US4994347A
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Storage stable photopolymerizable composition and element for refractive index imaging
Assignee: EIDP Inc
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Filing: 1988-12-23
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Granted: 1991-02-19
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Expires: 2008-12-23
Abstract
Abstract Solid storage stable photopolymerizable compositions are provided that are useful in preparing optical elements, and especially holograms. The composition contains a polymeric binder, N-vinyl carbazole and a photoinitiator system that has a hydrogen donor component.
Inventors
- 👤 William K. Smothers
Bibliographic Details
Application Number
—
Jurisdiction
US
Data Source
google_patents
Last Synchronized
2026-11-08 02:02
CPC Classifications
G; G03; G03F; G03F7/00; G03F7/004; G03F7/027; G03F7/028; G03F7/031; G03F7/0005; G03F7/001; Y; Y10; Y10S; Y10S430/00; Y10S430/1053; Y10S430/1055; Y10S430/106; Y10S430/11; Y10S430/111; Y10S430/112; Y10S430/113; Y10S430/114; Y10S430/117; Y10S430/12; Y10S430/121; Y10S430/122
Claims Analysis
Total Claims: 36
Claim 1
Independent Claim
92 words
A substantially solid, storage stable, photopolymerizable composition suited for forming a refractive-index image upon exposure to actinic radiation as the sole processing step, said composition consisting essentially of: (a) approximately 25 to 95% of a solvent soluble, thermoplastic, polymeric binder; (b) approximately 5 to 40% of N-vinyl carbazole; and (c) approximately 0.1 to 10% of a hexaarylbiimidazole photoinitiator system having a hydrogen donor component, wherein the hydrogen donor component is a mercapto compound having a pK HNP greater than 8.0, as measured in methanol with a glass electrode calibrated with aqueous buffer.
Claim 2
Dependent Claim
92 words
A substantially solid, storage stable, photopolymerizable composition suited for forming a refractive-index image upon exposure to actinic radiation as the sole processing step, said composition consisting essentially of: (a) approximately 25 to 95% of a solvent soluble, thermoplastic, polymeric binder; (b) approximately 5 to 40% of N-vinyl carbazole; and (c) approximately 0.1 to 10% of a hexaarylbiimidazole photoinitiator system having a hydrogen donor component, wherein the hydrogen donor component is a mercapto compound having a pK HNP greater than 8.0, as measured in methanol with a glass electrode calibrated with aqueous buffer.
Claim 3
Dependent Claim
22 words
The composition of claim 1 that will have a refractive index modulation of at least approximately 0.005 after exposure to actinic radiation.
Claim 4
Dependent Claim
26 words
The composition of claim 1 which also contains at least one liquid ethylenically unsaturated monomer capable of addition polymerization having a boiling point above 100° C.
Claim 5
Dependent Claim
46 words
The composition of claim 3 wherein the liquid monomer contains a substituent selected from the group consisting of phenyl, phenoxy, naphthyl, naphthyloxy, heteroaromatic containing up to three aromatic rings, chlorine and bromine and wherein the solvent soluble, thermoplastic, polymeric material is substantially free of said substituents.
Claim 6
Dependent Claim
42 words
The composition of claim 3 wherein the liquid monomer is selected from the group consisting of phenoxyalkyl acrylate or methacrylate; a phenol ethoxylate acrylate or methacrylate; a phenyl alkyl acrylate or methacrylate; 2-(1-naphthyloxy)ethyl acrylate; the di(2-acryloxyethyl)ether of bisphenol-A; and ethoxylated bisphenol-A diacrylate.
Claim 7
Dependent Claim
67 words
The composition of claim 3 wherein said binder is present in the amount of approximately 25 to 75%, N-vinyl carbazole is present in the amount of approximately 5 to 40% the ethylenically unsaturated monomers are present in the amount of approximately 5 to 60%, and said photoinitiator system is present in the amount of approximately 0.1 to 10% by weight, based on total weight of said composition.
Claim 8
Dependent Claim
15 words
The composition of claim 3 in which a solid ethylenically unsaturated monomer is also present.
Claim 9
Dependent Claim
16 words
The composition of claim 7 in which the solid ethylenically unsaturated monomer contains the carbazole group.
Claim 10
Dependent Claim
45 words
The composition of claim 7 wherein the solid ethylenically unsaturated monomer is selected from the group consisting of 3,6-dibromo-9-vinyl carbazole, 2,4,6-tribromophenyl acrylate or methacrylate, pentachlorophenyl acrylate or methacrylate, 2-naphthyl acrylate or methacrylate, 2-(2-naphthyloxy)ethyl acrylate or methacrylate, and the di-(2-acryloxyethyl)ether of tetrabromo-bisphenol A, and mixtures thereof.
Claim 11
Dependent Claim
82 words
The composition of claim 3 in which a plasticizer is also present, said plasticizer being selected from the group consisting of tris(2-ethylhexyl)phosphate, glyceryl tributyrate, and a compound having the general formula: ##STR3## wherein each of R 1 and R 2 is an alkyl group of 1 to 10 carbon atoms; R 3 is H or an alkyl group of 8 to 16 carbon atoms, R 4 is H or CH 3 ; x is 1-4; y is 2-20 and z is 1-20.
Claim 12
Dependent Claim
36 words
The composition of claim 10 wherein the plasticizer is selected from the group consisting of triethylene glycol dicaprylate, triethylene glycol bis(2-ethylhexanoate), diethyl adipate, dibutyl adipate, tetraethylene glycol diheptanoate, dibutyl suberate, diethyl sebacate, tris(2-ethylhexyl)phosphate, and glyceryl tributyrate.
Claim 13
Dependent Claim
22 words
The composition of claim 10 in which said plasticizer is substituted for at least a portion of the liquid ethylenically unsaturated monomer.
Claim 14
Dependent Claim
41 words
The composition of claim 1 wherein said binder is selected from the group consisting of cellulose acetate butyrate; an acrylate or methacrylate polymer or interpolymer; a vinyl butyral, acetal or formal polymer or interpolymer; and a vinyl acetate polymer or interpolymer.
Claim 15
Dependent Claim
173 words
A substantially solid, storage stable, photopolymerizable composition that will have a refractive index modulation of at least approximately 0.005 after exposure to actinic radiation, said composition consisting essentially of: (a) approximately 25 to 95% of a solvent soluble, thermoplastic binder; (b) approximately 5 to 40% of N-vinyl carbazole; (c) approximately 5 to 60% of a liquid ethylenically unsaturated monomer capable of addition polymerization and having a boiling point above 100° C; (d) approximately 0 to 25% of a plasticizer; and (e) approximately 0.1 to 10% of a hexaarylbiimidazole photoinitiator system having a hydrogen donor component, wherein the hydrogen donor component is a mercapto compound having a pK HNP greater than 8.0, as measured in methanol with a glass electrode calibrated with aqueous buffer, said percentages being weight percentages of the total composition, and one of said binder or said liquid monomer containing a substituent selected from the group consisting of phenyl, phenoxy, naphthyl, naphthyloxy, heteroaromatic containing up to three aromatic rings, chlorine and bromine, and the other being substantially free of said substituents.
Claim 16
Dependent Claim
173 words
A substantially solid, storage stable, photopolymerizable composition that will have a refractive index modulation of at least approximately 0.005 after exposure to actinic radiation, said composition consisting essentially of: (a) approximately 25 to 95% of a solvent soluble, thermoplastic binder; (b) approximately 5 to 40% of N-vinyl carbazole; (c) approximately 5 to 60% of a liquid ethylenically unsaturated monomer capable of addition polymerization and having a boiling point above 100° C; (d) approximately 0 to 25% of a plasticizer; and (e) approximately 0.1 to 10% of a hexaarylbiimidazole photoinitiator system having a hydrogen donor component, wherein the hydrogen donor component is a mercapto compound having a pK HNP greater than 8.0, as measured in methanol with a glass electrode calibrated with aqueous buffer, said percentages being weight percentages of the total composition, and one of said binder or said liquid monomer containing a substituent selected from the group consisting of phenyl, phenoxy, naphthyl, naphthyloxy, heteroaromatic containing up to three aromatic rings, chlorine and bromine, and the other being substantially free of said substituents.
Claim 17
Dependent Claim
112 words
A substantially solid, storage stable element adapted to record a refractive index image upon exposure to actinic radiation as the sole processing step, said element comprising a substrate that supports a substantially solid, storage stable composition consisting essentially of: (a) approximately 25 to 95% of a solvent soluble, thermoplastic, polymeric binder; (b) approximately 5 to 40% of N-vinyl carbazole; and (c) approximately 0.1 to 10% of a hexaarylbiimidazole photoinitiator system having a hydrogen donor component, wherein the hydrogen donor component is a mercapto compound having a pK HNP greater than 8.0, as measured in methanol with a glass electrode calibrated with aqueous buffer, said percentages being weight percentages of the total composition.
Claim 18
Dependent Claim
112 words
A substantially solid, storage stable element adapted to record a refractive index image upon exposure to actinic radiation as the sole processing step, said element comprising a substrate that supports a substantially solid, storage stable composition consisting essentially of: (a) approximately 25 to 95% of a solvent soluble, thermoplastic, polymeric binder; (b) approximately 5 to 40% of N-vinyl carbazole; and (c) approximately 0.1 to 10% of a hexaarylbiimidazole photoinitiator system having a hydrogen donor component, wherein the hydrogen donor component is a mercapto compound having a pK HNP greater than 8.0, as measured in methanol with a glass electrode calibrated with aqueous buffer, said percentages being weight percentages of the total composition.
Claim 19
Dependent Claim
23 words
The recording element of claim 15 that will have a refractive index modulation of at least approximately 0.005 after exposure to actinic radiation.
Claim 20
Dependent Claim
75 words
The recording element of claim 16 wherein said composition also contains approximately 5 to 60% of at least one liquid ethylenically unsaturated monomer capable of addition polymerization and having a boiling point above 100° C., one of said binder or said liquid monomer containing a substituent selected from the group consisting of phenyl, phenoxy, naphthyl, naphthyloxy, heteroaromatic containing up to three aromatic rings, chlorine and bromine, and the other being substantially free of said substituents.
Claim 21
Dependent Claim
42 words
The recording element of claim 17 wherein said binder contains the substituent selected from the group consisting of phenyl, phenoxy, naphthyl, naphthyloxy, heteroaromatic containing up to three aromatic rings, chlorine and bromine, and said liquid monomer is substantially free of said substituents.
Claim 22
Dependent Claim
42 words
The recording element of claim 17 wherein said liquid monomer contains the substituent selected from the group consisting of phenyl, phenoxy, naphthyl, naphthyloxy, heteroaromatic containing up to three aromatic rings, chlorine and bromine, and said binder is substantially free of said substituents.
Claim 23
Dependent Claim
68 words
The recording element of claim 17 wherein said binder is present in the amount of approximately 25 to 75%, N-vinyl carbazole is present in the amount of approximately 5 to 40% the ethylenically unsaturated monomers are present in the amount of approximately 5 to 60%, and said photoinitiator system is present in the amount of approximately 0.1 to 10% by weight, based on total weight of said composition.
Claim 24
Dependent Claim
19 words
The recording element of claim 16 in which a solid ethylenically unsaturated monomer is also present in said composition.
Claim 25
Dependent Claim
17 words
The recording element of claim 21 in which the solid ethylenically unsaturated monomer contains the carbazole group.
Claim 26
Dependent Claim
46 words
The recording element of claim 21 wherein the solid ethylenically unsaturated monomer is selected from the group consisting of 3,6-dibromo-9-vinyl carbazole, 2,4,6-tribromophenyl acrylate or methacrylate, pentachlorophenyl acrylate or methacrylate, 2-naphthyl acrylate or methacrylate, 2-(2-naphthyloxy)ethyl acrylate or methacrylate, and the di-(2-acryloxyethyl)ether of tetrabromo-bisphenol A, and mixtures thereof.
Claim 27
Dependent Claim
86 words
The recording element of claim 16 in which a plasticizer is also present in said composition, said plasticizer being selected from the group consisting of tris(2-ethylhexyl)phosphate, glyceryl tributyrate, and a compound having the general formula: ##STR4## wherein each of R 1 and R 2 is an alkyl group of 1 to 10 carbon atoms; R 3 is H or an alkyl group of 8 to 16 carbon atoms, R 4 is H or CH 3 ; x is 1-4; y is 2-20 and z is 1-20.
Claim 28
Dependent Claim
36 words
The composition of claim 24 wherein the plasticizer is selected from the group consisting of triethylene glycol dicaprylate, triethylene glycol bis(2-ethylhexanoate), diethyl adipate, dibutyl adipate, tetraethylene glycol diheptanoate, dibutyl suberate, diethyl sebacate, tris(2-ethylhexyl)phosphate, and glyceryl tributyrate.
Claim 29
Dependent Claim
22 words
The composition of claim 24 in which said plasticizer is substituted for at least a portion of the liquid ethylenically unsaturated monomer.
Claim 30
Dependent Claim
42 words
The recording element of claim 15 wherein said binder is selected from the group consisting of cellulose acetate butyrate; an acrylate or methacrylate polymer or interpolymer; a vinyl butyral, acetal or formal polymer or interpolymer; and a vinyl acetate polymer or interpolymer.
Claim 31
Dependent Claim
198 words
A substantially solid, storage stable element adapted to record a refractive index image upon exposure to actinic radiation as the sole processing step, said element comprising a substrate that supports a composition that will have a refractive index modulation of at least approximately 0.005 after exposure to actinic radiation, said composition consisting essentially of: (a) approximately 25 to 95% of a solvent soluble, thermoplastic binder; (b) approximately 5 to 40% of N-vinyl carbazole; (c) approximately 5 to 60% of a liquid ethylenically unsaturated monomer capable of addition polymerization and having a boiling point above 100° C; (d) approximately 0 to 25% of a plasticizer; and (e) approximately 0.1 to 10% of a hexaarylbiimidazole photoinitiator system having a hydrogen donor component, wherein the hydrogen donor component is a mercapto compound having a pK HNP greater than 8.0, as measured in methanol with a glass electrode calibrated with aqueous buffer, said percentages being weight percentages of the total composition, and one of said binder or said liquid monomer containing a substituent selected from the group consisting of phenyl, phenoxy, naphthyl, naphthyloxy, heteroaromatic containing up to three aromatic rings, chlorine and bromine, and the other being substantially free of said substituents.
Claim 32
Dependent Claim
198 words
A substantially solid, storage stable element adapted to record a refractive index image upon exposure to actinic radiation as the sole processing step, said element comprising a substrate that supports a composition that will have a refractive index modulation of at least approximately 0.005 after exposure to actinic radiation, said composition consisting essentially of: (a) approximately 25 to 95% of a solvent soluble, thermoplastic binder; (b) approximately 5 to 40% of N-vinyl carbazole; (c) approximately 5 to 60% of a liquid ethylenically unsaturated monomer capable of addition polymerization and having a boiling point above 100° C; (d) approximately 0 to 25% of a plasticizer; and (e) approximately 0.1 to 10% of a hexaarylbiimidazole photoinitiator system having a hydrogen donor component, wherein the hydrogen donor component is a mercapto compound having a pK HNP greater than 8.0, as measured in methanol with a glass electrode calibrated with aqueous buffer, said percentages being weight percentages of the total composition, and one of said binder or said liquid monomer containing a substituent selected from the group consisting of phenyl, phenoxy, naphthyl, naphthyloxy, heteroaromatic containing up to three aromatic rings, chlorine and bromine, and the other being substantially free of said substituents.
Claim 33
Dependent Claim
29 words
The composition of claim 1 wherein said hydrogen donor component is at least one mercapto compound selected from the group consisting of 5-chloro-2-mercaptobenzothiazole; 2-mercaptobenzothiazole; 1H-1,2,4-triazole-3-thiol; 6-ethoxy-2-mercaptobenzothiazole; 4-methyl-4H-1,2,4-triazole-3-thiol; and 1-dodecanethiol.
Claim 34
Dependent Claim
29 words
The composition of claim 14 wherein said hydrogen donor component is at least one mercapto compound selected from the group consisting of 5-chloro-2-mercaptobenzothiazole; 2-mercaptobenzothiazole; 1H-1,2,4-triazole-3-thiol; 6-ethoxy-2-mercaptobenzothiazole; 4-methyl-4H-1,2,4-triazole-3-thiol; and 1-dodecanethiol.
Claim 35
Dependent Claim
30 words
The recording element of claim 15 wherein said hydrogen donor component is at least one mercapto compound selected from the group consisting of 5-chloro-2-mercaptobenzothiazole; 2-mercaptobenzothiazole; 1H-1,2,4-triazole-3-thiol; 6-ethoxy-2-mercaptobenzothiazole; 4-methyl-4H-1,2,4-triazole-3-thiol; and 1-dodecanethiol.
Claim 36
Dependent Claim
31 words
The recording element of claim 28 wherein said hydrogen donor component is at least one mercapto compound selected from the group consisting of 5-chloro-b 2-mercaptobenzothiazole; 2-mercaptobenzothiazole; 1H-1,2,4-triazole-3-thiol; 6-ethoxy-2-mercaptobenzothiazole; 4-methyl-4H-1,2,4-triazole-3-thiol; and 1-dodecanethiol.
References Cited (Backward Citations)
USPTO Annuity & Maintenance Windows
| Annuity Stage | Window Opens | Payment Deadline | Surcharge Period Until | Estimated Fee | Status |
|---|---|---|---|---|---|
| 3.5 Years (Year 4) | 1994-02-18 | 1994-08-20 | 1995-02-19 | $2000.00 | Window Closed / Lapsed |
| 7.5 Years (Year 8) | 1998-02-18 | 1998-08-20 | 1999-02-19 | $3760.00 | Window Closed / Lapsed |
| 11.5 Years (Year 12) | 2002-02-18 | 2002-08-20 | 2003-02-19 | $7700.00 | Window Closed / Lapsed |