US3802888A - Light-stable sheet material for recording light-images - Google Patents

Light-stable sheet material for recording light-images Download PDF

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Publication number
US3802888A
US3802888A US00191803A US19180371A US3802888A US 3802888 A US3802888 A US 3802888A US 00191803 A US00191803 A US 00191803A US 19180371 A US19180371 A US 19180371A US 3802888 A US3802888 A US 3802888A
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US
United States
Prior art keywords
light
sheet material
exposed
silver
image
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Expired - Lifetime
Application number
US00191803A
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English (en)
Inventor
J Willits
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
3M Co
Original Assignee
Minnesota Mining and Manufacturing Co
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Priority to BE790370D priority Critical patent/BE790370A/xx
Application filed by Minnesota Mining and Manufacturing Co filed Critical Minnesota Mining and Manufacturing Co
Priority to US00191803A priority patent/US3802888A/en
Priority to CA152,476A priority patent/CA981513A/en
Priority to ES407529A priority patent/ES407529A1/es
Priority to SE7213145A priority patent/SE380909B/xx
Priority to AR244714A priority patent/AR197686A1/es
Priority to JP10516372A priority patent/JPS5435484B2/ja
Priority to AT898772A priority patent/AT326478B/de
Priority to PH14029*UA priority patent/PH9454A/en
Priority to IT53515/72A priority patent/IT966443B/it
Priority to FR7237235A priority patent/FR2156870B1/fr
Priority to ZA727489A priority patent/ZA727489B/xx
Priority to AU48021/72A priority patent/AU471936B2/en
Priority to CH1532372A priority patent/CH583922A5/xx
Priority to GB4855872A priority patent/GB1383604A/en
Priority to BR7370/72A priority patent/BR7207370D0/pt
Priority to DE2251554A priority patent/DE2251554C3/de
Application granted granted Critical
Publication of US3802888A publication Critical patent/US3802888A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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Classifications

    • 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
    • G03C1/498—Photothermographic systems, e.g. dry silver

Definitions

  • This invention relates to the recording of lightimages, with particular reference to novel sheet materials for use therein.
  • an initially substantially light-insensitive or light-stable sheet material which is rendered highly light-sensitive upon mere heating and which thereafter when first exposed to a light-image will develop a visible image under further restricted heating.
  • the sheet material may initially be manufactured, packed, and manipulated while exposed to light, and may thereafter, on demand, be quickly and easily made light-sensitive by simple heating. Sensitization may be accomplished by heating the entire sheet; alternatively, small segments of the lightstable sheet may independently be sensitized, exposed and developed.
  • the product is therefore particularly useful in the form of microfiche cards adapted for the cumulative recording of intelligence.
  • the present invention may and frequently does employ similar components and similar proportions but uses critically different procedures resulting in latent rather than immediate light-sensitivity.
  • the procedures employed serve to maintain the silver salt and the source of halide ion in interreactive proximity so as substantially to prevent any initial photosensitivity but so that, upon subsequent appropriate manipulation primarily involving the application of heat, interreaction occurs with formation of photosensitive silver halide in full catalytic proximity with the remaining organic silver salt.
  • the organic silver salt and the source of halide ion are laid down'in separate layers with an intervening separate thin layer of a'suitable film-forming thermoplastic binder.
  • the binder is incorporated with the silver salt and is of a specific type and in sufficient quantity to protect the salt from reaction with the halide until such time as the stratum is heated.
  • the polyvinyl acetal resins such as polyvinyl butyral and polyvinyl formal, are found to be particularly effective. Yet even these preferred materials must be employed with suitable precautions in order to avoid premature reaction between silver salt and halide ion. Thus it is necessary that the silver salt be protected with the binder prior to introduction of the halide.
  • Separation and avoidance of premature reaction of silver salt and halide may be achieve by coating in two layers, the first being dried prior to application of the second, the volatile vehicle of the second being preferably a nonsolvent for the dried first layer or at least being removed promptly so as to avoid any substantial contact produce a coated sheet showing no evidence of photosensitivity; whereas the same composition when first permitted to stand for as little as two to five hours prior to coating, or when inhibited from prompt evaporation of solvent after coating, is found to yield an obviously light-sensitive sheet.
  • Plasticizing of the polyvinyl acetal binder likewise has a tendency to permit migration and premature reaction of silver soap and halide; thus silver behenate half soap, a mixture of equimolar amounts of silver behenate and behenic acid, has been found ineffective in 7 sheets where prolonged stability is required, apparently due to the plasticizing effect of the free behenic acid.
  • mercuric halide may be used as the sole source of halide ion; but the necessary amount of halide ion is preferably here obtained in whole or in part from some other source.
  • Chlorides, bromides and iodides of calcium, nickel or cobalt are illustrative of other sources of halide ion which may be used.
  • the halide ions of these several compounds may be titrated with alcoholic silver nitrate solution and are found to be readily reactive with the organic silver soap.
  • the invention makes possible a microfiche card or transparency which may be handled under room light or used in appropriate viewing or pro- 40 jection apparatus without damage.
  • graphic intelligence is to be imparted to an initial or added small area of the card, the area is quickly and conveniently sensitized by brief heating, whereupon the desired image is imparted by exposure to a light-image followed by heat development, the remaining unheated areas of the card remaining non-light-sensitive.
  • EXAMPLE 1 Silver behenate, prepared by precipitation with silver nitrate from an equimolar proportion of the sodium salt of commercial behenic acid, is well dispersed in a mixture of toluene and methylethyl ketone by multiple passes through a homogenizer to form a thick slurry containing 20 weight percent of the silver soap.
  • a coating composition containing grams of methyl isobutyl ketone, and 20 ml. of a solution of 0.5 gram spectral sensitizing dye (RF-341) in 1,000 ml. of methanol, is coated on heat-resistant thin transparent polyethylene glycol terephthalate polyester film using a coating orifice of four mils. The coating is dried.
  • RF-341 0.5 gram spectral sensitizing dye
  • a second coating of a solution of 15 parts by weight of Vinylite VYLF ketone-soluble vinyl chloride-vinyl acetate copolymer in 100 parts of acetone, is applied at an orifice of 2 mils and allowed to dry.
  • a third coating also at an orifice of 2 mils, is then applied and permitted to dry at room temperature; it contains, in parts by weight:
  • Nonox WSO is a hindered phenol identified as l, l bis(2-hydroxy-3,S-dimethylphenyD-B,5,5- trimethylhexane.
  • Spectral sensitizers include merocyanine sensitizing dyes, such for example as 3-allyl-5-(3-ethyi-(2- naphthoxazoylidene)ethylidene)-l-pheny1-2- thiohydantoin.
  • the coated film is held for several seconds in contact with a platen maintained at 250 F., with no visible change. It is then exposed for 15 seconds to a light-image from a projection lamp, and reheated. A visible image develops within about ten seconds.
  • the sheet When heated at substantially higher temperatures, the sheet will darken uniformly due to a relatively slow oxidation-reduction reaction between the silver soap intensity of about 200 foot-candles, and heated by contact with a 250 F. platen for several seconds. Samples which remain unchanged in appearance after such treatment are next exposed to a light-image at the same intensity for 5 seconds and again heated at 250 F. for a time just sufficient to develop maximum darkening at image areas while avoiding as far as possible any significant darkening at the unexposed background areas. Further samples of the doubly coated film segments prior to initial heating are exposed to normal room light for two hours before being heated, exposed to a light-image, and heat-developed; and the test is repeated with a third set of samples, with preliminary exposure continued for 16 hours. Image and background areas of all pertinent specimens are measured for diffuse transmission optical density using the MacBeth Quantalog densitometer and the results are expressed as maximum (D max) and minimum (D min) densities respectively.
  • composition E employing a mixture of mercuric bromide and calcium bromide as the source of halide ion.
  • the reaction is catalytically EXAMPLE 3 accelerated at the exposed areas of the sensitized coating.
  • Application of heat during development is controlled to obtain maximum image density consistent with minimum backgrounding.
  • a first coating composition is prepared by adding grams of polyvinyl butyral (Butvar B 76") resin to a homogenatedye mixture prepared as in Example 1, with agitation in a high speed mixer. The resulting smooth liquid is coated on 5 mil transparent polyester film using a 5 mil orifice and allowed to dry.
  • Segments of the coated film are separately further coated at 3 mils with compositions each containing grams of a master batch prepared by mixing together 10 grams of cellulose acetate butyrate, 100 grams of methanol, 2 grams of phthalazinone, and a solution of 6 grams of hindered phenol (Nonox WSO) in 50 ml. of acetone, together with one or more halogencontaining salts as hereinafter tabulated, the salts being first dissolved in a small quantity of methanol for ease in mixing.
  • the doubly coated film segments are allowed to dry at room temperature.
  • a sheet prepared as above described but using 0.05 gram mercuric bromide and 0.03 gram of calcium bromide is first sensitized by brief heating at 245 F. under darkroom conditions, exposed to light from a UV sensitometer at separate areas for different times, and devel oped by heating for 5 seconds at 245? F. The image density is then measured. Maximum density is attained under these conditions with exposure of 25 seconds and the density is maintained at substantially the same level as time of exposure is increased to a maximum of 4 minutes. Under the same exposure and development conditions the unsensitized sheet shows a constant density of 0.05.
  • Example 1 The reaction between the halide salt and the silver salt to produce photosensitive silver halide is inhibited in Example 1 by the intervening film of vinyl chloridevinyl acetate copolymer, and much more effectively in Examples 2and 3 by the presence of the polyvinyl acetal resin.
  • Example 2and 3 The effect of variations in the proportions of this last-named material will now be further described.
  • EXAMPLE 4 A mixture of 13 parts by weight of silver behenate in 87 parts of mixed toluene and methylethyl ketone is homogenized and to each 100 grams of homogenate is added one ml. of sensitizer solution as defined in Example 1. Polyvinyl butyral resin is then added in different amounts to portions of the mixture and the well mixed compositions are separately coated at a thickness of 4 mils on polyester film, dried and overcoated at 3 mils with a composition containing 2 grams phthalazinone, 6 grams Nonox WSO reducing agent, and 1.4 ml. of a 10% solution of mercuric bromide in methanol, all dissolved in a mixture of 100 grams of acetone and 30 grams of methanol.
  • the coatings are dried at room temperature. Each segment is divided into two portions. One portion of each is exposed to light and is then heated at 260 F. to incipient backgrounding. The other portion is first heated at 260 F. for two seconds and is then exposed to light and again heated. Density measurements are made on all portions, with the following results:
  • EXAMPLE 5 A mixture of parts by weight of silver behenate in 85 parts of a 1:1 mixture of toluene and methylethyl ketone is homogenized to form a thick paste. To 17 parts by weight of the homogenate is added 35 parts of a 35% solution of polyvinyl butyral resin in methylethyl ketone with intensive mixing, resulting in -a milky liquid.
  • phthalazinone 0.1 part of mercuric bromide, and 0.8 part of a hindered phenol, in this instance bis( 2-hydroxy-3,5- ditertiarybutylphenyl) methane.
  • a hindered phenol in this instance bis( 2-hydroxy-3,5- ditertiarybutylphenyl) methane.
  • the well stirred mixture is promptly coated on 3 mil transparent polyester film using a coating blade at an orifice of 3 mils and the coating is promptly dried.
  • a protective coating of two mils of a 5% solution of cellulose acetate in acetone is applied over the silver-containing coating and the product is again promptly dried under forced ventilation at room temperature.
  • a portion of the coated film is first exposed to a lightimage at approximately 10 foot-candle-seconds from a tungsten filament source, and is then heated for 10 seconds at 138 C. No visible change is apparent, the optical density remaining at about 0.1.
  • Another portion of the film is first held for 15 seconds in contact with a metal block maintained at C. It is then exposed through a step wedge to tungsten radiation followed by heating for 10 seconds at 138 C resulting in a visible image having an optical density of 1.0 in the area exposed at 5 X 10 foot-candle-seconds.
  • the film may alternatively be rendered photosensitive by the action of a volatile solvent.
  • a volatile solvent As an example, acetone is applied to the surface of the film while exposed to light, and is permitted to dry slowly. The film is then heated. The solvent-treated area is darkened; the remaining areas remain unchanged.
  • Sheet material which after being exposed to normal indoor illumination for several hours and then heated for a few seconds at a photosensitizing temperature within the range 2 10- 285 F. remains visibly substantially unaltered but which when first thus heated and then exposed image-wise to said illumination for not more than a few minutes and then again heated undergoes substantial darkening at the light-struck image areas; said sheet material including a stratum containing an organic silver salt oxidizing agent, a hindered phenol reducing agent for silver ion, a source of mercury ions in significant small amount up to about 0.07 mol of mercury per mol of silver, and a source of halide ion in significant small amount equivalent to not more than about fifteen molar percent based on the amount of said silver salt, and wherein said silver salt and said source of. halide ion are held in closely spaced interreactive proximity by an intervening thermoplastic film-forming binder.

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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)
  • Heat Sensitive Colour Forming Recording (AREA)
  • Manufacture Of Macromolecular Shaped Articles (AREA)
US00191803A 1971-10-22 1971-10-22 Light-stable sheet material for recording light-images Expired - Lifetime US3802888A (en)

Priority Applications (17)

Application Number Priority Date Filing Date Title
BE790370D BE790370A (fr) 1971-10-22 Feuille stable a la lumiere pour l'enregistrement d'images lumineuses
US00191803A US3802888A (en) 1971-10-22 1971-10-22 Light-stable sheet material for recording light-images
CA152,476A CA981513A (en) 1971-10-22 1972-09-25 Light-stable sheet material for recording light-images
ES407529A ES407529A1 (es) 1971-10-22 1972-10-11 Metodo para fabricar un material en lamina.
SE7213145A SE380909B (sv) 1971-10-22 1972-10-12 Latent ljuskensligt arkmaterial och sett att framstella detta
AR244714A AR197686A1 (es) 1971-10-22 1972-10-19 Material laminar estable a la luz para el registro de imagenes luminosas y metodo para su produccion
CH1532372A CH583922A5 (ja) 1971-10-22 1972-10-20
PH14029*UA PH9454A (en) 1971-10-22 1972-10-20 Light-stable sheet material for recording light-images
JP10516372A JPS5435484B2 (ja) 1971-10-22 1972-10-20
FR7237235A FR2156870B1 (ja) 1971-10-22 1972-10-20
ZA727489A ZA727489B (en) 1971-10-22 1972-10-20 Light-stable sheet material for recording light-images
AU48021/72A AU471936B2 (en) 1971-10-22 1972-10-20 Light-stable sheet material for recording light-images
AT898772A AT326478B (de) 1971-10-22 1972-10-20 Photographisches aufzeichnungsmaterial und verfahren zu dessen herstellung
GB4855872A GB1383604A (en) 1971-10-22 1972-10-20 Light-stable sheet material for recording light-images
BR7370/72A BR7207370D0 (pt) 1971-10-22 1972-10-20 Material laminar e processo para sua obtencao
DE2251554A DE2251554C3 (de) 1971-10-22 1972-10-20 Lichtstabiles thermophotographisches Aufzeichnungsmaterial und Verfahren zu dessen Herstellung
IT53515/72A IT966443B (it) 1971-10-22 1972-10-20 Perfezionamento nei materiali in foglio atti alla registrazione di immagini di luce e relativo pro cedimento di produzione

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
US00191803A US3802888A (en) 1971-10-22 1971-10-22 Light-stable sheet material for recording light-images

Publications (1)

Publication Number Publication Date
US3802888A true US3802888A (en) 1974-04-09

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ID=22706992

Family Applications (1)

Application Number Title Priority Date Filing Date
US00191803A Expired - Lifetime US3802888A (en) 1971-10-22 1971-10-22 Light-stable sheet material for recording light-images

Country Status (17)

Country Link
US (1) US3802888A (ja)
JP (1) JPS5435484B2 (ja)
AR (1) AR197686A1 (ja)
AT (1) AT326478B (ja)
AU (1) AU471936B2 (ja)
BE (1) BE790370A (ja)
BR (1) BR7207370D0 (ja)
CA (1) CA981513A (ja)
CH (1) CH583922A5 (ja)
DE (1) DE2251554C3 (ja)
ES (1) ES407529A1 (ja)
FR (1) FR2156870B1 (ja)
GB (1) GB1383604A (ja)
IT (1) IT966443B (ja)
PH (1) PH9454A (ja)
SE (1) SE380909B (ja)
ZA (1) ZA727489B (ja)

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3960908A (en) * 1973-01-22 1976-06-01 Fuji Photo Film Co., Ltd. Process for preparing organosilver carboxylates
US4173482A (en) * 1977-03-16 1979-11-06 Asahi Kasei Kogyo Kabushiki Kaisha Dry image forming material containing an organic silver salt oxidizing agent, a reducing agent and a halogen molecule
US4188226A (en) * 1977-07-18 1980-02-12 Asahi Kasei Kogyo Kabushiki Kaisha Dry image forming material containing diarylhalomethane
DE2931920A1 (de) * 1978-08-11 1980-02-21 Asahi Chemical Ind Bilderzeugungsverfahren und vorrichtung hierfuer
US4332889A (en) * 1980-05-23 1982-06-01 Asahi Kasei Kogyo Kabushiki Kaisha Post-activation type dry image forming material
US4347310A (en) * 1977-10-14 1982-08-31 Asahi Kasei Kogyo Kabushiki Kaisha Heat developable silver image forming materials
US4395484A (en) * 1982-06-25 1983-07-26 Minnesota Mining And Manufacturing Company Roomlight-stable ultraviolet-response photothermographic imaging material
US4396712A (en) * 1980-05-30 1983-08-02 Asahi Kasei Kogyo Kabushiki Kaisha Dry image forming material
US4433037A (en) * 1982-07-15 1984-02-21 Eastman Kodak Company Heat erasable photographic element and process comprising silver halide
US4442202A (en) * 1979-04-16 1984-04-10 Asahi Kasei Kogyo Kabushiki Kaisha Post-activation type dry image forming material
US4893148A (en) * 1986-09-04 1990-01-09 Asahi Kasei Kogyo Kabushiki Kaisha Method for storing dry silver salt roll film for rotary type microphotography and rotary type microphotography camera system
US5279928A (en) * 1992-11-30 1994-01-18 Eastman Kodak Company Method for processing a photothermographic element

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JPS545687B2 (ja) * 1972-05-23 1979-03-20
JPS5264925A (en) * 1975-11-25 1977-05-28 Asahi Chemical Ind Image forming material
JPS52127326A (en) * 1976-04-19 1977-10-25 Asahi Chemical Ind Dry image forming material

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3589903A (en) * 1968-02-28 1971-06-29 Minnesota Mining & Mfg Silver halide,heat-developable image sheet containing mercuric ion
US3589901A (en) * 1968-02-28 1971-06-29 Minnesota Mining & Mfg Method of making a heat developable sheet containing mercury lens

Cited By (13)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3960908A (en) * 1973-01-22 1976-06-01 Fuji Photo Film Co., Ltd. Process for preparing organosilver carboxylates
US4173482A (en) * 1977-03-16 1979-11-06 Asahi Kasei Kogyo Kabushiki Kaisha Dry image forming material containing an organic silver salt oxidizing agent, a reducing agent and a halogen molecule
US4188226A (en) * 1977-07-18 1980-02-12 Asahi Kasei Kogyo Kabushiki Kaisha Dry image forming material containing diarylhalomethane
US4347310A (en) * 1977-10-14 1982-08-31 Asahi Kasei Kogyo Kabushiki Kaisha Heat developable silver image forming materials
DE2931920A1 (de) * 1978-08-11 1980-02-21 Asahi Chemical Ind Bilderzeugungsverfahren und vorrichtung hierfuer
US4287295A (en) * 1978-08-11 1981-09-01 Asahi Kasei Kogyo Kabushiki Kaisha Image forming method and apparatus therefor
US4442202A (en) * 1979-04-16 1984-04-10 Asahi Kasei Kogyo Kabushiki Kaisha Post-activation type dry image forming material
US4332889A (en) * 1980-05-23 1982-06-01 Asahi Kasei Kogyo Kabushiki Kaisha Post-activation type dry image forming material
US4396712A (en) * 1980-05-30 1983-08-02 Asahi Kasei Kogyo Kabushiki Kaisha Dry image forming material
US4395484A (en) * 1982-06-25 1983-07-26 Minnesota Mining And Manufacturing Company Roomlight-stable ultraviolet-response photothermographic imaging material
US4433037A (en) * 1982-07-15 1984-02-21 Eastman Kodak Company Heat erasable photographic element and process comprising silver halide
US4893148A (en) * 1986-09-04 1990-01-09 Asahi Kasei Kogyo Kabushiki Kaisha Method for storing dry silver salt roll film for rotary type microphotography and rotary type microphotography camera system
US5279928A (en) * 1992-11-30 1994-01-18 Eastman Kodak Company Method for processing a photothermographic element

Also Published As

Publication number Publication date
BR7207370D0 (pt) 1973-09-27
JPS5435484B2 (ja) 1979-11-02
GB1383604A (en) 1974-02-12
ZA727489B (en) 1973-07-25
DE2251554C3 (de) 1981-05-27
CA981513A (en) 1976-01-13
BE790370A (fr) 1973-04-20
JPS4851626A (ja) 1973-07-20
AT326478B (de) 1975-12-10
IT966443B (it) 1974-02-11
DE2251554A1 (de) 1973-05-03
AU4802172A (en) 1974-04-26
ES407529A1 (es) 1976-02-16
AU471936B2 (en) 1976-05-06
PH9454A (en) 1975-12-04
ATA898772A (de) 1975-02-15
SE380909B (sv) 1975-11-17
AR197686A1 (es) 1974-04-30
DE2251554B2 (de) 1980-09-04
CH583922A5 (ja) 1977-01-14
FR2156870A1 (ja) 1973-06-01
FR2156870B1 (ja) 1978-03-03

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