JP2013510336A - ホログラフィックフィルムの製造方法 - Google Patents
ホログラフィックフィルムの製造方法 Download PDFInfo
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- JP2013510336A JP2013510336A JP2012537368A JP2012537368A JP2013510336A JP 2013510336 A JP2013510336 A JP 2013510336A JP 2012537368 A JP2012537368 A JP 2012537368A JP 2012537368 A JP2012537368 A JP 2012537368A JP 2013510336 A JP2013510336 A JP 2013510336A
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- photopolymer
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- MHCLJIVVJQQNKQ-UHFFFAOYSA-N ethyl carbamate;2-methylprop-2-enoic acid Chemical class CCOC(N)=O.CC(=C)C(O)=O MHCLJIVVJQQNKQ-UHFFFAOYSA-N 0.000 description 1
- 230000005284 excitation Effects 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 229920001002 functional polymer Polymers 0.000 description 1
- 238000007646 gravure printing Methods 0.000 description 1
- 235000019382 gum benzoic Nutrition 0.000 description 1
- 229910052736 halogen Inorganic materials 0.000 description 1
- 150000002367 halogens Chemical class 0.000 description 1
- LNCPIMCVTKXXOY-UHFFFAOYSA-N hexyl 2-methylprop-2-enoate Chemical compound CCCCCCOC(=O)C(C)=C LNCPIMCVTKXXOY-UHFFFAOYSA-N 0.000 description 1
- 125000004051 hexyl group Chemical group [H]C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])* 0.000 description 1
- LNMQRPPRQDGUDR-UHFFFAOYSA-N hexyl prop-2-enoate Chemical compound CCCCCCOC(=O)C=C LNMQRPPRQDGUDR-UHFFFAOYSA-N 0.000 description 1
- 239000000852 hydrogen donor Substances 0.000 description 1
- 150000002440 hydroxy compounds Chemical class 0.000 description 1
- 238000005286 illumination Methods 0.000 description 1
- 238000003384 imaging method Methods 0.000 description 1
- 150000002460 imidazoles Chemical class 0.000 description 1
- 125000001841 imino group Chemical group [H]N=* 0.000 description 1
- 230000000977 initiatory effect Effects 0.000 description 1
- 239000000976 ink Substances 0.000 description 1
- 239000013067 intermediate product Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 229940119545 isobornyl methacrylate Drugs 0.000 description 1
- XJRAOMZCVTUHFI-UHFFFAOYSA-N isocyanic acid;methane Chemical compound C.N=C=O.N=C=O XJRAOMZCVTUHFI-UHFFFAOYSA-N 0.000 description 1
- 238000009533 lab test Methods 0.000 description 1
- 150000003951 lactams Chemical class 0.000 description 1
- 239000005001 laminate film Substances 0.000 description 1
- PBOSTUDLECTMNL-UHFFFAOYSA-N lauryl acrylate Chemical compound CCCCCCCCCCCCOC(=O)C=C PBOSTUDLECTMNL-UHFFFAOYSA-N 0.000 description 1
- 239000003446 ligand Substances 0.000 description 1
- 239000012669 liquid formulation Substances 0.000 description 1
- 239000011344 liquid material Substances 0.000 description 1
- VXWPONVCMVLXBW-UHFFFAOYSA-M magnesium;carbanide;iodide Chemical compound [CH3-].[Mg+2].[I-] VXWPONVCMVLXBW-UHFFFAOYSA-M 0.000 description 1
- FDZZZRQASAIRJF-UHFFFAOYSA-M malachite green Chemical compound [Cl-].C1=CC(N(C)C)=CC=C1C(C=1C=CC=CC=1)=C1C=CC(=[N+](C)C)C=C1 FDZZZRQASAIRJF-UHFFFAOYSA-M 0.000 description 1
- 229940107698 malachite green Drugs 0.000 description 1
- VZCYOOQTPOCHFL-UPHRSURJSA-N maleic acid Chemical compound OC(=O)\C=C/C(O)=O VZCYOOQTPOCHFL-UPHRSURJSA-N 0.000 description 1
- 150000002688 maleic acid derivatives Chemical class 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 238000011177 media preparation Methods 0.000 description 1
- 150000007522 mineralic acids Chemical class 0.000 description 1
- 229920006030 multiblock copolymer Polymers 0.000 description 1
- DLSOILHAKCBARI-UHFFFAOYSA-N n-benzyl-2-methylpropan-2-amine Chemical compound CC(C)(C)NCC1=CC=CC=C1 DLSOILHAKCBARI-UHFFFAOYSA-N 0.000 description 1
- CXOYJPWMGYDJNW-UHFFFAOYSA-N naphthalen-2-yl 2-methylprop-2-enoate Chemical compound C1=CC=CC2=CC(OC(=O)C(=C)C)=CC=C21 CXOYJPWMGYDJNW-UHFFFAOYSA-N 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 238000006386 neutralization reaction Methods 0.000 description 1
- 150000002825 nitriles Chemical class 0.000 description 1
- 229920001220 nitrocellulos Polymers 0.000 description 1
- 125000002347 octyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 238000005457 optimization Methods 0.000 description 1
- 150000002902 organometallic compounds Chemical class 0.000 description 1
- WPRDEDGZJLTOFJ-UHFFFAOYSA-N oxadiazin-4-imine Chemical group N=C1C=CON=N1 WPRDEDGZJLTOFJ-UHFFFAOYSA-N 0.000 description 1
- 150000002923 oximes Chemical class 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 125000003854 p-chlorophenyl group Chemical group [H]C1=C([H])C(*)=C([H])C([H])=C1Cl 0.000 description 1
- NWVVVBRKAWDGAB-UHFFFAOYSA-N p-methoxyphenol Chemical compound COC1=CC=C(O)C=C1 NWVVVBRKAWDGAB-UHFFFAOYSA-N 0.000 description 1
- 238000004806 packaging method and process Methods 0.000 description 1
- 239000003973 paint Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- QIWKUEJZZCOPFV-UHFFFAOYSA-N phenyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC1=CC=CC=C1 QIWKUEJZZCOPFV-UHFFFAOYSA-N 0.000 description 1
- WRAQQYDMVSCOTE-UHFFFAOYSA-N phenyl prop-2-enoate Chemical compound C=CC(=O)OC1=CC=CC=C1 WRAQQYDMVSCOTE-UHFFFAOYSA-N 0.000 description 1
- FAQJJMHZNSSFSM-UHFFFAOYSA-N phenylglyoxylic acid Chemical compound OC(=O)C(=O)C1=CC=CC=C1 FAQJJMHZNSSFSM-UHFFFAOYSA-N 0.000 description 1
- 238000006303 photolysis reaction Methods 0.000 description 1
- 230000015843 photosynthesis, light reaction Effects 0.000 description 1
- 239000002985 plastic film Substances 0.000 description 1
- 229920006255 plastic film Polymers 0.000 description 1
- 230000010287 polarization Effects 0.000 description 1
- 229920000233 poly(alkylene oxides) Polymers 0.000 description 1
- 229920003229 poly(methyl methacrylate) Polymers 0.000 description 1
- 229920002492 poly(sulfone) Polymers 0.000 description 1
- 229920002037 poly(vinyl butyral) polymer Polymers 0.000 description 1
- 229920002647 polyamide Polymers 0.000 description 1
- 229920001707 polybutylene terephthalate Polymers 0.000 description 1
- 239000004926 polymethyl methacrylate Substances 0.000 description 1
- 229920001155 polypropylene Polymers 0.000 description 1
- 229920001296 polysiloxane Polymers 0.000 description 1
- 229920002223 polystyrene Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- HJWLCRVIBGQPNF-UHFFFAOYSA-N prop-2-enylbenzene Chemical compound C=CCC1=CC=CC=C1 HJWLCRVIBGQPNF-UHFFFAOYSA-N 0.000 description 1
- 125000001325 propanoyl group Chemical group O=C([*])C([H])([H])C([H])([H])[H] 0.000 description 1
- AOHJOMMDDJHIJH-UHFFFAOYSA-N propylenediamine Chemical compound CC(N)CN AOHJOMMDDJHIJH-UHFFFAOYSA-N 0.000 description 1
- 239000011241 protective layer Substances 0.000 description 1
- 150000003217 pyrazoles Chemical class 0.000 description 1
- INCIMLINXXICKS-UHFFFAOYSA-M pyronin Y Chemical compound [Cl-].C1=CC(=[N+](C)C)C=C2OC3=CC(N(C)C)=CC=C3C=C21 INCIMLINXXICKS-UHFFFAOYSA-M 0.000 description 1
- 150000005838 radical anions Chemical class 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 238000007151 ring opening polymerisation reaction Methods 0.000 description 1
- 238000007142 ring opening reaction Methods 0.000 description 1
- 239000005060 rubber Substances 0.000 description 1
- 238000007650 screen-printing Methods 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 150000003335 secondary amines Chemical class 0.000 description 1
- 125000000467 secondary amino group Chemical group [H]N([*:1])[*:2] 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 239000000600 sorbitol Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- RWSOTUBLDIXVET-UHFFFAOYSA-O sulfonium Chemical compound [SH3+] RWSOTUBLDIXVET-UHFFFAOYSA-O 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- SJMYWORNLPSJQO-UHFFFAOYSA-N tert-butyl 2-methylprop-2-enoate Chemical compound CC(=C)C(=O)OC(C)(C)C SJMYWORNLPSJQO-UHFFFAOYSA-N 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
- DTIFFPXSSXFQCJ-UHFFFAOYSA-N tetrahexylazanium Chemical compound CCCCCC[N+](CCCCCC)(CCCCCC)CCCCCC DTIFFPXSSXFQCJ-UHFFFAOYSA-N 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 125000004149 thio group Chemical group *S* 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
- RYYWUUFWQRZTIU-UHFFFAOYSA-K thiophosphate Chemical compound [O-]P([O-])([O-])=S RYYWUUFWQRZTIU-UHFFFAOYSA-K 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical class 0.000 description 1
- 239000012780 transparent material Substances 0.000 description 1
- 150000003852 triazoles Chemical class 0.000 description 1
- 239000013638 trimer Substances 0.000 description 1
- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical compound OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 0.000 description 1
- 150000004072 triols Chemical class 0.000 description 1
- MDCWDBMBZLORER-UHFFFAOYSA-N triphenyl borate Chemical compound C=1C=CC=CC=1OB(OC=1C=CC=CC=1)OC1=CC=CC=C1 MDCWDBMBZLORER-UHFFFAOYSA-N 0.000 description 1
- AAAQKTZKLRYKHR-UHFFFAOYSA-N triphenylmethane Chemical compound C1=CC=CC=C1C(C=1C=CC=CC=1)C1=CC=CC=C1 AAAQKTZKLRYKHR-UHFFFAOYSA-N 0.000 description 1
- LENZDBCJOHFCAS-UHFFFAOYSA-N tris Chemical compound OCC(N)(CO)CO LENZDBCJOHFCAS-UHFFFAOYSA-N 0.000 description 1
- KGLSETWPYVUTQX-UHFFFAOYSA-N tris(4-isocyanatophenoxy)-sulfanylidene-$l^{5}-phosphane Chemical compound C1=CC(N=C=O)=CC=C1OP(=S)(OC=1C=CC(=CC=1)N=C=O)OC1=CC=C(N=C=O)C=C1 KGLSETWPYVUTQX-UHFFFAOYSA-N 0.000 description 1
- JEVGKYBUANQAKG-UHFFFAOYSA-N victoria blue R Chemical compound [Cl-].C12=CC=CC=C2C(=[NH+]CC)C=CC1=C(C=1C=CC(=CC=1)N(C)C)C1=CC=C(N(C)C)C=C1 JEVGKYBUANQAKG-UHFFFAOYSA-N 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- CHJMFFKHPHCQIJ-UHFFFAOYSA-L zinc;octanoate Chemical compound [Zn+2].CCCCCCCC([O-])=O.CCCCCCCC([O-])=O CHJMFFKHPHCQIJ-UHFFFAOYSA-L 0.000 description 1
- 229910052726 zirconium Inorganic materials 0.000 description 1
Images
Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N5/00—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid
- G01N5/04—Analysing materials by weighing, e.g. weighing small particles separated from a gas or liquid by removing a component, e.g. by evaporation, and weighing the remainder
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03H—HOLOGRAPHIC PROCESSES OR APPARATUS
- G03H1/00—Holographic processes or apparatus using light, infrared or ultraviolet waves for obtaining holograms or for obtaining an image from them; Details peculiar thereto
- G03H1/02—Details of features involved during the holographic process; Replication of holograms without interference recording
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03H—HOLOGRAPHIC PROCESSES OR APPARATUS
- G03H1/00—Holographic processes or apparatus using light, infrared or ultraviolet waves for obtaining holograms or for obtaining an image from them; Details peculiar thereto
- G03H1/04—Processes or apparatus for producing holograms
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B7/00—Recording or reproducing by optical means, e.g. recording using a thermal beam of optical radiation by modifying optical properties or the physical structure, reproducing using an optical beam at lower power by sensing optical properties; Record carriers therefor
- G11B7/24—Record carriers characterised by shape, structure or physical properties, or by the selection of the material
- G11B7/2403—Layers; Shape, structure or physical properties thereof
- G11B7/24035—Recording layers
- G11B7/24044—Recording layers for storing optical interference patterns, e.g. holograms; for storing data in three dimensions, e.g. volume storage
-
- G—PHYSICS
- G11—INFORMATION STORAGE
- G11B—INFORMATION STORAGE BASED ON RELATIVE MOVEMENT BETWEEN RECORD CARRIER AND TRANSDUCER
- G11B7/00—Recording or reproducing by optical means, e.g. recording using a thermal beam of optical radiation by modifying optical properties or the physical structure, reproducing using an optical beam at lower power by sensing optical properties; Record carriers therefor
- G11B7/24—Record carriers characterised by shape, structure or physical properties, or by the selection of the material
- G11B7/241—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material
- G11B7/242—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of recording layers
- G11B7/244—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of recording layers comprising organic materials only
- G11B7/245—Record carriers characterised by shape, structure or physical properties, or by the selection of the material characterised by the selection of the material of recording layers comprising organic materials only containing a polymeric component
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03H—HOLOGRAPHIC PROCESSES OR APPARATUS
- G03H1/00—Holographic processes or apparatus using light, infrared or ultraviolet waves for obtaining holograms or for obtaining an image from them; Details peculiar thereto
- G03H1/02—Details of features involved during the holographic process; Replication of holograms without interference recording
- G03H2001/026—Recording materials or recording processes
- G03H2001/0264—Organic recording material
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03H—HOLOGRAPHIC PROCESSES OR APPARATUS
- G03H2227/00—Mechanical components or mechanical aspects not otherwise provided for
- G03H2227/04—Production line for mass production
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03H—HOLOGRAPHIC PROCESSES OR APPARATUS
- G03H2260/00—Recording materials or recording processes
- G03H2260/12—Photopolymer
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- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03H—HOLOGRAPHIC PROCESSES OR APPARATUS
- G03H2260/00—Recording materials or recording processes
- G03H2260/50—Reactivity or recording processes
- G03H2260/54—Photorefractive reactivity wherein light induces photo-generation, redistribution and trapping of charges then a modification of refractive index, e.g. photorefractive polymer
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- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- Life Sciences & Earth Sciences (AREA)
- Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Polyurethanes Or Polyureas (AREA)
- Holo Graphy (AREA)
- Optical Record Carriers And Manufacture Thereof (AREA)
Abstract
Description
i)成分として、
A)マトリックスポリマー、
B)書込モノマー、
C)光開始剤系、
D)必要に応じて、非光重合性成分、および
E)必要に応じて、触媒、フリーラジカル安定剤、溶媒、添加剤および他の補助剤および/または添加剤
を含むフォトポリマー処方物を供給し、
ii)フォトポリマー処方物を、フィルムとして基材へ広範囲に塗布し、および
iii)フォトポリマー処方物を、60<T<120℃の温度にて基材上で乾燥させ、
フォトポリマー処方物について選択された成分は、TGA95値が、>100℃であり、および温度Tより少なくとも30℃高い化合物のみであり、および≧30000Paの平坦弾性率を有するフォトポリマー処方物を用いることを特徴とするホログラフィックフィルムの製造方法により達成される。
−CH2−CH(R)−O− 式I
〔式中、Rは、水素、置換されていてよい、またはヘテロ原子(例えばエーテル酸素等)により中断されていてよいアルキル基またはアリール基である〕
で示されるオキシアルキレン単位から構成され、Yは、基礎となるスターターであり、セグメントXiの割合は、セグメントXiおよびYの全量を基準に少なくとも50重量%を占める。
A)イソシアヌレート、ウレットジオン、イミノオキサジアンジンジオンおよび/またはHDIに基づく他のオリゴマーとの組み合わせにおいて、ブチロラクトン、ε−カプロラクトンおよび/またはメチル−ε−カプロラクトンと1.8〜3.1および200〜4000g/モルの数平均モル質量を有するポリエーテルポリオールとの付加物。特に好ましくは、HDIに基づくオリゴマー、イソシアヌレートおよび/またはイミノオキサジアジンジオンとの組み合わせにおいて、ε−カプロラクトンと1.9〜2.2および500〜2000g/モル(特に600〜1400g/モル)の数平均モル質量を有するポリ(テトラヒドロフラン)との付加物(その数平均全モル質量は800〜4500g/モル、特に1000〜3000g/モルである)。
を有し得、および単官能性書込モノマーは好ましくは、<0℃のガラス転移温度TGおよび好ましくは405nmにて>1.50の屈折率を有する。
を有し得る。さらに多官能性書込モノマーは好ましくは、>1.50の屈折率を405nmにて有し得る。
を有する場合には更に好ましい。本発明では、R10は、特に好ましくは、少なくとも1つのフッ素原子を有する有機基である。
I. まず、必要に応じて1以上の成分B)、C)、D)およびE)と混合した成分a)の輸送および計量、および次に、これとは別に、必要に応じて1以上の成分B)、C)、D)およびE)と混合した成分b)の輸送および計量、
II. I)に従って輸送、計量および必要に応じて予備混合した流れの脱蔵(devolatilization)、
III. II)に従って得られた混合物のろ過、
IV. III)に従って得られた混合物の均質化、
V. 基材物質の巻き出しおよび予備処理、
VI. 基材物質の、工程IV)に従って得られた混合物での被覆、
VII. VI)に従って被覆されたフィルムの乾燥、
VIII. VII)に従って得られた被覆フィルムの積層、
IX. VIII)に従って得られた積層フィルムの巻き取り
1 貯蔵容器
2 計量装置
3 真空脱蔵器
4 フィルター
5 静的ミキサー
6 被覆装置
7 乾燥器
8 ウェブ経路
9 生成物積層
フォトポリマー処方物は、以下のものを含む:
・3次元架橋有機マトリックスポリマーA)。特に好ましくは、3次元架橋ポリマーは、前駆体として、
・イソシアネート成分a)
・およびイソシアネート反応性成分b)
から構成され、
・通常、溶液中で添加する触媒成分E)を用いて架橋させる。
・化学線の作用下でエチレン性不飽和化合物と重合により反応する基(放射線硬化性基)を有し、上記マトリックス中で溶解または分配されるモノマーB)。
・少なくとも1つの光開始剤系C)。
・必要に応じて非光重合性成分D)。
必要に応じて触媒、フリーラジカル安定剤、溶媒、添加剤および他の助剤および/または添加剤E)。
・測定体:コーンCP 25、d=25mm、角度=1度
・コーンおよびプレート間の距離としての測定ギャップ:0.047mm
・測定の継続時間:10秒
・250 1/秒のせん断速度での粘度の決定
各成分のTGA95値は、各成分の試料の約10mgの量を70μLの容積を有するアルミニウムパン中へ計量投入し、小アルミニウムパンを熱天秤、好ましくはMettler−ToledoからのTG50熱天秤の炉へ導入し、試料の質量の損失を、開いた小アルミニウムパンにおいて20K/分の一定炉加熱速度にて計測し、炉の出発温度は30℃であり、終了温度は600℃であり、炉を、決定の間、200mL/分窒素流でフラッシュし、最初に計量した試料の量を基準に5重量%の試料の質量の損失が生じた温度を、各成分のTGA95値として決定することにより決定することができる。
ホログラフィック性能を測定するために、ホログラフィックフィルムの保護フィルムを剥がし、ホログラフィックフィルムをフォトポリマー側に、長さおよび幅が適当である1mm厚ガラス板上へゴムローラーを用いて穏やかな圧力で積層する。このガラスおよびフォトポリマーを含むサンドイッチを用いて、ホログラフィック性能パラメーターDEおよびΔnを決定することができる。
・暴露時間tの間、両シャッター(S)を開いた。
・次いで、シャッター(S)を閉じて、媒体のなお未重合の書込モノマーを5分間拡散させた。
α0=θ0+Ω記録
以下に記載の組成を有する未だ液体処方物を、レオメーター(Anton Paar PhysicaからのModel MCR 301、50℃に予備加熱した炉型CTD 450を有する)のプレート−プレート計測系に導入する。次いでフォトポリマー処方物のマトリックスの硬化性を、時間に関して以下の条件下で測定する:
・プレート空間250μm
・10rad/秒の一定の角振動数ω0および1%の調節変形振幅における振動測定モード
・温度50℃、0ニュートンにて設定した垂直力調節
・G’の一定値G最大に到達するまでまたは3時間以下の貯蔵弾性率G’の記録
物理層厚みを、市販の白色光干渉計、例えばIngenieursbuero FuchsからのFTM−Lite NIR層厚みゲージを用いて決定した。
用いたイソシアネート(成分A)
イソシアネート成分1(成分a1)は、Bayer MaterialScience AG(レーバークーゼン、独国)の実験生成物、ヘキサンジイソシアネート系ポリイソシアネート、イミノオキサジアジンジオンの割合少なくとも30%、NCO含量:23.5%である。
ポリオール1(成分b1)は、Bayer MaterialScience AG(レーバークーゼン、独国)の実験生成物であり、その製法は、以下に記載する。
アクリレート1(成分B1)は、Bayer MaterialScience AG(レーバークーゼン、独国)の実験生成物であり、その製法は、以下に記載する。
共開始剤1テトラブチルアンモニウムトリス(3−クロロ−4−メチルフェニル)(ヘキシル)ボレート、[1147315 11 4]は、Ciba Inc.(バーゼル、スイス)により製造された実験生成物である。
非光重合性成分(成分D1〜D10)は、Bayer MaterialScience AG(レーバークーゼン、独国)の実験生成物であり、その製法は、以下に記載する。
触媒1(成分E1):ウレタン化触媒、ジメチルビス[(1−オキソネオデシル)オキシ]スタンナン、Momentive Performance Chemicals(ウィルトン、コネチカット州、米国)の市販生成物(N−エチルピロリドン中10%濃度溶液として用いた)
BYK(登録商標)310:BYK−Chemie GmbH(ベーゼル、独国)のシリコーン系表面添加剤(成分G1)(キシレン中25%濃度溶液)
ポリオール1(成分b1)の製造
3.621kgの2官能性ポリテトラヒドロフランポリエーテルポリオール(当量500g/モルOH)を、撹拌機を有する20リットル反応容器中へ計量投入し、525mgのDMC触媒を添加した。次いで105℃まで約70rpmにて撹拌しながら加熱した。真空を適用しおよび窒素で3回圧抜きすることにより、空気を窒素に交換した。撹拌速度を300rpmへ上昇させた後、窒素を混合物へ下方より54分間真空ポンプを動かしながら約0.1バールの圧力にて通過させた。その後、0.2バールの圧力を窒素により確立し、363gのプロピレンオキシド(PO)を投入して重合を開始した。その結果、圧力は2.42バールへ増加した。7分後、圧力を0.34バールへ再び低下させ、更なる11.379kgのPOを2時間29分間にわたり2.9バールにて計量投入した。PO計量の終了から47分後、真空を1.9バールの残存圧にて適用し、完全な脱基を行った。生成物を、7.5gのIrganox1076の添加により安定化し、無色の粘性液体(OH価:27.6mgKOH/g、25℃での粘度:1498mPas)として得た。
2475gの2官能性ポリテトラヒドロフランポリエーテルポリオール(当量325g/モルOH)を、撹拌機を有する20リットル反応容器中へ計量投入し、452.6mgのDMC触媒を添加した。次いで105℃まで約70rpmにて撹拌しながら加熱した。真空を適用しおよび窒素で3回圧抜きすることにより、空気を窒素に交換した。撹拌速度を300rpmへ上昇させた後、窒素を混合物へ下方より57分間真空ポンプを動かしながら約0.1バールの圧力にて通過させた。その後、0.5バールの圧力を窒素により確立し、100gのエチレンオキシド(EO)および150gのPOを投入して同時に重合を開始した。その結果、圧力は2.07バールへ増加した。10分後、圧力を0.68バールへ再び低下させ、混合物として更なる5.116kgのEOおよび7.558kgのPOを1時間53分間にわたり2.34バールにて計量投入した。エポキシド計量の終了から31分後、真空を2.16バールの残存圧にて適用し、完全な脱気を行った。生成物を、7.5gのIrganox1076の添加により安定化し、僅かに濁った粘性液体(OH価:27.1mgKOH/g、25℃での粘度:1636mPas)として得た。
まず、0.18gのオクタン酸錫、374.8gのε−カプロラクトンおよび374.8gの2官能性ポリテトラヒドロフランポリエーテルポリオール(当量500g/モルOH)を1リットルフラスコへ導入し、120℃へ加熱し、この温度を、固形分(非揮発性成分の割合)が99.5重量%以上になるまで維持した。その後、冷却を行い、生成物をワックス状固体として得た。
2465gの2官能性ポリテトラヒドロフランポリエーテルポリオール(当量325g/モルOH)を、撹拌機を有する20リットル反応容器中へ計量投入し、450.5mgのDMC触媒を添加した。次いで105℃まで約70rpmにて撹拌しながら加熱した。真空を適用しおよび窒素で3回圧抜きすることにより、空気を窒素に交換した。撹拌速度を300rpmへ上昇させた後、窒素を混合物へ下方より72分間真空ポンプを動かしながら約0.1バールの圧力にて通過させた。その後、0.3バールの圧力を窒素により確立し、242gのプロピレンオキシド(PO)を投入して重合を開始した。その結果、圧力は2.03バールへ増加した。8分後、圧力を0.5バールへ再び低下させ、更なる12.538kgのPOを2時間11分にわたり2.34バールにて計量投入した。エポキシド計量の終了から17分後、真空を1.29バールの残存圧にて適用し、完全な脱気を行った。生成物を、7.5gのIrganox1076の添加により安定化し、無色の粘性液体(OH価:27.8mgKOH/g、25℃での粘度:1165mPas)として得た。
まず、0.1gの2,6−ジ−tert−ブチル−4−メチルフェノール、0.05gのジブチルスズジラウレート(Desmorapid(登録商標)Z、Bayer MaterialScience AG、レーバークーゼン、独国)と、213.07gの酢酸エチル中トリス(p−イソシアナトフェニル)チオホスフェート27%濃度溶液(Desmodur(登録商標)RFE、Bayer MaterialScience AG、レーバークーゼン、独国の生成物)を500ml容丸底フラスコに仕込み、60℃まで加熱した。続いて、42.37gの2−ヒドロキシエチルアクリレートを滴下し、混合物は、イソシアネート含有量が0.1%未満に低下するまで60℃で保持した。この後、冷却し、酢酸エチルを真空により完全に除去した。生成物は、半結晶質固体として得られた。
まず、0.02gの2,6−ジ−tert−ブチル−4−メチルフェノール、0.01gのDesmorapid(登録商標)Z、11.7gの3−(メチルチオ)フェニルイソシアネートを100ml容丸底フラスコに投入し、60℃まで加熱した。続いて、8.2gの2−ヒドロキシエチルアクリレートを滴下し、混合物は、イソシアネート含有量が0.1%未満に低下するまで60℃で更に保持した。次いで冷却した。生成物は淡黄色液体として得られた。
まず、430.2gのDenacol EX 142(Nagase−Chemtex、日本)、129.7gのアクリル酸、1.18gのトリフェニルホスフィンおよび0.0056gの2,6−ジ−tert−ブチル−4−メチルフェノールを、還流冷却器および撹拌器を有する3口フラスコ中へ導入した。空気を混合物へ徐々に通過させ、60℃にて温度制御した。続いて、撹拌を24時間90℃にて行う。157.8mgKOH/gのOH価を有する透明液体を得た。まず、21.3gの該中間生成物および5.2gの2,4−および2,6−トルイデンジイソシアネートの混合物((Desmodur T80、Bayer MaterialScience AG、レーバークーゼン、独国)を還流冷却器および撹拌器を有する3口フラスコ中へ導入した。空気を混合物へ徐々に通過させ、60℃にて温度制御した。初期発熱反応後、生成物を24時間60℃にて撹拌した。0%のNCOを有する無色透明のガラス状生成物を得た。
暗い場所でまたは適当な照明の下で、0.05gの染料1、0.05gの染料2、0.05gの染料4、1.50gの共開始剤1を、3.50gのN−エチルピロリドンにビーカー中で溶解した。この溶液の対応する重量パーセントを、実施例媒体を製造するために用いた。
暗い場所でまたは適当な照明の下で、0.05gの染料1、0.05gの染料3、0.05gの染料4、1.50gの共開始剤1を、3.50gのN−エチルピロリドンにビーカー中で溶解した。この溶液の対応する重量パーセントを、実施例媒体を製造するために用いた。
暗い場所でまたは適当な照明の下で、0.10gの染料1、1.00gの共開始剤1を、3.50gのN−エチルピロリドンにビーカー中で溶解した。この溶液の対応する重量パーセントを、実施例媒体を製造するために用いた。
まず、0.02gのジブチルスズジラウレート(Desmorapid(登録商標)Z、Bayer MaterialScience AG、レーバークーゼン、独国)および3.6gの2,4,4−トリメチルヘキサン1,6−ジイソシアネート(TMDI)を50ml丸底フラスコに仕込み、60℃まで加熱した。続いて、11.9gの2,2,3,3,4,4,5,5,6,6,7,7−ドデカフルオロヘプチル)−1−オールを滴下し、混合物を、イソシアネート含有量が0.1%未満に低下するまで60℃で更に保持した。次いで冷却した。生成物を無色油として得た。
フォトポリマーの平坦弾性率G0を決定するための光開始剤C)を含まないフォトポリマー処方物(F)の製造
弾性率G0を決定するためのフォトポリマー処方物の製造のために、種々の書込モノマー(成分B)および必要に応じて添加剤(成分Eの一部)を、イソシアネート反応性成分b)(成分Aの一部として)中に、必要に応じて60℃にて溶解する。必要に応じて、60℃への加熱は、10分未満、乾燥炉中で行う。次いでイソシアネート成分a)(成分Aの他の部分)を、添加し、混合を、1分間Speedmixer中で行う。その後、酢酸ブチル中での成分E1の溶液を添加し、混合をSpeedmixer中で1分間再び行う(成分Eの他の部分)。酢酸ブチル中の成分E1)の濃度は、10重量%である。表2に記載のこの溶液の量を用いた。
以下のG0(Pa)についての測定値および巻取性の品質を得た。これらを表4に示す。
++ 層厚みのシフトがなく、フィルムを乱さない保護フィルムの極めて容易な取り外し。
+ 層厚みのシフトがなく、フィルムを乱さない保護フィルムの容易な取り外し。
− 端領域での軽微な層厚み変形、保護フィルムは、表面を破壊せずに剥離することが困難である。
− 端領域での顕著な層厚み変形、被覆端の深刻な「ほころび」、保護フィルムは、剥離することが困難でありフォトポリマーに乱れが起こる。
以下のTGA95測定値は、非光重合性成分D)に記載の式IIおよびIIIに従って書込モノマーB)について決定した。
表3に記載のホログラフィック媒体の以下の測定値を表6に示す。
Claims (17)
- ホログラフィックフィルムの製造方法であって、
i)成分として、
A)マトリックスポリマー、
B)書込モノマー、
C)光開始剤系、
D)必要に応じて、非光重合性成分、および
E)必要に応じて、触媒、フリーラジカル安定剤、溶媒、添加剤および他の補助剤および/または添加剤
を含むフォトポリマー処方物を供給し、
ii)フォトポリマー処方物を、フィルムとして基材フィルムへ広範囲に塗布し、および
iii)フォトポリマー処方物を、60<T<120℃の温度にて基材フィルム上で乾燥させ、
該フォトポリマー処方物について選択された成分は、TGA95値が、>100℃であり、および温度Tより少なくとも30℃高い化合物のみであり、≧0.030MPaの平坦弾性率を有するフォトポリマー処方物を用いる、方法。 - フォトポリマー処方物を、70<T<100℃の温度にて乾燥させることを特徴とする、請求項1に記載の方法。
- 個々の成分のTGA95値を、各成分の試料の約10mgの量を70μLの容積を有する小アルミニウムパン中へ計量投入し、該小アルミニウムパンを熱天秤、好ましくはMettler−ToledoからのTG50熱天秤の炉へ導入し、試料の質量の損失を、開いた小アルミニウムパン中で20K/分の一定炉加熱速度にて計測し、炉の出発温度は30℃であり、終了温度は600℃であり、炉を、決定の間、200mL/分窒素流でフラッシュし、試料の最初に計量した量を基準に5重量%の試料の質量の損失が生じた温度を、各成分のTGA95値として決定することにより決定することを特徴とする、請求項1および2のいずれかに記載の方法。
- ≧0.03MPaおよび≦1MPa、好ましくは≧0.05MPaおよび≦1MPa、特に好ましくは≧0.1MPaおよび≦1MPa、とりわけ好ましくは≧0.1MPaおよび≦0.6MPaの平坦弾性率を有するフォトポリマー処方物を用いることを特徴とする、請求項1〜3のいずれかに記載の方法。
- 積層フィルムを、工程iii)における乾燥後にフィルムへ適用することを特徴とする、請求項1〜4のいずれかに記載の方法。
- フィルムを、積層フィルムと共に巻き取ることを特徴とする、請求項5に記載の方法。
- マトリックスポリマーは、ポリウレタンであることを特徴とする、請求項1〜6のいずれかに記載の方法
- ポリウレタンは、イソシアネート成分a)およびイソシアネート反応性成分b)を反応させることにより得られることを特徴とする、請求項7に記載の方法。
- 書込モノマーは、アクリレートおよび/またはメタ(アクリレート)であることを特徴とする、請求項1〜8のいずれかに記載の方法。
- 単官能性書込モノマーおよび多官能性書込モノマーの組み合わせを、書込モノマーとして用いることを特徴とする、請求項1〜9のいずれかに記載の方法。
- 単官能性書込モノマーは、一般式(II):
を有し、および該単官能性書込モノマーは、好ましくは、<0℃のガラス転移温度TGおよび好ましくは405nmにおいて>1.50の屈折率を有することを特徴とする、請求項10に記載の方法。 - 以下のプロセス工程:
I. まず、必要に応じて成分B)、C)、D)およびE)の1以上と混合した成分a)の輸送および計量、および次いで、これとは別に、必要に応じて成分B)、C)、D)およびE)の1以上と混合した成分b)の輸送および計量、
II. I)に従って輸送、計量および必要に応じて予備混合した流れの脱蔵、
III. II)に従って得られた混合物のろ過、
IV. III)に従って得られた混合物の均質化、
V. 基材物質の巻き出しおよび予備処理、
VI. 基材物質の、工程IV)に従って得られた混合物での被覆、
VII. VI)に従って被覆されたフィルムの乾燥、
VIII. VII)に従って得られた被覆フィルムの積層、
IX. VIII)に従って得られた積層フィルムの巻き取り
を行うことを特徴とする、請求項8〜13のいずれかに記載の方法。 - フォトポリマー処方物を、印刷法により基材フィルムへ適用することを特徴とする、請求項1〜14のいずれかに記載の方法。
- 請求項1〜15のいずれかに記載の方法により得られるホログラフィックフィルム。
- 光学要素として、画像として、または画像表示または投射のための、請求項16に記載のホログラフィックフィルムの使用。
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- 2010-11-02 KR KR1020127011403A patent/KR101727769B1/ko active IP Right Grant
- 2010-11-02 PT PT107789406T patent/PT2497085E/pt unknown
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- 2010-11-02 RU RU2012122585/04A patent/RU2542984C2/ru not_active IP Right Cessation
- 2010-11-02 TW TW099137560A patent/TWI488877B/zh not_active IP Right Cessation
- 2010-11-02 PL PL10778940T patent/PL2497085T3/pl unknown
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- 2010-11-02 WO PCT/EP2010/066630 patent/WO2011067057A1/de active Application Filing
- 2010-11-02 CN CN201080060482.XA patent/CN102870157B/zh active Active
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Also Published As
Publication number | Publication date |
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KR20120101642A (ko) | 2012-09-14 |
RU2542984C2 (ru) | 2015-02-27 |
CN102870157A (zh) | 2013-01-09 |
IN2012DN03900A (ja) | 2015-09-04 |
US20140302426A1 (en) | 2014-10-09 |
CN102870157B (zh) | 2016-01-20 |
JP5923041B2 (ja) | 2016-05-24 |
TW201132662A (en) | 2011-10-01 |
BR112012010472A2 (pt) | 2016-03-15 |
RU2012122585A (ru) | 2013-12-10 |
KR101727769B1 (ko) | 2017-04-17 |
PT2497085E (pt) | 2014-03-27 |
ES2453267T3 (es) | 2014-04-07 |
US20120214089A1 (en) | 2012-08-23 |
WO2011067057A1 (de) | 2011-06-09 |
TWI488877B (zh) | 2015-06-21 |
PL2497085T3 (pl) | 2014-07-31 |
EP2497085B1 (de) | 2014-02-12 |
US8771903B2 (en) | 2014-07-08 |
EP2497085A1 (de) | 2012-09-12 |
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