US3109737A - Silver halide print-out emulsions combining cadmium iodide - Google Patents

Silver halide print-out emulsions combining cadmium iodide Download PDF

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Publication number
US3109737A
US3109737A US737758A US73775858A US3109737A US 3109737 A US3109737 A US 3109737A US 737758 A US737758 A US 737758A US 73775858 A US73775858 A US 73775858A US 3109737 A US3109737 A US 3109737A
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United States
Prior art keywords
silver
iodide
sensitive
cadmium iodide
silver halide
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Expired - Lifetime
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US737758A
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English (en)
Inventor
Troy A Scott
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Honeywell Inc
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Honeywell Inc
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Publication date
Priority to US3123474D priority Critical patent/US3123474A/en
Application filed by Honeywell Inc filed Critical Honeywell Inc
Priority to US737758A priority patent/US3109737A/en
Priority to GB16791/59A priority patent/GB924658A/en
Priority to DEM41595A priority patent/DE1125278B/de
Priority to SE5007/59A priority patent/SE302078B/xx
Application granted granted Critical
Publication of US3109737A publication Critical patent/US3109737A/en
Anticipated expiration legal-status Critical
Expired - Lifetime legal-status Critical Current

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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
    • G03C1/005—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein
    • G03C1/49—Print-out and photodevelopable emulsions

Definitions

  • the present invention relates broadly to photographic sensitive compositions and more particularly to photographic compositions of the printout type.
  • print-out refers to that type of photosensitive substance upon which a visible image is obtained after an initial eX- posure to light or electromagnetic radiation has been utilized to form a latent image, the visible image being obtained initially or simply by an additional exposure to such radiation.
  • Print-out emulsion or dispersions are distinguished from development emulsions which require a development treatment such as a chemical development after initial exposure to produce a visible image, inasmuch as this image is produced by an additional exposure in print-out emulsions.
  • the specific print-out papers coated with a film, comprising a dispersion or emulsion of the compositions of the present invention are particularly sensitive to a high intensity beam of light or other electromagnetic energy of either visible or invisible wavelength radiated across a portion of the area of the film. While the material of the present invention is particularly sensitive to such exposure, the background or non-exposed area is sufficiently stable to render a highly contrasting image upon subsequent latensification.
  • a photosensitive silver halide is used as the basic sensitive ingredient of the composition, and a quantity of cadmium iodide is added to the silver halide in order to improve the photo response thereof.
  • the cadmium iodide sensitizes the silver halide parti ularly to brief exposures, in the range of microseconds, from a high intensity source, but causes very little sensitization of composition to relatively lower
  • a high degree of sensitivity to the trace coupled with a highly stable background produces a maximum contrast between the image and the background when applied to recording operations.
  • the present invention provides this desirable combination of high image sensitivity and high degree of background stability.
  • the intensity of the radiation source utilized in latensification is not as critical with the sensitive mixtures of the present invention as it is with available compositions of the prior art. in other words, the accumulated quantity or intensity of illumination or radiation to which the sensitized paper is exposed during latensification is not particularly critical.
  • the latensification rate obtainable by an intense exposure to ordinary fluorescent lamp lighting conditions has been found to be satisfactory for the silver halide compositions of the present invention, while this intensity of light is generally too great for available emulsions produced prior to the present invention.
  • halide as used throughout the specification is intended to encompass bromides, chlorides and iodides, fluorides being specifically excluded. Accordingly various silver halides may be employed, silver halides consisting mainly of or entirely of silver bromide being generally referred.
  • the sensitive paper exhibit a certain degree of permanence in order that any record prepared thereon will have a sufiiciently long and usable lifetime without losing its contrast. It is also desirable to have a sensitive paper which responds substantially uniformly to applied radiation without regard to varying intensities and different writing speeds and yet which exhibits a substantially uniform degree of contrast against the background upon latensification.
  • the sensitive films posses a sensitivity capable of writing in a wide range of speeds, including very slow speeds as well as speeds ranging up to more than 200,000 lineal inches per second. In spite of the varying requirements relative to different writing speeds, a uniform, relatively permanent and highly contrasting image is produced upon latensification.
  • Latensification may be accomplished through exposure to radiation within the sensitive range for the paper for a very short period of time. For example, several seconds or less under an ordinary fluorescent lamp is suiticient to latensify or print-out certain images or traces made on paper prepared in accordance with the present invention.
  • FIGURE 1 is a schematic illustration of a preferred process for preparation of sensitive dispersions in accordance with the present invention.
  • FIGURE 2 is a cross sectional view showing the sensitive material as a coating on a support member.
  • compositions of the present invention are not entirely understood.
  • silver halides generally, and in particular silver bromide
  • exposure to light produces elemental silver and free bromine, this phenomenon probably being carried out in accordance with the reversible equation shown below.
  • the free silver indicates the exposed area and a darkening of the area occurs.
  • the reaction in general may tend to reverse and therefore proceed to the left with a consequent loss of indicated exposed area.
  • Silver halide emulsions have long been employed in the photographic art, including silver bromide and silver brom-o-iodide as employed in the present invention. The presence of cadmium iodide is believed to prevent reverse reactions from occurring and hence increase sensitivity.
  • Other halides of cadmium not within the scope of this invention form a composition with silver halides which is less sensitive than the cadmium iodide doped material. The writing speed of compositions containing other cadmium salts is lower, and the trace, if formed, tends to fade and in some cases is substantially assimilated into the background.
  • the cadmium iodide additive as noted above performs substantially as a bromine acceptor, and hence there is no polyvinyl alcohol are suitable.
  • the invention is operable using a single halide salt, e.g., AgBr, with a mechanical mixture of AgBr plus AgI, or the co -precipitated silver bromo-iodide.
  • compositions of the present invention may be further sensitized if desired, by adding from .01 to .2% (by weight based on total solids) of an organic sensitizer such as thiourea which is the preferred sensitizer for this composition.
  • an organic sensitizer such as thiourea which is the preferred sensitizer for this composition.
  • Thiocarbamide, tbiosemicarbazide, paramethylamino phenol sulphate and mercapta succinic acid are useful and may be employed if desired.
  • inert carriers or binders may be employed in order to facilitate application and adhesion of the sensitive composition to paper in dispersion or emulsion fnom either aqueous compatible or aqueous incompatible carriers.
  • aqueous compatible or aqueous incompatible carriers In an aqueous system, pregelatinized dextrin, gelatin, starch, dextrin, thickening agents such as sea-weed extracts or In the nonsoluble systems, silicones may be employed.
  • coatings without a binder may be applied in dry form e.g. by electrostatic application and subsequently covered with a suitable conventional protective film.
  • the car-riers do not substantially affect the photographic properties of the compositions, but are merely used to adhere the composition to the base material.
  • Heat treating the coated paper when carriers other than gelatin have been used has been found advantageous in increasing top writing speeds and retarding the rate of background rise.
  • heating to a temperature of about 400 'F. or greater for a period of from 10 to 30 seconds produces beneficial results, it being necessary to avoid scorching the paper.
  • a temperature of about 400 F. for a period of about 20 seconds has been considered the optimum for compositions prepared in accordance with the present invention.
  • Somewhat lower temperatures, in the range of from about 300 F. to 400 F. may be employed for somewhat longer periods of time.
  • Temperatures as low as 200 F. have been found to improve the qualities of the coated paper, this improvement being somewhat less than that achieved when higher temperatures are employed. For example, one coated paper was heat treated at 200 F.
  • the maximum sensitivity of the paper is found to be below about 5000 angstroms, and mainly below about 4400 angstroms.
  • Various commercially available high intensity light sources may be conveniently employed for producing the trace image, such as for example the Osram lamp manufactured by Osram, Kunststoff, West Germany, as hereinafter identified in Example I.
  • high intensity radiation reference is made to electromagnetic radiations having an intensity of about 10 ergs/sec./cm. or greater. In order to obtain a useful trace, this radiation 'is applied to the material for a period of about 10- seconds or greater.
  • lower intensity sources may be satisfactorily utilized, these sources may require substantially higher total enengics inasmuch as the material exhibits a low intensity reciprocity failure.
  • the sensitive films are particularly sensitive to radiations of relatively high intensity, they are also suitable for use at lower intensities, with a corresponding drop in writing speed.
  • For latensification a less intense source of light available generally across the extent of the paper is desired. Ordinary fluorescent lighting at close range is useful both in its intensity and its output wave lengths characteristic for latensification operations. For example, latensification may be carried out under the influence of illumination of the order of 75 foot candles of coolwhite fluorescent light.
  • the silver nitrate was weighed and dissolved in the prescribed amount of distilled water. Then the ammonia solution was added with stirring until the solution cleared as the precipitate of silver oxide formed by the first added portions of the ammonia was redissolved.
  • Potassium Halide Solution Compound Amount Kl 1.66 gr. (0.0l0 mol). liBr 143 gr. (1.20 mol). H O (distilled) 300cc.
  • the potassium iodide was weighed carefully in order to insure precise control over the iodide content of the resultant silver halide mixture.
  • the potassium halides were dissolved in the prescribed amount of water contained in a two-liter beaker which was set in a waterethylene glycol bath. The bath was heated on a hot plate to about 70-80 C. The solution of potassium halide was stirred mechanically with a stainless steel stirrer.
  • Ammonia and potassium bromide act as solvents for the silver halides formed and promote crystal growth.
  • the smaller silver halide crystals may dissolve and be re-deposited on the surfaces of larger crystals by a process known as Ostwald ripening. This process can occur during the slow precipitation step.
  • the mixture was stirred vigorously with a mechanical stirrer during the precipitation period.
  • the silver halide mixture was filtered by suction on a Biichner funnel and was washed five times with distilled water. It is not normally necessary to dry the silver halides after filtering and washing.
  • Cadmium iodide to increase the print-out effect and to suppress background during latensification.
  • Starch to bind the ocating to the paper support.
  • various application techniques may be employed, such as transfer roller coating, dip coating using an air-knife to wipe oh the excess upon emergence from the bath, or by conventional spreading using a doctor knife to control the thickness of the film.
  • thickness of the coatings to be applied to paper or other supports is dependent on the characteristics desired in the end product, it has been found that the composition disclosed above was when applied in layers calculated to be in the range of about 0.5 mil in thickness useful. As the thickness of the wet film is diflicult to measure, it is somewhat easier to use the weight per unit area of solids deposited as a reference. About 2 grams of solids per square foot of the dried film appears to be satisfactory.
  • the critical features are that the coating be uniform, flexible, and adherent to the base material. After application to the base paper, the coating was dried and was subjected to a temperature of about 400 F. for a period of 20 seconds.
  • FIGURE 2 of the drawings wherein there is illustrated a photosensitive paper having a base support and a sensitive coating. This coating was prepared as in Example 1 above.
  • Sensitive papers prepared according to this process were capable of writing speeds equivalent to more than 200,000 inches per second when illuminated from a source having an intensity of about 100,000 candles/sq. cm. under the spectrum distribution obtainable from a high pressure mercury vapor arc lamp such as the Osram lamp manufactured by Osram, Kunststoff, West Germany, and identified as their model HBOAOV/l High Pressure Mercury Lamp, this lamp being employed as specified in the aforementioned application of Mahoney et al. A high proportion of this radiation is in the ultraviolet.
  • Mahoney et al. application A complete system for recording is described and disclosed in the aforementioned Mahoney et al. application.
  • EXAMPLE 2 A silver nitrate solution was prepared in accordance with the procedures of Example 1, and a potassium halide solution was prepared as follows.
  • EXAMPLE 3 Identical techniques, preparations, and compositions were followed as in Example 1, with the exception that 2% of cadmium iodide was added to the composition rather than the as added therein.
  • the resultant material provided a good recording paper capable of recording a distinct trace at writing speeds about as fast as those in Example 1, under the identical conditions set forth therein, the background being somewhat less stable. This trace is also uniform in color and contrast upon latensification.
  • Example 4 Identical techniques, preparations and compositions were followed as in Example l'above with the exception that rather than 5% of cadmium iodide was added to the composition. This resulted in a recording paper capable of recording a uniform distinct trace at /2 as fast as those in Example 1.
  • the silver halides may be precipitated in cold Water or even ice water.
  • the crystal ripening and milling processes may be dispensed with, although the character istics of the material, for the purposes of this disclosure may be aifected adversely to some extent.
  • the present invention makes possible the production of sensitive papers capable of giving a sharp visible image at Writing speeds of up to 200,000 in./sec.
  • the latent image becomes visible a short time after exposure to fluorescent light, and maintains good contrast against the background "for extended periods of time.
  • Such papers find extensive use in modern recording instruments.
  • a process for the production of photographic printout compositions sensitive to high intensity radiation of short duration and including an inert colloid carrier having a photosensitive substance consisting of silver halide and cadmium iodide dispersed theretlhrough comprising coprecipitating a slurry of silver halide salts where at least 95 molar percent of the silver halideis silver bromide and the balance silver iodide, Washing said precipitate, adding between about /2% to 20% by Weight of cadmium iodide to the Washed silver halide precipitate, and forming a dispersion of said silver halide and cadmium iodide in an inert colloid carrier.
  • a process for the production of photographic printout paper sensitive to high intensity radiation and substantially insensitive to relatively low intensity radiation including a support element coated with an inert colloid carrier and having a photosensitive substance consisting of silver halide and cadmium iodide dispersed therethrough, said process comprising coprecipitating a slurry of silver halide salts where at least 95 molar percent of the silver halide is silver bromide and the balance silver iodide, Washing said precipitate, adding between about /2% and 20% by weight of cadmium iodide based on the Weight or" the silver salts in the Washed silver halide precipitate, forming a.
  • dispersion of silver halide and cadmium iodide in an inert colloid carrier coating a support member With a film of said dispersion, and heating said film to a temperature of from about 200 F. up to about 400 F. for a period in excess of about 10 seconds.
  • a photographic print-out composition comprising an inert carrier having dispersed therein a photosensitive substance consisting essentially of from up to 99.5% by weight of precipitated, Washed silver bromide, the balance being cadmium iodide which is added thereto, said composition being characterized in that it is particularly sensitive to high intensity radiation of less than about 4,400 angstroms and in being substantially insensitive to ambient light intensity and wave length.
  • a photographic print-out composition comprising an inert carrier having dispersed therein a photosensitive substance, said photosensitive substance consisting essentially of about 95% by weight of a precipitated, Washed silver bromide, the balance being cadmium iodide Which is added thereto, said substance being characterized in that it is particularly sensitive to high intensity radiation of less than about 4,400 angstroms and in being substantially insensitive to ambient light intensity and Wave length.
  • a photo-graphic print-out composition comprising an.
  • photosensitive substance consisting essentially of from between 80% and 99.5% by Weight of precipitated Washed silver halides, said halides consisting of silver bromide containing up to about 5 molar percent silver iodide; the balance being cadmium iodide which is added thereto, said substance characterized in that it is particularly sensitive to high intensity radiation of less than about 4,400 angstroms and in being substantially insensitive to ambient light intensity and wave length.
  • a photographic print-out composition consisting essentially or" from up to 98% by Weight precipitated Washed silver halides dispersed in an inert colloid carrier, said halides consisting of silver bromide containing up to 5 molar percent of silver iodide, the balance being cadmium iodide which is added thereto, said substance characterized in that it is particularly sensitive to high intensity radiation of less than about 4,400 angstroms and in being substantially insensitive to ambient light intensity and Wave length.

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Silver Salt Photography Or Processing Solution Therefor (AREA)
  • Non-Silver Salt Photosensitive Materials And Non-Silver Salt Photography (AREA)
  • Paper (AREA)
US737758A 1958-05-26 1958-05-26 Silver halide print-out emulsions combining cadmium iodide Expired - Lifetime US3109737A (en)

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Application Number Priority Date Filing Date Title
US3123474D US3123474A (en) 1958-05-26 byrne
US737758A US3109737A (en) 1958-05-26 1958-05-26 Silver halide print-out emulsions combining cadmium iodide
GB16791/59A GB924658A (en) 1958-05-26 1959-05-15 Improved photographic material
DEM41595A DE1125278B (de) 1958-05-26 1959-05-22 Auskopiermaterial
SE5007/59A SE302078B (de) 1958-05-26 1959-05-26

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US73783158A 1958-05-26 1958-05-26
US737758A US3109737A (en) 1958-05-26 1958-05-26 Silver halide print-out emulsions combining cadmium iodide
US6419260A 1960-10-21 1960-10-21

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Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3241971A (en) * 1961-08-01 1966-03-22 Eastman Kodak Co Photographic silver halide emulsions
US3249440A (en) * 1963-03-15 1966-05-03 Du Pont Radiation-sensitive elements and their preparation
US3305365A (en) * 1962-11-12 1967-02-21 Oriental Photo Ind Co Ltd Photosensitive material
US3647456A (en) * 1968-12-23 1972-03-07 Ibm Method of making conductive silver images and emulsion therefor
US3874881A (en) * 1972-03-14 1975-04-01 Fuji Photo Film Co Ltd Sensitizing a mixture of silver halide and lead halide by heat
US3976489A (en) * 1972-03-24 1976-08-24 Polaroid Corporation Silver halide photographic products with semiconductor sensitizers
US3996053A (en) * 1975-07-21 1976-12-07 Eastman Kodak Company Photosensitive composition containing a mixture of cadmium iodide and cuprous iodide
US4009041A (en) * 1974-10-03 1977-02-22 Polaroid Corporation Fogged, direct-positive silver halide emulsion containing a gallium sulfide semiconductor
US4045227A (en) * 1972-08-04 1977-08-30 Fuji Photo Film Co., Ltd. Method for stabilizing silver halide photographic material
US4207103A (en) * 1978-06-26 1980-06-10 Eastman Kodak Company Photographic print-out silver halide process

Families Citing this family (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB1059782A (en) * 1962-09-11 1967-02-22 Eastman Kodak Co Photographic silver halide emulsions and sensitive materials prepared therefrom
US3367780A (en) * 1963-08-19 1968-02-06 Eastman Kodak Co Direct-print photographic silver halide emulsions
CA731575A (en) * 1964-06-01 1966-04-05 A. Sprung Joseph Light-sensitive silver halide print-out emulsions
FR1408303A (fr) * 1964-07-01 1965-08-13 Kodak Pathe Nouvelle émulsion photographique à noircissement direct et procédé pour l'utilisation de cette émulsion
US3317322A (en) * 1965-08-27 1967-05-02 Eastman Kodak Co Photographic emulsions having high internal sensitivity
US3511662A (en) * 1965-10-28 1970-05-12 Eastman Kodak Co Method of preparing silver halide grains having high internal sensitivity
US3531291A (en) * 1967-04-07 1970-09-29 Eastman Kodak Co Silver halide emulsions capable of being chemically or photo developed
US3725073A (en) * 1967-05-25 1973-04-03 Xerox Corp Light developable,direct writing,silver halide emulsions containing gold,iodine,lead and copper
BE754323A (fr) * 1969-08-04 1971-01-18 Fuji Photo Film Co Ltd Procede pour la fabrication d'un materiel sensible electrophotographique
US3852072A (en) * 1972-05-11 1974-12-03 Polaroid Corp Photographic products and processes comprising synthetic nuclear isotopes
CN102212000A (zh) * 2011-05-25 2011-10-12 原平市同利化工有限责任公司 2-氟-3羟基丙酸烷基酯的合成方法

Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB108193A (en) * 1916-07-26 1917-07-26 Edouard Blondel La Rougery Improvements in or relating to Photography.
US2126318A (en) * 1937-02-09 1938-08-09 Eastman Kodak Co Print-out emulsion
US2816029A (en) * 1955-03-08 1957-12-10 Eastman Kodak Co Supersensitizing combinations comprising simple cyanine dyes and metal salts
US2839405A (en) * 1955-03-08 1958-06-17 Eastman Kodak Co Inorganic salt antifoggants for photographic emulsions
US2843490A (en) * 1955-03-08 1958-07-15 Eastman Kodak Co Supersensitizing combinations comprising meso-substituted carbocyanine dyes and polyvalent metal salts
US3047392A (en) * 1960-02-01 1962-07-31 Honeywell Regulator Co Photographic hydroxyethyl starch silver halide print-out composition

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2950972A (en) * 1954-11-24 1960-08-30 Gen Aniline & Film Corp Photographic emulsions having increased sensitivity to x-ray and gamma ray radiation
US3039871A (en) * 1961-03-02 1962-06-19 Honeywell Regulator Co Photographic composition

Patent Citations (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
GB108193A (en) * 1916-07-26 1917-07-26 Edouard Blondel La Rougery Improvements in or relating to Photography.
US2126318A (en) * 1937-02-09 1938-08-09 Eastman Kodak Co Print-out emulsion
US2816029A (en) * 1955-03-08 1957-12-10 Eastman Kodak Co Supersensitizing combinations comprising simple cyanine dyes and metal salts
US2839405A (en) * 1955-03-08 1958-06-17 Eastman Kodak Co Inorganic salt antifoggants for photographic emulsions
US2843490A (en) * 1955-03-08 1958-07-15 Eastman Kodak Co Supersensitizing combinations comprising meso-substituted carbocyanine dyes and polyvalent metal salts
US3047392A (en) * 1960-02-01 1962-07-31 Honeywell Regulator Co Photographic hydroxyethyl starch silver halide print-out composition

Cited By (10)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3241971A (en) * 1961-08-01 1966-03-22 Eastman Kodak Co Photographic silver halide emulsions
US3305365A (en) * 1962-11-12 1967-02-21 Oriental Photo Ind Co Ltd Photosensitive material
US3249440A (en) * 1963-03-15 1966-05-03 Du Pont Radiation-sensitive elements and their preparation
US3647456A (en) * 1968-12-23 1972-03-07 Ibm Method of making conductive silver images and emulsion therefor
US3874881A (en) * 1972-03-14 1975-04-01 Fuji Photo Film Co Ltd Sensitizing a mixture of silver halide and lead halide by heat
US3976489A (en) * 1972-03-24 1976-08-24 Polaroid Corporation Silver halide photographic products with semiconductor sensitizers
US4045227A (en) * 1972-08-04 1977-08-30 Fuji Photo Film Co., Ltd. Method for stabilizing silver halide photographic material
US4009041A (en) * 1974-10-03 1977-02-22 Polaroid Corporation Fogged, direct-positive silver halide emulsion containing a gallium sulfide semiconductor
US3996053A (en) * 1975-07-21 1976-12-07 Eastman Kodak Company Photosensitive composition containing a mixture of cadmium iodide and cuprous iodide
US4207103A (en) * 1978-06-26 1980-06-10 Eastman Kodak Company Photographic print-out silver halide process

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SE302078B (de) 1968-07-01
DE1125278B (de) 1962-03-08
GB924658A (en) 1963-05-01
US3123474A (en) 1964-03-03

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