US3589903A - Silver halide,heat-developable image sheet containing mercuric ion - Google Patents

Silver halide,heat-developable image sheet containing mercuric ion Download PDF

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Publication number
US3589903A
US3589903A US708989A US3589903DA US3589903A US 3589903 A US3589903 A US 3589903A US 708989 A US708989 A US 708989A US 3589903D A US3589903D A US 3589903DA US 3589903 A US3589903 A US 3589903A
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United States
Prior art keywords
silver
mercuric
heat
silver halide
ion
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Expired - Lifetime
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US708989A
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English (en)
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Stephen P Birkeland
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3M Co
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Minnesota Mining and Manufacturing 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
    • G03C1/494—Silver salt compositions other than silver halide emulsions; Photothermographic systems ; Thermographic systems using noble metal compounds
    • G03C1/498—Photothermographic systems, e.g. dry silver

Definitions

  • a light-sensitive heat-developable imaging sheet containing catalytic amounts of light-sensitive silver halide in catalytic association with organic silver salt oxidation-reduction image-forming means is given increased speed, stability and contrast by incorporation of mercuric ion.
  • This invention relates to the visible recording of lightimages and to light-sensitive and heat-developable sheet materials useful therein.
  • sensitive sheet materials of the class indicated may be significantly improved in a number of respects by the incorporation in the sensitive layer of sources of small but highly significant amounts of mercuric ion.
  • the invention has made possible the recording of cathode ray tube single field exposures on photosensitive heat-developable dry silver sheet material.
  • the mercuric ion may be introduced in any desired manner.
  • a mercuric compound may be added to the coating composition containing either the organic silver salt, or the reducing agent, or both; or it may be applied as a separate coating. It has been found particularly convenient to introduce the mercuric ion in the form of mercuric halide under conditions which permit the halide ion to react with a small proportion of the organic silver salt to form the required photosensitive silver halide, the latter remaining in catalytic proximity with the remainder of the silver salt.
  • the mercuric ion may be introduced in the form of compounds of anions other than the halide, for example acetate, behenate, benzoate, bromate, chromate, citrate, chloranilate, iodate, lactate, nitrate, oxalate, phthalate, salicylate, succinate, sulfate, or as mercury compounds of hexamethylenetetramine, pentachlorophenol, or phthalazinone.
  • anions other than the halide for example acetate, behenate, benzoate, bromate, chromate, citrate, chloranilate, iodate, lactate, nitrate, oxalate, phthalate, salicylate, succinate, sulfate, or as mercury compounds of hexamethylenetetramine, pentachlorophenol, or phthalazinone.
  • Any compound capable of providing mercuric ions in the system employed is operable in the practice of the invention; but compounds of extremely low solubility, or dark color, or Whose anions have a deleterious effect, such for example as mercuric sulfide or thiocyanate, will ordinarily be avoided.
  • Silver behenate half soap is a mixture of equimolar proportions of silver lbehenate and behenic acid, obtained by precipitation with silver nitrate and nitric acid from the sodium salt of commercial behenic acid. Other ratios of silver salt and free acid may be used, or the free acid may be omitted, particularly where transparency is desired. Silver salts of other long chain fatty acids, e.g. silver stearate, may be used. Other organic silver salt oxidizing agents, e.g. silver p-hexoxybenzoate, silver octadecoxybenzoate, silver p-methoxycinnamate, which likewise provide a visible image on reduction, are also contemplated for use in this invention.
  • the sheet containing mercuric ion produces a substantially equally dense image but with a much lighter background than does a comparable sheet free of mercuric ion when both are stored, exposed, and developed under identical test conditions.
  • Sheet materials of this invention which contain Waterinsoluble sterically hindered normally solid o-alkyl substituted phenols or the like as reducing agents for the organic silver salt, and particularly those which additionally contain phthalazinone or equivalent materials, are found to have further advantages over sheets containing these same components but in the absense of mercuric ion.
  • the novel photosensitive heat-developable print papers of the invention containing these materials are found to possess a significantly higher photographic speed.
  • the photographic speed may be defined* Where E is the exposure in meter-candle-seconds. Exposure and density values are obtained in accordance with Wellknown sensitometric principles, development in each instance bein-g accomplished by heating for the specified time at the speciiied temperature. Uniform heating is obtained by holding the sheet in uniform pressure-contact with the smooth surface of a uniformly heated drum or roller, or in any other equivalent manner.
  • Phthalazinone has previously been found to provide a toning action in copy-sheet coatings containing silver soap and reducing agent, as shown for example in U.S. Pat. No. 3,080,254. Although a similar effect is undoubtedly provided in the compositions of the present invention, an additional and apparently catalytic effect is also obtained whereby the hindered phenols, which otherwise react only with diliiculty with the silver ion, are enabled to react much more rapidly and effectively.
  • the amount of phthalazinone may vary from about one-half to about ten percent of the total Weight of the coating.
  • Solid Water-insoluble o-alkyl phenols which have been shown to be useful in these compositions include a number of compounds commercially available as anti-oxidant or preservative materials and identifiables as:
  • Methyl alcohol sensitizing dye .0015 Acetone (solvent for dye) 2.93
  • the two compositions are prepared by mixing the components in a ball mill to provide a smooth mixture which spreads evenly under a knife coater.
  • the sensitizing dye is 3-allyl-5-[3-ethyl (2 naphthoxazoylidene) ethylidene]-l-phenyl-Z-thiohydantoin.
  • Other useful spectral sensitizers are listed in application Ser. No. 693,714.
  • Sensitive strips are prepared by coating paper with a iirst layer of composition A at 1.25 g./sq. ft. dry weight followed by a second layer of composition B at 0.30 g./sq. ft. dry weight. Additional strips are similarly prepared but with the addition of mercuric acetate to composition A, and also with the addition of phthalazinone to composition B. For most accurate comparison the strips are coated side-by-side in each test series and are then simultaneously exposed and developed under identical conditions in a Quadrant dry-silver printing machine, wherein development is obtained by contacting the back of the sheet for three seconds With the smooth surface of a metal drum maintained at 212i2 F. Density is determined at unexposed and at fully exposed areas with a reectometer. Density readings are recorded under D min. for the lightest and D max. for the heaviest density areas of each strip.
  • the iirst series shows the effect of mercuric acetate in suppressing the background darkening or fog obtained on sheets which have been subjected to accelerated aging prior to exposure, e.g. by holding in an oven for periods equivalent to several months of normal room-temperature aging. The image densities will be seen to remain essentially constant.
  • the amount of mercuric acetate is shown as grams per 100 grams of composition A.
  • composition B In a second series, 0.5% of phthalazinone is added to composition B (second layer) and a similar suppression of fog is achieved by incorporation of the mercuric salt in the rst layer.
  • EXAMPLE 2 In this example the halide ion is added in the form of calcium bromide to the rst coating composition and following the addition of the indicated amount of mercuric acetate.
  • the two compositions are applied to paper at dry coating weights of 1.25 and 0.30 g./sq. ft. respectively as in Example 1.
  • Prints are prepared by exposure at 300 foot-candles through a step wedge for 10 seconds and development at 235 F. for 25 seconds, and density measurements are obtained and reported as in Example 1 except that the density is given in terms of the range of readings for both the unexposed area (D min.) and the fully exposed area (D max). The wide range of values in some samples indicates a mottled or non-uniform appearance. Formulations and results are as tabulated below.
  • the blue dye may be added as a solution in methyl alcohol.
  • the merocyanine spectral sensitizing dye is added as a solution in a small portion of the acetone.
  • the water-insoluble solid o-alkyl-substitutedphenol reducing agent is present in an amount substantially stoichiometrically equivalent to the amount of silver salt.
  • Another control sample i.e. containing no mercury, is similarly treated but with an exposure of one second and with a critical and very carefully controlled development time of ten seconds. A recognizable print with fair contrast is obtained, but the image areas have a brownish cast rather than the rich black appearance obtained with the longer development time.
  • Composition A A:
  • Composition -A is applied at a coating weight, after drying, of 1.0 g./ sq. ft. and composition B at .30 g./sq. ft.
  • sensitometric characteristics of coated paper prepared as thus described are determined by exposure, development, measurement of densities, and plotting of D log E curves. Values taken from these curves are compared with those obtained from sheet materials in which an equal molar proportion of calcium bromide is substituted for the mercuric bromide.
  • FIG. l graphically represents the maximum and minimum densities developed in the two sheets at increasing times of development and at different temperatures
  • FIG. 2 is a graph representing the values of gamma. obtained for the two sheets when developed for different times.
  • lFIG. 3 indicates the relative photographic speeds of the two sheets.
  • the components are mixed in a ball mill to provide uniform dispersion and the mixture is coated on paper at a thickness sucient to provide a coating weight of 1.0 ⁇ g./sq. ft. after drying.
  • the sheet is exposed in a sensitometer through a 0 to 3 optical density wedge for 10 seconds to tungsten lilament light at l95 foot-candles, and developed by heating for ten seconds at an optimum temperature of C.
  • the optimum temperature is selected as that temperature which in ten seconds will produce a iirst faint visible dan-kening of the previously unexposed sheet.
  • Control sheets containing no mercury are similarly prepared and tested, the mercuric bromide being replaced by 10.15 part of cadmium bromide and by 0.16 part of barium bromide respectively, the optimum development temperature being 77 C. in each instance. As shown in Table V, both speed and maximum density are significantly increased in the presence of mercuric ion.
  • Example 4 uses a single mixture of all components and the stratum is produced in a single application. These coatings may be applied to paper, transparent flexible films or glass plates, or other suitable carriers or baokings. It is also possible to separate the components, for example by combining the photosensitive silver halide, the organic silver salt oxidizing agent, and the mercuric salt with a. suitable binder on a light-.sensitive sheet which ⁇ after exposure must then be heated in contact with a separately prepared developer sheet containing the organic reducing agent.
  • Silver bromide is a particularly useful silver halide photosensitive material but silver chloride and silver iodide, and mixed silver halides, are also useful. These materials may further be spectrally sensitized to any desired portion of the visible range of the spectrum by the addition of suitable sensitizers such as the merocyanne spectral sensitizing dyes.
  • suitable sensitizers such as the merocyanne spectral sensitizing dyes.
  • Sheet material useful in the recording of light-images including a stratum containing (a) photosensitive silver halide catalyst-forming means, (b) heat-sensitive reactant image-forming 'means including an organic silver salt oxidizing agent and a reducing agent for silver ion, the oxidation-reduction reaction of which to produce a visible change' is accelerated by said catalyst, and (o) a source of mercuric ion in significant small amount up to about .O7 mol of mercury per mol of silver.
  • Sheet material of claim 1 wherein the amount of mercury is between about .005 and about .05 mol per mol of silver.
  • Sheet material of claim 1 wherein the reducing agent is a normally solid, Water-insoluble, o-alkyl substituted phenol.
  • Sheet material of claim 4 wherein the reducing agent is a normally solid, water-insoluble, o-alkyl substituted phenol.

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Materials Engineering (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Non-Silver Salt Photosensitive Materials And Non-Silver Salt Photography (AREA)
  • Heat Sensitive Colour Forming Recording (AREA)
US708989A 1968-02-28 1968-02-28 Silver halide,heat-developable image sheet containing mercuric ion Expired - Lifetime US3589903A (en)

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US70898968A 1968-02-28 1968-02-28

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US (1) US3589903A (de)
AT (1) AT287485B (de)
BE (1) BE729043A (de)
BR (1) BR6906698D0 (de)
CH (1) CH514155A (de)
DE (1) DE1908761C2 (de)
DK (1) DK137615B (de)
ES (1) ES363775A1 (de)
FR (1) FR2002790A1 (de)
GB (1) GB1264532A (de)
SE (1) SE356377B (de)

Cited By (25)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3748137A (en) * 1970-12-10 1973-07-24 Eastman Kodak Co Photosensitive and thermosensitive elements and process for development
US3844797A (en) * 1972-04-27 1974-10-29 Agfa Gevaert Photosensitive recording material
US3847612A (en) * 1973-02-02 1974-11-12 Minnesota Mining & Mfg Light-sensitive heat-developable sheet material
JPS5126019A (ja) * 1974-08-27 1976-03-03 Canon Kk Kankozairyo
US3951660A (en) * 1972-12-16 1976-04-20 Agfa-Gevaert, A.G. Dry copying material
US4028129A (en) * 1974-01-08 1977-06-07 Fuji Photo Film Co., Ltd. Heat-developable photosensitive materials
US4069759A (en) * 1974-07-27 1978-01-24 Canon Kabushiki Kaisha Light and heat formation of conductive image printing plate
US4123282A (en) * 1975-09-08 1978-10-31 Minnesota Mining And Manufacturing Company Photothermographic toners
US4668612A (en) * 1984-09-04 1987-05-26 Fuji Photo Film Co., Ltd. Heat-developable color photosensitive material
US4725534A (en) * 1981-05-13 1988-02-16 Oriental Photo Industrial Co., Ltd. Process for producing a heat-developable photosensitive material
US4820617A (en) * 1986-04-28 1989-04-11 Oriental Photo Industrial Co., Ltd. Heat-developable photosensitive material
US5028523A (en) * 1990-06-04 1991-07-02 Minnesota Mining And Manufacturing Company Photothermographic elements
US5260180A (en) * 1992-09-02 1993-11-09 Minnesota Mining And Manufacturing Company Photothermographic imaging media employing silver salts of tetrahydrocarbyl borate anions
US5369000A (en) * 1993-04-29 1994-11-29 Minnesota Mining And Manufacturing Company Post-processing stabilizers for photothermographic articles
US5382504A (en) * 1994-02-22 1995-01-17 Minnesota Mining And Manufacturing Company Photothermographic element with core-shell-type silver halide grains
US5409798A (en) * 1991-08-30 1995-04-25 Canon Kabushiki Kaisha Plate blank, process for producing printing plate from plate blank, and printing method and apparatus using plate
US5482814A (en) * 1993-07-15 1996-01-09 Canon Kabushiki Kaisha Thermal developing photosensitive member and image forming method using the thermal developing photosensitive member
US5599648A (en) * 1990-08-03 1997-02-04 Canon Kabushiki Kaisha Surface reforming method, process for production of printing plate, printing plate and printing process
EP0802178A2 (de) 1996-02-23 1997-10-22 Fuji Photo Film Co., Ltd. Komplexe von Schiffschen Basen von Chinonen und optische Aufzeichnungsmaterialien, die sie enthalten
US5939249A (en) * 1997-06-24 1999-08-17 Imation Corp. Photothermographic element with iridium and copper doped silver halide grains
US20060003272A1 (en) * 2004-06-09 2006-01-05 Konica Minolta Medical & Graphic, Inc. Photothermographic material, development method and thermal development device thereof
US20060088785A1 (en) * 2004-10-22 2006-04-27 Konica Minolta Medical & Graphic, Inc. Silver salt photothermographic dry imaging material, thermal development method of the same, and thermal development apparatus for the same
WO2007010777A1 (ja) 2005-07-20 2007-01-25 Konica Minolta Medical & Graphic, Inc. 画像形成方法
US7267934B2 (en) 2004-07-15 2007-09-11 Konica Minolta Medical & Graphic, Inc. Method of forming an image
EP1953592A1 (de) 2007-02-02 2008-08-06 Konica Minolta Medical & Graphic, Inc. Photothermographisches Material

Families Citing this family (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
BE790370A (fr) * 1971-10-22 1973-04-20 Minnesota Mining & Mfg Feuille stable a la lumiere pour l'enregistrement d'images lumineuses
GB1590678A (en) 1976-08-18 1981-06-03 Canon Kk Image-forming member
DE2914474A1 (de) * 1979-04-10 1980-10-23 Eberspaecher J Ausstellbares rahmenloses dachfenster aus kunststoff

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
DE1572203C3 (de) * 1964-04-27 1978-03-09 Minnesota Mining And Manufacturing Co., Saint Paul, Minn. (V.St.A.) Verfahren zur Herstellung eines wärmeentwickelbaren Blattmaterials mit einem strahlungsempfindlichen Überzug
DE1547850A1 (de) * 1965-08-05 1969-11-20 Fuji Photo Film Co Ltd Durch Waerme entwickelbares lichtempfindliches Element

Cited By (30)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US3748137A (en) * 1970-12-10 1973-07-24 Eastman Kodak Co Photosensitive and thermosensitive elements and process for development
US3844797A (en) * 1972-04-27 1974-10-29 Agfa Gevaert Photosensitive recording material
US3951660A (en) * 1972-12-16 1976-04-20 Agfa-Gevaert, A.G. Dry copying material
US3847612A (en) * 1973-02-02 1974-11-12 Minnesota Mining & Mfg Light-sensitive heat-developable sheet material
US4028129A (en) * 1974-01-08 1977-06-07 Fuji Photo Film Co., Ltd. Heat-developable photosensitive materials
US4069759A (en) * 1974-07-27 1978-01-24 Canon Kabushiki Kaisha Light and heat formation of conductive image printing plate
JPS5126019A (ja) * 1974-08-27 1976-03-03 Canon Kk Kankozairyo
JPS532771B2 (de) * 1974-08-27 1978-01-31
US4123282A (en) * 1975-09-08 1978-10-31 Minnesota Mining And Manufacturing Company Photothermographic toners
US4725534A (en) * 1981-05-13 1988-02-16 Oriental Photo Industrial Co., Ltd. Process for producing a heat-developable photosensitive material
US4668612A (en) * 1984-09-04 1987-05-26 Fuji Photo Film Co., Ltd. Heat-developable color photosensitive material
US4820617A (en) * 1986-04-28 1989-04-11 Oriental Photo Industrial Co., Ltd. Heat-developable photosensitive material
US5028523A (en) * 1990-06-04 1991-07-02 Minnesota Mining And Manufacturing Company Photothermographic elements
US5599648A (en) * 1990-08-03 1997-02-04 Canon Kabushiki Kaisha Surface reforming method, process for production of printing plate, printing plate and printing process
US5409798A (en) * 1991-08-30 1995-04-25 Canon Kabushiki Kaisha Plate blank, process for producing printing plate from plate blank, and printing method and apparatus using plate
US5260180A (en) * 1992-09-02 1993-11-09 Minnesota Mining And Manufacturing Company Photothermographic imaging media employing silver salts of tetrahydrocarbyl borate anions
US5369000A (en) * 1993-04-29 1994-11-29 Minnesota Mining And Manufacturing Company Post-processing stabilizers for photothermographic articles
US5464737A (en) * 1993-04-29 1995-11-07 Minnesota Mining And Manufacturing Company Post-processing stabilizers for photothermographic articles
US5482814A (en) * 1993-07-15 1996-01-09 Canon Kabushiki Kaisha Thermal developing photosensitive member and image forming method using the thermal developing photosensitive member
US5382504A (en) * 1994-02-22 1995-01-17 Minnesota Mining And Manufacturing Company Photothermographic element with core-shell-type silver halide grains
EP0802178A2 (de) 1996-02-23 1997-10-22 Fuji Photo Film Co., Ltd. Komplexe von Schiffschen Basen von Chinonen und optische Aufzeichnungsmaterialien, die sie enthalten
US5939249A (en) * 1997-06-24 1999-08-17 Imation Corp. Photothermographic element with iridium and copper doped silver halide grains
US6060231A (en) * 1997-06-24 2000-05-09 Eastman Kodak Company Photothermographic element with iridium and copper doped silver halide grains
US20060003272A1 (en) * 2004-06-09 2006-01-05 Konica Minolta Medical & Graphic, Inc. Photothermographic material, development method and thermal development device thereof
US7445884B2 (en) 2004-06-09 2008-11-04 Konica Minolta Medical & Graphic, Inc. Photothermographic material, development method and thermal development device thereof
US7267934B2 (en) 2004-07-15 2007-09-11 Konica Minolta Medical & Graphic, Inc. Method of forming an image
US20060088785A1 (en) * 2004-10-22 2006-04-27 Konica Minolta Medical & Graphic, Inc. Silver salt photothermographic dry imaging material, thermal development method of the same, and thermal development apparatus for the same
US7220536B2 (en) 2004-10-22 2007-05-22 Konica Minolta Medical & Graphic, Inc. Silver salt photothermographic dry imaging material, thermal development method of the same, and thermal development apparatus for the same
WO2007010777A1 (ja) 2005-07-20 2007-01-25 Konica Minolta Medical & Graphic, Inc. 画像形成方法
EP1953592A1 (de) 2007-02-02 2008-08-06 Konica Minolta Medical & Graphic, Inc. Photothermographisches Material

Also Published As

Publication number Publication date
DK137615C (de) 1978-09-18
SE356377B (de) 1973-05-21
BR6906698D0 (pt) 1973-01-11
BE729043A (de) 1969-08-27
GB1264532A (de) 1972-02-23
DE1908761C2 (de) 1984-03-01
FR2002790A1 (de) 1969-10-31
AT287485B (de) 1971-01-25
DE1908761A1 (de) 1969-09-11
ES363775A1 (es) 1971-07-01
DK137615B (da) 1978-04-03
CH514155A (de) 1971-10-15

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