US2743183A - Chemical sensitization of photographic emulsions - Google Patents
Chemical sensitization of photographic emulsions Download PDFInfo
- Publication number
- US2743183A US2743183A US319617A US31961752A US2743183A US 2743183 A US2743183 A US 2743183A US 319617 A US319617 A US 319617A US 31961752 A US31961752 A US 31961752A US 2743183 A US2743183 A US 2743183A
- Authority
- US
- United States
- Prior art keywords
- stannous
- emulsions
- emulsion
- sulfur
- silver halide
- 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
Links
- 239000000839 emulsion Substances 0.000 title description 44
- 239000000126 substance Substances 0.000 title description 6
- 206010070834 Sensitisation Diseases 0.000 title description 2
- 230000008313 sensitization Effects 0.000 title description 2
- 229910052709 silver Inorganic materials 0.000 description 23
- 239000004332 silver Substances 0.000 description 23
- -1 silver halide Chemical class 0.000 description 21
- 239000003795 chemical substances by application Substances 0.000 description 20
- 230000001235 sensitizing effect Effects 0.000 description 20
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 17
- 239000011593 sulfur Substances 0.000 description 17
- 229910052717 sulfur Inorganic materials 0.000 description 17
- 150000001875 compounds Chemical class 0.000 description 16
- 150000003839 salts Chemical class 0.000 description 10
- SDKPSXWGRWWLKR-UHFFFAOYSA-M sodium;9,10-dioxoanthracene-1-sulfonate Chemical compound [Na+].O=C1C2=CC=CC=C2C(=O)C2=C1C=CC=C2S(=O)(=O)[O-] SDKPSXWGRWWLKR-UHFFFAOYSA-M 0.000 description 10
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 description 6
- 229910021626 Tin(II) chloride Inorganic materials 0.000 description 6
- 230000035945 sensitivity Effects 0.000 description 6
- 239000001119 stannous chloride Substances 0.000 description 6
- 235000011150 stannous chloride Nutrition 0.000 description 6
- 108010010803 Gelatin Proteins 0.000 description 5
- 229910052783 alkali metal Inorganic materials 0.000 description 5
- 150000001340 alkali metals Chemical class 0.000 description 5
- 230000029087 digestion Effects 0.000 description 5
- 229920000159 gelatin Polymers 0.000 description 5
- 239000008273 gelatin Substances 0.000 description 5
- 235000019322 gelatine Nutrition 0.000 description 5
- 235000011852 gelatine desserts Nutrition 0.000 description 5
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 5
- 239000010931 gold Substances 0.000 description 5
- 229910052737 gold Inorganic materials 0.000 description 5
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 description 3
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 3
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 description 3
- 230000002301 combined effect Effects 0.000 description 3
- KYRUBSWVBPYWEF-UHFFFAOYSA-N copper;iron;sulfane;tin Chemical compound S.S.S.S.[Fe].[Cu].[Cu].[Sn] KYRUBSWVBPYWEF-UHFFFAOYSA-N 0.000 description 3
- 239000000203 mixture Substances 0.000 description 3
- 229910052700 potassium Inorganic materials 0.000 description 3
- 239000011591 potassium Substances 0.000 description 3
- UMGDCJDMYOKAJW-UHFFFAOYSA-N thiourea Chemical compound NC(N)=S UMGDCJDMYOKAJW-UHFFFAOYSA-N 0.000 description 3
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 3
- 239000004372 Polyvinyl alcohol Substances 0.000 description 2
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Natural products NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 description 2
- 229910052946 acanthite Inorganic materials 0.000 description 2
- ZOJBYZNEUISWFT-UHFFFAOYSA-N allyl isothiocyanate Chemical compound C=CCN=C=S ZOJBYZNEUISWFT-UHFFFAOYSA-N 0.000 description 2
- HTKFORQRBXIQHD-UHFFFAOYSA-N allylthiourea Chemical compound NC(=S)NCC=C HTKFORQRBXIQHD-UHFFFAOYSA-N 0.000 description 2
- 229960001748 allylthiourea Drugs 0.000 description 2
- 239000002585 base Substances 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 150000004820 halides Chemical class 0.000 description 2
- 238000010438 heat treatment Methods 0.000 description 2
- 238000000034 method Methods 0.000 description 2
- 230000003647 oxidation Effects 0.000 description 2
- 238000007254 oxidation reaction Methods 0.000 description 2
- 229920002451 polyvinyl alcohol Polymers 0.000 description 2
- 238000012545 processing Methods 0.000 description 2
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 description 2
- 229940056910 silver sulfide Drugs 0.000 description 2
- XUARKZBEFFVFRG-UHFFFAOYSA-N silver sulfide Chemical compound [S-2].[Ag+].[Ag+] XUARKZBEFFVFRG-UHFFFAOYSA-N 0.000 description 2
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 description 2
- 150000003464 sulfur compounds Chemical class 0.000 description 2
- ZSUXOVNWDZTCFN-UHFFFAOYSA-L tin(ii) bromide Chemical compound Br[Sn]Br ZSUXOVNWDZTCFN-UHFFFAOYSA-L 0.000 description 2
- JKFYKCYQEWQPTM-UHFFFAOYSA-N 2-azaniumyl-2-(4-fluorophenyl)acetate Chemical compound OC(=O)C(N)C1=CC=C(F)C=C1 JKFYKCYQEWQPTM-UHFFFAOYSA-N 0.000 description 1
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 1
- 229920008712 Copo Polymers 0.000 description 1
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 1
- FCSHMCFRCYZTRQ-UHFFFAOYSA-N N,N'-diphenylthiourea Chemical compound C=1C=CC=CC=1NC(=S)NC1=CC=CC=C1 FCSHMCFRCYZTRQ-UHFFFAOYSA-N 0.000 description 1
- 206010034960 Photophobia Diseases 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- 229910021612 Silver iodide Inorganic materials 0.000 description 1
- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 description 1
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 235000016720 allyl isothiocyanate Nutrition 0.000 description 1
- GCPXMJHSNVMWNM-UHFFFAOYSA-N arsenous acid Chemical class O[As](O)O GCPXMJHSNVMWNM-UHFFFAOYSA-N 0.000 description 1
- 230000003190 augmentative effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 239000003638 chemical reducing agent Substances 0.000 description 1
- 239000011248 coating agent Substances 0.000 description 1
- 238000000576 coating method Methods 0.000 description 1
- 239000000084 colloidal system Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- FDWREHZXQUYJFJ-UHFFFAOYSA-M gold monochloride Chemical compound [Cl-].[Au+] FDWREHZXQUYJFJ-UHFFFAOYSA-M 0.000 description 1
- XMBWDFGMSWQBCA-UHFFFAOYSA-N hydrogen iodide Chemical compound I XMBWDFGMSWQBCA-UHFFFAOYSA-N 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- CBEQRNSPHCCXSH-UHFFFAOYSA-N iodine monobromide Chemical compound IBr CBEQRNSPHCCXSH-UHFFFAOYSA-N 0.000 description 1
- 208000013469 light sensitivity Diseases 0.000 description 1
- 238000009740 moulding (composite fabrication) Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000001603 reducing effect Effects 0.000 description 1
- ZUNKMNLKJXRCDM-UHFFFAOYSA-N silver bromoiodide Chemical compound [Ag].IBr ZUNKMNLKJXRCDM-UHFFFAOYSA-N 0.000 description 1
- 229940045105 silver iodide Drugs 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 235000010265 sodium sulphite Nutrition 0.000 description 1
- AKHNMLFCWUSKQB-UHFFFAOYSA-L sodium thiosulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=S AKHNMLFCWUSKQB-UHFFFAOYSA-L 0.000 description 1
- 235000019345 sodium thiosulphate Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- LSNNMFCWUKXFEE-UHFFFAOYSA-L sulfite Chemical class [O-]S([O-])=O LSNNMFCWUKXFEE-UHFFFAOYSA-L 0.000 description 1
- YUKQRDCYNOVPGJ-UHFFFAOYSA-N thioacetamide Chemical compound CC(N)=S YUKQRDCYNOVPGJ-UHFFFAOYSA-N 0.000 description 1
- DLFVBJFMPXGRIB-UHFFFAOYSA-N thioacetamide Natural products CC(N)=O DLFVBJFMPXGRIB-UHFFFAOYSA-N 0.000 description 1
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
- G03C1/06—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein with non-macromolecular additives
- G03C1/08—Sensitivity-increasing substances
- G03C1/09—Noble metals or mercury; Salts or compounds thereof; Sulfur, selenium or tellurium, or compounds thereof, e.g. for chemical sensitising
Definitions
- one object of our invention is to provide chemically sensitized emulsions of enhanced light sensitivity. Another object is to provide emulsions having sensitivity enhanced by the combined effect of sulfur, gold and stannous compound sensitizing agents. A further object is to provide the methods of augmenting cmulsion sensitivity utilizing the novel combination of sensitizing agents. Further objects of our invention will become apparent from consideration of the following description.
- the objects of our invention are accomplished by the incorporation into silver halide emulsions of a mixture of (A) a sulfur sensitizing agent such as disclosed in Sheppard U. S. Patents 1,574,944 granted March 2, 1926, and 1,623,499 granted April 5, 1927, e. g., allyl isothiocyanate, thiocarbanilide, thiourea, sodium thiosulfate, dio-tolyl thiourea, thioacetamide and allyl thiourea, (B) a gold salt sensitizing agent such as disclosed in Waller and Dodd U. S. Patent 2,399,083, e. g., gold chloride,
- A a sulfur sensitizing agent such as disclosed in Sheppard U. S. Patents 1,574,944 granted March 2, 1926, and 1,623,499 granted April 5, 1927, e. g., allyl isothiocyanate, thiocarbanilide,
- stannous chloride stannous bromide, iodide, fluoride and sulfate are preferred.
- the stannous compounds are used in silver halide emul: sions in quantities of the order of from 1 l0-" to 44 l0- mol per mol silver halide.
- stannous salts such as stannous halides
- stannous salts we prefer to use from about; l l0- mol per mol silver halide up to about 44x10 mol per mol silver halide, the higher quantities sometimesbeing required when the conditions of operation cause excessive aerial oxidation of the stannite solutions.
- concentration of stannous salts are used with the faster emulsions and up to about 20 10- mol per mol silver halide with slower fine-grained emulsions except when using stannite solutions.
- Other factors well known to those skilled in the art will be found to influence the optimum concentration of stannous salt to obtain the characteristics desired for a given photographicemulsion.
- the appearance of fog with a given emulsion and concentration of stannous salt is a good criterion to follow indicating that too much salt has been used.
- Thequantities of sulfur and gold salt sensitizing agents in the "silver halide emulsions are not especially critical: and can be varied from the optimum amounts indicated in the following examples.
- the novel sensitizers are incorporated into emulsions digestion is complete. That is, the emulsion can first be sensitized with a sulfur sensitizing agent and a gold salt sensitizing agent followed by one of the stannous compounds or the addition'of the stannous compound can be made prior to addition of the gold salt.
- Example 1 A In a positive type of silver bromoiodide emulsion were incorporated 20 milligrams of allyl thiourea per mol of silver halide and 2 milligrams of potassium chloroaurate per mol of silver halide and the emulsion was digested for 61 minutes at 62 C. A sample of the emulsion was coated onto film base.
- a tine-grained positive type of silver 'bromoiodide gelatin emu si was. sen t ed n a con nt n l' er w th. a sul r n t e: suc a esc dabq e b new tastie 3. m nut M 0 6- scaled @040 n coa e a'film- E A. s m e of he same.
- ri n emuls o was en ii e n a coii t oaa manne w t he sulfur e i i used in D and a gold salt sensitizer such as described above, by heating for 30. minutes at 60 C., cooled to 40 and coated on film. Upon exposure, processing, and sensitometric evaluation, the emulsion was found to' have twice the speed of emulsion D. The combined effect of sulfur and gold salt sensitizing agents is thus illustrated.
- many types of silver halide emulsions may be. treated with the novel combination of sulfur, gold and stannous sensitizing agents.
- the novel sensitizers may, in general, be employed in hydrophilic colloid emulsion vehicles; for example, gelatin, polyvinyl alcohol, partially hydrolyzed s ll osc ster suc as cellu os acetate and copo y of polyvinyl alcohol, The sensitigersare suitable for the well lrnown types of; silver chloride, silver bromide and silver iodide.
- emulsions and emulsions containing mixtures of these halides containing the usual emulsion addenda such as nntifoggants, spreading agents, coupler qomnoun a. u h. emulsions, are suitable to use.
- such color films carry at least one emulsion layer containing the mentioned combination of sensitizing agents.
- a ligh t sensitive, photographic emulsion comprising silver halide sensitized, with a sulfur sensitizing agent, a gold salt sensitizing agent, and: from 1x10 to 2O 10- mol. of stanuous chloride per mol of silver halide.
Landscapes
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- General Physics & Mathematics (AREA)
- Silver Salt Photography Or Processing Solution Therefor (AREA)
Priority Applications (5)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| BE523958D BE523958A (US20100268047A1-20101021-C00003.png) | 1952-11-08 | ||
| US319617A US2743183A (en) | 1952-11-08 | 1952-11-08 | Chemical sensitization of photographic emulsions |
| FR64778D FR64778E (fr) | 1952-11-08 | 1953-11-05 | Nouvelles émulsions photographiques |
| GB30699/53A GB734473A (en) | 1952-11-08 | 1953-11-06 | Improvements in sensitized photographic emulsions |
| DEE8091A DE939422C (de) | 1952-11-08 | 1953-11-08 | Sensibilisiertes photographisches Material |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US319617A US2743183A (en) | 1952-11-08 | 1952-11-08 | Chemical sensitization of photographic emulsions |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| US2743183A true US2743183A (en) | 1956-04-24 |
Family
ID=23243014
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| US319617A Expired - Lifetime US2743183A (en) | 1952-11-08 | 1952-11-08 | Chemical sensitization of photographic emulsions |
Country Status (5)
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3000739A (en) * | 1957-04-02 | 1961-09-19 | Du Pont | Process for preparing silver halide emulsions |
| US3128184A (en) * | 1960-01-25 | 1964-04-07 | Eastman Kodak Co | Antifoggants for gold sensitized emulsions in the presence of reduction sensitizers |
| US3320069A (en) * | 1966-03-18 | 1967-05-16 | Eastman Kodak Co | Sulfur group sensitized emulsions |
| EP0563985A1 (en) | 1992-04-03 | 1993-10-06 | Fuji Photo Film Co., Ltd. | Silver halide color photographic material |
Families Citing this family (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS58125612A (ja) * | 1982-01-14 | 1983-07-26 | Konishiroku Photo Ind Co Ltd | ハロゲン化銀乳剤の製造方法 |
| US5641621A (en) * | 1996-01-11 | 1997-06-24 | Eastman Kodak Company | Process for preparation of silver halide emulsion employing a double heat-cycle during finishing |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2399083A (en) * | 1942-02-13 | 1946-04-23 | Ilford Ltd | Photographic materials |
| US2487850A (en) * | 1948-07-23 | 1949-11-15 | Eastman Kodak Co | Chemical sensitization of photographic emulsions |
| US2540086A (en) * | 1948-06-17 | 1951-02-06 | Silver halibe emulsions | |
| US2597856A (en) * | 1949-09-24 | 1952-05-27 | Eastman Kodak Co | Stabilization of photographic emulsions sensitized with gold compounds |
-
0
- BE BE523958D patent/BE523958A/xx unknown
-
1952
- 1952-11-08 US US319617A patent/US2743183A/en not_active Expired - Lifetime
-
1953
- 1953-11-05 FR FR64778D patent/FR64778E/fr not_active Expired
- 1953-11-06 GB GB30699/53A patent/GB734473A/en not_active Expired
- 1953-11-08 DE DEE8091A patent/DE939422C/de not_active Expired
Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US2399083A (en) * | 1942-02-13 | 1946-04-23 | Ilford Ltd | Photographic materials |
| US2540086A (en) * | 1948-06-17 | 1951-02-06 | Silver halibe emulsions | |
| US2487850A (en) * | 1948-07-23 | 1949-11-15 | Eastman Kodak Co | Chemical sensitization of photographic emulsions |
| US2597856A (en) * | 1949-09-24 | 1952-05-27 | Eastman Kodak Co | Stabilization of photographic emulsions sensitized with gold compounds |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US3000739A (en) * | 1957-04-02 | 1961-09-19 | Du Pont | Process for preparing silver halide emulsions |
| US3128184A (en) * | 1960-01-25 | 1964-04-07 | Eastman Kodak Co | Antifoggants for gold sensitized emulsions in the presence of reduction sensitizers |
| US3320069A (en) * | 1966-03-18 | 1967-05-16 | Eastman Kodak Co | Sulfur group sensitized emulsions |
| EP0563985A1 (en) | 1992-04-03 | 1993-10-06 | Fuji Photo Film Co., Ltd. | Silver halide color photographic material |
Also Published As
| Publication number | Publication date |
|---|---|
| DE939422C (de) | 1956-02-23 |
| BE523958A (US20100268047A1-20101021-C00003.png) | |
| GB734473A (en) | 1955-08-03 |
| FR64778E (fr) | 1955-12-02 |
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