US3790390A - Photographic silver halide light-sensitive materials - Google Patents

Photographic silver halide light-sensitive materials Download PDF

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Publication number
US3790390A
US3790390A US00214216A US3790390DA US3790390A US 3790390 A US3790390 A US 3790390A US 00214216 A US00214216 A US 00214216A US 3790390D A US3790390D A US 3790390DA US 3790390 A US3790390 A US 3790390A
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US
United States
Prior art keywords
group
silver halide
halide photographic
emulsion
photographic emulsion
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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
US00214216A
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English (en)
Inventor
K Shiba
M Hinata
K Yamasue
A Sato
T Ikeda
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Fujifilm Holdings Corp
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Fuji Photo Film Co Ltd
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Publication of US3790390A publication Critical patent/US3790390A/en
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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
    • G03C1/06—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein with non-macromolecular additives
    • G03C1/08—Sensitivity-increasing substances
    • G03C1/10—Organic substances
    • G03C1/12—Methine and polymethine dyes
    • G03C1/22—Methine and polymethine dyes with an even number of CH groups
    • 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

  • R, R L and L are a s defi ned in the specification.
  • light sources used in these instruments there have been used combinations of light sources having high illuminance, such as a xenon arc lamp, and high speed shutters; xenon flash light-sources; and cathode raytube light sources. Amount these, cathode ray-tubes, especially those having fluorescent substance with short-time afterglow, are generally used for flying spot.
  • P-IS various fluorescent substances referred to as P-IS, P-l 1-, P-16, P-24 etc.
  • P-l5, P-lli, P-l6, and P-24 are known to have their maximum spectral energy distribution of emission at 505 nm, 460 nm, 385 nm and 520 nm, respectively.
  • the afterglow time of the emission of the aforesaid cathode ray-tube is usually as short as 1/l0,000,000 to 1/l00,000 second.
  • Xenon flash lamps having an emission time similarly short are frequently used.
  • the above-mentioned short-time exposure by a light source of this kind is generically referred to as flashlight exposure.
  • the room wherein such light-sensitive materials are used is generally comparatively bright so that the operation can be conducted with ease.
  • These materials are often used under comparatively bright yellowish-green safety light such as a Fuji Safe Light No. 2A (the percent transmission curve thereof is given in the drawing); and hence light-sensitive materials having a low sensitivity to safety lights of this kind are desirable.
  • Oneobject of the present invention is to provide a silver halide light-sensitive material having a high sensitivity to blue light in flashlight exposure.
  • Another object of the present invention is to provide a light-sensitive material having high sensitivity to blue light which is capable of being dealt with under bright yellowish-green safety light.
  • the blue-light-sensitive region (mainly the wavelength region of from 380 to 520 nm) corresponds to the light-sensitive region intrinsic to silver halide.
  • processes for increasing the sensitivity by making the grain size of the silver halide large processes for increasing the sensitivity by chemical sensitization, etc., were investigated.
  • the process comprising making the grain size large the granular properties and the sharpness of the image formed were greatly deteriorated.
  • the stability thereof to v the safety light was deteriorated.
  • the objects of the present invention were attained by using a silver halide emulsion containing light-sensitive silver halide grains whose mean grain size by diameter (and by number) is equal to or smaller than 0.9 micron; at least one compound containing .a group VIII metal in the periodic table in an amount of 10 to 10' mol per 1 gram mol of the silver halide; and at least one sensitizing dye represented by the general formula:
  • R and R each represents a hydrogen atom, an alkyl group, a substituted alkyl group or an aryl group
  • Y represents an oxygen atom or N R
  • R being a hydrogen atom, an alkyl group, a substituted alkyl group, an aryl group, a substituted aryl group or an allyl group
  • L and L each represents a methinegroup
  • Z represents the non-metallic atoms necessary to complete a series of oxazoline nuclei; in a binder such as gelatin.
  • sensitizing dyes used in the present invention are known and are described, for example, in British Pat. No. 1,074,433, and can be readily synthesized by reference to said specification.
  • dyes represented by the general formula are set out below, but the dyes used in the present invention are not to be thereby limited.
  • the grain size of the sil- .ver halide is, more effectively, smaller than 0.8 micron, most especially not larger than 0.6 micron, on the average.
  • the production of the light-sensitive silver halide grain that is, the production of the silver halide emulsion, comprising forming the crystals of silver halide grains in a dispersed state in the binder, and developing the crystals into a suitable grain size, is conducted according to conventional methods.
  • the group Vlll metals of the periodic table include iron, cobalt, nickel, ruthenium, rhodium, palladium, osmium, iridium and platinum and, as the compounds containing these metals which are rnost preferably used in the present invention, there are iron, iridium and rhodium compounds.
  • group VIII metal compounds are used in an amount of 10 mol to 10' mol per 1 mol of silver halide, independently or in combinations of more than one of these compounds.
  • a gold compound can be preferably added to the emulsion in combination with any of those compounds of the group VIII metal.'The addition of these compounds is properly' conducted at the formation of the silver halide grains, at the start of the ripening of the emulsion or in the course thereof in the production of the silver halide emulsion. Otherwise, they may be.
  • -a known stabilizer such as 2- mercaptobenzimidazole, I I l-phenyl-5 mercaptotetrazole, 5-methyl7-hydroxy-l ,3,4- triazoindolizene, etc., antifogging .ag'ents, toning agents, coating assistants such as sodium alkylbenzenesulfonate, saponin, etc., plasticizers, hardeners such as 1 formaldehyde, mucochloric acid, delustering agents, development accelerators, fluorescent brightening agents, color couplers or developing agents for activator development, etc. These materials are added,,when desired, for their'art-recognized function.
  • -a known stabilizer such as 2- mercaptobenzimidazole, I I l-phenyl-5 mercaptotetrazole, 5-methyl7-hydroxy-l ,3,4- triazoindolizene, etc.
  • antifogging .ag'ents such
  • the sensitizing dyes used in he present invention are used in an amount of 10".to 10 mol per mol of silver halide contained in the silver halide-emulsion, either,
  • sensitizing dyes to the emulsion is carried out inthe. same manner as the aforesaid metal compounds. They may-be added to the emulsion simultaneously with the said metal compounds, or may be added independently regardless of the order.
  • the light-sensitive material prepared in this way can be developed and fixed in the conventionalmanner, or may be treated in the manner generally known as the diffusion transfer process, or may be treated according to the developing yantageously not larger than 0.9 micron.
  • the sensitizing dyes represented by the general formula are capable of spectrally sensitizing light-sensitive materials.
  • the sensitizing effect of the emulsion not containing abovementioned metal compounds is small while in the usual exposure, the emulsion not containing said metal compounds shows at least about the same sensitizing effect as that of the emulsion containing said metal compounds.
  • the group VIII metal compounds of the present invention a remarkable sensitizing effect is produced as is shown in the following examples.
  • the light-sensitive material whose sensitivity in flashlight exposure is increased by chemical sensitization or by the process whereby the grain size is made larger, has an increased sensitivity to safety light, and under a safety light is deteriorated, as is shown in the -following examples.
  • the mean grain size of the silver halide is quite important for use under a safe light, and the mean grain size of the silver halide is ad- A bright safety light is desirable and it is the prerequisite for the light-sensitive material used in the present invention that it can be safely dealt with under a yellowish-green safety light, and hence it can of course be dealt with under red light, such as a Fuji Safe Light No. 2, or under'the light passed through a safety light filter which transmits light of longer wavelengths.
  • control emulsion (I) was prepared in the presence of l X 10' mol of ammonia per 1 mol of silver halide, and an emulsion having about the same sensitivity as that of the control emulsion (l) was prepared with the same prescription with adding 3 X 10 5 mol of ammonium hexachlororhodate (Ill) per 1 mol of silver halide contained in the said emulsion upon. forming the silver halide grains and further adding 2 X mol of potassium chloroplatinate per 1 mol of silver halide upon post-ripening.
  • the above-described samples were imagewise exposed for 1/100 and l/l,000,000 second using a Mark Ill sensitometer made by EG G Co. in the U.S.A.
  • the exposed samples were developed with the following de- Water to make up 1 liter mined as the reciprocal of the quantity of light which After fixing, washing and drying, the transmission density was measured.
  • the sensitivity value was deter- 40 gave a density of 2.5.
  • the sensitivity of the control emulsion (I) was calculated as 100, and the relative sensitivities of the other emulsions based on that of the control emulsion (I) are given in Table l.
  • Vlll metal+ Dye l Control emulsion 150 v emulsion to flashlight is remarkably increased by the combined use of rhodium salt, platinum salt and the Dye i'farfi the safetytothe saletyTi g'htis not so poor. It is also seen that, in the emulsion whose grain 'size was made big to obtain about the same sensitivity, the safety thereof under the safety light deteriorated.
  • the sensitivity and the fog under a No. 2A Safe Light were measured in the same manner as in 'Example l.
  • Control emulsion loo 100 0.0 0.03 g' 0 (l) Control emulsion loo 105 0 0.01 Control emulsion 98 100 0.0 0.02 921+ t e group (l) the group metal vm metal v I v fi?)nf+i:OIl);;nl2llSl0n I50 I15 0 0.03 Control emulsion 130 HO 0.0 0.04 Comm] emulsion 130 0 0 (I) D 1 (ll) the group Control emulsion I50 0.0 0.0l Dr 2 (I) the group Control emulsion I60 0.01 1.2
  • group VIII metal Dye 4 As is obvious from Table 2, a remarkable sensitizing effect to flashlight exposure was recognized by the combined use of the group -VIII metal salts and Dye 2 without deteriorating safety under a safety light, whereas emulsion (II') showed badly deteriorated safety under the safety light.
  • Example 3 An emulsion was prepared according to the procedure described in Example 2 using the Dye 3 instead of Dye 2, and tested in the manner described in Example 1. By the combined use of the group VIII metal salts and the Dye 3, a similar synergistic'effect was recognized.
  • Example 4 process, and to an emulsion prepared with the same prescription but with adding l X 10 mol of potassium hexacyanoferrate (III) per 1 mol of silver halide contained in the emulsion'upon forming the silver halide grains, and 7 X 10 mol of the Dye 4 per 1 molof silver halide in the same manner as in Example 1, there were v added, a stabilizer, a hardener and a coating assistant and the emulsions coated on PET films.
  • the dye sensitization degree "of the samples thus obtained was measured in the same manner as in Example 1 to obtain the following results:
  • R and R each represents a hydrogen atom, al-
  • Y represents an oxygen atom, N-R,
  • R being a hydrogen atom, alkyl, aryl, or allyl group
  • L and L each. represents methine group, Z represents non-metallic atom group necessary to complete aseries of oxazoline nucleus 2.
  • 1 l 12 group is selected from the group consisting of 2- I 15.

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  • 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)
  • Fax Reproducing Arrangements (AREA)
US00214216A 1970-12-30 1971-12-30 Photographic silver halide light-sensitive materials Expired - Lifetime US3790390A (en)

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
JP45123036A JPS4914265B1 (enrdf_load_stackoverflow) 1970-12-30 1970-12-30

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US (1) US3790390A (enrdf_load_stackoverflow)
JP (1) JPS4914265B1 (enrdf_load_stackoverflow)
BE (1) BE777530A (enrdf_load_stackoverflow)
CA (1) CA971815A (enrdf_load_stackoverflow)
DE (1) DE2165764A1 (enrdf_load_stackoverflow)
FR (1) FR2121086A5 (enrdf_load_stackoverflow)
GB (1) GB1367700A (enrdf_load_stackoverflow)

Cited By (22)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3982950A (en) * 1971-12-28 1976-09-28 Fuji Photo Film Co., Ltd. Silver halide photographic emulsion for use in flash exposure
US4160669A (en) * 1975-03-17 1979-07-10 Teiji Habu Argon laser flash exposure of spectrally sensitized silver halide photographic material
US4173483A (en) * 1975-05-27 1979-11-06 Konishiroku Photo Industry Co., Ltd. Silver halide photographic emulsions for use in flash exposure
US4828962A (en) * 1986-10-15 1989-05-09 Minnesota Mining And Manufacturing Company High contrast scanner photographic elements employing ruthenium and iridium dopants
US4835093A (en) * 1988-04-08 1989-05-30 Eastman Kodak Company Internally doped silver halide emulsions
US4847191A (en) * 1986-04-15 1989-07-11 Minnesota Mining And Manufacturing Company Silver halide photographic materials having rhodium cyanide dopants
US4857450A (en) * 1986-04-28 1989-08-15 Minnesota Mining And Manufacturing Company Silver halide photographic materials
US4933272A (en) * 1988-04-08 1990-06-12 Eastman Kodak Company Photographic emulsions containing internally modified silver halide grains
US4937180A (en) * 1988-04-08 1990-06-26 Eastman Kodak Company Photographic emulsions containing internally modified silver halide grains
US4945035A (en) * 1988-04-08 1990-07-31 Eastman Kodak Company Photographic emulsions containing internally modified silver halide grains
US4981781A (en) * 1989-08-28 1991-01-01 Eastman Kodak Company Photographic emulsions containing internally modified silver halide grains
US5037732A (en) * 1989-08-28 1991-08-06 Eastman Kodak Company Photographic emulsions containing internally modified silver halide grains
US5132203A (en) * 1991-03-11 1992-07-21 Eastman Kodak Company Tabular grain emulsions containing laminar halide strata
US5264336A (en) * 1991-04-10 1993-11-23 Eastman Kodak Company Silver brom(oiod)ide emulsions of increased sensitivity in the near infrared
US5268264A (en) * 1991-04-10 1993-12-07 Eastman Kodak Company Spectrally sensitized octahedral emulsions with buried shell sensitization
US5320938A (en) * 1992-01-27 1994-06-14 Eastman Kodak Company High chloride tabular grain emulsions and processes for their preparation
US5360712A (en) * 1993-07-13 1994-11-01 Eastman Kodak Company Internally doped silver halide emulsions and processes for their preparation
US5391474A (en) * 1992-04-30 1995-02-21 Eastman Kodak Company Iridium and bromide in silver halide grain finish
US5457021A (en) * 1994-05-16 1995-10-10 Eastman Kodak Company Internally doped high chloride {100} tabular grain emulsions
US5462849A (en) * 1994-10-27 1995-10-31 Eastman Kodak Company Silver halide emulsions with doped epitaxy
US5518872A (en) * 1994-11-09 1996-05-21 Eastman Kodak Company Emulsion and photographic element
US5695909A (en) * 1995-10-26 1997-12-09 Fuji Photo Film Co., Ltd. Silver halide photographic material

Families Citing this family (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US5434043A (en) * 1994-05-09 1995-07-18 Minnesota Mining And Manufacturing Company Photothermographic element with pre-formed iridium-doped silver halide grains

Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2078233A (en) * 1934-09-14 1937-04-27 Eastman Kodak Co Photographic emulsion
US2448060A (en) * 1945-08-30 1948-08-31 Eastman Kodak Co Photographic emulsions sensitized with salts of metals of group viii of the periodicarrangement of the elements
US2566245A (en) * 1945-08-30 1951-08-28 Eastman Kodak Co Complex compounds of the platinum group as photographic fog inhibitors
GB1074433A (en) * 1964-08-11 1967-07-05 Ilford Ltd Merocyanine dyestuffs
US3480439A (en) * 1964-10-15 1969-11-25 Agfa Gevaert Ag Light-sensitive materials optically sensitized with chloropropylsulfonic acid substituted merocyanines

Patent Citations (5)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US2078233A (en) * 1934-09-14 1937-04-27 Eastman Kodak Co Photographic emulsion
US2448060A (en) * 1945-08-30 1948-08-31 Eastman Kodak Co Photographic emulsions sensitized with salts of metals of group viii of the periodicarrangement of the elements
US2566245A (en) * 1945-08-30 1951-08-28 Eastman Kodak Co Complex compounds of the platinum group as photographic fog inhibitors
GB1074433A (en) * 1964-08-11 1967-07-05 Ilford Ltd Merocyanine dyestuffs
US3480439A (en) * 1964-10-15 1969-11-25 Agfa Gevaert Ag Light-sensitive materials optically sensitized with chloropropylsulfonic acid substituted merocyanines

Cited By (23)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3982950A (en) * 1971-12-28 1976-09-28 Fuji Photo Film Co., Ltd. Silver halide photographic emulsion for use in flash exposure
US4160669A (en) * 1975-03-17 1979-07-10 Teiji Habu Argon laser flash exposure of spectrally sensitized silver halide photographic material
US4173483A (en) * 1975-05-27 1979-11-06 Konishiroku Photo Industry Co., Ltd. Silver halide photographic emulsions for use in flash exposure
US4847191A (en) * 1986-04-15 1989-07-11 Minnesota Mining And Manufacturing Company Silver halide photographic materials having rhodium cyanide dopants
US4857450A (en) * 1986-04-28 1989-08-15 Minnesota Mining And Manufacturing Company Silver halide photographic materials
US4828962A (en) * 1986-10-15 1989-05-09 Minnesota Mining And Manufacturing Company High contrast scanner photographic elements employing ruthenium and iridium dopants
JP2761028B2 (ja) 1988-04-08 1998-06-04 イーストマン コダック カンパニー ハロゲン化銀写真乳剤
US4835093A (en) * 1988-04-08 1989-05-30 Eastman Kodak Company Internally doped silver halide emulsions
US4933272A (en) * 1988-04-08 1990-06-12 Eastman Kodak Company Photographic emulsions containing internally modified silver halide grains
US4937180A (en) * 1988-04-08 1990-06-26 Eastman Kodak Company Photographic emulsions containing internally modified silver halide grains
US4945035A (en) * 1988-04-08 1990-07-31 Eastman Kodak Company Photographic emulsions containing internally modified silver halide grains
US4981781A (en) * 1989-08-28 1991-01-01 Eastman Kodak Company Photographic emulsions containing internally modified silver halide grains
US5037732A (en) * 1989-08-28 1991-08-06 Eastman Kodak Company Photographic emulsions containing internally modified silver halide grains
US5132203A (en) * 1991-03-11 1992-07-21 Eastman Kodak Company Tabular grain emulsions containing laminar halide strata
US5264336A (en) * 1991-04-10 1993-11-23 Eastman Kodak Company Silver brom(oiod)ide emulsions of increased sensitivity in the near infrared
US5268264A (en) * 1991-04-10 1993-12-07 Eastman Kodak Company Spectrally sensitized octahedral emulsions with buried shell sensitization
US5320938A (en) * 1992-01-27 1994-06-14 Eastman Kodak Company High chloride tabular grain emulsions and processes for their preparation
US5391474A (en) * 1992-04-30 1995-02-21 Eastman Kodak Company Iridium and bromide in silver halide grain finish
US5360712A (en) * 1993-07-13 1994-11-01 Eastman Kodak Company Internally doped silver halide emulsions and processes for their preparation
US5457021A (en) * 1994-05-16 1995-10-10 Eastman Kodak Company Internally doped high chloride {100} tabular grain emulsions
US5462849A (en) * 1994-10-27 1995-10-31 Eastman Kodak Company Silver halide emulsions with doped epitaxy
US5518872A (en) * 1994-11-09 1996-05-21 Eastman Kodak Company Emulsion and photographic element
US5695909A (en) * 1995-10-26 1997-12-09 Fuji Photo Film Co., Ltd. Silver halide photographic material

Also Published As

Publication number Publication date
FR2121086A5 (enrdf_load_stackoverflow) 1972-08-18
BE777530A (fr) 1972-04-17
JPS4914265B1 (enrdf_load_stackoverflow) 1974-04-06
CA971815A (en) 1975-07-29
GB1367700A (en) 1974-09-18
DE2165764A1 (de) 1972-07-20

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