US3142567A - Photographic product and process - Google Patents

Photographic product and process Download PDF

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US3142567A
US3142567A US182991A US18299162A US3142567A US 3142567 A US3142567 A US 3142567A US 182991 A US182991 A US 182991A US 18299162 A US18299162 A US 18299162A US 3142567 A US3142567 A US 3142567A
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silver
gold
optical transmission
metallic coating
photosensitive
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US182991A
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Meroe M Morse
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Polaroid Corp
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Polaroid Corp
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    • G—PHYSICS
    • G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
    • G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
    • G03C1/00—Photosensitive materials
    • G03C1/494—Silver salt compositions other than silver halide emulsions; Photothermographic systems ; Thermographic systems using noble metal compounds
    • G03C1/496—Binder-free compositions, e.g. evaporated
    • G03C1/4965—Binder-free compositions, e.g. evaporated evaporated
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10—TECHNICAL SUBJECTS COVERED BY FORMER USPC
    • Y10S—TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y10S430/00—Radiation imagery chemistry: process, composition, or product thereof
    • Y10S430/133—Binder-free emulsion

Definitions

  • the present invention relates to novel photographic products, their production and use, and more particularly, to novel photosensitive elements, their production and use.
  • the primary objects of the present invention are the production and use of novel photographic elements comprising photosensitive materials formed, at least in part, by the vacuum deposition of their components upon their support. It has been found that such photosensitive materials possess characteristics, including virtually grainless structure and small mass per unit area, that unexpectedly make feasible a variety of unusual processing techniques and pictorial results.
  • the invention accordingly comprises the process possessing the several steps and the relation and order of one or more of such steps with respect to each of the others and the product possessing the features, properties and the relation of elements which are exemplified in the following detailed disclosure, and the scope of the application of which will be indicated in the claims.
  • FIGURE 1 shows successive, exaggerated diagrammatic cross-sectional, views of materials undergoing a process of the present invention
  • FIG. 2 shows successive, exaggerated cross-sectional views of the product of the process of FIGURE 1 being used in accordance with the present invention.
  • the processes and products of the present in vention herein disclosed are based upon the production of a photosensitive stratum by vacuum depositing at least a metal of a photosensitive salt on a supportand then subjecting the metal on the support to halogen vapor.
  • the support for example, is composed of a suitable plastic such as hydrolyzed cellulose acetate, a suitable paper such as baryta paper or a suitable glass.
  • the step of vacuum depositing involves either evaporating or sputtering at pressures below one hundred microns of mercury, and usually within the range of from 0.1 to 100 microns of mercury, these pressures being produced by continuous evacuation to ensure the rapid removal of any gases produced during the vacuum deposition process.
  • the metallic distribution of the stratum initially formed preferably is in sufiicient concentration per unit area to give rise to an optical transmission ofat most 40%. Unusually useful results are achieved when the metal distribution includes both gold and silver deposited in either sequence or together.
  • Halogenation is effected by subjecting the metallic stratum produced in the foregoing way to the vapor of elemental halogen, e.g., chlorine, bromine, iodine or combinations thereof or t) volatile halogen salts, e.g., hydroice gen bromide, hydrogen iodide or combinations thereof at a suitable temperature, for example, room temperature.
  • elemental halogen e.g., chlorine, bromine, iodine or combinations thereof or t
  • volatile halogen salts e.g., hydroice gen bromide, hydrogen iodide or combinations thereof
  • the metallic stratum preferably, is subjected to the halogen vapor for a period sufficient to effect substantially complete halogenation, a condition that is indicated when the optical transmission of the stratum has increased substantially to between about and
  • photosensitive strata may be prepared, in accordance with this invention, by evaporating silver alone or in combination with gold, followed by halogenation.
  • the resulting photosensitive silver halide stratum may be developed by the application of heat alonetoform a negative silver image; this method of development is disclosed and claimed in the copending application of Edwin H. Land, Serial No. 733,754, filed May 7, 1958 (now abandoned in favor of a continuation application, Serial No. 176,844, filed February 14, 1962).
  • the exposed photosensitive stratum may be developed to a negative silver image by the application of vapors of a silver halide developing agent, particularly a silver halide developing agent which exhibits appreciable volatility at room temperature, e.g., volatile hydroxylamines and hydrazines.
  • a silver halide developing agent particularly a silver halide developing agent which exhibits appreciable volatility at room temperature
  • volatile hydroxylamines and hydrazines e.g., volatile hydroxylamines and hydrazines.
  • a volatile hydroxylamine such as, N,N-diethyl-hydroxylamine.
  • the vapor of a volatile alkali for example, an amine, such as diethylamine, also may be used.
  • the silver and gold may be deposited in either sequence or together, with the silver being deposited in a concentration that by itself would give rise to an optical transmission of from about 10% to about 30%, and the gold being deposited in a concentration sufficient per unit area to give rise to an optical transmission of at most 40%.
  • best results including highest sensitivity and speed of development, are achieved when said silver and gold each are deposited in a concentration which by itself would provide an optical transmission of from about 10% to about 30%, the coating of gold and silver together having a total optical transmission of from about 0.01% to about 1.0%, and thereafter halogenating the metallic coating to provide a halogenated metallic coating having an optical transmission of from about 85% to about 100%.
  • Photosensitivestrata prepared in accordance with this invention and containing both gold and silver also may be developed by the application of heat alone, asdisclosed and claimed in the abovementioned copending application, Serial No, 733,754.
  • FIGURE 1 illustrates the production of a photosensitive element in accordance with the present invention.
  • the support is a hydrolyzed cellulose acetate sheet 20, approximately 1 millimeter thick, 3 inches wide and 6 /2 inches long.
  • the photosensitive element of Example I is photoexposed. Thereafter under a bell jar, this element is sub- J jected to the vapor of diethylamine as an alkali and N,N-diethyl-hydroxylamine as a developer.
  • the partial pressures of the diethylamine and the N,N-diethyl-hydroxylamine are the normal partial pressures of those compounds at room temperature.
  • a negative print of delicate gradation is produced in approximately five minutes.
  • Example III A negative print is obtained in approximately 1 minute when the procedure of Example 11 is repeated with a photosensitive element prepared in the manner described in Example I, except that the optical transmissions of the gold stratum and the gold and silver stratum, respectively, are 39% and 0.80%, and halogenation is eifected by iodine vapors.
  • Example V A negative print is obtained in approximately 35 seconds when the procedure of Example II is repeated with a photosensitive element prepared in the manner described in Example I, except that the optical transmissions of the gold stratum and the gold and silver stratum, respectively, are 29% and 0.10%, and halogenation is effected by iodine vapors. Similar results are obtained when substantially the same concentrations of silver and gold are applied but in the reverse sequence.
  • the prints of the above examples may be fixed by reacting the unreduced silver with a fixing vapor, e.g., hydrogen sulfide, to form a stable silver salt or by coating with a washing and protecting formulation including water and a film-forming polymer.
  • a fixing vapor e.g., hydrogen sulfide
  • Photosensitive materials prepared in accordance with this invention may be developed by aqueous alkaline solutions of a silver halide developing agent, e.g., hydroquinone, which may be applied by spraying or lightly swabbing the developer solution onto the exposed photosensitive material; and they also may be employed in diffusion transfer processes, wherein a water-soluble silver complex is formed by a silver halide solvent with unexposed and undeveloped silver halide, and said water-soluble silver complex is transferred by diffusion to a superposed silverreceptive stratum to provide a silver transfer image.
  • a silver halide developing agent e.g., hydroquinone
  • a process of forming a photosensitive element comprising the steps of vacuum depositing gold and silver on a support to form a metallic coating, said silver being deposited in a concentration which, by itself, would provide an optical transmission of from about 10% to about 30%, said gold being deposited in a concentration which, by itself, would be a metallic coating having an optical transmission of from about 10% to at most 40%, said coating of gold and silver together having a total optical transmission of from about 0.01% to about 1.0%, and halogenating said metallic coating by contacting said metallic coating with halogen vapors provided by a member of the group consisting of elemental chlorine, elemental bromine, elemental iodine, and volatile salts of said elemental halogens for a time sufficient to provide a halogenated metallic coating having an optical transmission of from about to about 2.
  • said volatile organic silver halide developing agent is selected from the class consisting of hydroxylamines and hydrazines.
  • Glafkides Photograph Chemistry, 1., Fountain Press, London (1958), page 319.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Non-Silver Salt Photosensitive Materials And Non-Silver Salt Photography (AREA)

Description

July 28, 1964 M. M. MORSE 7 3,142,567
PHOTOGRAPHIC PRODUCT AND PROCESS Filed March 9, 1962 2O Suppor'l' TTTTTTTT Vacuum Deposl'l'ion of Gold Vacuum Deposil'i'on of Silver Pholosensllive l TTTTTTTT" Halogen Vapor P h o l'oexpose FIG. 2
T u a r a v :9 {Developed Ep- 7 Negaflve T 'T T T T T T T Evaporal'lon pf Volal'lle Alkali and Volcrl'ile Developer INVENTOR imam- ATTORNEYS United States Patent H Delaware Filed Mar. 9, 1962, Ser. No. 182,991
8 Claims. (Cl. 9666) The present invention relates to novel photographic products, their production and use, and more particularly, to novel photosensitive elements, their production and use.
The primary objects of the present invention are the production and use of novel photographic elements comprising photosensitive materials formed, at least in part, by the vacuum deposition of their components upon their support. It has been found that such photosensitive materials possess characteristics, including virtually grainless structure and small mass per unit area, that unexpectedly make feasible a variety of unusual processing techniques and pictorial results.
Other objects of the invention will in part be obvious and will in part appear hereinafter.
The invention accordingly comprises the process possessing the several steps and the relation and order of one or more of such steps with respect to each of the others and the product possessing the features, properties and the relation of elements which are exemplified in the following detailed disclosure, and the scope of the application of which will be indicated in the claims.
For a fuller understanding of the nature and objects of the present invention, reference should be had to the following detailed description taken in connection with the accompanying drawing wherein:
FIGURE 1 shows successive, exaggerated diagrammatic cross-sectional, views of materials undergoing a process of the present invention; and
FIG. 2 shows successive, exaggerated cross-sectional views of the product of the process of FIGURE 1 being used in accordance with the present invention.
Generally the processes and products of the present in vention herein disclosed are based upon the production of a photosensitive stratum by vacuum depositing at least a metal of a photosensitive salt on a supportand then subjecting the metal on the support to halogen vapor. The support, for example, is composed of a suitable plastic such as hydrolyzed cellulose acetate, a suitable paper such as baryta paper or a suitable glass.
The step of vacuum depositing involves either evaporating or sputtering at pressures below one hundred microns of mercury, and usually within the range of from 0.1 to 100 microns of mercury, these pressures being produced by continuous evacuation to ensure the rapid removal of any gases produced during the vacuum deposition process. The metallic distribution of the stratum initially formed preferably is in sufiicient concentration per unit area to give rise to an optical transmission ofat most 40%. Unusually useful results are achieved when the metal distribution includes both gold and silver deposited in either sequence or together. Best results are achieved when the silver is vacuum deposited in a concentration that by itself would give rise to an optical transmission of from about 10% to about 30%, the gold is deposited in a concentration that by itself would give rise to an optical transmission of from about 10% to about 30% and the gold and silver are deposited in concentrations which together give rise to an optical transmission of from about 0.01% to about 1.0%.
Halogenation is effected by subjecting the metallic stratum produced in the foregoing way to the vapor of elemental halogen, e.g., chlorine, bromine, iodine or combinations thereof or t) volatile halogen salts, e.g., hydroice gen bromide, hydrogen iodide or combinations thereof at a suitable temperature, for example, room temperature. The metallic stratum, preferably, is subjected to the halogen vapor for a period sufficient to effect substantially complete halogenation, a condition that is indicated when the optical transmission of the stratum has increased substantially to between about and As noted above, photosensitive strata may be prepared, in accordance with this invention, by evaporating silver alone or in combination with gold, followed by halogenation. Where the photosensitive stratum is prepared by evaporating silver as the only metal, the resulting photosensitive silver halide stratum may be developed by the application of heat alonetoform a negative silver image; this method of development is disclosed and claimed in the copending application of Edwin H. Land, Serial No. 733,754, filed May 7, 1958 (now abandoned in favor of a continuation application, Serial No. 176,844, filed February 14, 1962).
Where the photosensitive stratum prepared in accordance with this invention includes both silver and gold, it has been found that the exposed photosensitive stratum may be developed to a negative silver image by the application of vapors of a silver halide developing agent, particularly a silver halide developing agent which exhibits appreciable volatility at room temperature, e.g., volatile hydroxylamines and hydrazines. Particularly useful results are obtained with a volatile hydroxylamine, such as, N,N-diethyl-hydroxylamine. In conjunction with the volatile silver halide developing agent, the vapor of a volatile alkali, for example, an amine, such as diethylamine, also may be used. The silver and gold may be deposited in either sequence or together, with the silver being deposited in a concentration that by itself would give rise to an optical transmission of from about 10% to about 30%, and the gold being deposited in a concentration sufficient per unit area to give rise to an optical transmission of at most 40%. As noted above, best results, including highest sensitivity and speed of development, are achieved when said silver and gold each are deposited in a concentration which by itself would provide an optical transmission of from about 10% to about 30%, the coating of gold and silver together having a total optical transmission of from about 0.01% to about 1.0%, and thereafter halogenating the metallic coating to provide a halogenated metallic coating having an optical transmission of from about 85% to about 100%.
Photosensitivestrata prepared in accordance with this invention and containing both gold and silver also may be developed by the application of heat alone, asdisclosed and claimed in the abovementioned copending application, Serial No, 733,754.
Example I V 5 FIGURE 1 illustrates the production of a photosensitive element in accordance with the present invention.-
As shown, the support is a hydrolyzed cellulose acetate sheet 20, approximately 1 millimeter thick, 3 inches wide and 6 /2 inches long. First, 5 milligrams of gold is evapo-' The photosensitive element of Example I is photoexposed. Thereafter under a bell jar, this element is sub- J jected to the vapor of diethylamine as an alkali and N,N-diethyl-hydroxylamine as a developer. The partial pressures of the diethylamine and the N,N-diethyl-hydroxylamine are the normal partial pressures of those compounds at room temperature. A negative print of delicate gradation is produced in approximately five minutes.
Example III Example IV A negative print is obtained in approximately 1 minute when the procedure of Example 11 is repeated with a photosensitive element prepared in the manner described in Example I, except that the optical transmissions of the gold stratum and the gold and silver stratum, respectively, are 39% and 0.80%, and halogenation is eifected by iodine vapors.
Example V A negative print is obtained in approximately 35 seconds when the procedure of Example II is repeated with a photosensitive element prepared in the manner described in Example I, except that the optical transmissions of the gold stratum and the gold and silver stratum, respectively, are 29% and 0.10%, and halogenation is effected by iodine vapors. Similar results are obtained when substantially the same concentrations of silver and gold are applied but in the reverse sequence.
The prints of the above examples may be fixed by reacting the unreduced silver with a fixing vapor, e.g., hydrogen sulfide, to form a stable silver salt or by coating with a washing and protecting formulation including water and a film-forming polymer.
When the development procedure of, e.g., Example II, was repeated employing a photoexposed photosensitive stratum prepared by vacuum deposition of only silver, very little silver image density was observed. This comparison demonstrates the unexpected results obtained where both silver and gold are employed in preparing photosensitive materials in accordance with this embodiment of the invention.
Photosensitive materials prepared in accordance with this invention may be developed by aqueous alkaline solutions of a silver halide developing agent, e.g., hydroquinone, which may be applied by spraying or lightly swabbing the developer solution onto the exposed photosensitive material; and they also may be employed in diffusion transfer processes, wherein a water-soluble silver complex is formed by a silver halide solvent with unexposed and undeveloped silver halide, and said water-soluble silver complex is transferred by diffusion to a superposed silverreceptive stratum to provide a silver transfer image.
This application is a continuation-in-part of my copending application, Serial No. 733,753, filed May 7, 1958 (now abandoned).
Since certain changes may be made in the above product and process without departing from the scope of the invention herein involved, it is intended that all matter contained in the above description and shown in the accompanying drawing shall be interpreted as illustrative and not in a limiting sense.
What is claimed is:
1. A process of forming a photosensitive element, said process comprising the steps of vacuum depositing gold and silver on a support to form a metallic coating, said silver being deposited in a concentration which, by itself, would provide an optical transmission of from about 10% to about 30%, said gold being deposited in a concentration which, by itself, would be a metallic coating having an optical transmission of from about 10% to at most 40%, said coating of gold and silver together having a total optical transmission of from about 0.01% to about 1.0%, and halogenating said metallic coating by contacting said metallic coating with halogen vapors provided by a member of the group consisting of elemental chlorine, elemental bromine, elemental iodine, and volatile salts of said elemental halogens for a time sufficient to provide a halogenated metallic coating having an optical transmission of from about to about 2. A photosensitive element prepared by the process of claim 1.
3. The process of developing a photoexposed photosensitive stratum formed by the process of claim 1, said development being effected by contacting said exposed photosensitive stratum with the vapor of a volatile organic silver halide developing agent.
4. The process of claim 3, wherein said development is effected at room temperature.
5. The process of claim 3, wherein said volatile organic silver halide developing agent is selected from the class consisting of hydroxylamines and hydrazines.
6. The process of claim 3, including the step of treating the developed photosensitive stratum with hydrogen sulfide vapors.
7. The process which comprises photoexposing a photosensitive element formed by the process of claim 1, and developing said photoexposed photosensitive element by contacting it, at room temperature, with vapors of diethylamine and N,N-diethyl-hydroxylamine.
8. The process as defined in claim 1, wherein said gold is deposited prior to said silver, said gold layer having an optical transmission of about 30%, and said halogen vapors are iodine vapors.
References Cited in the file of this patent UNITED STATES PATENTS 2,153,628 Knoll Apr. 11, 1939 2,239,452 William et al. Apr. 22, 1941 2,399,083 Waller Apr. 22, 1946 2,439,983 Morgan et al. Apr. 20, 1948 2,706,157 Sainsbury et al Apr. 12, 1955 OTHER REFERENCES Yamada et al.: Chemical Abstracts, vol. 50, pages 11147-8.
Glafkides: Photograph Chemistry, 1., Fountain Press, London (1958), page 319.

Claims (2)

1. A PROCESS OF FORMING A PHOTOSENSITIVE ELEMENT, SAID PROCESS COMPRISING THE STEPS OF VACUUM DEPOSITING GOLD AND SILVER ON A SUPPORT TO FORM A METALLIC COATING, SAID SILVER BEING DEPOSITED IN A CONCENTRATION WHICH, BY ITSELF, WOULD PROVIDE AN OPTICAL TRANSMISSION OF FROM ABOUT 10% TO ABOUT 30%, SAID GOLD BEING DEPOSITED IN A CONCENTRATION WHICH, BY ITSELF, WOULD BE A METALLIC COATING HAVING AN OPTICAL TRANSMISSION OF FROM ABOUT 10% TO AT MOST 40%, SAID COATING OF GOLD AND SILVER TOGETHER HAVING A TOTAL OPTICAL TRANSMISSION OF FROM ABOUT 0.01% TO ABOUT 1.0%, AND HALOGENATING SAID METALLIC COATING BY CONTACTING SAID METALLIC COATING WITH HALOGEN VAPORS PROVIDED BY A MEMBER OF THE GROUP CONSISTING OF ELEMENTAL CHLORINE, ELEMENTAL BROMINE, ELEMENTAL IODINE, AND VOLATILE SALTS OF SAID ELEMENTAL HALOGENS FOR A TIME SUFFICIENT TO PROVIDE A HALOGENATED METALLIC COATING HAVING AN OPTICAL TRANSMISSION OF FROM ABOUT 85% TO ABOUT 100%.
3. THE PROCESS OF DEVELOPING A PHOTOEXPOSED PHOTOSENSITIVE STRATUM FORMED BY THE PROCESS OF CLAIM 1, SAID DEVELOPMENT BEING EFFECTED BY CONTACTING SAID EXPOSED PHOTOSENSITIVE STRATUM WITH THE VAPOR OF A VOLATILE ORGANIC SILVER HALIDE DEVELOPING AGENT.
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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3416920A (en) * 1963-03-14 1968-12-17 Zindler Lumoprint Kg Photographic method of producing a copy from an endless silver surface
US3505066A (en) * 1966-10-05 1970-04-07 Polaroid Corp Photographic print-out process utilizing binder-free silver fluoride
US3537855A (en) * 1966-10-05 1970-11-03 Polaroid Corp Photosensitive silver fluoride element

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2153628A (en) * 1935-03-13 1939-04-11 Telefunken Gmbh Electron tube
US2239452A (en) * 1937-03-13 1941-04-22 Robley C Williams Method and apparatus for producing semitransparent coatings
US2399083A (en) * 1942-02-13 1946-04-23 Ilford Ltd Photographic materials
US2439983A (en) * 1944-01-15 1948-04-20 Libbey Owens Ford Glass Co Means for thermally evaporating various materials in vacuums for coating purposes
US2706157A (en) * 1951-07-21 1955-04-12 Grant Photo Products Inc Processing photographic paper and film

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2153628A (en) * 1935-03-13 1939-04-11 Telefunken Gmbh Electron tube
US2239452A (en) * 1937-03-13 1941-04-22 Robley C Williams Method and apparatus for producing semitransparent coatings
US2399083A (en) * 1942-02-13 1946-04-23 Ilford Ltd Photographic materials
US2439983A (en) * 1944-01-15 1948-04-20 Libbey Owens Ford Glass Co Means for thermally evaporating various materials in vacuums for coating purposes
US2706157A (en) * 1951-07-21 1955-04-12 Grant Photo Products Inc Processing photographic paper and film

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3416920A (en) * 1963-03-14 1968-12-17 Zindler Lumoprint Kg Photographic method of producing a copy from an endless silver surface
US3505066A (en) * 1966-10-05 1970-04-07 Polaroid Corp Photographic print-out process utilizing binder-free silver fluoride
US3537855A (en) * 1966-10-05 1970-11-03 Polaroid Corp Photosensitive silver fluoride element

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