CN1158660A - Laser addressable thermographic elements - Google Patents
Laser addressable thermographic elements Download PDFInfo
- Publication number
- CN1158660A CN1158660A CN95195324A CN95195324A CN1158660A CN 1158660 A CN1158660 A CN 1158660A CN 95195324 A CN95195324 A CN 95195324A CN 95195324 A CN95195324 A CN 95195324A CN 1158660 A CN1158660 A CN 1158660A
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- China
- Prior art keywords
- silver
- dyestuff
- alkyl
- image density
- radiation
- Prior art date
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- Pending
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- 230000005855 radiation Effects 0.000 claims abstract description 31
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- FOIXSVOLVBLSDH-UHFFFAOYSA-N Silver ion Chemical compound [Ag+] FOIXSVOLVBLSDH-UHFFFAOYSA-N 0.000 claims abstract description 17
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- ZINOCYHIHYTAND-UHFFFAOYSA-N 4-methylbenzoic acid;silver Chemical compound [Ag].CC1=CC=C(C(O)=O)C=C1 ZINOCYHIHYTAND-UHFFFAOYSA-N 0.000 description 1
- DAOLGZTXBRODCV-UHFFFAOYSA-N 4-phenyl-1h-1,2,4-triazole-5-thione;silver Chemical compound [Ag].SC1=NN=CN1C1=CC=CC=C1 DAOLGZTXBRODCV-UHFFFAOYSA-N 0.000 description 1
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- 235000021357 Behenic acid Nutrition 0.000 description 1
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- 238000005057 refrigeration Methods 0.000 description 1
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- DCKVNWZUADLDEH-UHFFFAOYSA-N sec-butyl acetate Chemical compound CCC(C)OC(C)=O DCKVNWZUADLDEH-UHFFFAOYSA-N 0.000 description 1
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- NBYLLBXLDOPANK-UHFFFAOYSA-M silver 2-carboxyphenolate hydrate Chemical compound C1=CC=C(C(=C1)C(=O)O)[O-].O.[Ag+] NBYLLBXLDOPANK-UHFFFAOYSA-M 0.000 description 1
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 description 1
- 229940045105 silver iodide Drugs 0.000 description 1
- RTFVIAGNZNCYMZ-UHFFFAOYSA-N silver;1,2,2-trimethylcyclopentane-1,3-dicarboxylic acid Chemical compound [Ag].CC1(C)C(C(O)=O)CCC1(C)C(O)=O RTFVIAGNZNCYMZ-UHFFFAOYSA-N 0.000 description 1
- MNMYRUHURLPFQW-UHFFFAOYSA-M silver;dodecanoate Chemical compound [Ag+].CCCCCCCCCCCC([O-])=O MNMYRUHURLPFQW-UHFFFAOYSA-M 0.000 description 1
- ORYURPRSXLUCSS-UHFFFAOYSA-M silver;octadecanoate Chemical compound [Ag+].CCCCCCCCCCCCCCCCCC([O-])=O ORYURPRSXLUCSS-UHFFFAOYSA-M 0.000 description 1
- FDBMFXMFZNNOQV-UHFFFAOYSA-N silver;tetradecanoic acid Chemical compound [Ag].CCCCCCCCCCCCCC(O)=O FDBMFXMFZNNOQV-UHFFFAOYSA-N 0.000 description 1
- 235000009518 sodium iodide Nutrition 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 239000011877 solvent mixture Substances 0.000 description 1
- PWEBUXCTKOWPCW-UHFFFAOYSA-N squaric acid Chemical compound OC1=C(O)C(=O)C1=O PWEBUXCTKOWPCW-UHFFFAOYSA-N 0.000 description 1
- 239000011145 styrene acrylonitrile resin Substances 0.000 description 1
- 125000005504 styryl group Chemical group 0.000 description 1
- 125000000446 sulfanediyl group Chemical group *S* 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 239000000057 synthetic resin Substances 0.000 description 1
- LRBQNJMCXXYXIU-NRMVVENXSA-N tannic acid Chemical compound OC1=C(O)C(O)=CC(C(=O)OC=2C(=C(O)C=C(C=2)C(=O)OC[C@@H]2[C@H]([C@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)[C@@H](OC(=O)C=3C=C(OC(=O)C=4C=C(O)C(O)=C(O)C=4)C(O)=C(O)C=3)O2)OC(=O)C=2C=C(OC(=O)C=3C=C(O)C(O)=C(O)C=3)C(O)=C(O)C=2)O)=C1 LRBQNJMCXXYXIU-NRMVVENXSA-N 0.000 description 1
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Images
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
- G03C1/494—Silver salt compositions other than silver halide emulsions; Photothermographic systems ; Thermographic systems using noble metal compounds
- G03C1/498—Photothermographic systems, e.g. dry silver
- G03C1/4989—Photothermographic systems, e.g. dry silver characterised by a thermal imaging step, with or without exposure to light, e.g. with a thermal head, using a laser
-
- 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
Abstract
A thermographic imaging element containing a substrate which is coated on at least one surface thereof with a thermographic imaging system having at least one layer containing light-insensitive organic silver salt; reducing agent for silver ion; a binder; toner; and a dye which absorbs radiation in the wavelength range of about 750-1100 nm. Preferably, there is a layer adjacent to the one containing the light-insensitive organic silver salt, etc., which contains binder and additional dye which absorbs radiation in the range of about 750-1100 nm. When the thermographic imaging element is exposed to radiation of 750-1100 nm of 0.10-2.0 joules/cm<2> for 0.20-200 microseconds, an image density of about 1.0 or greater is formed. When imaging a thermographic imaging element with radiation-absorbing dye in both adjacent layers or only the layer containing binder and dye, the radiation is directed through the layer containing the light-insensitive organic silver salt, etc., before striking the adjacent layer containing radiation-absorbing dye and binder.
Description
Field of the present invention
The present invention relates to new Ying's heat-sensitive imaging element, more specifically, the present invention relates to the heat-sensitive imaging element of available infra-red laser diode direct imaging.The invention further relates to infra-red laser diode and make heat-sensitive imaging element imaging method of the present invention.
Background of the present invention
In imaging field, can be known by the image-forming component of light or heat one-tenth image exposure.The conventional photosensitive and photothermographic elements of silver halide is the most representative photosensitive material class component.In routine photosensitive (" wet silver ") and photo-thermal quick (" doing silver ") element, the little silver atoms (Ag °) of the silver halide exposure generation in the photosensitive emulsion bunch.The one-tenth image of these bunches is distributed in this area and is called latent image.Usually, the latent image of formation can not see by conventional methods that photosensitive emulsion must further be processed to generate visible image simultaneously.In doing and wetting silver-colored system, visible image generates by the reduction silver ion, and described silver ion catalysis has the silver halide particle of silver atom cluster (being latent image) near (catalytic proximity).So generate soot-and-whitewash.
The conventional photothermographic silver halide element developing method that need wet makes developable latent image.The wet-chemical reagent that uses in this method needs special operational and handles waste chemical reagent.The piping system that the equipment of this method is big and needs are special.
In photothermographic elements, the reducible silver material (for example ， behenic acid silver) of the approaching non-sensitization of Photoactive silver-halide catalysis, when generating galactic nucleus when exposing like this by silver halide, but the reduction of the reducible silver material of these galactic nucleus catalysis.By evenly being imposed on this element, heat makes latent image visible.The firing equipment that is used for photothermographic elements is developed encounters problems by adopting dry method to solve conventional light activated element.Yet the photothermographic elements that uses these equipment to develop can have uneven image density, image distortion and/or surface abrasion defective.The reason that can occur non-homogeneous image fault in developing process is that the surface of (for example) heating element changes, has foreign matter and fully do not get rid of the volatile matter that produces in the developing process on photothermographic elements or heating element.The reason that pattern distortion occurs is the change in size of unsteered photothermographic elements base material in photothermographic elements heating and/or the cooling procedure.Photothermographic elements dragged the retaining element in the firing equipment surface abrasion or fuzzy can occur.In a lot using as text or stick figure, these defectives are acceptable.Yet, all even high-quality image of the application need of medical diagnosis, industry, Plate making printing, printed circuit board (PCB) and other imaging.
US5,041,369 has described a kind of method, has emphasized that wherein the advantage of dry process photothermographic elements is not need to make the surface to contact with firing equipment.Photothermographic elements is become image through the laser explosure with secondary harmonic generation (SHG) equipment split beam.In the method,, carry out thermal activation by light-Re simultaneously at another wavelength place absorbing dye near infrared (NIR) with the light exposure of element with a kind of wavelength.Expose simultaneously and heat-developed advantage although this method has the image of making, the equipment that needs is complicated and be subjected to producing the restriction of the laser output of two kinds of different wavelength availables.In addition, photosensitive emulsion still needs the light and heat activation to generate image.
The photosensitive emulsion that contains silver halide known in this field can cause high minimum density (D at the visible of spectrum and ultraviolet (UV) part
Min).High UV D
MinBe silver halide (particularly silver bromide and silver iodide) the intrinsic absorption of nearly UV and the high optical haze when silver halide and organic silver salts exist simultaneously extremely.High UV D
MinFor Plate making printing scanning and image fixedly egative film be undesirable because it with other medium such as UV sensitization printed panel, draw a design egative film and paper contact exposure process in increased the required time shutter.The photothermographic elements for the treatment of as image is used as when contacting egative film, and high optical haze also can cause image definition to reduce.Well-known in photothermographic elements silver halide also can cause the bad light stability of background video density, cause atomizing.
A class image-forming component that does not rely on based on the chemical reagent of silver halide is a thermal sensing element.These materials are widely used in the figure of facsimile recorder, label, bill, record medicine output or angles of science monitoring instrument etc.In modal form, thermal sensing element comprises the carrier that scribbles heat-sensitive composition, and described composition comprises colour coupler (being generally a kind of colourless basically electron stain precursor of giving) and color developer (being generally a kind of electron compound that is subjected to).By heating head, heating pen or laser beam, heat imposed on make it become image on the element, when using heat and become image, colour coupler forms image with the color developer reaction immediately.US 4,904, and 572 have described a kind of thermal sensing element, and it uses the image of leuco dye with intensifying processing.Leuco dye is the reduction form of band look dyestuff, and it is generally colourless or unusual light color.， behenic acid silver plays lewis acidic effect among the application, and the leuco dye reaction through heating on it and the image forms chromatic image.Obtain the black image by the combination of losing lustre (cyan, yellow and magenta).The black image that reaches the high density neutral-tone with losing lustre very difficulty this be well known in the art.Owing to generate image by forming coloured dye, image is a little less than the absorption of ultraviolet region, therefore for providing very little practicality as the UV masking-out with film.
Conventional temperature-sensitive egative film needs 1 to 5 second imaging dead time usually.This, scope was unpractiaca for using laser imaging process time.For the suitable imaging that can the adopt laser dead time is provided, requirement can be in microsecond the on-the-spot temperature-sensitive chassis construction that forms image.
There are some shortcomings in above-mentioned all kinds of image-forming component.For example, conventional siliver halide photosensitive material is serious because of the environmental pollution of wet processing chemical reagent; Photothermal sensitive material has lower image fastness, limited optical density and bad dimensional stability; The silver halide base emulsion uses the visible light-sensitive agent that needs bleaching or remove also need operate in darkroom or sheen usually; Conventional photosensitive and photothermographic elements needs two-stage process (exposure and development); Reach the high imaging energy of conventional thermal sensing element needs, long thermographic dead time, and have lower image fastness and limited optical density.
Industrial needs be image-forming component and the method that helps to overcome the problems referred to above, just be based on this background and finishing the present invention.
The present invention's general introduction
In one embodiment, the invention provides a kind of heat-sensitive imaging element, comprise the base material that scribbles thermosensitive imaging system, this thermosensitive imaging system comprises the one deck at least that contains following component: non-photosensitivity organic silver salts, silver ion with reductive agent, bonding agent, toner and in the about 750-1100nm of wavelength coverage the dyestuff of absorbed radiation, comprising one deck at least of non-photosensitivity organic silver salts, when at 0.10-2.0J/cm
2Radiation (wavelength coverage is in about 750-1100nm) forms the image density greater than about 1.0 when exposing the 0.2-200 microsecond down.
In another embodiment, the invention provides a kind of heat-sensitive imaging element, be included in the base material that scribbles thermosensitive imaging system at least one surface, this thermosensitive imaging system comprises at least two adjacent layers, wherein the one deck in the adjacent layer comprises the non-photosensitivity organic silver salts, the silver ion reductive agent, bonding agent, toner and non-essential in the about 750-1100nm of wavelength coverage the dyestuff of absorbed radiation, another layer is made up of the dyestuff and the bonding agent of absorbed radiation in the about 750-1100nm of wavelength coverage basically, the layer that comprises the non-photosensitivity organic silver salts like this is when at 0.10-2.0J/cm
2Radiation (wavelength coverage is in about 750-1100nm) forms the image density greater than about 1.0 when exposing the 0.2-200 microsecond down.
In a scheme again, the invention provides the method that forms image, comprise step with heat-sensitive imaging element radiant exposure in the about 750-1100nm of wavelength coverage, described image-forming component comprises the base material that scribbles thermosensitive imaging system, described thermosensitive imaging system comprises the one deck at least that contains following component: non-photosensitivity organic silver salts, silver ion with reductive agent, bonding agent, in the about 750-1100nm of wavelength coverage the dyestuff and the toner of absorbed radiation, the one deck at least that comprises the non-photosensitivity organic silver salts like this is when at 0.10-2.0J/cm
2Radiation (wavelength coverage is in about 750-1100nm) forms the image density greater than about 1.0 when exposing the 0.2-200 microsecond down.
In yet another embodiment, the invention provides the method that forms image, comprise step with heat-sensitive imaging element radiant exposure in the about 750-1100nm of wavelength coverage, described image-forming component comprises the base material that scribbles thermosensitive imaging system, this thermosensitive imaging system comprises adjacent two-layer at least, wherein the one deck in the adjacent layer comprises the non-photosensitivity organic silver salts, the silver ion reductive agent, bonding agent, toner and non-essential in the about 750-1100nm of wavelength coverage the dyestuff of absorbed radiation, another layer basically by bonding agent and in the about 750-1100nm of wavelength coverage the dyestuff of absorbed radiation form, described radiation is before the adjacent layer that irradiation is made up of bonding agent and dyestuff basically, through comprising the described heat-sensitive imaging element of layer irradiation of non-photosensitivity organic silver salts, the layer that comprises the non-photosensitivity organic silver salts like this is when at 0.10-2.0J/cm
2Radiation (wavelength coverage is in about 750-1100nm) forms the image density greater than about 1.0 when exposing the 0.2-200 microsecond down.
In the preferred embodiment of such scheme of the present invention, by at 0.10-2.0J/cm
2Radiation (wavelength coverage is in about 750-1100nm) is exposure 0.2-200 microsecond down, in comprising the layer of non-photosensitivity organic silver salts, reductive agent etc., form greater than about 2.00, more preferably greater than about 2.50, most preferably greater than about 2.75 image density.
In disclosed all embodiments of the present invention, comprise that non-photosensitivity organic silver salts, silver ion can comprise the silver halide of about 1.0wt% (by the general assembly (TW) of this layer) at the most with the layer (" a thermal sensitivity silver emulsion layer ") of reductive agent etc. in the above.
Money base heat-sensitive imaging element provided by the invention and use heat-sensitive imaging element are as adopting the method for the write-through egative film of laser to overcome a lot of problems that run in the existing system.Since heat-sensitive imaging element be temperature-sensitive and therefore non-photosensitivity can be operated under white light and not need to remove the visible light-sensitive agent.Different with wet silver-colored method element with photothermographic elements, do not need to make the post-processing step of developing.When making the scanned heat-sensitive imaging element of high-power laser diode, can in the thermal sensitivity silver emulsion, shine black-and-white image in the scene, therefore make it have a lot of useful purposes, for example be used for the online detection system of printed circuit board (PCB) photograph processing curtain cover.Simultaneously, do not change relatively owing to only heat the temperature of emulsion imaging moiety and base material, so the thermal shrinkage of egative film is reduced to minimum.This wherein writes down important field for being used for, as reproduces colored imaging fixedly egative film and printed circuit board (PCB) photograph instrument particular importance.In addition, heat-sensitive imaging element can generate the high definition half tone image that can be used for color dub.
Others of the present invention, advantage and benefit are apparent from following detailed description, embodiment, accompanying drawing and claim.
Brief description of the drawings
Fig. 1 represents the synoptic diagram of laser sensitometer.
Fig. 2 represents the relative density figure of distance to laser diode, comprises the theory and the actual curve data value of the flat-top taper laser spot on the egative film plane.
Fig. 3 a is illustrated in laterally/and the direction of scanning is along the total incident exposure energy figure that describes by the distance of laser beam.
Fig. 3 b represents with the microphotometer curve of the imaging line of the energy trace of describing among Fig. 3 a on thermal sensing element (embodiment 16, and sample N does not show).
Fig. 4 represents the figure of density to the logarithm value of exposure energy data shown in Fig. 3 a.
Fig. 5 represents the figure (embodiment 16, sample N do not show) of the absorption of the imaging of comparison heat-sensitive imaging element and non-imaging region to wavelength
Detailed description of the present invention
" heat-sensitive imaging element " used herein refers to scribble at least one surface the base material of " thermosensitive imaging system ". Thermosensitive imaging system comprises at least one thermal sensitivity silver emulsion layer, this emulsion layer contain non-photosensitivity organic silver salts, silver ion with reducing agent, adhesive, toner and in the about 750-1100nm of wave-length coverage the dyestuff of radiation-absorbing. In addition, thermosensitive imaging system can comprise the layer adjacent with thermal sensitivity silver emulsion layer, and this layer further contains dyestuff and the adhesive of radiation-absorbing.
Among the present invention, the thermal sensitivity silver emulsion of use comprise non-photosensitivity organic silver salts, silver ion with reducing agent, in the about 750-1100nm of wave-length coverage dyestuff, toner, adhesive and the non-essential development accelerant of radiation-absorbing.
The non-photosensitivity silver salt is for reducing the material of formation silver metal under such as 60 °-225 ℃ at higher temperature in the presence of the reducing agent. These materials are preferably and contain 4 to 30 carbon atoms, more preferably 8 to 28 carbon atoms, the silver salt of the long-chain alkanoic acid of 10 to 22 carbon atoms (being called again long chain aliphatic carboxylic acid or aliphatic acid) most preferably. The latter also is called " silver-colored soap " in this area.
The non-limitative example of the silver salt of aliphatic carboxylic acid comprises behenic acid silver, silver stearate, oleic acid silver, erucic acid silver, laurate silver, caproic acid silver, myristic acid silver, palmitic acid silver, maleic acid silver, fumaric acid silver, silver tartrate, linoleic acid silver, camphoric acid silver and composition thereof. Also can use the overall stability constant of ligand wherein is the complex of 4.0 to 10.0 organic or inorganic silver salt. Also can use the silver salt of aromatic carboxylic acid and other carboxy-containing acid group's compound to comprise silver benzoate, the silver benzoate that replaces is such as 3,5-dihydroxy-benzoic acid silver, o-toluic acid silver, m-methyl benzoic acid silver, p-methylbenzoic acid silver, 2,4-dichlorobenzoic acid silver, acetaminobenzoic acid silver, to Phenylbenzoic acid silver etc., gallate silver, tannic acid silver, phthalic acid silver, terephthalic acid (TPA) silver, silver salicylate, phenylacetic acid silver, 1,2,4,5-benzenetetracarboxylic acid silver, 3-carboxymethyl-4-methyl-4-thiazoline-2-thioketones or (for example) US 3,785, the analog of describing in 830 and (for example) US 3, the disclosed silver salt that contains the aliphatic carboxylic acid of sulfide group in 330,663. Can also use the silver salt of the compound or derivatives thereof that contains sulfydryl or thioketones group. The preferred example of these compounds comprises 3-sulfydryl-4-phenyl-1,2,4-triazole silver, 2-mercaptobenzimidazole silver, the amino thiadiazoles silver of 2-sulfydryl-5-, 2-(S-ethohexadiol acylamino-) benzothiazole silver, the silver salt of the silver salt of TGA such as S-alkyl-TGA (wherein alkyl has 12-22 carbon atom), the silver salt of carbodithioic acid such as methyl-carbithionic acid silver, thio acylamino silver, 1-methyl-2-phenyl-4-sulfo-pyridine-5-silver carboxylate, triazine thiolic acid silver, 2-sulfo-benzoxazole silver and US 4, disclosed silver salt in 123,274. In addition, can use the silver salt of the compound of amido-containing group. The preferred example of these compounds comprises the silver salt of BTA, the silver salt of the silver salt of the BTA that the silver salt of the BTA that replaces such as BTA silver, alkyl such as methylbenzotrazole silver etc., halogen replace such as 5-chlorobenzotriazole silver etc., carbon imido grpup BTA etc., (for example) US 4,220, in 709 disclosed 1, the silver salt of 2,4-triazole and 1-H-tetrazolium, the silver salt of imidazoles etc. Non-photosensitivity silver salt material preferably should account for about 5 to 60% (weight), more preferably from about 30 to 50% (weight) by the gross weight of thermal sensitivity silver emulsion layer.
Any reducing agent that is applicable to silver ion all can be used among the present invention. These reducing agents are that those skilled in the art are known. The example of these reducing agents includes but not limited to methyl gallate, hindered phenol, catechol, pyrogallol, quinhydrones, replacement quinhydrones, ascorbic acid, ascorbic acid derivates, leuco dye etc. Most preferred reducing agent comprises methyl gallate, gallate butyl ester and propyl gallate. Which kind of reducing agent no matter the present invention use, and its consumption is preferably about 5.0 to 25.0 % (weight), more preferably from about 10.0 to 20.0% (weight) by the gross weight of thermal sensitivity silver emulsion layer.
Toner also is used for thermal sensitivity silver emulsion layer. The example of toner comprises 2,3-phthalazone (phthalazinone), 2,3-benzodiazine, barbituric acid, succinimide and phthalimide. Found the mixture particularly suitable of toner, preferred mixture is the mixture of 2,3-phthalazone and barbituric acid and the mixture of phthalimide and barbituric acid, and most preferred mixture is the mixture of succinimide and barbituric acid. By the gross weight of thermal sensitivity silver emulsion layer, the consumption of toner is preferably about 0.2 to 10.0% (weight), more preferably from about 1.0 to 8.0% (weight), most preferably from about 2.0 to 6.0% (weight).
Can optionally comprise reduction auxiliary agent or development accelerant in thermal sensitivity silver emulsion layer, this depends on used silver material. The reduction auxiliary agent preferably includes 3-indazole quinoline ketone (3-indazolinone) or carbamide compound as development accelerant.
Be used for 3-indazole quinoline ketonic compound of the present invention and preferably have following structure:
Wherein R is selected from following group: the alkyl of hydrogen, 1 to 4 carbon atom, halogen ,-COOH and-R1COOH (R wherein1For having the alkyl of 1 to 4 carbon atom), R is preferably the alkyl of hydrogen or 1 to 4 carbon atom, and R most preferably is hydrogen.
These 3-indazole quinoline ketonic compounds can be synthetic according to the known method of synthetic organic chemistry field those of skill in the art.In addition, these compounds can be commercial, as available from Aldrich chemical company (AldrichChemical Company), Milwaukee, Wei Sikangxin; Lancaster chemical company (Lancaster Chemical Company), Windham, New Hampshire; And K﹠amp; KLaboratories of Cleveland, Ohio.
As well known in the art, a large amount of replace, be not only permission, and advocate.Therefore, term used herein " group " not only comprises pure hydrocarbon substituent such as methyl, ethyl etc.And comprise the hydrocarbon substituent that has the conventional substituting group in this area such as hydroxyl, alkoxy, phenyl, halogen (F, Cl, Br, I), cyano group, nitro, amino etc.
The carbamide compound that uses among the present invention preferably has following general formula:
R wherein
2And R
3Represent hydrogen, C independently of one another
1-C
10Alkyl or cycloalkyl or phenyl, or R
2And R
3Form together and contain the heterocyclic group of 6 annular atomses at the most.R
2And R
3Preferred hydrogen, the C of representing
1To C
5Alkyl or cycloalkyl or phenyl, or R
2And R
3Form together and contain the heterocyclic group of 5 annular atomses at the most.These carbamide compounds can synthesize easily and be commercially available.The non-limitative example of these carbamide compounds comprises urea, 1,3-diphenyl urea, 1,3-diethyl urea, Butylurea and 2-diimidazole alkane ketone.Most preferred development accelerant is a 2-diimidazole alkane ketone.
Heat-sensitive imaging element of the present invention is commonly referred to be non-photosensitivity, does not therefore contain photosensitizer such as silver halide, light trigger, photoproduction bleaching agent.Thermal sensitivity silver emulsion layer can have and is lower than 1%, is lower than 0.75%, is lower than 0.5% or be 0% (weight) (pressing the general assembly (TW) agent of thermal sensitivity emulsion), and performance is good.It is believed that if not catalysis of silver halide forms latent image, then is not effective.
Light stabilizer such as benzotriazole, phenyl mercapto-tetrazole and other light stabilizer known in the art can add in the photosensitivity silver emulsion.Preferred light stabilizer is a benzotriazole.The addition of light stabilizer preferably should be the about 0.1 to 3.0% of photosensitivity silver emulsion layer, and more preferably from about 0.3 to 2.0wt%.
Be used for thermal sensitivity silver emulsion layer of the present invention and also use bonding agent.Can use the known any conventional polymer bonding agent of those skilled in the art.For example, bonding agent can be selected from any known natural and synthetic resin such as gelatin, Pioloform, polyvinyl acetal, Polyvinylchloride, cellulose acetate, polyolefin, polyester, polystyrene, polyacrylonitrile, polycarbonate etc.Certainly, comprise multipolymer and ter-polymers in these definition, its example includes but not limited to Pioloform, polyvinyl acetal, as polyvinyl acetal, polyvinyl butyral, polyvinyl formal and ethylenic copolymer.The addition of bonding agent preferably should be 10 to 60% (weight) by the general assembly (TW) of thermal sensitivity silver emulsion layer, more preferably 15 to 50% (weight).
Thermal sensing element of the present invention uses and absorbs about 750-1100nm, preferably about 750-900nm, the dyestuff of the electromagnetic radiation of 750-870nm wavelength coverage most preferably from about.
Dyestuff should dissolve in coating solvent, in preferred ketone or arsol such as methyl ethyl ketone or the toluene.Dyestuff also should be with bonding agent miscible and with emulsion in the silver salt, activator and the developer that use compatible.For being used for UV (ultraviolet ray) contact egative film or mask, the optical density of dyestuff is preferably greater than 1.0 ODUs, has the weak absorption that is lower than 0.2 ODU in the UV zone (250-450nm) corresponding to the exposure tool wavelength that is used as mask simultaneously.Optical density is measured with the MacBeth Model TD523 densitometer that state 18A filter is housed.Also needing (but not necessarily) to have low visible background for dyestuff absorbs.
The dyestuff of absorbed radiation can be used for in one deck with reductive agent, toner and bonding agent are the same with non-photosensitivity organic silver salts, silver ion.In addition, dyestuff can be used in above-mentioned layer and the adjacent layer or is mainly used in the adjacent layer.The dyestuff of absorbed radiation can directly add in the thermal sensitivity silver emulsion layer, or in the heat-sensitive imaging element process by making dyestuff from the adjacent layer that contains dyestuff, move to come out to add indirectly in the thermal sensitivity silver emulsion layer.
Suitable dyestuff includes but not limited to oxonol, squarylium, chalcogenopyrylarylidene, bis (chalcogenopyrylo) polymethine, two (ammonia aryl) polymethine, merocyanine, three nuclear cyanine, indenes bridge joint polymethine, the oxygen indolizine, iron complex, quinoid, nickel dithiode alkene complex and cyanine dye such as carbocyanine, the azepine carbocyanine, half cyanine, styryl, the diaza carbocyanine, three azepine carbocyanines, dinitrogen diaze hemicyanine, the polymethine cyanine, azepine polymethine cyanine, full cyanine, indocyanine green and dinitrogen diaze hemicyanine.
The amount of dye that exists in the heat-sensitive imaging element depends on that dyestuff only adds in the thermal sensitivity silver emulsion layer or adds in the adjacent layer simultaneously.When dyestuff existed only in the thermal sensitivity silver emulsion layer, its amount was counted 0.10-5.0wt% by the general assembly (TW) of thermal sensitivity silver emulsion layer, preferred 0.2-3.0wt%.
In the time of in being present in adjacent layer, the amount of dyestuff in thermal sensitivity silver emulsion layer counted 0-5.0wt% by the general assembly (TW) of thermal sensitivity silver emulsion layer, preferred 0-1.0wt%.In the adjacent layer that contains dyestuff and bonding agent, the amount of dyestuff is counted 1-25wt% by the general assembly (TW) of adjacent layer, preferred 5-20wt%.
Known any suitable substrates or the stroma ground substance of those skilled in the art can be used among the present invention.These materials can be opaque, translucent or transparent.Be used for the substrate commonly used in temperature-sensitive field or stroma ground substance and include but not limited to that paper, opaque or transparent polyester and polycarbonate egative film and specific light reflective metals matrix are as silver, gold and aluminium.Term used herein " specific light reflective metals matrix " is meant when metal matrix is used rayed, at specific angle reflected light, rather than in certain angle scope reflects light.
Can optionally use the protection or the adherent layer that are positioned at the heat-sensitive imaging element top.Any conventional preventing viscosity substance all can be used among the present invention.The example of these preventing viscosity substances includes but not limited to paraffin, silica dioxide granule, contain cinnamic elastomeric block copolymers such as s-B-S, styrene-isoprene-phenylethene, and the blend of they and (for example) cellulose acetate, cellulose acetate-butyrate, cellulose-acetate propionate and poly-(ethene butyral).
Other layers can be included in the thermal sensing element of the present invention as prime coat or antistatic layer.Simultaneously, antistatic or adherent layer can optionally be applied to the back side of base material.The material that is used for this purpose is that those skilled in the art are known.
Being used for thermosensitive imaging system of the present invention, antiseized, infrared or hear-infrared absorption dye and antistatic layer can be by coatings such as conventional method such as blade coating, roller coat, dipping, curtain coating, hopper coatings.If need, can be coated with two layers or multilayer simultaneously by the method for describing among US 2,761,791 and the GB 837,095.
Heat-sensitive imaging element of the present invention generally passes through with infrared or near-infrared laser radiant image infrared or that the near-infrared laser diode produces.Known as the thermographic field, infrared or near-infrared laser diode can advantageously form a line to improve image taking speed.Can be used for providing laser instrument infrared or the near-infrared laser radiation consist essentially of can be in the infrared and near infrared region of about 750 to 1100nm electromagnetic wave spectrums lasing any laser instrument, comprise that dye laser, solid state diode lasers are as the aluminum gallium arsenide diode laser of emission laser in 780 to 870nm zones and diode bleed solid-state laser such as Nd:YAG, Nd:YLF or Nd: glass.
Following non-limiting examples further specifies the present invention.
Embodiment
The material that is used for the following example, except as otherwise noted can available from normal business mechanism such as Aldrich chemical company (Milwaukee, W1).
Behenic acid silver and lauric acid silver homogenate can be by US 4,210,710 (the 2nd hurdle 55-57 is capable) or Us3, the preparation of 457,075 (the 4th hurdle 23-44 is capable and the 6th hurdle 37-44 is capable) disclosed method.
Preparation dyestuff 1: according to US 4,062, the method for describing in 682 prepares 5-sulfonamide-2,3, the 3-tri-methyl indole false.With 37.0g 5-sulfonamide-2,3, the potpourri of 3-tri-methyl indole false, 16.7mL 2-ethyl chloride sulfonic acid chloride and 200mL acetonitrile refluxed 6 hours.After adding 18.5mL water, the potpourri stirring is spent the night.Filter to isolate solid, with the acetonitrile washing, the dry then quaternary salt intermediate that obtains 11.0g 1-sulfoalkylization.
The potpourri of 6.5g chlorine cyclopentene dialdehyde, the 26g quaternary salt intermediate, 108mL acetic anhydride and the 72mL acetate that prepare was previously at room temperature stirred 10 minutes.After adding the 12.8mL diisopropylethylamine, this potpourri stirring is spent the night.Filter to isolate solid, with the solvent mixture washing, drying obtains 20.0g dyestuff 1 then.
Dyestuff 2 preparation dyestuffs 2: in the 3L flask, add 385g trimethyl sulfonamide indolenine and 250ml butyronitrile.Under the condition of not heat release, in this potpourri, add 225mL (364g) butyl iodide, then add other 750mL butyronitrile.This potpourri was under agitation heated 22.5 hours.Except that reducing phlegm and internal heat and this potpourri being cooled to about 40 ℃.Continue to stir 1 hour.After adding 1L ethyl acetate, filter out solid, with the ethyl acetate washing, drying obtains 595.6g N-butyl-2,3 then, 3-trimethyl-5-sulfonamide indolenine iodide.
In 1 hour to the 370mL methylene chloride and the 558mL N that are cooled to below 5 ℃, be added dropwise to the 277mL phosphoryl chloride phosphorus oxychloride in the solution of dinethylformamide, rate of addition should make temperature be no more than 5 ℃, after charging is finished, removes external refrigeration and this potpourri was stirred 1 hour.In 30 minutes, divide 2 batches to add the 75mL cyclopentanone.After adding first, observe temperature and slowly rise to about 35 ℃ and color (variation), add second portion and cause a large amount of heat releases this moment.After heat release reduces, this mixture heated was refluxed 4 hours.After adding 1L ethyl acetate this potpourri is distilled under slight underpressure.When beginning to form precipitation, collect about 250mL liquid, to wherein adding 700mL ethyl acetate.This potpourri stirring is spent the night, solid filtering is come out,, then use heptane wash,, obtain the thick chlorine cyclopentene of 115.8g dialdehyde then 35 ℃ of following vacuum drying 4 hours with the washing of 1L ethyl acetate.
This thick cyclopentadiene dialdehyde is dissolved in the 1250mL water.Begin to occur crystallization after about 1 hour.This potpourri was left standstill 2 days.Filter out brown solid, this solid is washed with water,, obtain 61.0g chlorine cyclopentene dialdehyde 35 ℃ of following vacuum drying 7 hours.
In the solution of 450mL acetate and 450mL acetic anhydride, add 278.7g N-butyl-2,3,3-trimethyl-5-sulfonamide indolenine iodide and 47.6g cyclopentene dialdehyde.In stirring the mixture, this in 5 minutes, is being added dropwise to the 90mL triethylamine under 60-65 ℃.Do not observe a large amount of heat releases.This potpourri was heated 30 minutes again.Then except that reducing phlegm and internal heat and potpourri being cooled to 15 ℃.Filter out the golden yellow solid of gained and use acetate: potpourri washing in 1: 1 of acetic anhydride, till washings is green rather than purple.Solid suspension is removed acetate and acetic anhydride in 1L ethyl acetate, then stirred 90 minutes.Filter out solid and, leach thing and be pink with ethyl acetate washing.This solid is obtained 250.0g dyestuff 2 by vacuum drying under 45 ℃.
Dyestuff 3 preparation dyestuffs 3: dyestuff 2,0.1mol sodium tetraphenylborate and 500mL methanol mixture that 0.1mol is prepared above under agitation refluxed 10 minutes.Filter out solid and use methanol wash, then wash with water, drying obtains 0.97mol dyestuff 3 then.
Dyestuff 4 preparation dyestuffs 4: with 26.05g 1, the reflux 5 hours of stirring the mixture under nitrogen atmosphere of 8-diaminonaphthalene, 32.66g methyl n-undecyl ketone, 55mg p-toluenesulfonic acid monohydrate and 250mL toluene is removed the water of emitting from reaction with Dean-Stark trap.Then this potpourri is washed with saturated sodium bicarbonate solution, dry on Anhydrous potassium carbonate, filter, and under reduced pressure remove and desolvate.The product distillation is made the 48.86g dihydro
Pyridine intermediate, its boiling point are 192-213 ℃ under 0.3 to 0.4 torr.
The dihydro that 8.0g is prepared above
The heating that stirs the mixture of pyridine intermediate, 1.48g squaric acid, 64mL normal butyl alcohol and 64mL toluene makes it reflux 3 hours to remove the water of emitting from reaction with dean stark trap under nitrogen atmosphere.This potpourri is filtered, pour in the 600mL sherwood oil (b.p.35-60 ℃), and kept 18 hours down at 5 ℃.Filter out product, use petroleum ether, make 6.45g dyestuff 4 at air drying then.
The preparation of dyestuff 5 dyestuffs 5: under agitation, with 28g 2,3,3-trimethyl-5-methoxyl indolenine adds 80mL oleum (10%SO
3) in.This potpourri at room temperature stirred spend the night, be poured on then on the 500g trash ice.This aqueous solution is extremely done with neutralization of 30% sodium hydroxide solution and vaporising under vacuum.With the residue methanol extraction, and with solution evaporation.Solid is added in the ethanol, filter,, make 20g indolenine sulfate intermediate, be yellow prism thing with ethanol washing and dry under vacuum.
With the 20g indolenine sulfate intermediate, the 20g 2 that prepare above, the potpourri of 4-butane sulfone and 80mL benzonitrile under agitation refluxed 5 hours.With the solids wash that forms, with the ethyl acetate washing, and drying makes 25g sulfoalkyl quaternary salt intermediate under vacuum, is light brown prism thing.
With 14.2g sulfoalkyl quaternary salt intermediate, the 7.5g N-(2-chloro-3-(dimethylamino) methylene)-1-cyclohexene-1-yl for preparing above) methylene)-potpourri of N-methyl chloromethane ammonium (methanaminiumchloride) (according to the method preparation of describing among the EPO application No.0288261), 5.4mL dicyclohexyl ethamine and 75mL benzonitrile at room temperature stirs and spends the night.Add in the ethyl acetate with this potpourri filtration and with filtrate.Filter out solid and be dried.Be dissolved in solid in the 50mL ethanol and add the 3g sodium iodide.Filter out sediment, with the acetonitrile washing, drying makes 3g dyestuff 5 then, is green prism thing.
Dyestuff 6 dyestuffs 6 can be from Eastman Kodak Co., Rochester, and NY has bought.Embodiment 1-3 is used for following coating solution the preparation method of embodiment 1-3.Silver emulsion: behenic acid silver homogenate 160g
(in methyl ethyl ketone, 10wt%) Butvar
TMB76 gathers (vinyl butyral), available from Monsanto Co. 20g thermal sensitivity coating solution:
Following component is mixed the thermal sensitivity coating solution of preparation embodiment 1-3 with the above-mentioned silver emulsion of 20g. material embodiment 1 embodiment 2 embodiment 3 methyl gallate 0.6g 0.6g 0.6g pyrogallol 0.2g 0.2g 0.2g2,3-phthalazone 0.2g 0.2g 0.2g succinimide 0.1g 0.1g 0.1g2-imidazolidinone 0.1g 0.1g 0.1g barbituric acid 0.05g 0.05g BTA 0.02g
Each solution is applied on the polyester base material of 0.08mm (3 mil) with the wet thickness of 0.1mm (4 mil) and under 60 ℃ air drying 3 minutes.
0.08g dyestuff 1,1.0g CA 398-6 cellulose acetate resin and 20.0g MEK are mixed, and preparation absorbs ultrared finish paint solution.Be applied to heat-sensitive layer on the wet thickness of 0.05mm (2 mil) this finish paint solution and under 60 ℃ air drying 3 minutes.
Embodiment 4-6
The preparation method who following coating solution is used for embodiment 4-6.Silver emulsion: the full soap homogenate 160g of lauric acid silver (in methyl ethyl ketone, 10wt%) BX-1 poly-(vinyl butyral), available from Sekisui Chemical Co. 10g thermal sensitivity coating solution:
Following component is mixed the thermal sensitivity coating solution of preparation embodiment 4-6 with the above-mentioned silver emulsion of 20g. material embodiment 4 embodiment 5 embodiment 6 methyl gallate 0.6g 0.6g 0.6g pyrogallol 0.2g 0.2g 0.2g2,3-phthalazone 0.2g 0.2g 0.2g succinimide 0.1g 0.1g 0.1g2-imidazolidinone 0.1g 0.1g 0.1g barbituric acid 0.05g 0.05g BTA 0.02g
The wet thickness of each solution with 0.1mm (4 mil) is applied on the polyester base material of 0.08mm (3 mil), and under 60 ℃ air drying 3 minutes.
0.08g dyestuff 1,1.0g CA 398-6 cellulose acetate resin and 20.0g MEK are mixed, and preparation absorbs ultrared finish paint solution.Be applied to heat-sensitive layer on the wet thickness of 0.05mm (2 mil) this finish paint solution and under 60 ℃ air drying 3 minutes.
Table 1 is generally listed with 810 nanometer laser diodes (available from Spectra Diode Labs of SanJose, CA) with 1.75J/cm
2Focus on the result that (with 7 microns bright spot size) exposes the material of embodiment 1-6 on the egative film plane.Measure visible light density and measure the UV optical density with Perkin Elmer microphotometer PDS 1010M with the MacBeth TD523 densitometer that state 18A filter is housed.The UV light stability leaves standstill 24 hours mensuration by sample is in fluorescence (1,000 foot candle, the 90) case.
Table 1
| Embodiment | ???1 | ????2 | ???3 | ???4 | ???5 | ???6 |
| As seen Dmax | ??3.06 | ??3.23 | ??3.25 | ??3.87 | ??3.84 | ??3.83 |
| As seen Dmin | ??0.05 | ??0.05 | ??0.05 | ??0.07 | ??0.07 | ??0.07 |
| UV?Dmin | ??0.15 | ??0.14 | ??0.13 | ??0.19 | ??0.15 | ??0.16 |
| UV Dmin 24hr stability | ??0.55 | ??0.61 | ??0.23 | ??0.53 | ??0.59 | ??0.25 |
Embodiment 3 and 6 clearlys show and works as that benzotriazole has significantly improved UV Dmin light stability when adding in the thermal sensitivity silver emulsion.
Embodiment 7
Following coating solution is used for the preparation of embodiment 7: silver emulsion: behenic acid silver homogenate 160g is (in methyl ethyl ketone, 10wt%) BX-1 poly-(vinyl butyral), available from Sekisui Chemicai Co. 10g thermal sensitivity coating solution:
The 20g silver emulsion is joined preparation thermal sensitivity coating solution among 0.6g methyl gallate, 0.1g succinimide, 0.1g phthalimide, 0.1g tetrachlorophthalic tetrachlorophthalic anhydrid, 0.02g benzotriazole, 0.05g barbituric acid in 4mL methyl alcohol and the 1mL MEK.The wet thickness of this solution with 0.08mm (3 mil) is applied on the polyester base material of 0.08mm (3 mil), and under 60 ℃ air drying 3 minutes.
0.08g dyestuff 1,0.5g Sekisui BX-1 poly-(vinyl butyral) and 20.0g MEK are mixed with the ultrared finish paint solution of absorption.Be applied to heat-sensitive layer on the wet thickness of 0.05mm (2 mil) this finish paint solution and under 60 ℃ air drying 3 minutes.
With embodiment 7 usefulness 810 nanometer laser diodes (available from Spectra Diode Labs of SanJose, CA) with 1.75J/cm
2Focus on (with 7 microns bright spot size) exposure on the egative film plane.The visible Dmax that this imaging egative film has is 3.4, visible Dmin is 0.08, UV Dmax be 3.6 and UV Dmin be 0.17.Visible light density is measured with Perkin Elmer microphotometer PDS1010M.The UV optical density is measured with the MacBeth TD523 densitometer that state 18A filter is housed.
Embodiment 8
Following coating solution is used for the preparation of embodiment 8.(in methyl ethyl ketone, 10wt%) BX-1 poly-(vinyl butyral) is available from Sekisui Chemical Co. 15gAcryloid for silver emulsion: behenic acid silver homogenate 160g
TMThe A-21 acryl resin, available from Rohm and Haas 6g methyl ethyl ketone (MEK) 50g thermal sensitivity coating solution:
The 15g silver emulsion is joined 0.6g methyl gallate, 0.1g 2, preparation thermal sensitivity coating solution in 3-phthalazone, 0.1g 2-miaow alkane ketone, 0.1g tetrachlorophthalic tetrachlorophthalic anhydrid, the 0.05g barbituric acid in 4mL methyl alcohol, 1mLMEK and the 1mL tetrahydrofuran.Before the coating, 0.13g dyestuff 1 is added in the solution.The wet thickness of this solution with 0.08mm (3 mil) is applied on the polyester base material of 0.08mm (3 mil), and under 50 ℃ air drying 3 minutes.
The finish paint solution that will contain poly-(vinyl butyral) solution of BX-1 of 2.4% (weight) is applied on the temperature-sensitive coating with the wet thickness face of 0.05mm (2 mil), and under 50 ℃ air drying 3 minutes.
Embodiment 9-10
Following coating solution is used for the preparation of embodiment 9-10.Silver emulsion: behenic acid silver homogenate 160g (in methyl ethyl ketone, 10wt%) BX-1 poly-(vinyl butyral), available from Sekisui Chemical Co. 5g thermal sensitivity coating solution:
The 15g silver emulsion is joined preparation thermal sensitivity coating solution among 0.6g methyl gallate, 0.1g succinimide, 0.1g 2-imidazolidinone, 0.1g tetrachlorophthalic tetrachlorophthalic anhydrid, 0.05g barbituric acid and 4mL methyl alcohol and the 1mL MEK.Before the coating, will add in the solution of embodiment 3 in the solution of 0.08g dyestuff 2 adding embodiment 2 and with 0.08g dyestuff 3.The wet thickness of this solution with 0.08mm (3 mil) is applied on the polyester base material of 0.08mm (3 mil), and under 50 ℃ air drying 3 minutes.
The finish paint solution that will contain poly-(vinyl butyral) solution of BX-1 of 2.4% (weight) is applied on the temperature-sensitive coating with the wet thickness face of 0.05mm (2 mil), and under 50 ℃ air drying 3 minutes.
Embodiment 11-12
Following coating solution is used for the preparation of embodiment 11-12.Silver emulsion: behenic acid silver homogenate 160g (in methyl ethyl ketone, 10wt%) Butvar
TMB-76 gathers (vinyl butyral) 20g thermal sensitivity coating solution:
The 15g silver emulsion is joined 0.8g methyl gallate, 0.2g succinimide, 0.1g 2, preparation thermal sensitivity coating solution in 3-phthalazone, the 0.1g 2-imidazolidinone in 4mL methyl alcohol and the 1mL methyl ethyl ketone.Before the coating, will add in the solution of embodiment 12 in the solution of 0.05g dyestuff 4 adding embodiment 11 and with 0.08g dyestuff 5.This solution is applied on the polyester base material of 0.08mm (3 mil) with the wet thickness of 0.1mm (4 mil) and under 21 ℃ air drying 10 minutes.
The finish paint solution that will contain 2.4% (weight) CA 398-6 cellulose acetate (available from Eastman KodakCo.) solution is applied on the heat-sensitive layer with the wet thickness of 0.05mm (2 mil), and under 21 ℃ air drying 20 minutes.
Table 2 is generally listed with 810 nanometer laser diodes (available from Spectra Diode Labs of SanJose) with 1.75J/cm
2Focus on the result that (with 7 microns bright spot size) exposes the material of embodiment 8-12 on the egative film plane.Measure maximum (D with the MacBeth TD523 densitometer that state 18A filter is housed
Max) and minimum (D
Min) optical density.
Table 2
| Embodiment # | ??8 | ??9 | ??10 | ??11 | ??12 |
| Time shutter (microsecond) | ??72 | ??45 | ??45 | ??45 | ??72 |
| D max | ??3.2 | ??3.0 | ??1.55 | ??2.5 | ??3.1 |
| UV?D min | ??0.19 | ??0.16 | ??0.13 | ??0.18 | ??0.18 |
| As seen D min | ??0.07 | ??0.07 | ??0.07 | ??0.07 | ??0.13 |
Embodiment 13
For the effect that has halide ion in the thermal sensitivity emulsion layer is described, the 0.2g calcium bromide is added in the thermal sensitivity coating solution of embodiment 9.When the complete blackening of heat-sensitive layer in the time of 3 minutes of drying under 21 ℃.
Embodiment 14
Following coating solution is used for the preparation of embodiment 14.Silver emulsion: behenic acid silver homogenate 160g (in methyl ethyl ketone, 10wt%) Butvar
TMB-76 gathers (vinyl butyral) 20g thermal sensitivity coating solution:
With 0.6g methyl gallate, 0.2g 2,3-phthalazone, 0.1g succinimide, 0.1g 2-imidazolidinone and 0.2g pyrogallol add preparation thermal sensitivity coating solution in the 20g silver emulsion.The wet thickness of this solution with 0.1mm (4 mil) is applied on the polyester base material of 0.08mm (3 mil), and under 21 ℃ air drying 10 minutes.
0.03g dyestuff 6,1.0g CA398-6 cellulose acetate resin and 20.0g MEK are mixed, and preparation absorbs ultrared finish paint solution.Be applied to heat-sensitive layer on the temperature thickness of 0.05mm (2 mil) this finish paint solution and under 60 ℃ air drying 3 minutes.
Embodiment 15
Following coating solution is used for the preparation of embodiment 15.Silver emulsion: behenic acid silver homogenate 160g (in methyl ethyl ketone, 10wt%) Butvar
TMB-76 gathers (vinyl butyral) 20g thermal sensitivity coating solution:
0.6g methyl gallate, 0.1g succinimide, 0.1g 2-imidazolidinone and 0.2g L-ascorbyl palmitate are added preparation thermal sensitivity coating solution in the 20g silver emulsion.The wet thickness of this solution with 0.1mm (4 mil) is applied on the polyester base material of 0.08mm (3 mil), and under 60 ℃ air drying 3 minutes.
0.03g dyestuff 6,1.0g CA398-6 cellulose acetate resin and 21.0g MEK are mixed, and preparation absorbs ultrared finish paint solution.Be applied to heat-sensitive layer on the wet thickness of 0.05mm (2 mil) this finish paint solution and under 60 ℃ air drying 3 minutes.
Table 3 is generally listed the laser explosure result of each embodiment.Measure minimum and maximum optical density with the MacBeth TD523 densitometer that state 18A filter is housed.
Table 3
| Embodiment | ????14 | ????15 |
| ??D max | ????3.73 | ????2.73 |
| ??D min | ????0.09 | ????0.10 |
The dyestuff of absorbed radiation can mainly be included in the thermal sensitivity silver emulsion layer.It is believed that thermal sensitivity silver emulsion layer is heated to more than the glass transition temperature, so make silver ion migrate into the interior non-photosensitivity organic silver salts (behenic acid silver of layer with reductive agent) in.Behenic acid silver is reduced into elemental silver with reductive agent, forms brown/black image.To obtain more neutral black in the toner adding batching.The elemental silver that forms in imaging region not only provides the image that does not see through UV in final element, and is the infrared absorbing agents that quickens the image forming process.Infrared laser beam in infiltrating thermal sensitivity silver emulsion layer the time its intensity exponentially weaken.The thickness of thermal sensitivity silver emulsion layer and the concentration of Infrared dyes will influence the sharpness of image, and reason is that intensity of laser beam reduces with the distance of passing layer.The thickness of thermal sensitivity silver emulsion layer is preferably about 1 to 10 μ m, more preferably from about 2 to 6 μ m.It is about 20% to 99% that the thickness of regulating the concentration of Infrared dyes and layer absorbs the IR of layer to be generally, preferred 50-90%, more preferably 60-85%.
Under the high-resolution imaging condition (this moment the pixel residence time short and laser peak intensity height), if Infrared dyes can occur ablating when only adding in the thermal sensitivity emulsion layer of structure.The rate of heat addition is higher on the surface that laser beam enters thermal sensitivity silver emulsion layer.Because forming element silver, the absorption of laser beam increases, and this can cause thermal sensitivity silver emulsion layer overheated, causes a fog, damages or ablate.
Add in the layer adjacent by the concentration of the Infrared dyes in elimination or the minimizing thermal sensitivity silver emulsion layer with Infrared dyes, can increase the laser beam that penetrates in the thermal sensitivity silver emulsion layer with thermal sensitivity silver emulsion layer.Making laser beam pass through thermal sensitivity silver emulsion layer before irradiation contains the adjacent layer of Infrared dyes exposes the thermal sensitivity image-forming component.With respect to base material, infrared absorption layer can be positioned on the thermal sensitivity silver emulsion layer or under, wherein adjacent layer is deposited on the base material.The concentration of the infrared absorbing dye of choosing in infrared absorption layer should make the maximum heat-up rate appear between infrared absorption layer and the thermal sensitivity silver emulsion layer at the interface.The concentration of Infrared dyes depends on the physical property of the thickness and the dyestuff of thermal sensitivity layer.For example, regulating the concentration of Infrared dyes in the thick thermal sensitivity layer of 1 μ m makes it preferably obtain about 90% or bigger absorption.
In imaging laser pulse process, elemental silver forms on the interface.The elemental silver that forms increases infrared absorption and play the effect of the thermal source of imagery zone in thermal sensitivity silver emulsion layer in this zone of thermal sensitivity silver emulsion layer.Because the density of elemental silver is being set up adjacent to infrared absorption layer, therefore in the weakened near the infrared absorption layer another side, reduces the overheated of this zone thus.The profile of pixel image will be similar to a hour glass shape (hour-glass shape), so obtain image more clearly.
Embodiment 16
The concentration of the thickness of present embodiment explanation thermal sensitivity silver emulsion layer, resin/silver-colored ratio, Infrared dyes and finish paint type are to the influence of the imaging characteristic of heat-sensitive imaging element of the present invention.
Following coating solution is used to prepare sample A-P.X represents the variable that provides in the table 4.Silver emulsion: behenic acid silver homogenate 160g (in methyl ethyl ketone, 10wt%) Butvar
TMB-76 gathers (vinyl butyral) Xg thermal sensitivity coating solution:
The 15g silver emulsion is added 0.8g methyl gallate, 0.2g succinimide, 0.1g 2, in 3-phthalazone, the 0.1g 2-imidazolidinone and 1mL methyl ethyl ketone in 4mL methyl alcohol, preparation thermal sensitivity coating solution.Before the coating, Xg dyestuff 2 is added in the solution.This solution is applied on the polyester base material of 0.08mm (3 mil) with the X wet thickness and under 70 ℃ air drying 3 minutes.
The CA398-6 cellulose acetate that will comprise 2.4% (weight) is available from the Scripset of Monsanto Company
TM540 styrene-maleic anhydride copolymers are available from the Tyril of Dow Chemical Company
TMThe 8808B styrene-acrylonitrile resin, or poly-(vinyl alcohol) is (PVA), available from AirProducts and Chemicals, the Airvol of Inc.
TM523, the finish paint solution of PA and X% dyestuff 2 is applied on the heat-sensitive layer with X wet thickness face, and under 50 ℃ air drying 3 minutes.
Sample A-P is scanned with the different scanning speed in 20-60cm/s with laser sensitometer.Measure the density size of these lines with Perkin Elmer microphotometer PDS 1010M at the 415nm place.Measure the not optical density measurements of image-forming component with Shimadzu spectrophotometer MPC-3100/UV3101PC at 826nm (laser diode wavelength) and 415nm place.
Table 4
| Sample # | ?A | ?B | ??C | ?D | ?E | ?F | ?G | ?H |
| Heat-sensitive layer thickness (wet, mm) | ?0.10 | ?0.05 | ??0.10 | ?0.05 | ?0.10 | ?0.05 | ?0.10 | ?0.10 |
| Top coat layer thickness (wet, mm) | ?0 | ?0 | ??0 | ?0 | ?0 | ?0 | ?0.05 | ?0.05 |
| The top-coat resin type | Do not have | Do not have | Do not have | Do not have | Do not have | Do not have | ?PVA | ?PVA |
| The content of Butvar in the silver layer | ?20g | ?20g | ?10g | ?10g | ?5g | ?5g | ?0 | ?0 |
| Infrared dyes in the heat-sensitive layer | ?0.05g | ?0.05g | ?0.05g | ?0.05g | ?0.05g | ?0.05 ?g | ?0 | ?0.01g |
| Infrared dyes in the top coat layer | ?0 | ?0 | ?0 | ?0 | ?0 | ?0 | ?0.10g | ?0.15g |
| Dmin(415nm) | ?0.95 | ?0.14 | ?1.1 | ?0.3 | ?1.24 | ?0.75 | ?0.34 | ?0.53 |
| Guang Midu @825nm | ?0.65 | ?0.34 | ?0.7 | ?0.36 | ?0.79 | ?0.27 | ?1.80 | ?3.20 |
| Sample # | I | J | K | L | M | N | O | P |
| Heat-sensitive layer thickness (wet, mm) | 0.10 | 0.05 | 0.10 | 0.05 | 0.10 | 0.10 | 0.10 | 0.10 |
| Top coat layer thickness (wet, mm) | 0.05 | 0.05 | 0.05 | 0.05 | 0.05 | 0.05 | 0.05 | 0.05 |
| The top-coat resin type | Cellulose acetate | Cellulose acetate | Cellulose acetate | Cellulose acetate | Tyril TM | Scripset TM | Scripset TM | Scripset TM |
| The content of Butvar in the silver layer | 10g | 10g | 10g | 10g | 0 | 0 | 0 | 0 |
| Infrared dyes in the heat-sensitive layer | 0.07g | 0.07g | 0.10g | 0.10g | 0.05g | 0.01g | 0.01g | 0 |
| Infrared dyes in the top coat layer | 0 | 0 | 0 | 0 | 0 | 0.10g | 0.15g | 0.10g |
| ?Dmin (415nm) | 0.23 | 0.07 | 0.42 | 0.12 | 0.55 | 0.35 | 0.29 | 0.42 |
| Guang Midu @825nm | 0.75 | 0.30 | 1.40 | 0.84 | 0.76 | 0.84 | 1.45 | 1.11 |
Laser sensitometer as shown in Figure 1 (1) is used for assessing the heat-sensitive imaging element of embodiment 16.The 700 milliwatt laser beam (2) that the laser diode that 2361-P2 optical fiber is coupled (3) (available from Spectra Diode Labs) sends focus on the rotary drum (4).The core diameter of optical fiber (5) is 100 μ m, and the wavelength of laser diode (3) is 826 nm.Power on the rotary drum (4) is 210 milliwatts, and light spot form is for locating to have the flat-top awl of 45 μ m spot sizes in overall with half maximum (FWHM).The flat-top cone-shaped is characterised in that r
0(the peak intensity radius of taper) and r
1(intensity approaches the external radius of 0 o'clock taper).Scanning slit bundle section tester is used for the shape of Laser Measurement point.Because the section tester is in the direction integrated intensity that moves perpendicular to slit, the actual point shape is from section tester inferred from input data.Fig. 2 represents the contrast of the profile data (7) of section tester data (6) and calculating, the r that flat-top taper intensity has
0Equal 10 microns, r
1Equal 36 microns.Curve negotiating is bored intensity section integration and varying sized calculating in a direction to the model flat-top.
Because by film scanning, being positioned at naming a person for a particular job of minute planting, intensity distributions accepts fixedly exposure energy.This exposure energy depends on this position and spot scan speed with respect to analyzing spot.Fig. 3 a is illustrated in laterally/and the total incident exposure energy in direction of scanning is to the figure of the distance of transmitted beam.The sensitometer model harness shape calculated curve coupled to optical fiber supposes that sweep velocity is 40cm/ second.In Fig. 3 b, the expression microphotometer figure (embodiment 16, and sample N is not shown) of the line of the energy distribution imaging on thermal sensing element shown in Fig. 3 a.Density data is collected at the 415nm place with the arrowband filter.Density limit among Fig. 3 b shows greater than the gradient of the exposure of the incident shown in Fig. 3 a section, shows that this thermal sensing element (embodiment 16, and sample N is not shown) has high contrast.
The contrast of thermal sensing element can be shown with the more quantitative face of land of D-logE curve.The D-logE curve is the logarithmic graph of imaging egative film density and incident exposure energy.The theoretical shape of this curve is by D=γ log (EE
F/ E
O) provide, wherein, γ equals the D-logE slope of a curve, and E equals incident exposure energy, E
FEqual the effective energy of mist or background level, E
0The required least energy of expression beginning developing, the optical density of element when D equals to expose under exposure energy E.Background density equals γ log E
FWith data computation D-logE curve shown in Figure 3 and in Fig. 4, draw.Prove that by the model curve of describing by the optical density equation γ of element or contrast are consistent with the D-logE slope of a curve.The γ value of D-logE curve is 34 among Fig. 4.For relatively, the γ value of the wet processing silver halide egative film of fast selecting is about 10 usually.Higher contrast ratio is an advantage for using in the figure field, because the half tone dot of high-contrast is required for constant hue curve controlled and new random screening process.Confers similar advantages is applicable in the printed circuit board (PCB) photograph instrument.
D-logE curve representation density among Fig. 4 is developed in about 0.9J/cm
2Place beginning and at maximal density (D
Max) the density saturation value located appears at 1.2J/cm
2As can be seen, for the specific scanner that is used for the thermal sensing element imaging, optimum image taking speed and scan exposure condition are unique.
To scan under each sample laser sensitometer (1) several different scanning speed in 20 to 60cm/s scopes of describing in the table 4 with Fig. 1.Calculate D-logE curve in the density data at 415nm place by Perkin Elmer microphotometer with taking from these lines.Model parameter in the above-mentioned optical density equation is by the D-logE curve determination and generally be listed in the table below in 5.
Table 5
MD E
o, 50=E
o, its value is taken from the D-logE curve, sweep velocity 20 cels (cm/s) mD E
Sat, 50=E
Sat, its value is taken from the D-logE curve, sweep velocity 20cm/smD D
Max, 50=maximal density, sweep velocity 20cm/smD D
Min, 50=minimum density, sweep velocity 20cm/s γ, the γ value mD E when the 50=sweep velocity is 20cm/s
o, 100=E
o, its value is taken from the D-logE curve, sweep velocity 40 cels (cm/s) mD E
Sat, 100=E
Sat, its value is taken from the D-logE curve, sweep velocity 40cm/smD D
Max, 100=maximal density, sweep velocity 40cm/smD D
Min, 100=minimum density, sweep velocity 40cm/s γ, the γ value γ when the 100=sweep velocity is 40cm/s, 100/ γ, 50=(the γ value during 40cm/s)/(the γ value during 20cm/s)
| Sample # | ????A | ????B | ????C | ????D | ????E |
| D max(415nm) | ????4.5 | ||||
| mD?Eo，50 | ????0.77 | ????0.85 | ????0.74 | ????0.93 | ????0.60 |
| mD?Esat，50 | ????1.30 | ????1.40 | ????1.40 | ????1.80 | ????1.23 |
| mD?Dmax，50 | ????3.50 | ????3.50 | ????3.65 | ????3.50 | ????3.60 |
| mD?Dmin，50 | ????0.85 | ????0.40 | ????0.55 | ????0.65 | ????0.80 |
| γ，50 | ????11.65 | ????14.30 | ????11.19 | ????9.93 | ????8.98 |
| mD?Eo，100 | ????0.966 | ????0.94 | ????0.96 | ????1.00 | ????1.03 |
| mD?Dsat，100 | ????1.27 | ????1.30 | ????1.26 | ????10.00 | ????1.32 |
| mD?Dmax，100 | ????3.5 | ????3.0 | ????3.4 | ????0.0 | ????3.6 |
| mD?Dmin，100 | ????0.80 | ????0.35 | ????0.80 | ????0.00 | ????0.80 |
| γ，100 | ????22.72 | ????18.82 | ????22.02 | ????0.00 | ????25.99 |
| γ100 /γ50 | ????1.95 | ????1.32 | ????1.97 | ????0.00 | ????2.89 |
| Sample # | ????F | ????I | ????J | ????K | ????L |
| Dmax(415nm) | |||||
| mD?E0，50 | ????0.65 | ????0.80 | ????1.13 | ????0.56 | ????0.35 |
| mD?Esat，50 | ????1.60 | ????1.26 | ????2.00 | ????1.30 | ????1.00 |
| mD?Dmax，50 | ????3.70 | ????3.60 | ????3.50 | ????3.70 | ????3.60 |
| mD?Dmin，50 | ????0.70 | ????0.40 | ????0.30 | ????0.60 | ????0.35 |
| γ，50 | ????7.80 | ????16.22 | ????12.90 | ????8.47 | ????7.12 |
| mD?Eo，100 | ????1.00 | ????0.90 | ????1.00 | ????0.66 | ????0.661 |
| mD?Dsat，100 | ????10.00 | ????1.16 | ????10.00 | ????1.00 | ????1.042 |
| mD?Dmax，100 | ????0.0 | ????3.5 | ????0.0 | ????3.6 | ????3.5 |
| mD?Dmin，100 | ????0.00 | ????0.30 | ????0.00 | ????0.70 | ????0.40 |
| γ，100 | ????0.00 | ????29.03 | ????0.00 | ????16.07 | ????15.88 |
| γ100 /γ50 | ????0.00 | ????1.79 | ????0.00 | ????1.90 | ????2.20 |
| Sample # | ????N | ????O |
| Dmax(415?nm) | ????5.00 | ????4.4 |
| mD?Eo，50 | ????0.95 | ????0.88 |
| mD?Esat，50 | ????1.65 | ????1.26 |
| mD?Dmax，50 | ????3.70 | ????3.80 |
| mD?Dmin，50 | ????0.70 | ????0.50 |
| γ，50 | ????12.51 | ????21.16 |
| mD?Eo，100 | ????0.96 | ????0.97 |
| mD?Dsat，100 | ????1.20 | ????1.26 |
| mD?Dmax，100 | ????3.7 | ????3.8 |
| mD?Dmin，100 | ????0.40 | ????0.50 |
| γ，100 | ????34.05 | ????29.05 |
| γ100 /γ50 | ????2.72 | ????1.37 |
The mean value E of sample A to L
oWhen sweep velocity 20cm/s, be 0.8 ± 0.2J/cm
2, when sweep velocity 40cm/s, be 0.9 ± 0.2J/cm
2The required minimum exposure energy of beginning density development is relatively independent of sweep velocity.E
SatValue is also irrelevant with speed.E
SatMean value when sweep velocity 20cm/s, be 1.3 ± 0.2J/cm
2, when sweep velocity 40cm/s, be 1.2 ± 0.1J/cm
2The evidence of γ value explanation imaging performance difference under these two speed.The average γ value of sample A to L is 12 ± 4J/cm when sweep velocity 20cm/s
2, when sweep velocity 40cm/s, be 24 ± 6J/cm
2Therefore show that the γ value increases obviously increase with sweep velocity.When sweep velocity was low, thermal diffusion was more remarkable, caused the sharpness on limit to reduce, and reduced the γ value of image thus.Different with the quick silver-colored medium of photo-thermal, the exposure effect of thermal sensitivity silver dollar spare more depends on conditions of exposure.
Sample C, I are coated with different Infrared dyes concentration with K.Sample C and I have 80% absorption at 826nm laser diode wavelength place.Sample K is applied to identical thickness, but the more Infrared dyes of load so absorbs 96% at the 826nm place.The average E of sample C and I
oAnd E
SatWhen sweep velocity 40cm/s, be respectively 0.93J/cm
2And 1.21J/cm
2The E of sample K
oAnd E
SatValue is respectively 0.66J/cm
2And 1.0J/cm
2The photonasty of egative film absorbs proof and slightly improves because of increasing by 16% layer.
Thin coating result is more remarkable.The coating thickness of sample D, J and L is half of thickness of C, I and K.Sample D and J only absorb about 50% incidenting laser radiation, not imaging when the 40cm/s sweep velocity.Sample L absorbs 85% incidenting laser radiation.The average E of D and J
oAnd E
SatValue is respectively 1.0J/cm when 20cm/s
2And 1.9J/cm
2, and the E of sample L
oAnd E
SatValue is respectively 0.35J/cm
2And 1.0J/cm
2The exposure energy value of L is lower than the exposure energy of D and J.Photonasty strengthens by increasing the laser absorption in the thermal sensitivity emulsion layer or passing through to increase Infrared dyes concentration.The limit of the imaging line that scans with 40cm/s in sample K and L is more smooth than the outer sample in other Shan Hong.
Have different-thickness, but the relatively proof with sample of similar percent absorption has the thinner layer of high IR dye strength more than the thicker easier sensitization of coating.The E of K
oAnd E
SatValue is respectively 0.56J/cm when 20cm/s
2And 1.3J/cm
2, and the E of L
oAnd E
SatValue is respectively 0.35J/cm
2And 1.0J/cm
2The thickness of sample L is half of K, but its absorbs 85% laser emission, it basically with K quite.The concentration that increases Infrared dyes can cause ablation because of the peak temperature that raises in the heat-sensitive layer.The photonasty that contains single thermal sensitivity silver emulsion layer of Infrared dyes can increase to greatest extent by the thin as far as possible thermal sensitivity silver emulsion layer with accessible high IR dye strength of coating, keeps required maximal density simultaneously.
The quality of imaging line is subjected to the influence of the ratio of resin and silver.Shown in sample A, C and E in the table 5, the not obvious influence that is subjected to the ratio variation of resin and silver of exposure energy value and γ value.Yet, the microphoto proof resin of these samples and the quality of image of the scale effect line of silver.Along with the ratio of resin with silver reduces, the edge roughening of line and uneven, the horizontal and vertical density uniformity of imaging line reduces simultaneously.Reduce resin concentration and answer the photonasty of reinforcing material, reason is to heat less discrete material.Yet this advantage can be offset in rough limit.Resin is preferably about 25-50wt% with the ratio of silver.
Another embodiment of the present invention comprises in the layer of Infrared dyes adding adjacent to thermal sensitivity silver emulsion layer.Sample N, O among the embodiment 16, G, H and P estimate the effect that adds Infrared dyes in the finish paint of thermal sensing element.Because some unknown reason, sample M, G become aberration with H, therefore are not included in the table 4.Compare with the sample that only contains Infrared dyes in the thermal sensitivity layer, sample N, O and P show improved line mass.Thermal sensitivity silver layer in sample N, O and the P Scripset that contains the high concentration Infrared dyes
TMThe resin face is coated with the thick coating of 0.05mm.The pressure sensitive adhesive strap is used for the thermal sensitivity emulsion layer is separated with finish paint to prove two-layer not fusion.The γ value of sample N and O at sweep velocity 40cm/s respectively greater than 34 and 30.These γ values can be compared with conventional silver halide duplicate film.In order to contrast, the γ value of conventional fast selecting silver halide egative film is about 10.The performance of sample P and N and O are similar, although do not calculate the D-logE curve of this sample.Sample N and O present the clear fair line limit with about 1 μ m edge roughness.The sample that only contains Infrared dyes in the thermal sensitivity silver layer has more coarse limit than sample N and O.The density uniformity of sample N, O and P is in ± 5% scope.The photonasty of sample N and O can with the analogy of the finish paint sample that does not contain Infrared dyes.In sample N, O and P, do not observe ablation.Can improve limit contrast, limit sharpness and density uniformity by in the layer adjacent, adding Infrared dyes with the thermal sensitivity silver layer.Simultaneously, in this structure, also can avoid ablation phenomen.The concentration of Infrared dyes in the thermal sensitivity silver layer should make heat-sensitive layer that the absorption of laser emission preferably is less than or equal to 40%, is more preferably less than or equals 35%.
Fig. 5 represents imaging (8) and not imaging (background) (9) transmittance spectrum of embodiment 16 sample N.Enhancing Infrared dyes absorption peak at the 820nm place is very tangible.Density at laser diode wavelength 826nm place increases to 1.26 (transmitances 5.5%) from 0.84 (transmitance, 14.5%), and the density at 415nm place increases to 5.0 (transmissivity is near 0) from 0.355 (transmissivity 44.2%) simultaneously.The elemental silver that forms in heat-sensitive layer in the exposure process provides enhanced absorption poor in ultraviolet (UV) line, and this is favourable for using in the UV mask.In the table 5, by the D of microphotometer measurement
MaxBe 3.7, be lower than the value that records with spectrophotometer.Obviously, can be limited to about 3.7 by the maximum optical density that microphotometer is measured.This shows in the γ value of calculating in the table 5 many actual values that are lower than, and therefore should be taken as conservative estimated value.
In order relatively to have very little or not have the imaging characteristic of the thermal sensing element of dissipation of heat influence, be used in 150 luminous milliwatts of 811nm place (is 110 milliwatts at image plane) laser diode (SDL-5422 is available from Spectra Diode Labs) and make embodiment 1,2,3,4,5,6 and 16 (sample N) imaging.Focus the laser beam on the 8mm spot definition (at 1/e
2Amount place overall with) and with 213cm/s sweep velocity and the interval scan of 4.5mm horizontal scan line.Table 6 is generally listed the result of this evaluation.
Table 6
| Embodiment | ??Dmax， ??365nm | ??Dmin， ??365nm | ??Dmax- ??Dmin， ??365nm | ??Dmax， ??415nm | ??Dmin， ??415nm | ??Dmax- ??Dmin， ??415nm |
| ????1 | ??2.17 | ??0.31 | ??1.85 | ??2.48 | ??0.25 | ??2.23 |
| ????2 | ??2.58 | ??0.39 | ??2.19 | ??2.94 | ??0.29 | ??2.65 |
| ????3 | ??1.78 | ??0.39 | ??1.39 | ??1.85 | ??0.29 | ??1.56 |
| ????4 | ??3.05 | ??0.63 | ??2.42 | ??3.13 | ??0.57 | ??2.56 |
| ????5 | ??4.50 | ??0.57 | ??3.93 | ??5.00 | ??0.42 | ??4.58 |
| ????6 | ??4.04 | ??0.90 | ??3.14 | ??5.00 | ??0.59 | ??4.01 |
| 16, sample N | ??4.40 | ??0.47 | ??3.92 | ??5.00 | ??0.53 | ??4.46 |
Digital proof in the table, (embodiment 16 in the time of in lauric acid silver being used in combination (embodiment 5 and 6) in the thermal sensitivity silver emulsion with barbituric acid or the sour methyl esters of higher concentration prepared burden with Yushan Hill Yu Yin acid, sample N), make the egative film of higher contrast (Dmax-Dmin).Use in order to provide machinable UV to shrink, contrast is preferably greater than about 2.50.These data also prove, add the speed that benzotriazole can suppress egative film; Yet the speed reduction can reduce to minimum when lauric acid silver is used as silver-colored soap.As shown in table 1, in the thermal sensitivity silver emulsion, add benzotriazole, though the speed that can be observed has reduction slightly, provide the advantage of improving light stability.
By top disclosing, under the spirit and scope of the invention condition of not leaving the claim qualification, can carry out various reasonable change and improvement.
Claims (45)
1. heat-sensitive imaging element, be included in the base material that scribbles thermosensitive imaging system at least one surface, this thermosensitive imaging system comprises the one deck at least that contains following component: non-photosensitivity organic silver salts, silver ion with reductive agent, bonding agent, toner and in wavelength coverage 750-1100nm the dyestuff of absorbed radiation, wherein said one deck at least that comprises described non-photosensitivity organic silver salts is when at 0.10-2.0J/cm
2Radiation forms the image density greater than about 1.0 when exposing the 0.20-200 microsecond down.
2. the element of claim 1, wherein said image density be greater than about 2.00, and comprise argent.
3. the element of claim 1, wherein said image density be greater than about 2.50, and comprise argent.
4. the element of claim 1, wherein said image density be greater than about 2.75, and comprise argent.
5. the element of claim 1, wherein said dyestuff is absorbed radiation in wavelength 750 to 900nm scopes.
6. the element of claim 1, wherein said thermosensitive imaging system further comprises development accelerant.
7. the element of claim 1, wherein said non-photosensitivity organic salt is the silver salt that contains the carboxylic acid of 10-30 carbon atom.
8. the element of claim 7, wherein said silver salt Wei behenic acid silver or lauric acid silver.
9. the element of claim 6, wherein said development accelerant is selected from:
(i) the 3-indazole quinoline ketonic compound of following formula institute formula:
Wherein R is selected from following group: the alkyl of hydrogen, 1 to 4 carbon atom, halogen ,-COOH and R
1COOH, wherein R
1For having the alkyl of 1 to 4 carbon atom; With
The (ii) carbamide compound shown in the following formula:
R wherein
2And R
3Represent hydrogen, C independently of one another
1-C
10Alkyl or cycloalkyl or phenyl, or R
2And R
3Form together and contain the heterocyclic group of 6 annular atomses at the most.
10. the element of claim 9, wherein R represents hydrogen, R
2And R
3Represent C independently of one another
1-C
5Alkyl or cycloalkyl or phenyl, or R
2And R
3Form together and contain the heterocyclic group of 5 annular atomses at the most.
11. the element of claim 1, wherein said toner be for being selected from 2,3-phthalazone, 2, at least a in 3-benzodiazine, barbituric acid, succinimide and the phthalimide.
12. heat-sensitive imaging element, comprise the base material that scribbles thermosensitive imaging system, described thermosensitive imaging system comprises at least two adjacent layers, one of them described adjacent layer comprise non-photosensitivity organic silver salts, silver ion with reductive agent, toner, bonding agent and non-essential in the about 750-1100nm of wavelength coverage the dyestuff of absorbed radiation, described another layer basically by bonding agent and in the about 750-1100nm of wavelength coverage the dyestuff of absorbed radiation form, the wherein said layer that comprises the non-photosensitivity organic silver salts is when at 0.10-2.0J/cm
2Described radiation forms the image density greater than about 1.0 when exposing the 0.20-200 microsecond down.
13. the element of claim 12, wherein said non-photosensitivity organic salt is the silver salt that contains the carboxylic acid of 10-30 carbon atom.
14. the element of claim 12, the silver salt Wei behenic acid silver or the lauric acid silver of wherein said carboxylic acid.
15. the element of claim 12, wherein said thermosensitive imaging system further comprises development accelerant.
16. the element of claim 15, wherein said development accelerant is selected from:
(i) the 3-indazole quinoline ketonic compound shown in the following formula:
Wherein R is selected from following group: the alkyl of hydrogen, 1 to 4 carbon atom, halogen ,-COOH and R
1COOH, wherein R
1For having the alkyl of 1 to 4 carbon atom;
The carbamide compound that (ii) is shown below:
R wherein
2And R
3Represent hydrogen, C independently of one another
1-C
10Alkyl or cycloalkyl or phenyl, or R
2And R
3Form together and contain the heterocyclic group of 6 annular atomses at the most.
17. the element of claim 16, wherein R represents hydrogen, R
2And R
3Represent C independently of one another
1-C
5Alkyl or cycloalkyl or phenyl, or R
2And R
3Form together and contain the heterocyclic group of 5 annular atomses at the most.
18. the element of claim 12, wherein said dyestuff is absorbed radiation in about 750 to the 900nm scopes of wavelength.
19. the element of claim 12, wherein said image density be greater than about 2.00, and comprise argent.
20. the element of claim 12, wherein said image density be greater than about 2.50, and comprise argent.
21. the element of claim 12, wherein said image density be greater than about 2.75, and comprise argent.
22. the element of claim 12, wherein said toner be for being selected from 2,3-phthalazone, 2, at least a in 3-benzodiazine, barbituric acid, succinimide and the phthalimide.
23. method that forms image, comprise step with heat-sensitive imaging element radiant exposure in the about 750-1100nm of wavelength coverage, described image-forming component comprises the base material that scribbles thermosensitive imaging system, described thermosensitive imaging system comprises the one deck at least that contains following component: non-photosensitivity organic silver salts, silver ion with reductive agent, in the about 750-1100nm of wavelength coverage dyestuff, toner and the bonding agent of absorbed radiation, described one deck at least that comprises the non-photosensitivity organic silver salts is when at 0.10-2.0J/cm
2Radiation forms the image density greater than about 1.0 when exposing the 0.20-200 microsecond down.
24. the method for claim 23, wherein said non-photosensitivity organic salt is the silver salt that contains the carboxylic acid of 10-30 carbon atom.
25. the method for claim 24, the silver salt Wei behenic acid silver or the lauric acid silver of wherein said carboxylic acid.
26. the method for claim 23, wherein said thermosensitive imaging system further comprises development accelerant.
27. the method for claim 26, wherein said development accelerant is selected from: (i) the 3-indazole quinoline ketonic compound shown in the following formula:
Wherein R is selected from following group: the alkyl of hydrogen, 1 to 4 carbon atom, halogen ,-COOH and R
1COOH, wherein R
1For having the alkyl of 1 to 4 carbon atom;
The (ii) carbamide compound shown in the following formula:
R wherein
2And R
3Represent hydrogen, C independently of one another
1-C
10Alkyl or cycloalkyl or phenyl, or R
2And R
3Form together and contain the heterocyclic group of 6 annular atomses at the most.
28. the method for claim 27, wherein R represents hydrogen, R
2And R
3Represent C independently of one another
1-C
5Alkyl or cycloalkyl or phenyl, or R
2And R
3Form together and contain the heterocyclic group of 5 annular atomses at the most.
29. the method for claim 23, wherein said dyestuff is absorbed radiation in about 750 to the 900nm scopes of wavelength.
30. the method for claim 23, wherein said image density be greater than about 2.00, and comprise argent.
31. the method for claim 23, wherein said image density be greater than about 2.50, and comprise argent.
32. the method for claim 23, wherein said image density be greater than about 2.75, and comprise argent.
33. the method for claim 23, wherein said toner be for being selected from 2,3-phthalazone, 2, at least a in 3-benzodiazine, barbituric acid, succinimide and the phthalimide.
34. method that forms image, comprise step with heat-sensitive imaging element radiant exposure in the about 750-1100nm of wavelength coverage, described image-forming component comprises the base material that scribbles thermosensitive imaging system, described thermosensitive imaging system comprises at least two adjacent layers, one of them described adjacent layer comprises the non-photosensitivity organic silver salts, the silver ion reductive agent, toner, bonding agent and non-essential in the about 750-1100nm of wavelength coverage the dyestuff of absorbed radiation, another layer basically by bonding agent and in the about 750-1100nm of wavelength coverage the dyestuff of absorbed radiation form, described radiation is before the adjacent layer that irradiation is made up of the dyestuff of bonding agent and absorbed radiation basically, through comprising the described heat-sensitive imaging element of layer irradiation of non-photosensitivity organic silver salts, the layer that comprises the non-photosensitivity organic silver salts like this is when at 0.10-2.0J/cm
2Radiation forms the image density greater than about 1.0 when exposing 0.2 0-200 microsecond down.
35. the method for claim 34, wherein said non-photosensitivity organic silver salts is the silver salt that contains the carboxylic acid of 10-30 carbon atom.
36. the method for claim 34, the silver salt Wei behenic acid silver or the lauric acid silver of wherein said carboxylic acid.
37. the method for claim 34, wherein said thermosensitive imaging system further comprises development accelerant.
38. the method for claim 37, wherein said development accelerant is selected from:
(i) the 3-indazole quinoline ketonic compound shown in the following formula:
Wherein R is selected from following group: the alkyl of hydrogen, 1 to 4 carbon atom, halogen ,-COOH and R
1COOH, wherein R
1For having the alkyl of 1 to 4 carbon atom; With
The (ii) carbamide compound shown in the following formula:
R wherein
2And R
3Represent hydrogen, C independently of one another
1-C
10Alkyl or cycloalkyl or phenyl, or R
2And R
3Form together and contain the heterocyclic group of 6 annular atomses at the most.
39. the method for claim 38, wherein R represents hydrogen, R
2And R
3Represent C independently of one another
1-C
5Alkyl or cycloalkyl or phenyl, or R
2And R
3Form together and contain the heterocyclic group of 5 annular atomses at the most.
40. the method for claim 34, wherein said dyestuff is absorbed radiation in wavelength 750 to 900nm scopes.
41. the method for claim 34, wherein said image density be greater than about 2.00, and comprise argent.
42. the method for claim 34, wherein said image density be greater than about 2.50, and comprise argent.
43. the method for claim 34, wherein said image density is greater than about 2.75.
44. the method for claim 34, wherein said toner be for being selected from 2,3-phthalazone, 2, at least a in 3-benzodiazine, barbituric acid, succinimide and the phthalimide.
45. according to the method for claim 34, the dyestuff of the radiation in the about 750-1100nm wavelength of wherein said absorption is present in two adjacent layers.
Applications Claiming Priority (2)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| US31301194A | 1994-09-27 | 1994-09-27 | |
| US08/313,011 | 1994-09-27 |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1158660A true CN1158660A (en) | 1997-09-03 |
Family
ID=23213996
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN95195324A Pending CN1158660A (en) | 1994-09-27 | 1995-08-01 | Laser addressable thermographic elements |
Country Status (10)
| Country | Link |
|---|---|
| EP (1) | EP0783726B1 (en) |
| JP (1) | JPH10506339A (en) |
| KR (1) | KR970706523A (en) |
| CN (1) | CN1158660A (en) |
| BR (1) | BR9509042A (en) |
| CA (1) | CA2197469A1 (en) |
| DE (1) | DE69515496T2 (en) |
| IL (1) | IL115056A0 (en) |
| MX (1) | MX9702044A (en) |
| WO (1) | WO1996010213A1 (en) |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102275399A (en) * | 2010-06-08 | 2011-12-14 | 何仁城 | Temperature-sensitive printing method and apparatus utilizing light |
| CN101750870B (en) * | 2008-12-17 | 2012-05-30 | 中国科学院理化技术研究所 | Application of niacin compound serving as toner in direct thermographic material |
| CN112882335A (en) * | 2021-01-08 | 2021-06-01 | 中国乐凯集团有限公司 | Silver-containing thermosensitive imaging layer, thermosensitive printing medical film and preparation method thereof |
| CN112882335B (en) * | 2021-01-08 | 2024-05-14 | 中国乐凯集团有限公司 | Silver-containing thermosensitive imaging layer, thermosensitive printing medical film and preparation method thereof |
Families Citing this family (19)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5780483A (en) * | 1995-02-17 | 1998-07-14 | Smithkline Beecham Corporation | IL-8 receptor antagonists |
| EP0809492A4 (en) | 1995-02-17 | 2007-01-24 | Smithkline Beecham Corp | Il-8 receptor antagonists |
| GB2305509A (en) * | 1995-09-19 | 1997-04-09 | Minnesota Mining & Mfg | Heat sensitive elements |
| US6005008A (en) * | 1996-02-16 | 1999-12-21 | Smithkline Beecham Corporation | IL-8 receptor antagonists |
| US6211373B1 (en) | 1996-03-20 | 2001-04-03 | Smithkline Beecham Corporation | Phenyl urea antagonists of the IL-8 receptor |
| US6262113B1 (en) | 1996-03-20 | 2001-07-17 | Smithkline Beecham Corporation | IL-8 receptor antagonists |
| DE69734077T2 (en) | 1996-05-21 | 2006-06-29 | Agfa-Gevaert | Production process for a thermographic recording material with increased stability and improved image tone |
| EP0809142B1 (en) * | 1996-05-21 | 2005-08-31 | Agfa-Gevaert | Production process for a thermographic recording material with improved stability and image-tone |
| US6133319A (en) * | 1996-06-27 | 2000-10-17 | Smithkline Beecham Corporation | IL-8 receptor antagonists |
| EP0915651A4 (en) | 1996-06-27 | 2001-10-24 | Smithkline Beecham Corp | Il-8 receptor antagonists |
| US5840469A (en) * | 1997-05-13 | 1998-11-24 | Imation Corp. | Gallic acid as a laser direct thermal developer |
| US6348308B1 (en) | 1997-09-03 | 2002-02-19 | Agfa-Gevaert | Substantially light-insensitive thermographic recording material with improved stability and image-tone |
| EP1006403B1 (en) * | 1998-11-30 | 2004-10-20 | Agfa-Gevaert | Use of direct thermal transparent imaging materials including an organic silver salt for producing labels |
| US6908731B2 (en) | 2002-11-14 | 2005-06-21 | Agfa-Gevaert | Stabilizers for use in substantially light-insensitive thermographic recording materials |
| US7060655B2 (en) | 2002-11-14 | 2006-06-13 | Agfa Gevaert | Stabilizers for use in substantially light-insensitive thermographic recording materials |
| US6902880B2 (en) | 2002-11-14 | 2005-06-07 | Agfa-Gevaert | Stabilizers for use in substantially light-insensitive thermographic recording materials |
| US7018786B2 (en) | 2002-12-19 | 2006-03-28 | Agfa Gevaert | Toning agents for use in thermographic recording materials |
| ITSV20060002A1 (en) * | 2006-01-19 | 2007-07-20 | Ferrania Technologies Spa | FLUORESCENT DYE OF CIANIN TYPE |
| US7582403B2 (en) * | 2006-07-17 | 2009-09-01 | E. I. Du Pont De Nemours And Company | Metal compositions, thermal imaging donors and patterned multilayer compositions derived therefrom |
Family Cites Families (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| DE69310045T2 (en) * | 1992-08-03 | 1997-12-11 | Minnesota Mining & Mfg | Laser addressable heat sensitive recording material |
-
1995
- 1995-08-01 EP EP95927547A patent/EP0783726B1/en not_active Expired - Lifetime
- 1995-08-01 KR KR1019970702019A patent/KR970706523A/en not_active Application Discontinuation
- 1995-08-01 BR BR9509042A patent/BR9509042A/en not_active Application Discontinuation
- 1995-08-01 JP JP8511726A patent/JPH10506339A/en active Pending
- 1995-08-01 DE DE69515496T patent/DE69515496T2/en not_active Expired - Fee Related
- 1995-08-01 MX MX9702044A patent/MX9702044A/en unknown
- 1995-08-01 WO PCT/US1995/009659 patent/WO1996010213A1/en not_active Application Discontinuation
- 1995-08-01 CN CN95195324A patent/CN1158660A/en active Pending
- 1995-08-01 CA CA002197469A patent/CA2197469A1/en not_active Abandoned
- 1995-08-24 IL IL11505695A patent/IL115056A0/en unknown
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101750870B (en) * | 2008-12-17 | 2012-05-30 | 中国科学院理化技术研究所 | Application of niacin compound serving as toner in direct thermographic material |
| CN102275399A (en) * | 2010-06-08 | 2011-12-14 | 何仁城 | Temperature-sensitive printing method and apparatus utilizing light |
| CN112882335A (en) * | 2021-01-08 | 2021-06-01 | 中国乐凯集团有限公司 | Silver-containing thermosensitive imaging layer, thermosensitive printing medical film and preparation method thereof |
| CN112882335B (en) * | 2021-01-08 | 2024-05-14 | 中国乐凯集团有限公司 | Silver-containing thermosensitive imaging layer, thermosensitive printing medical film and preparation method thereof |
Also Published As
| Publication number | Publication date |
|---|---|
| KR970706523A (en) | 1997-11-03 |
| MX9702044A (en) | 1997-06-28 |
| CA2197469A1 (en) | 1996-04-04 |
| WO1996010213A1 (en) | 1996-04-04 |
| DE69515496T2 (en) | 2000-09-14 |
| BR9509042A (en) | 1997-09-30 |
| EP0783726A1 (en) | 1997-07-16 |
| DE69515496D1 (en) | 2000-04-13 |
| IL115056A0 (en) | 1995-12-08 |
| EP0783726B1 (en) | 2000-03-08 |
| JPH10506339A (en) | 1998-06-23 |
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