008-08-21 | Pentax Corporation | Dust-proof, reflecting mirror and optical apparatus comprising same |
JP5279344B2 (ja) * | 2007-06-06 | 2013-09-04 | キヤノン株式会社 | 光学素子の製造方法 |
JP5078470B2 (ja) | 2007-07-05 | 2012-11-21 | ペンタックスリコーイメージング株式会社 | 光学ローパスフィルタ及びそれを具備する撮像装置 |
WO2012140744A1 (ja) * | 2011-04-13 | 2012-10-18 | 三共化成株式会社 | 成形回路部品 |
JP2014048526A (ja) * | 2012-08-31 | 2014-03-17 | Dexerials Corp | 光学体、表示装置、入力装置および電子機器 |
JP6979994B2 (ja) * | 2017-09-26 | 2021-12-15 | デクセリアルズ株式会社 | 光学体、及び窓材 |
JP2019061026A (ja) * | 2017-09-26 | 2019-04-18 | デクセリアルズ株式会社 | 光学体、及び窓材 |
JP2023165649A (ja) * | 2022-05-06 | 2023-11-16 | 東ソー・ファインケム株式会社 | 酸化亜鉛被膜を有する物品およびその製造方法ならびに脱臭方法 |
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