EP0233396B1 - Photographische Silberhalogenidemulsionen mit Kornoberfläche - Google Patents

Photographische Silberhalogenidemulsionen mit Kornoberfläche Download PDF

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Publication number
EP0233396B1
EP0233396B1 EP19860306829 EP86306829A EP0233396B1 EP 0233396 B1 EP0233396 B1 EP 0233396B1 EP 19860306829 EP19860306829 EP 19860306829 EP 86306829 A EP86306829 A EP 86306829A EP 0233396 B1 EP0233396 B1 EP 0233396B1
Authority
EP
European Patent Office
Prior art keywords
silver halide
icositetrahedral
grains
emulsion
crystal faces
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
Application number
EP19860306829
Other languages
English (en)
French (fr)
Other versions
EP0233396A3 (en
EP0233396A2 (de
Inventor
Joe Edward Maskasky
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.)
Eastman Kodak Co
Original Assignee
Eastman Kodak 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 claimed from US06/882,113 external-priority patent/US4724200A/en
Application filed by Eastman Kodak Co filed Critical Eastman Kodak Co
Publication of EP0233396A2 publication Critical patent/EP0233396A2/de
Publication of EP0233396A3 publication Critical patent/EP0233396A3/en
Application granted granted Critical
Publication of EP0233396B1 publication Critical patent/EP0233396B1/de
Expired 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
    • G03C1/005—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein
    • G03C1/04—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein with macromolecular additives; with layer-forming substances
    • G03C1/047—Proteins, e.g. gelatine derivatives; Hydrolysis or extraction products of proteins
    • 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
    • G03C1/0051—Tabular grain 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
    • G03C1/035—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein characterised by the crystal form or composition, e.g. mixed grain
    • 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
    • G03C1/06—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein with non-macromolecular additives
    • G03C1/07—Substances influencing grain growth during silver salt formation
    • 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
    • G03C1/0051—Tabular grain emulsions
    • G03C2001/0055—Aspect ratio of tabular grains in general; High aspect ratio; Intermediate aspect ratio; Low aspect ratio
    • 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
    • G03C1/035—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein characterised by the crystal form or composition, e.g. mixed grain
    • G03C2001/03511—Bromide content
    • 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
    • G03C2200/00—Details
    • G03C2200/03—111 crystal face

Definitions

  • silver halide grains have been the subject of intense investigation. Although high iodide silver halide grains, those containing at least 90 mole percent iodide, based on silver, are known and have been suggested for photographic applications, in practice photographic emulsions almost always contain silver halide grains comprised of bromide, chloride, or mixtures of chloride and bromide optionally containing minor amounts of iodide. Up to about40 mole percent iodide, based on silver, can be accomodated in a silver bromide crystal structure without observation of a separate silver iodide phase. However, in practice silver halide emulsions rarely contain more than about 15 mole percent iodide, with iodide well below 10 mole percent being most common.
  • the silver halide emulsions as well as other layers of the photographic elements of this invention can contain as vehicles hydrophilic colloids, employed alone or in combination with other polymeric materials (e.g., lattices).
  • Suitable hydrophilic materials include both naturally occurring substances such as proteins, protein derivatives, cellulose derivatives ⁇ e.g., cellulose esters, gelatin ⁇ e.g., alkali treated gelatin (cattle, bone, or hide gelatin) or acid treated gelatin (pigskin gelatin), gelatin derivatives ⁇ e.g., acetylated gelatin, phthalated gelatin, and the like, polysaccharides such as dextran, gum arabic, zein, casein, pectin, collagen derivatives, collodion, agar-agar, arrow-root, and albumin.
  • Processing of the imagewise exposed photographic elements can be accomplished in any convenient conventional manner. Processing procedures, developing agents, and development modifiers are illustrated by Research Disclosure, Item 17643, cited above, Sections XIX, XX, and XXI, respectively.
  • This emulsion illustrates the preparation of a silver bromide icositetrahedral emulsion having a ⁇ 311 ⁇ Miller index by the Ostwald ripening of a small grain size AgBr emulsion onto a mixture of cubic and octahedral host grains in the presence of Compound X acting as a growth modifier.
  • This example illustrates the preparation of a silver bromide icositetrahedral emulsion having ⁇ 533 ⁇ Miller index crystal faces, using a cubic host emulsion and Compound XI, 2-mercaptoimidazole as a growth modifier.
  • the emulsion was prepared by a procedure similar to that described in Example 13, but with the following changes :
  • the growth modifier was 2.0 millimoles/Ag mole of Compound I, dissolved in 2 mL. methanol and 2 drops of triethylamine.
  • the pH was maintained at 5.92 at 50°C, and the pAg was maintained at 7.9 during the precipitation.
  • This emulsion was prepared by the procedure described for Example 15, but using 3.0 millimoles/Ag mole of Compound I as a growth modifier, dissolved in 3 mL. methanol and 3 drops of triethylamine. The pH was maintained at 5.87 at 60°C.
  • Emulsion Example 20 illustrates the preparation of a ruffled tabular grain silver bromide emulsion using as a growth modifier Compound 81, 5-(3-ethyl-2-benzothiazolinylidene)-3-p-sulfoethyl rhodanine, which is known to be useful as a blue spectral sensitizing dye.
  • the temperature was raised to 60°C, and the pAg adjusted to 8.5 at 60°C with KBr and maintained at that value during the precipitation.
  • a 2.0M solution of AgN0 3 was introduced at a constant rate over a period of 20 min while a 2M solution of KBr was added as needed to hold the pAg constant.
  • a total of 0.02 mole Ag was added.
  • Figures 29A, B, and C show electron micrographs of the resulting grains.
  • addition of the growth modifier after the precipitation resulted in o growth of ruffles on the host emulsion grains.
  • Example 21 B with the same amount of growth modifier added prior to the precipitation, produced uniform, closely arranged, small ruffles.
  • Example 21C with a higher level of growth modifier, produced a similar result, but with slightly better defined ruffles (pyramids).
  • Figures 31 A and 31 B are electron micrographs of the resulting emulsions grains produced by Examples 23A and 23B, respectively.
  • Figure 31A shows a pattern of growths covering the crystal faces.
  • Figure 31 B illustrates the formation of ⁇ 533 ⁇ icositetrahedral grains with continued precipitation.
  • Portion A This half was gently centrifuged and the solid portion resuspended in 300g of 3.7% bone gelatin solution.
  • Portions A and B were further treated as listed below and coated on acetate support at 1.08 g Ag/m 2 , 4.31 g bone gelatin/m 2 , and 0.81 glm 2 of a dispersion of the coupler 2-benzamido-5-[2-(4-butanesulfonylami- dophenoxy)tretradecanamido]-4-chlorophenol, 0.14g saponinlm 2 as spreading agent, and 18mg bis(vinylsulfonylmethyl)ether/g gelatin as hardener.
  • the emulsion exhibits no measurable sensitivity in the 470 to 510 nm region of the spectrum, but exhibits a marked increase in spectral sensitiviity beyond 650 nm.
  • the curves demonstrate that the spectral sensitivity imparted by the growth modifier can be destroyed to allow spectral sensitization of the icositetrahedral emulsions according to the invention to a differing portion of the visible spectrum, if desired.
  • Emulsion A To prepare Emulsion A, to a reaction vessel supplied with a stirrer was added 0.05 mole of the above icositetrahedral host emulsion. Distilled water was added to make a total contents weight of 50g. The contents were heated to 40°C and 0.92 mmole of NaCl was added. An 0.50M solution of AgN0 3 and a 0.52M solution of NaCI was then introduced with a constant silver addition rate over a period of 10 min, consuming 2.5 mmole of silver. During the precipitation, the pAg was held constant at 7.5 and the temperature held constant at 40°C.
  • Emulsion A and Emulsion B showed discrete epitaxial deposits.
  • Emulsion B which was precipitated in the presence of the site director, the cubic ⁇ 100 ⁇ crystal faces on the epitaxy were quite distinct.
  • site director such as Compound XII, is essential to achieving selective site epitaxy, but an adsorbed site director can be advantageous in achieving better definition of crystal faces.

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  • Chemical & Material Sciences (AREA)
  • Physics & Mathematics (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • General Physics & Mathematics (AREA)
  • Spectroscopy & Molecular Physics (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Silver Salt Photography Or Processing Solution Therefor (AREA)

Claims (11)

1. Photographische Silberhalogenidemulsion mit strahlungsempfindlichen Silberhalogenidkörnern einer kubischen Kristallgitterstruktur mit icositetraedrischen Kristallflächen.
2. Photographische Silberhalogenidemulsion nach Anspruch 1, in der die Silberhalogenidkömer mit icositetraedrischen Kristallflächen Silberbromidkörner sind.
3. Photographische Silberhalogenidemulsion nach Anspruch 1, in der die Silberhalogenidkömer mit icositetraedrischen Kristallflächen Silberchloridkömer sind.
4. Photographische Silberhalogenidemulsion nach Anspruch 1, in der die Silberhalogenidkömer mit icositetraedrischen Kristallflächen mindestens einen lonentyp bestehend aus Bromidionen und Chloridionen und gegebenenfalls eine untergeordnete Menge von lodidionen, bezogen auf Gesamtsilber, enthalten.
5. Photographische Silberhalogenidemulsion nach einem der Ansprüche 1 bis 4, in der die Silberhalogenidkörner zusätzlich mindestens eine Kristallfläche bestehend aus kubischen order oktaedrischen Kristallflächen aufweisen.
6. Photographische Silberhalogenidemulsion nach einem der Ansprüche 1 bis 4, in der die Silberhalogenidkörner reguläre icositetraedrische Körner sind.
7. Photographische Silberhalogenidemulsion nach einem der Ansprüche 1 bis 6, in der die icositetraedrischen Kristallflächen ein Komwachstumsmodifizierungsmittel adsorbiert enthalten.
8. Photographische Silberhalogenidemulsion nach einem der Ansprüche 1 bis 7, in der die icositetraedrischen Kristallflächen der Miller-Indexangabe {hll} genügen, in der h und I ganze Zahlen größber als Null sind, h größer als I und h nicht größer als 5 ist.
9. Photographische Silberhalogenidemulsion nach Anspruch 8, in der die icositetraedrischen Kristallflächen einen {211}, {311}, {322}, {522} oder {533} Miller-Index aufweisen.
10. Photographische Silberhalogenidemulsion nach Anspruch 9, in der ein Kornwachstumsmodifizierungsmittel in der Emulsion vorhanden ist, das ausgewählt ist aus : 4-Hydroxy-6-methyl-1,3,3a,7-tetraazainden, Natriumsalz ; 2-Mercaptoimidazol ; 4-Hydroxy-6-methyl-2-methylmercapto-1,3,3a,7-tetraazainden 7-Ethoxycarbonyl-6-methyl-2-methylthio-4-oxo-1,3,3a-7-tetraazainden ; 2-Methyl-5-nitro-1-H-benzimidazol ; 3-Ethyl-5-(3-ethyl-2-benzothiazolinyliden)rhodanin ; 5-(1,3-Dithiolan-2-yliden)-3-ethylrhodanin ; 5-(3-Ethyl-2-benzothiazolinyliden)-3-ß-sulfoethylrhodanin ; 5-Anilinomethylen-3-(2-sulfoethyl)rhodanin ; 3-(1-Carboxyethyl)-5-[(3-ethyl-2-benzoxazolinyliden)ethyliden]rhodanin; 3-(3-Carboxypropyl)-5-[(3-ethyl-2-benzo- xazolinyliden)ethyliden]rhodanin ; 3-(2-Carboxyethyl)-5-(1-ethyl-4-pyridinyliden)rhodanin ; 3-Carboxymethyl-5-(2-pyrrolino-1-cyclopenten-1-ylmethylen)-rhodanin, Natriumsalz, 3-Ethyl-5-(3-methyl-2-thiazoli-dinyliden)rhodanin ; 3-Carboxymethyl-5-(2,6-dimethyl-4(H)-pyran-4-yliden)rhodanin ; 5-(5-Methyl-3-propyl-2-thiazolinyliden)-3-propylrhodanin oder 3-Ethyl-5-[3-(3-sulfopropyl)2-benzothiazolinyliden]-rhodanin, Triethylaminzalz.
11. Photographisches Element, das eine Emulsion nach einem der Ansprüche 1 bis 10 aufweist.
EP19860306829 1985-09-03 1986-09-03 Photographische Silberhalogenidemulsionen mit Kornoberfläche Expired EP0233396B1 (de)

Applications Claiming Priority (8)

Application Number Priority Date Filing Date Title
US77223085A 1985-09-03 1985-09-03
US772230 1985-09-03
US81113385A 1985-12-19 1985-12-19
US81113285A 1985-12-19 1985-12-19
US811132 1985-12-19
US811133 1985-12-19
US882113 1986-07-03
US06/882,113 US4724200A (en) 1985-09-03 1986-07-03 Emulsions and photographic elements containing silver halide grains having icositetrahedral crystal faces

Publications (3)

Publication Number Publication Date
EP0233396A2 EP0233396A2 (de) 1987-08-26
EP0233396A3 EP0233396A3 (en) 1988-12-28
EP0233396B1 true EP0233396B1 (de) 1991-07-31

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Application Number Title Priority Date Filing Date
EP19860306829 Expired EP0233396B1 (de) 1985-09-03 1986-09-03 Photographische Silberhalogenidemulsionen mit Kornoberfläche

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EP (1) EP0233396B1 (de)
CA (1) CA1281227C (de)
DE (1) DE3680661D1 (de)

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
JP2851206B2 (ja) * 1992-05-01 1999-01-27 富士写真フイルム株式会社 ハロゲン化銀写真乳剤およびこれを用いるハロゲン化銀写真感光材料

Family Cites Families (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE342528A (de) * 1926-05-20
US3519426A (en) * 1966-12-27 1970-07-07 Eastman Kodak Co Preparation of silver halide emulsions having high covering power
US4011083A (en) * 1974-12-10 1977-03-08 Eastman Kodak Company Surface sensitive silver halide emulsion containing a silver complexing azaindene to reduce desensitization of optical sensitizing dye incorporated therein
US4183756A (en) * 1978-05-03 1980-01-15 Eastman Kodak Company Pre-precipitation spectral sensitizing dye addition process
US4225666A (en) * 1979-02-02 1980-09-30 Eastman Kodak Company Silver halide precipitation and methine dye spectral sensitization process and products thereof
JPS6054662B2 (ja) * 1981-09-28 1985-11-30 富士写真フイルム株式会社 ハロゲン化銀乳剤
JPS60222843A (ja) * 1984-04-19 1985-11-07 Fuji Photo Film Co Ltd ハロゲン化銀乳剤の製造方法及びハロゲン化銀写真感光材料

Also Published As

Publication number Publication date
EP0233396A3 (en) 1988-12-28
CA1281227C (en) 1991-03-12
DE3680661D1 (de) 1991-09-05
EP0233396A2 (de) 1987-08-26

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