US2592250A - Photographic silver bromide emulsion containing some silver iodide - Google Patents

Photographic silver bromide emulsion containing some silver iodide Download PDF

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Publication number
US2592250A
US2592250A US82914A US8291449A US2592250A US 2592250 A US2592250 A US 2592250A US 82914 A US82914 A US 82914A US 8291449 A US8291449 A US 8291449A US 2592250 A US2592250 A US 2592250A
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silver
emulsion
bromide
iodide
chloride
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US82914A
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Davey Edward Philip
Knott Edward Bowes
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Eastman Kodak Co
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Eastman Kodak Co
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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
    • G03C1/015—Apparatus or processes for the preparation of emulsions
    • 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
    • G03C1/485—Direct positive emulsions
    • G03C1/48538—Direct positive emulsions non-prefogged, i.e. fogged after imagewise exposure

Definitions

  • This invention relates to photographic emulsions which are capable of forming an internal latent image upon exposure to light.
  • the emulsions which form an internal latent image are known (Mees, The Theory of the Photographic Process (1942), page 166; Berg, Marriage and Stevens Journal Optical Society of America, vol. 31 (1941), page 385).
  • Knott and Stevens U. S. application Serial No. 528,738, filed March 30, 1944, now abandoned, continuation-in-part application Serial No. 756,636 now U. S. Patent 2,456,956, a process is described employing this type of emulsion which is designated therein as type I.
  • the emulsion of the present invention is useful in the process of the Knott and Stevens application.
  • Photographic emulsions are usually made by the following series of operations: (1) emulsification or digestion or ripening of the silver halide, (2) freeing the emulsion from excess soluble salts usually by washing, (3) the second digestion or after-ripening step.
  • Silver nitrate or other soluble silver salt solution is added to a solution of the halide in the presence of a small amount of gelatin.
  • the silver halide produced in this way is usually silver bromide containing a smallamount of iodide.
  • Gelatin is added to the emulsion during or before the second digestion and the content of the sensitizers, usually sulfur compounds, normally present in the gelatin acts to increase the sensitivity of the final emulsions.
  • Photographic emulsions may be either neutral or ammoniacal emulsions.
  • Ammonia is ordinarily used during emulsification but if a neutral emulsion is being prepared, no ammonia is used thereand temperatures in the neighborhood of 70-90 C. are used in the precipitation of the silver halide.
  • the precipitation of the silver halide is carried out with an excess of soluble halide, it is necessary to wash the excess soluble halide and other soluble salts from the emulsion after emulsification and digestion. This operation removes the potassium nitrate and any excess of potassium bromide or other soluble halide present in the emulsion.
  • the emulsion is then subjected to the second digestion or after-ripening during which the sensitivity continues to increase.
  • the emulsion may then be coated or stored for future coating.
  • a method of making a sensitive photographic silver halide emulsion which comprises first forming in the presence of inert gelatin, and in one or more stages, an emulsion of silver salt grains consisting at least partly of a. silver salt which is more soluble in water than is silver 2 Claims.
  • bromide subsequently converting the whole of such grains to silver bromide or iodobromide and preferably if the silver iodide content of the emulsion is less than 6% of the total amount ofzrsilyer halide, treating such grains with an iodine compound to bring the silver iodide content upto at least 6%, ripening the emulsion and then either washing out some of the soluble salts or washing out the whole of the soluble salts followed by addition of soluble salts such as soluble chloride or,
  • the soluble halide content of the finished emulsion should be above 0.03 gram of potassium bromide per liter (preferably between 0.03 and 0.3 gram per liter) or the equivalent of any other bromide or chloride or mixture thereof.
  • equivalent as used here means that there is the same suppressing action on the silver ion pounds which have labile sulfur atoms have been removed (Steigmann, Journal Society Chemical Industry,- vol. 61, 1942, page 162).
  • ripening may be performed before the addition of iodide in those cases where such addition is necessary.
  • iodide content of the final emulsion should be at least 10 to 20%. are made in the following general way.
  • Thefirst step is to form in the presence of a small amount of inert gelatin '2.
  • silver salt which is more soluble in water than silver bromide, that is, silver chloride or silver thiocyanate. This is accomplished by'adding separate solutions of potassium chloride in water, and silver nitrate in water, to a solution of gelatin containing a silverchloride or other silver salt more soluble in water than silver bromide, to a silver halide less soluble in water than silver chloride, that is,. silver bromide, silver iodide or silver iodobromide.”
  • the silver iodide content of the emulsion should preferably be at least 6% of the total amount of silver halide and if the iodide content is less than 6%, it can be brought up to at least 6% by treating the emulsion with an iodine compound such as potassium iodide. It is preferable to bring the iodide content to at least 10 to 20% of the total halide content of the emulsion.
  • the next step in our process is to add additional gelatin and ripen the emulsion for about 15 minutes at a low temperature.
  • the final step is the washing to remove a portion of the soluble salts.
  • a distinction over the usual emulsion making procedure is that a portion of the soluble salts are left in the emulsion. Either some of the soluble salts may be removed by washing or the whole of the soluble salts may be removed followed by addition of the required amount of soluble salts such as soluble chloride or bromide.
  • the temperature of the solutions and emulsions should not be above about 50 C.
  • An example of an emulsion made according to the present invention is as follows:
  • a sensitive silver halide emulsion which comprises the addition of aqueous silver nitrate solution to at least an equivalent amount of aqueous alkali chloride solution and gelatin, which alkali chloride reacts substantially completely with all of the silver to form silver chloride, then adding an aqueous mixture of alkali bromide and iodide in an amount which will completely convert substantially all of the silver chloride to silver bromide and silver iodide so that the resulting emulsion will contain at least approximately 5 per cent silver iodide, the remainder being essentially all silver bromide, ripening the emulsion, and washing out at least some of the soluble salts and bringing the soluble halide content of the emulsion to a potassium bromide equivalent concentration above 0.03 gram per liter, all of the operation being conducted at less than about C.

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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)
  • Compositions Of Macromolecular Compounds (AREA)

Description

Patented Apr. 8, 1952 PHOTOGRAPHIC SILVER BROMIDE EMUL- SION CONTAINING SOME SILVER IODIDE Edward Philip Davey and Edward BowesKnott, Wealdstone, England, assignors to Eastman Kodak Company, Roch-ester, N. Y., a corporation of New Jersey No Drawing. Application March 22, 1949, Serial No. 82,914. In Great Britain May 13, 1947 This invention relates to sensitive photographic silver halide emulsions.
This invention relates to photographic emulsions which are capable of forming an internal latent image upon exposure to light. The emulsions which form an internal latent image are known (Mees, The Theory of the Photographic Process (1942), page 166; Berg, Marriage and Stevens Journal Optical Society of America, vol. 31 (1941), page 385). In Knott and Stevens, U. S. application Serial No. 528,738, filed March 30, 1944, now abandoned, continuation-in-part application Serial No. 756,636 now U. S. Patent 2,456,956, a process is described employing this type of emulsion which is designated therein as type I. The emulsion of the present invention is useful in the process of the Knott and Stevens application.
Photographic emulsions are usually made by the following series of operations: (1) emulsification or digestion or ripening of the silver halide, (2) freeing the emulsion from excess soluble salts usually by washing, (3) the second digestion or after-ripening step. Silver nitrate or other soluble silver salt solution is added to a solution of the halide in the presence of a small amount of gelatin. The silver halide produced in this way is usually silver bromide containing a smallamount of iodide. Gelatin is added to the emulsion during or before the second digestion and the content of the sensitizers, usually sulfur compounds, normally present in the gelatin acts to increase the sensitivity of the final emulsions.
Photographic emulsions may be either neutral or ammoniacal emulsions. Ammonia is ordinarily used during emulsification but if a neutral emulsion is being prepared, no ammonia is used thereand temperatures in the neighborhood of 70-90 C. are used in the precipitation of the silver halide.
Since the precipitation of the silver halide is carried out with an excess of soluble halide, it is necessary to wash the excess soluble halide and other soluble salts from the emulsion after emulsification and digestion. This operation removes the potassium nitrate and any excess of potassium bromide or other soluble halide present in the emulsion. The emulsion is then subjected to the second digestion or after-ripening during which the sensitivity continues to increase. The emulsion may then be coated or stored for future coating.
According to the present invention, there is provided a method of making a sensitive photographic silver halide emulsion which comprises first forming in the presence of inert gelatin, and in one or more stages, an emulsion of silver salt grains consisting at least partly of a. silver salt which is more soluble in water than is silver 2 Claims. (Cl. 95--7) bromide, subsequently converting the whole of such grains to silver bromide or iodobromide and preferably if the silver iodide content of the emulsion is less than 6% of the total amount ofzrsilyer halide, treating such grains with an iodine compound to bring the silver iodide content upto at least 6%, ripening the emulsion and then either washing out some of the soluble salts or washing out the whole of the soluble salts followed by addition of soluble salts such as soluble chloride or,
bromide.
The soluble halide content of the finished emulsion should be above 0.03 gram of potassium bromide per liter (preferably between 0.03 and 0.3 gram per liter) or the equivalent of any other bromide or chloride or mixture thereof. The term equivalent as used here means that there is the same suppressing action on the silver ion pounds which have labile sulfur atoms have been removed (Steigmann, Journal Society Chemical Industry,- vol. 61, 1942, page 162).
It is also desirable to avoid digestion, that is,.
treatments after washing which increase sensie tivity such as heat treatment. Some ripeningmay be performed before the addition of iodide in those cases where such addition is necessary. Preferably the iodide content of the final emulsion should be at least 10 to 20%. are made in the following general way.
Thefirst step is to form in the presence of a small amount of inert gelatin '2. silver salt which is more soluble in water than silver bromide, that is, silver chloride or silver thiocyanate. This is accomplished by'adding separate solutions of potassium chloride in water, and silver nitrate in water, to a solution of gelatin containing a silverchloride or other silver salt more soluble in water than silver bromide, to a silver halide less soluble in water than silver chloride, that is,. silver bromide, silver iodide or silver iodobromide."
This isaccomplished by'adding to the silver chloride emulsion a solution of an excess of potassium Our emulsions bromide or a mixture of potassium bromide and potassium iodide or other soluble bromide or iodide. The silver iodide content of the emulsion should preferably be at least 6% of the total amount of silver halide and if the iodide content is less than 6%, it can be brought up to at least 6% by treating the emulsion with an iodine compound such as potassium iodide. It is preferable to bring the iodide content to at least 10 to 20% of the total halide content of the emulsion.
The next step in our process is to add additional gelatin and ripen the emulsion for about 15 minutes at a low temperature.
The final step is the washing to remove a portion of the soluble salts. A distinction over the usual emulsion making procedure is that a portion of the soluble salts are left in the emulsion. Either some of the soluble salts may be removed by washing or the whole of the soluble salts may be removed followed by addition of the required amount of soluble salts such as soluble chloride or bromide. During all of the emulsion-making procedure, the temperature of the solutions and emulsions should not be above about 50 C. An example of an emulsion made according to the present invention is as follows:
, Example I Solution No. 1:
Inert gelatin gms 102.6l KCl gms 102.6 at 40 C. Water ccs 2873] Solution N o. 2:
KCl gms 513 a Water ccs 2668} 45 Solution No. 3:
AgNOz gms 1000 Water ccs 2668} 45 Solution No. 4:
KBr gms 820.8 M KI gms 205.2 at 45 C. Water ccs 2565 Run Solutions Nos. 2 and 3 simultaneously into Solution No. 1 in a vessel, taking 90 seconds to do this. Then ripen for 1 minute at 45 C. Next add Solution No. 4 then ripen for 20 minutes at 45 C. Next add 1206 gms. of inert gelatin (dry). Then ripen at 45 C. for 15 minutes during which time the gelatin dissolves. Set and shred the emulsion and then wash until free from all soluble bromide and then add about 770 cos. of 10% solution of KCl (by weight), and then add water to make 18 litres.
Example I I Solution N o. 1:
Inert gelatin gm 128 KCl gms 10.2]at45C.
Water ccs 2873 Solution No. 2:
KCl gms 513 Water ccs 2668 at Solution No. 3:
AgNO; gms 1000 0 Water ccs 2668} C Solution No. 4:
KBr -gms 61.6
KCl ms 20.5
KI Ema- 51.3
Water ccs-- 257 Solution No. 5:
KBr gms 770 KI gms 154 at45C.
Water ccs 1796' Number Run Solutions Nos. 2 and 3 simultaneously into Solution No. 1 in a vessel, taking 90 seconds to do this. Then ripen for 30 seconds at C. Next add Solution No. 4 taking 2 minutes to do this and ripen for 15 minutes at 45 C. Next add Solution No. 5 taking 25 minutes to do this, and ripen for 1 minute at 45 C. Then add 51.3 cos. of ammonia (S. G. 0.935) and 1180 gms. of dry inert gelatin at 45 C. and ripen for 15 minutes at 45 C. during which time the gelatin dissolves. Set, wash and shred, add 770 cos. of 10% solution of KCl, and then add water to make 18 litres.
It will be understood that the examples and modifications included herein are illustrative only and that our invention is to be taken as limited only by the scope of the appended claims.
This application is a continuation-in-part of our application Serial No. 790,232, filed December 6, 1947, now abandoned.
We claim:
1. The method of making a sensitive silver halide emulsion which comprises the addition of aqueous silver nitrate solution to at least an equivalent amount of aqueous alkali chloride solution and gelatin, which alkali chloride reacts substantially completely with all of the silver to form silver chloride, then adding an aqueous mixture of alkali bromide and iodide in an amount which will completely convert substantially all of the silver chloride to silver bromide and silver iodide so that the resulting emulsion will contain at least approximately 5 per cent silver iodide, the remainder being essentially all silver bromide, ripening the emulsion, and washing out at least some of the soluble salts and bringing the soluble halide content of the emulsion to a potassium bromide equivalent concentration above 0.03 gram per liter, all of the operation being conducted at less than about C.
, 2. The method of makinga sensitive silver halide emulsion which comprises the addition of aqueous silver nitrate solution to at least an equivalent amount of aqueous potassium chloride solution and gelatin, which potassium chloride reacts completely with all of the silver to form silver chloride, then adding an aqueous mixture of potassium bromide and iodide in an amount which will completely convert substantially all 01 the silver chloride to silver bromide and silver iodide so that the resulting emulsion will contain approximately 6 per cent silver iodide, the re mainder being silver bromide, ripening the emulsion, and washing the emulsion to bring the soluble halide content to a potassium bromide equivalent concentration above 0.03 gram per litre, all
- of the operations being conducted at less than about 50 C.
EDWARD PHILIP DAVEY. EDWARD BOWES KNO'IT.
REFERENCES CITED The following references are of record in the file of this patent:
UNITED STATES PATENTS Name Date Crouse et al. May 28, 1946 OTHER REFERENCES Huse and Muelendyke, The Spectral Sensitivity of Mixtures of Silver Iodide and Silver Bromide, The Photographic Journal (Gr. Britain), June 1926, N. S. vol. 50, pp. 306-309.
Photographic Emulsions Wall American Photographic Publishing Co., 1929, Boston, Massachusetts; pages 52 and 53; footnote 3.

Claims (1)

1. THE METHOD OF MAKING A SENSITIVE SILVER HALIDE EMULSION WHICH COMPRISES THE ADDITION OF AQUEOUS SILVER NITRATE SOLUTION TO AT LEAST AN EQUIVALENT AMOUNT OF AQUEOUS ALKALI CHLORIDE REACTS SUBAND GELATIN, WHICH ALKALI CHLORIDE REACTS SUBSTANTIALLY COMPLETELY WITH ALL OF THE SILVER TO FORM SILVER CHLORIDE, THEN ADDING AN AQUEOUS MIXTURE OF ALKALI BROMIDE AND IODIDE IN AN AMOUNT WHICH WILL COMPLETELY CONVERT SUBSTANTIALLY ALL OF THE SILVER CHLORIDE TO SILVER BROMIDE AND SILVER IODIDE SO THAT THE RESULTING EMULSION WILL CONTAIN AT LEAST APPROXIMATELY 6 PER CENT SILVER IODIDE, THE REMAINDER BEING ESSENTIALLY ALL SILVER BROMIDE,RIP ENING THE EMULSION, AND WASHING OUT AT LEAST SOME OF THE SOLUBLE SALTS AND BRINGING THE SOLUBLE HALIDE CONTENT OF THE EMULSION TO A POTASSIUM BROMIDE EQUIVALENT CONCENTRATION ABOVE 0.03 GRAM PER LITER, ALL OF THE OPERATION BEING CONDUCTED AT LESS THAN ABOUT 50* C.
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US3000739A (en) * 1957-04-02 1961-09-19 Du Pont Process for preparing silver halide emulsions
US3031304A (en) * 1958-08-20 1962-04-24 Albert J Oliver Fine grain nuclear emulsion
US3237008A (en) * 1961-01-19 1966-02-22 Eastman Kodak Co Roomlight handling radiographic element including an x-ray sensitive layer overcoated with a dye desensitized silver halide emulsion
US3531288A (en) * 1966-03-11 1970-09-29 Eastman Kodak Co Direct positive silver halide emulsions containing excess iodide
US3531290A (en) * 1966-03-11 1970-09-29 Eastman Kodak Co Direct positive silver halide emulsions containing excess halide
DE2112729A1 (en) * 1970-03-20 1971-09-30 Eastman Kodak Co Color photographic recording material
US3837857A (en) * 1970-05-14 1974-09-24 Eastman Kodak Co Photographic materials curve shape stabilized with carboxy substituted 4-thiouracils
DE2436101A1 (en) * 1973-07-27 1975-02-06 Polaroid Corp PHOTOGRAPHIC PRODUCT AND PROCESS
DE2436180A1 (en) * 1973-07-27 1975-02-13 Polaroid Corp SILVER HALOGENIDE EMULSIONS WITH SUBSTITUTED HALOGENIDE AND PRODUCTS THAT CONTAIN THESE EMULSIONS
US3894871A (en) * 1973-07-27 1975-07-15 Polaroid Corp Photographic products and processes for forming silver and additive color transparencies
US3917485A (en) * 1973-01-18 1975-11-04 Eastman Kodak Co Method of making photographic silver halide emulsions and products thereof
DE2528638A1 (en) * 1974-06-26 1976-01-15 Minnesota Mining & Mfg PIVALYL ACETANILIDE AND PHOTOGRAPHICAL RECORDING MATERIAL CONTAINING THESE COMPOUNDS
US3935014A (en) * 1973-02-20 1976-01-27 Agfa-Gevaert Aktiengesellschaft Direct-positive photographic emulsion containing, unfogged, monodispersed silver halide grains having a layered grain structure of specific silver chloride content
US3957488A (en) * 1973-06-28 1976-05-18 Agfa-Gevaert, A.G. Photographic emulsion containing unfogged, heterodisperse layered silver halide grains having a prodominantly bromide core and total chloride content less than 30 mole percent
US3966476A (en) * 1973-02-09 1976-06-29 Agfa-Gevaert, A.G. Spectrally sensitized silver halide emulsion containing more than 50% of the grains with ripening nuclei in cavities
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US3979213A (en) * 1972-06-19 1976-09-07 Gilman Jr Paul B Spectrally sensitized silver halide emulsion containing an internal metal dopant
US3990895A (en) * 1974-04-23 1976-11-09 Polaroid Corporation Silver halide, color screen elements and their use in forming negative color images and diffusion transfer positive silver images
US4030920A (en) * 1976-04-12 1977-06-21 Eastman Kodak Company Processing compositions containing glycols for color transfer processes comprising direct positive silver halide developement
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US4070190A (en) * 1973-09-03 1978-01-24 E. I. Du Pont De Nemours And Company Process for producing photographic silver halide emulsions having a core/shell structure
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US4184877A (en) * 1976-06-10 1980-01-22 Ciba-Geigy Ag Process for the manufacture of photographic silver halide emulsions containing silver halide crystals of the twinned type
US4279987A (en) * 1978-11-14 1981-07-21 Konishiroku Photo Industry Co., Ltd. Light-sensitive, direct positive silver halide photographic material
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US4335199A (en) * 1980-02-19 1982-06-15 E. I. Du Pont De Nemours And Company High contrast by imagewise iodide infection in a mixed silver halide system
US4444874A (en) * 1982-09-15 1984-04-24 Eastman Kodak Company Photographic elements containing direct-positive emulsions and processes for their use
US4444865A (en) * 1981-11-12 1984-04-24 Eastman Kodak Company Blended grain direct-positive emulsions and photographic elements and processes for their use
US4459351A (en) * 1983-06-22 1984-07-10 Eastman Kodak Company Photographic element and process employed combination of surface and internal latent image silver halide
US4504570A (en) * 1982-09-30 1985-03-12 Eastman Kodak Company Direct reversal emulsions and photographic elements useful in image transfer film units
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Publication number Publication date
FR966221A (en) 1950-10-04
DE851716C (en) 1952-10-06
CH284107A (en) 1952-07-15
GB635841A (en) 1950-04-19

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