JP5889294B2 - 微細構造を有する表面を作製する方法 - Google Patents
微細構造を有する表面を作製する方法 Download PDFInfo
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- JP5889294B2 JP5889294B2 JP2013517380A JP2013517380A JP5889294B2 JP 5889294 B2 JP5889294 B2 JP 5889294B2 JP 2013517380 A JP2013517380 A JP 2013517380A JP 2013517380 A JP2013517380 A JP 2013517380A JP 5889294 B2 JP5889294 B2 JP 5889294B2
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- mold
- acid
- meth
- substrate
- acrylate
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- 238000000691 measurement method Methods 0.000 claims 1
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- IQPQWNKOIGAROB-UHFFFAOYSA-N isocyanate group Chemical group [N-]=C=O IQPQWNKOIGAROB-UHFFFAOYSA-N 0.000 description 9
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- C09J—ADHESIVES; NON-MECHANICAL ASPECTS OF ADHESIVE PROCESSES IN GENERAL; ADHESIVE PROCESSES NOT PROVIDED FOR ELSEWHERE; USE OF MATERIALS AS ADHESIVES
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Description
1.金型への急速、完全かつ一様な流入を可能にするポリマーブレンドの低い粘度;
2.好ましくは、即時の特に迅速な硬化のための放射線硬化性ポリマー。計画された基板と構造マスター(金型)との間の接触時間では、熱硬化又は化学的硬化は、想定され得るとしても、あまり好ましくはない;
3.正確な構造の複製(すなわち、金型の構造の複製)が基板の表面構造の最終特性に特に重要であるため、放射線硬化前の状態と放射線硬化後の状態とで高い成形忠実度及び低い材料収縮率;
4.最適な乾燥接着表面構造を得るための、硬化したポリマー材料の硬度及び弾性。
a)少なくとも1つのコーティング化合物を、少なくとも1つの基板上に塗布する工程と、
b)微細構造のネガを有する金型を用いて微細構造を形成する工程であって、
b1)前記金型を前記基板上の前記コーティング化合物に押し付けるか、又は
b2)工程a)の前記基板が前記金型を含有する、
微細構造を形成する工程と、
c)得られた微細構造を有するコーティング化合物を硬化させるとともに、実質的に硬化したコーティングを得る工程と、
d)前記微細構造を有するコーティングを前記金型から分離する工程と、
を含み、工程d)と工程c)とを逆の順序で行ってもよく、
前記コーティング化合物が、前記基板への塗布前の無溶媒状態で、10Pas未満、好ましくは1Pas未満、特に好ましくは20mPas〜1Pasの粘度(25℃でのプレート/円錐形状を用いたDIN 53018−1に従う回転粘度測定法、温度制御:ペルチェ、測定装置:10l×s−1〜1000 l×s−1、好ましくは400l×s−1の剪断速度(剪断勾配)DでのHC 60/1)を有し、
前記硬化したコーティングが、少なくとも1MPa、最大で2000MPa、好ましくは1MPa〜1000MPa、特に好ましくは2MPa〜100MPaの弾性係数(ベルコビッチチップ、試験片の係数に応じて0.1mN〜1mNの荷重を用いた押込み、押込み時間:10秒、保持時間:30秒、及び後退時間:10秒、ポリカーボネートに対する較正)を有する、
接着性に影響を与えるための、好ましくはアスペクト比が少なくとも0.5の、微細構造を有するコーティング表面を作製する方法によって解決される。
1)イソシアヌレート基を有する芳香族、脂肪族及び/又は脂環式ジイソシアネートのポリイソシアネート。対応する脂肪族及び/又は脂環式イソシアナト−イソシアヌレート、殊にヘキサメチレンジイソシアネート及びイソホロンジイソシアネートをベースとするイソシアネート−イソシアヌレートが殊に好ましい。本発明のイソシアヌレートは、特にジイソシアネートの環状三量体であるトリスイソシアナトアルキル又はトリスイソシアネートシクロアルキルイソシアヌレート、又は2つ以上のイソシアヌレート環を有するそれらの高級同族体との混合物である。イソシアネート−イソシアヌレートは概して、10wt%〜30wt%、殊に15wt%〜25wt%のNCO含有量、及び2.6〜8の平均NCO官能価を有する。
2)イソシアネート基が芳香族結合、脂肪族結合及び/又は脂環式結合した、好ましくは脂肪族結合及び/又は脂環式結合したウレトジオン基を有するポリイソシアネート、殊にヘキサメチレンジイソシアネート又はイソホロンジイソシアネートに由来するポリイソシアネート。ウレトジオンジイソシアネートはジイソシアネートの環状二量化生成物である。ウレトジオン基を有するポリイソシアネートは、本発明の文脈では、他のポリイソシアネート、殊に1)で述べたポリイソシアネートと混合して得られる。そのために、ジイソシアネートを、ウレトジオン基及び他のポリイソシアネートの両方が形成されるか、又はウレトジオン基が最初に形成され、それらが続いて他のポリイソシアネートへと変換されるか、又はジイソシアネートが最初に他のポリイソシアネートへと変換され、それらが続いてウレトジオン基を含有する生成物へと変換される反応条件下で反応させることができる。
3)イソシアネート基が芳香族結合、脂環式結合又は脂肪族結合した、好ましくは脂環式結合又は脂肪族結合したビウレット基、殊にトリス(6−イソシアナトヘキシル)ビウレット又はその高級同族体との混合物を有するポリイソシアネート。これらのビウレット基を有するポリイソシアネートは概して、18wt%〜22wt%のNCO含有量及び2.8〜6の平均NCO官能価を有する。
4)イソシアネート基が芳香族結合、脂肪族結合又は脂環式結合した、好ましくは脂肪族結合又は脂環式結合したウレタン基及び/又はアロファネート基を有するポリイソシアネート、例えば過剰量のジイソシアネート、例えばヘキサメチレンジイソシアネート又はイソホロンジイソシアネートと、一価アルコール又は多価アルコールとの反応によるポリイソシアネート。これらのウレタン基及び/又はアロファネート基を有するポリイソシアネートは概して、12wt%〜24wt%のNCO含有量及び2.5〜4.5の平均NCO官能価を有する。これらのウレタン基及び/又はアロファネート基を有するポリイソシアネートは、無触媒で、又は好ましくは触媒、例えばカルボン酸アンモニウム若しくは水酸化アンモニウム、若しくはアロファネート化(allophanatization)触媒、例えばZn(II)化合物の存在下で、いずれの場合にも一価アルコール、二価アルコール又は多価アルコール、好ましくは一価アルコールの存在下で生成することができる。
5)オキサジアジントリオン基を含有し、好ましくはヘキサメチレンジイソシアネート又はイソホロンジイソシアネートに由来するポリイソシアネート。これらのオキサジアジントリオン基を含有するポリイソシアネートは、ジイソシアネート及び二酸化炭素から得ることができる。
6)イミノオキサジアジンジオン基を含有し、好ましくはヘキサメチレンジイソシアネート又はイソホロンジイソシアネートに由来するポリイソシアネート。これらのイミノオキサジアジンジオン基を含有するポリイソシアネートは、特殊な触媒を用いてジイソシアネートから生成することができる。
7)ウレトンイミン修飾ポリイソシアネート。
8)カルボジイミド修飾ポリイソシアネート。
9)例えば独国特許出願公開第10013186号又は独国特許出願公開第10013187号から知られるもののような、超分岐(Hyperbranched)ポリイソシアネート。
10)アルコールとのジイソシアネート及び/又はポリイソシアネート由来のポリウレタン−ポリイソシアネートプレポリマー。
11)ポリ尿素−ポリイソシアネートプレポリマー。
12)調製した後、ポリイソシアネート1)〜11)、好ましくは1)、3)、4)及び6)を、イソシアネート基が芳香族結合、脂環式結合又は脂肪族結合した、好ましくは(脂環式)脂肪族結合したビウレット基又はウレタン/アロファネート基を有するポリイソシアネートへと転換させることができる。ビウレット基は、例えば水を添加するか、又はアミンと反応させることによって形成される。ウレタン基及び/又はアロファネート基は、必要に応じて好適な触媒の存在下での一価アルコール、二価アルコール又は多価アルコール、好ましくは一価アルコールとの反応によって形成される。これらのビウレット基又はウレタン/アロファネート基を有するポリイソシアネートは概して、18wt%〜22wt%のNCO含有量及び2.8〜6の平均NCO官能価を有する。
13)親水性に改質した(Hydrophilically modified)ポリイソシアネート、すなわち、1〜12に記載される基に加えて、形式的には分子のイソシアネート基に、NCO反応基及び親水化(hydrophilizing)基を付加することによって形成される基を含有するポリイソシアネート。親水化基は、アルキルポリエチレンオキサイド等の非イオン基、及び/又はリン酸、ホスホン酸、硫酸若しくはスルホン酸、若しくはその塩に由来するイオン基である。
14)二重硬化用途のために改質したポリイソシアネート、すなわち、1〜12に記載される基に加えて、形式的には分子のイソシアネート基に、NCO反応基及びUV又は化学線によって架橋可能な基を付加することによって形成される基を含有するポリイソシアネート。これらの分子は、例えばヒドロキシアルキル(メタ)アクリレート及び他のヒドロキシビニル化合物である。
N−ビニルホルムアミド:
50wt%〜100wt%、好ましくは80wt%〜99.5wt%、特に好ましくは90wt%〜99wt%、とりわけ好ましくは95wt%〜99wt%。
水溶性カチオンモノマー(複数も可):
0wt%〜20wt%、好ましくは0.5wt%〜10wt%、特に好ましくは1wt%〜5wt%、とりわけ好ましくは1wt%〜5wt%。
他のモノマー(複数も可):
0wt%〜30wt%、好ましくは0wt%〜10wt%、特に好ましくは0wt%〜5wt%、とりわけ好ましくは0wt%。
エチレン−イミンのホモポリマー、
少なくとも二官能性の架橋剤で架橋されるポリエチレン−イミン、
エチレン−イミンでグラフトされ、少なくとも二官能性の架橋剤で架橋されるポリアミドアミン、
アミド化ポリエチレン−イミンを生成する、モノカルボン酸とのポリエチレン−イミンの反応生成物、
エチレン性不飽和酸、モノエチレン性不飽和酸の塩、エステル、アミド又はニトリル上へのポリエチレン−イミンのマイケル付加生成物、
ホスホノメチル化ポリエチレン−イミン、
カルボキシル化ポリエチレン−イミン、及び
アルコキシル化ポリエチレン−イミン
である。
(a1)マレイン酸又はその誘導体、
(a2)少なくとも1つの環状ジカルボン酸又はその誘導体、
(a3)少なくとも1つの脂肪族ジオール又は脂環式ジオール。
モノマー形態又は同様にポリマー形態の問題の無水物、
モノアルキルエステル若しくはジアルキルエステル、好ましくはモノ−C1〜C4−アルキルエステル若しくはジ−C1〜C4−アルキルエステル、特に好ましくはモノメチルエステル若しくはジメチルエステル、又は対応するモノエチルエステル若しくはジエチルエステル、
他のモノビニルエステル及びジビニルエステル、並びに、
混合エステル、好ましくは種々のC1〜C4−アルキル成分を含む混合エステル、特に好ましくは混合メチルエチルエステル。
(a1)(a)中に存在する全てのカルボキシル基及びその誘導体に対して30mol%〜70mol%、好ましくは40mol%〜60mol%、
(a2)(a)中に存在する全てのカルボキシル基及びその誘導体に対して30mol%〜70mol%、好ましくは40mol%〜60mol%、
(a3)(a)中に存在する全てのヒドロキシル基に対して80mol%〜100mol%、好ましくは100mol%、
(a4)(a)中に存在する全てのカルボキシル基及びその誘導体に対して0mol%〜20mol%、好ましくは0mol%、
(a5)(a)中に存在する全てのカルボキシル基及びその誘導体に対して0mol%〜5mol%、好ましくは0mol%、
(a6)(a)中に存在する全てのヒドロキシル基に対して0mol%〜20mol%、好ましくは0mol%、並びに、
(a7)(a)中に存在する全てのヒドロキシル基に対して0mol%〜5mol%、好ましくは0mol%。但し、全てのヒドロキシル基の合計は100mol%であり、全てのカルボキシル基の合計は100mol%であり、ヒドロキシル基対カルボキシル基の化学量論比は、1:0.85〜1:1.25、好ましくは1:0.9〜1:1.2、特に好ましくは1:0.95〜1:1.15である。
(a)少なくとも1つの有機脂肪族、芳香族又は脂環式ジイソシアネート又はポリイソシアネート、例えば二成分コーティング化合物について上記で記載したポリイソシアネートのうちの少なくとも1つ、
(b)イソシアネートに反応性の少なくとも1つの基を有する少なくとも1つの化合物、好ましくはポリアクリレートポリオールについて上記で記載したヒドロキシル基、及び少なくとも1つのラジカル重合性不飽和基を保有するモノマーのうちの1つ、並びに、
(c)必要に応じて、イソシアネートに反応性の少なくとも2つの基を有する少なくとも1つの化合物、例えばポリエステロールについて上記で記載した多価アルコールのうちの1つ。
少なくとも1つのポリエステル(メタ)アクリレート、ポリエーテル(メタ)アクリレート、カーボネート(メタ)アクリレート、エポキシ(メタ)アクリレート及び/又はウレタン(メタ)アクリレート、又は不飽和ポリエステル樹脂、
必要に応じて少なくとも1つの反応性シンナー、
必要に応じて少なくとも1つの光開始剤、
必要に応じて少なくとも1つの溶媒、
必要に応じて少なくとも1つの安定化剤、
必要に応じて少なくとも1つの、活性化剤、充填剤、顔料、染料、増粘剤、チキソトロープ剤、界面活性剤、粘度調整剤、可塑剤及びキレート剤からなる群から選択される添加剤。
40wt%〜100wt%の少なくとも1つのポリエステル(メタ)アクリレート、ポリエーテル(メタ)アクリレート、カーボネート(メタ)アクリレート、エポキシ(メタ)アクリレート若しくはウレタン(メタ)アクリレート、又は不飽和ポリエステル樹脂、
0wt%〜60wt%の少なくとも1つの反応性シンナー、
0wt%〜5wt%の少なくとも1つの光開始剤、
0wt%〜20wt%の少なくとも1つの溶媒、
0wt%〜5wt%の少なくとも1つの安定化剤、
活性化剤、充填剤、顔料、染料、増粘剤、チキソトロープ剤、界面活性剤、粘度調整剤、可塑剤及びキレート剤からなる群から選択される、0wt%〜5wt%の少なくとも1つの添加剤(但し、合計が常に100wt%となる)。
R5及びR6は互いに独立して、水素、又はアリール、アルキル、アリールオキシ、アルキルオキシ、ヘテロ原子及び/若しくは複素環で任意に置換されるC1〜C18−アルキルを表し、
u、v、w、xは各々、互いに独立して、1〜10、好ましくは1〜5、特に好ましくは1〜3の整数を表し、
uに対してi=1、vに対してi=1、wに対してi=1、xに対してi=1の場合の各Xiは互いに独立して、−CH2−CH2−O−、−CH2−CH(CH3)O−、−CH(CH3)CH2−O−、−CH2−C(CH3)2−O−、−C(CH3)2−CH2−O−、−CH2−CHVin−O−、−CHVin−CH2−O−、−CH2−CHPh−O−及び−CHPh−CH2−O−の群から、好ましくは−CH2−CH2−O−、−CH2−CH(CH3)O−及び−CH(CH3)CH2−O−の群から選択することができ、特に好ましくは−CH2−CH2−O−であり、
Phはフェニルを表し、Vinはビニルを表す)
の化合物である。
−ビス(ジメチルアミノ)ベンゾフェノン、4−フェニルベンゾフェノン、4−クロロベンゾフェノン、ミヒラーケトン、o−メトキシベンゾフェノン、2,4,6−トリメチルベンゾフェノン、4−メチルベンゾフェノン、2,4−ジメチルベンゾフェノン、4−イソプロピルベンゾフェノン、2−クロロベンゾフェノン、2,2’−ジクロロベンゾフェノン、4−メトキシベンゾフェノン、4−プロポキシベンゾフェノン又は4−ブトキシベンゾフェノンであり、α−ヒドロキシ−アルキル−アリールケトンは、例えば、1−ベンゾイルシクロヘキサン−1−オール(1−ヒドロキシ−シクロヘキシル−フェニルケトン)、2−ヒドロキシ−2,2−ジメチルアセトフェノン、(2−ヒドロキシ−2−メチル−1−フェニル−プロパン−1−オン)、1−ヒドロキシアセトフェノン、1−[4−(2−ヒドロキシエトキシ)フェニル]−2−ヒドロキシ−2−メチル−1−プロパン−1−オン、又は重合によって組み込まれる2−ヒドロキシ−2−メチル−1−(4−イソプロペン−2−イル−フェニル)プロパン−1−オンを含有するポリマーである。
2−フェノキシエチルアクリレート(POEA);
ジプロピレングリコールジアクリレート(DPGDA);
ジプロピレングリコール及びアジピン酸(等モル)から構成される、約600g/molの分子量を有するポリエステロールと、1.2当量(ヒドロキシル基当たりのカルボン酸基)のアクリル酸とを反応させた後、未反応のアクリル酸と1当量(カルボン酸基当たりのエポキシ基)のビスフェノール−A−ジグリシジルエーテルとを反応させ、アクリレート基を2wt%のエチレンジアミンで活性化することによって得ることが可能なアミン修飾ポリエステルアクリレート(PESA);
2当量のアクリル酸とブタンジオールジグリシドエーテル(BDGEA)との反応生成物;
トリメチロールプロパンホルマールモノアクリレート(TMPFMA);
およそ500g/molの分子量を有する、アジピン酸及びネオペンチルグリコールに由来するポリエステルジオールと、2当量のイソホロンジイソシアネート及び2当量のヒドロキシエチルアクリレートとの反応の生成物(UA 1);
トリメチロールプロパンと、3当量のエチレンオキサイド及び3当量のアクリル酸との反応の生成物(ETMPTA);
トリメチロールプロパンと、3当量のエチレンオキサイド及び3当量のアクリル酸との反応、並びに4wt%のジエタノールアミンによるアクリレート基の活性化の生成物(ETMPTA−A);
およそ400g/molの分子量を有するカプロラクトンジオールと、イソフタル酸との、OH価が36mg KOH/gのポリエステルジオールへの反応、並びにポリエステルジオールと、各々2当量のイソホロンジイソシアネート及びヒドロキシエチルアクリレートとの反応の生成物(UA 2)。
5wt%〜80wt%、好ましくは10wt%〜50wt%、又は15wt%〜30wt%の含有量のPOEA;
5wt%〜35wt%、好ましくは7wt%〜30wt%、又は15wt%〜25wt%の含有量のDPGDA;
10wt%〜80wt%、好ましくは15wt%〜75wt%、又は50wt%〜75wt%の含有量のPESA
を有するが、ただし、既に記載された考え得る添加剤を加えた値が合計100wt%となる。
30wt%のETMPTA及び3.5%のLucirin(商標)TPO−L(エチル−2,4,6−トリメチルベンゾイルフェニルホスフィネート、BASF SE(Ludwigshafen)の光開始剤)を添加した、58wt%のn−ブチルアクリレート、40wt%のメチルメタクリレート及び2wt%のアクリル酸の重合によって得られるポリアクリレートの分散液(ポリアクリレートのガラス転移温度:0℃)を、基板に20μmの厚さでコーティングした。この混合物の粘度は10kPasであった。
接着性の決定のために、直径2.5mmのサファイア球を試料に2μm/秒の速度で押し付けた。入力パラメータは「圧電変位」である。これは、測定時の試料の変位を与えるものである。サファイア球を固定した測定ばねの偏向が出力信号として得られる。較正によって、測定時に生じる力を決定することが可能となる。図5では、正の力は試料に負荷した荷重に対応し、負の力は接着性を表す。予荷重に応じた接着性の測定については、球を試料に最大で対応する予荷重(測定ばねの偏向×ばね定数に対応する)まで押し付けた。接着力(引き離し力)は、球を引いた際の測定ばねの偏向から得ることができる。
硬化したブレンドの押込み弾性率を、TI950 Nanoindenter機器(Hysitron Inc.(Minneapolis,MN,USA))を用いて測定した。ベルコビッチチップを使用した。試料の予荷重は500nNであった。各々の測定の前に、チップを試料と所与の予荷重で10分間接触させて、系を安定させ、熱ドリフトを最小限に抑えた。押込みは以下の3部荷重曲線を用いて変位制御下で行った:最初に、侵入深さ2000nmまでの200nm/秒での第1の線形荷重(押込み時間:10秒)、続いて最大荷重で30秒の保持時間、その後200nm/秒での荷重低減(後退時間:10秒)。ベルコビッチチップの面積は、侵入深さ30nm〜140nmを用いた石英標準(石英ガラス)に対する測定によって推定した。算出されたベルコビッチチップのチップ直径は50nm〜60nmであった。1つの試料当たり20回の試験を行った。Oliver−Pharr法を、硬化した試料の弾性係数の算出に用いた。
ポリジメチルシロキサン(PDMS)からの金型の作製(「オリジナル構造」)
組成物を、10:1の比率のPDMS Sylgard 184ベース及びPDMS Sylgard 184硬化剤(どちらもDow Corning(Midland,MI))から調製した。混合物を、気泡形成を防止するために真空下で1時間脱気した。混合物を、構造化シリコン表面(ウエハー上の構造はフォトリソグラフィー及び「反応性イオンエッチング(Elmar)」によって作製した)に塗布し、95℃で14時間硬化した。
実施例1からのPDMS金型の表面を、作製した構造化表面からの金型の良好な剥離性を確実にするために、トリクロロ(1H,1H,2H,2H−ペルフルオロオクチル)シランの自己組織化単分子層(SAM)で処理した。
構造化ニッケル表面はTemicon社から購入した。これは、直径4μm、長さ15μmのミクロ構造を有する。
実施例3からの金型の表面を、プラズマで活性化した後、金型の容易な剥離を確実にするためにトリクロロ(1H,1H,2H,2H−ペルフルオロオクチル)シランで改質した。
形成による構造の作製
軟質形成(Soft forming)は、実施例2からのPDMS金型を用いて行った。厚さ75μmのPETフィルムのフレームを金型に適用した。このPETフィルムの厚さは、続くポリアクリレート層のエンボス加工されていない部分の厚さに比例する。UV硬化ポリアクリレートブレンド(ブレンド1、ブレンド2、ブレンド3及びブレンド4)を、フレームによって区切られた金型の領域に投入した。次いで、PETフィルムをブレンドに押し付けた。このPETフィルムは後に構造化表面の基板となる。ポリアクリレートブレンドにUV光を5分間照射した後、金型から剥離した。使用した光源は、短波1000 W Hg(Xe)ランプ(Lot-Oriel instruments)であった。UVランプの強度は、試料とランプとの距離が4cmで28.4mWであった。300秒間に144.676mW/cm2というスペクトル照射密度で、43402.8mJ/cm2の光エネルギーが表面に伝達した。照射時に、金型及びポリアクリレート層を接触させた。作製した構造を図9〜図11に示す。a)の場合、鋳物がPDMSから作製した。
硬質金型を用いた形成による微細構造の作製
方法は、実施例3からのニッケル金型を用いて行った。厚さ75μmのPETフィルムのフレームを、スペーサーとして金型上に適用した。フィルムの厚さは、ポリアクリレート層の後にエンボス加工されない部分の厚さに比例する。UV硬化ポリアクリレートブレンド(ブレンド2)を、フレームによって囲まれる母型の領域に投入した。次いで、PETフィルムを液状塊に押し付けた。このフィルムは、後に構造化したコーティングの支持基板ともなる。5分後に、PETフィルム及び硬化したポリアクリレートブレンドを金型から剥離した。曝露に使用した光源は、短波1000 W Hg(Xe)ランプ(Lot-Oriel instruments)であった。UVランプの強度は、試料とランプとの距離が4cmで28.4mWであった。300秒間に144.676mW/cm2というスペクトル照射密度で、43402.8mJ/cm2の光エネルギーが基板に伝達した。曝露時に、ポリアクリレート層及び金型を接触させた。
構造S1用の金型を、干渉リソグラフィを用いて六角形構造(六角形配置)のための3波セットアップで作製した。そのために、3つのビームを重畳して干渉パターンを作製する。これにより、鋭い六角形の構造を作製することが可能となる。3つのレンズからの3つのビームは、曝露される表面に規定の角度で衝突する。この角度は、得られるパターンのピッチを規定する。3つのレンズを正三角形の形態で配置して、対称なパターンを得ることができる。レンズからの基板の距離及びレンズ間の距離は角度、したがって干渉の強度分布のピッチを決定する。例えば、18.4cmという三角形の辺に沿うレンズの距離、及び3.5mという基板からの距離では、8μmの標的ピッチを得ることができる(レーザーの波長は363.8nm)。使用したフォトレジストは、AZ Electronic Materials社のフォトレジストAZ9260であった。水酸化カリウム溶液を現像に使用した。PDMSにおけるレプリカを図1に示す。
構造S2用の金型を実施例7と同様に作製した。ただし、ラインを得るために、単純な曝露を用いる2波セットアップのみを使用した。図2はPDMSにおけるレプリカを示す。
構造S3用の金型の作製は実施例7と同様であるが、90度の試料の回転による二重曝露を用いる2波セットアップの干渉リソグラフィを用いた。このようにして突起の十字格子構造が得られる。
ニッケル製の金型(実施例3と同様;穴径5μm;深さ15μm)を、ロールツーロール印刷機のロールに取り付けた。ブレンド3をPETフィルムに400μmの厚さで塗布し、圧力をかけずに金型と接触させた。ブレンドを金型と接触させながら、光に5分間曝露した。1000Wアークランプ(Thermo-Oriel instruments)を使用した。UVランプの強度は、試料とランプとの距離が4cmで20.3mWであった。300秒間に103.41mW/cm2というスペクトル照射密度で、31023.94mJ/cm2の光エネルギーが表面に伝達した。図7及び図8に示される構造が得られた。金型はきれいに複製されたが、金型の僅かに不完全な充填が存在した。
構造化PETフィルム片の可能な剪断負荷を測定した。そのために、構造をブレンド5(5分間のUV硬化による印刷プロセス(UV硬化前の粘度:39mPas、弾性係数:4MPa)及びブレンド6(5分間のUV硬化による印刷プロセス(UV硬化前の粘度:91mPas、弾性係数:3MPa)という2つの試料を用いて作製した。図23(ブレンド5)及び図24(ブレンド6)は作製した構造を示す。
50 レーザー干渉計
52 ガラスばね及び測定基板
54 圧電素子
56 6軸テーブル
60 アプローチ
62 予荷重
64 試料を反対方向に戻す(後退)
66 試料剥離力(引き離し力)
100 光に対する曝露の強度分布
101 金型基板
102 ネガ型フォトレジストの層
104 ネガ型フォトレジストの層
106 曝露の強度分布(ピッチ)
108 台座構造
110 全ての層の現像
112 微細構造を有する金型
114 金型の複製
116 複製されたエラストマー
130 曝露されたフォトレジスト
132 曝露されないフォトレジスト
134 エラストマー
200 スタンプ
202 エンボス加工したフォトレジストの層
204 フォトレジスト
206 エンボス加工したフォトレジストの層
208 曝露の強度分布
210 台座構造
212 全ての層の現像
214 微細構造を有する金型
216 金型の複製
218 複製されたエラストマー
300 金型基板
310 レーザ
320 ビーム分割器
330 反射鏡
340 レンズ
350 干渉領域
400 金型基板
410 レーザ
420 ビーム分割器
430 反射鏡
440 λ/2−プレート
450 レンズ
460 ダイヤフラム
470 干渉領域
Claims (3)
- アスペクト比が少なくとも0.5の微細構造を有するコーティング表面を作製する方法であって、
a)少なくとも1つの放射線硬化性コーティング化合物を、少なくとも1つの基板上に塗布する工程と、
b)微細構造のネガを有する金型を用いて微細構造を形成する工程であって、
b1)前記金型を前記基板上の前記放射線硬化性コーティング化合物に押し付けるか、又は
b2)工程a)の前記基板が前記金型を含有する、
微細構造を形成する工程と、
c)得られた微細構造を有する放射線硬化性コーティング化合物を硬化させるとともに、実質的に硬化したコーティングを得る工程と、
d)前記微細構造を有するコーティングを前記金型から分離する工程と、
を含み、工程d)と工程c)とを逆の順序で行ってもよく、
前記放射線硬化性コーティング化合物が、アクリル酸エステル、メタクリル酸エステル又は不飽和ポリエステル樹脂であり、
前記放射線硬化性コーティング化合物が、無溶媒状態で、600mPas以下の粘度(25℃でのプレート/円錐形状を用いたDIN 53018−1に従う回転粘度測定法、温度制御:ペルチェ、測定装置:10〜1000 l×s−1の剪断勾配DでのHC 60/1)を有し、
前記放射線硬化性コーティング化合物が、多くとも6.0mol/kgの二重結合密度を有し、
前記硬化したコーティングが、少なくとも1MPa、最大で20MPaの弾性係数(ベルコビッチチップ、試験片の係数に応じて0.1mN〜1mNの予荷重を用いた押込み、押込み時間:10秒、保持時間:30秒、及び後退時間:10秒、ポリカーボネートに対する較正)を有する、
アスペクト比が少なくとも0.5の微細構造を有するコーティング表面を作製する方法。 - 前記基板がPET、PP、PE及びPMMAからなる群から選択されることを特徴とする、請求項1に記載の方法。
- 前記金型が、幅2μm〜20μmの円筒状の窪みを1以上有し、該窪みの底面に幅200nm〜1μmの別の円筒状の窪みを1以上有する階層微細構造を有する金型であることを特徴とする、請求項1又は2に記載の方法。
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- 2011-07-06 WO PCT/EP2011/061440 patent/WO2012004319A1/de active Application Filing
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CN103209770B (zh) | 2014-12-17 |
PL2590757T3 (pl) | 2017-06-30 |
DE102010026490A1 (de) | 2012-01-12 |
EP2590757B1 (de) | 2016-09-07 |
CN103209770A (zh) | 2013-07-17 |
EP2590757A1 (de) | 2013-05-15 |
JP2013539201A (ja) | 2013-10-17 |
WO2012004319A1 (de) | 2012-01-12 |
US10005103B2 (en) | 2018-06-26 |
ES2605956T3 (es) | 2017-03-17 |
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