CN1932641A - Plate shape silver halide emulsion adapted to ray photography, producing method and use thereof - Google Patents
Plate shape silver halide emulsion adapted to ray photography, producing method and use thereof Download PDFInfo
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- CN1932641A CN1932641A CN 200510086439 CN200510086439A CN1932641A CN 1932641 A CN1932641 A CN 1932641A CN 200510086439 CN200510086439 CN 200510086439 CN 200510086439 A CN200510086439 A CN 200510086439A CN 1932641 A CN1932641 A CN 1932641A
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- silver halide
- halide emulsion
- plate shape
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- salt
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Abstract
This invention particularly relates to the high-energy radiography, the high sensitivity, high contrast of the silver halide emulsion coating plate's photosensitive materials which the high-speed photographic technique uses and the silver halide emulsion's preparation method and its use. The stated silver halide emulsion contains the iodine silver bromide which has the silver bromide as the main part, the proportion of the Br and I is 95~98%mol to 5~2%mol, the weight proportion of the photo indolent glue and the silver is 0.7 ~ 1.5 to 1, the iridium salt and rhodium salt or strontium salt's concentration is10-3~10-6mol/molAgBrI, the particle size is 1.5-2.0 mum.. The double beam emulsion preparation method which adopts the computer control uses the silver halide as the main iodine silver bromide crystallite emulsion, on the emulsification or the chemical.
Description
Technical field
The invention belongs to the image science and technology field, particularly relate to the photosensitive material of the plate shape silver halide emulsion coating of high-energy ray photography, ISO that high speed photography uses, hard contrast, and the preparation method of plate shape silver halide emulsion and purposes.
Background technology
External extraordinary ray photosensitive material (medical, industrial, scientific research with) various in style, performance are different, and the fertile scientific research of Kodak just reaches kind more than 20 with radiographic film.In the research of high-speed photography, nuclear explosion ballistic trajectory and life process, solve the high illumination reciprocity failure of film, require high light sensitivity.Use the photographic film of long-time weak light source, the essential low-light (level) reciprocity failure that solves film requires high detective quantum efficiency.In the development of ray photosensitive material, what solve is how high energy particle and nuclear blast Hong the various signal records that produced to be got off.Extraordinary radiographic film has been indispensable instrument and means in many productions, scientific research and the military project research field.As Wang Yongming at " photosensitive material " 1998, (6) .41～45 " present situation of homemade medical X-ray film and development trend "; Cui Haiping etc. are at " chemistry circular " VOL.68, w025,2005 " in the silver emulsion preparations metallic ion and complex doped dose "; Jap.P. JP7219102-A is disclosed.
China is also lagging behind far away aspect the radiographic film research abroad, particularly ISO, high definition radiographic film.At present, China can only produce medical, industrial radiographic film, and product variety is single, and quality and the big gap of external like product existence.The research of ISO, high definition radiographic film is blank especially at home with production.
Summary of the invention
The object of the invention one is to provide the plate shape silver halide emulsion that is applicable to that radiography is used, with secondary electron ability to accept and the raising silver-colored hiding rare of increase silver emulsion to the intensifying screen radiation, thus the light sensitivity of raising film.
The object of the invention two is to provide the preparation method of the plate shape silver halide emulsion that is applicable to that radiography is used according to silver halide precipitation procedural theory and control crystal technique.
The object of the invention three is to provide the purposes of the plate shape silver halide emulsion that is applicable to that radiography is used.
The present invention is applicable to the plate shape silver halide emulsion that radiography is used, and is the rare metal that mixes in plate shape silver halide emulsion, to improve the ability to accept of silver emulsion to the secondary electron radiation.
The present invention is applicable to the silver emulsion (iodine silver bromide emulsion) that contains in the plate shape silver halide emulsion that radiography uses based on silver bromide, distribution of particles uniformly the size of plate shape silver halide emulsion particle at 1.5～2.0 μ m.
Wherein, the Br in the plate shape silver halide emulsion: I is 95～98%mol: 5～2%mol, and the weight ratio of take a picture lazy glue and silver is 0.7～1.5: 1; Iridium salt (ammonium chloroiridate), rhodium salt (chlorine rhodium acid ammonium (NH
4)
3RhCl
6) or strontium salt (SrCl
2) concentration 10
-3～10
-6Mol/molAgBrI.
The present invention is applicable to that the preparation method of the plate shape silver halide emulsion that radiography is used may further comprise the steps:
(1) add take a picture lazy glue, potassium iodide and ammonium bromide in reaction pot and obtain potpourri, wherein, the concentration expressed in percentage by weight of the lazy glue of taking a picture in the potpourri is 2～5%, and the concentration of potassium iodide is 0.018～0.03mol, and the concentration of ammonium bromide is 0.05～0.1mol;
(2) preparation 1～2mol liquor argenti nitratis ophthalmicus and 1～2mol ammonium bromide solution;
(3) material that step (1) and step (2) are obtained according to the flow velocity of setting, prepares plate shape silver halide emulsion by computer-controlled two emulsification instruments of annotating.The temperature range of emulsification is at 50 ℃～70 ℃, emulsification times 50～70 minutes, and PAg is controlled at 6.8～10.0, and stirring rate is 1500 to change～2500 rev/mins; After emulsification finished, sedimentation (making its sedimentation as the kayexalate that adds 5～10wt% and the acetic acid of 5～10wt%) washing added the lazy glue remelt of taking a picture; Take a picture lazy glue with silver weight ratio be 0.7～1.5: 1;
Remelt emulsion is adjusted pH=6～6.8 with 5～10wt% acetic acid or 5～10wt% sodium carbonate down at 40～50 ℃, adjust PAg=8.4～9 with 2～10wt% potassium bromide, adding sulphur aurification sensitizer (the golden volume ratio of sulphur be preferably 1: 2～5) carries out chemical ripening and adds stabilizing agent (5-methyl-7-hydroxyl-1 after 60～120 minutes, 3,4-three nitrogen Yin Duo Li piperazines), stop chemical ripening; Be cooled to then below 40 ℃, the emulsion cooling is standby; In the emulsion preparation process or in the chemical ripening process, add iridium salt (ammonium chloroiridate), rhodium salt (chlorine rhodium acid ammonium (NH
4)
3RhCl
6) or strontium salt (SrCl
2), iridium salt, rhodium salt or the concentration of strontium salt in plate shape silver halide emulsion are 10
-3～10
-6Mol/AgBrImol.
Described sulphur aurification sensitizer is that sodium thiosulfate, gold chloride and ammonium thiocyanate mix the chemical sensitizer that forms complex compound.
Plate shape silver halide emulsion of the present invention adds coating additive (surfactant, antifoggant, antistatic agent, stabilizing agent etc.) in use, paints the ray film of double emulsion layer on extrusion coating machine.
The invention has the advantages that: plate shape silver halide emulsion provided by the present invention, light sensitivity can reach 33DIN, uses the film of this silver emulsion coating, can be used for high-technology fields such as high-speed photography, high energy strobo photography.
Description of drawings
Fig. 1. the plate shape silver halide emulsion particle electromicroscopic photograph of the embodiment of the invention 1.
Embodiment
The invention will be further described below in conjunction with comparative example and embodiment.
Comparative example 1
Two emulsification instruments of annotating of appliance computer control prepare silver emulsion, are example with two kilograms of emulsification prescriptions.Take by weighing 16 gram lazy glue of photograph and 800 ml deionized water, add in the reaction pot, and adding potassium iodide 2.0 restrains and ammonium bromide 4.0 grams obtain potpourri, wherein, the concentration expressed in percentage by weight of the lazy glue of photograph is 2～5% in the potpourri, the concentration of potassium iodide is 0.018～0.03mol, and the concentration of ammonium bromide is 0.05～0.1mol.Other prepares 2mol liquor argenti nitratis ophthalmicus and 2mol ammonium bromide solution, the PAg of emulsion process (electrode potential of emulsion) is controlled at 6.8～10.0, emulsifying temperature is controlled at 50 ℃～70 ℃, stirring rate is～2500 rev/mins of 1500 commentaries on classics, inject liquor argenti nitratis ophthalmicus and ammonium bromide solution with infusion pump with the two beam speed of 5.0 ml/min, emulsification times is 50 minutes～70 minutes, obtain tabular iodine silver bromide emulsion, its average-size is 1.5～2.0 μ m, after emulsification finishes, with emulsion cooling and add sinking agent--16 milliliters of 10% kayexalates and 10% an amount of acetic acid make its sedimentation, treat that the sedimentation mother liquor washes four times after limpid again, add the lazy glue of taking a picture then and carry out remelt, glue is silver-colored in transferring to 1.0, add 10% sodium carbonate and regulate pH=6～6.5 and 2% potassium bromide adjusting PAg=8.4～9.0, the emulsion remelt is stirred, it is standby to stop to stir cooling emulsion at last.
Get emulsion 100 grams of remelt, use acetic acid, sodium carbonate and bromide are regulated pH=6.5, PAg=8.4; Under 50 ℃, carry out sulphur aurification sensitizing, 2 milliliters of 0.5 milliliter in 0.1% sodium thiosulfate and 0.0167% gold chlorides, 2 milliliters of maturations of 0.2% ammonium thiocyanate 100 minutes, add stabilizing agent 2%5-methyl-7-hydroxyl-1,3,1.5 milliliters of 4-three nitrogen Yin Duo Li piperazines, 50% phenol 0.5 milliliter (antiseptic) stops chemical ripening, be cooled to 40 ℃ of adding 0.01%B114-3 dyestuffs then and carry out spectral sensitization (to green light sensitive), adsorb smear after 30 minutes, the emulsion cooling is standby.
We use the small-sized coating machine in laboratory, and the emulsion after the sensitizing is added the coating additive, 2%5-methyl-7-hydroxyl-1,3, and 2.0 milliliters of 4-three nitrogen Yin Duo Li piperazines, 0.5 milliliter of 0.1% tetrazole, 4%1,292 0.5 milliliters of coating weights are 8～16 gram silver/m
2, be coated with dry post-exposure, develop, photographic fixing, washing and drying is measured wedge density at different levels with densitometer again, calculates photosensitive property, and gained photosensitive property test result sees Table 1.
Embodiment 1
Two emulsification instruments of annotating of appliance computer control prepare silver emulsion, are example with two kilograms of emulsification prescriptions.
(1) takes by weighing 16 gram lazy glue of photograph and 800 ml deionized water, add in the reaction pot, and adding potassium iodide 2.0 restrains and ammonium bromide 4.0 grams obtain potpourri, wherein, the concentration expressed in percentage by weight of the lazy glue of photograph is 2～5% in the potpourri, the concentration of potassium iodide is 0.018～0.03mol, and the concentration of ammonium bromide is 0.05～0.1mol.
(2) preparation 2mol liquor argenti nitratis ophthalmicus and 2mol ammonium bromide solution;
(3) PAg of emulsion process (electrode potential of emulsion) is controlled at 6.8～10.0, emulsifying temperature is controlled at 50 ℃～70 ℃, stirring rate is～2500 rev/mins of 1500 commentaries on classics, the material that step (1) and step (2) obtain is mixed with the two beam speed of 5.0 ml/min with infusion pump, emulsification times is 50 minutes～70 minutes, obtain tabular iodine silver bromide emulsion, its average-size is 1.5～2.0 μ m; After emulsification finishes, with emulsion cooling and add sinking agent--16 milliliters of 10% kayexalates and 10% an amount of acetic acid make its sedimentation, treat that the sedimentation mother liquor washes four times after limpid again, add the lazy glue of taking a picture then and carry out remelt, glue silver than transferring to 1.0, is added 10% sodium carbonate and regulates pH=6～6.5, regulate PAg=8.4～9.0 with 2% potassium bromide, the emulsion remelt is stirred, and it is standby to stop to stir cooling emulsion at last.
Get emulsion 100 grams of remelt, with 5wt% acetic acid or 10wt% sodium carbonate and potassium bromide adjusting pH=6.5, PAg=8.4; Under 50 ℃, carry out sulphur aurification sensitizing, 2 milliliters of 0.5 milliliter in 0.1% sodium thiosulfate and 0.0167% gold chlorides, 2 milliliters of maturations of 0.2% ammonium thiocyanate 100 minutes add stabilizing agent 2%5-methyl-7-hydroxyl-1,3,1.5 milliliters of 4-three nitrogen Yin Duo Li piperazines, 0.5 milliliter of 50% phenol (antiseptic) stops chemical ripening, is cooled to 40 ℃ of adding 0.01%B114-3 dyestuffs then and carries out spectral sensitization (to green light sensitive), adsorb smear after 30 minutes, the emulsion cooling is standby.
In emulsifying stage (during total silver amount 80% left and right sides), add 5.0 * 10
-4～5.0 * 10
-7Mol (Ircl
6)
-3/ molAgBrI, 3.0 milliliters, other test condition is identical with comparative example 1, and gained photosensitive property test result sees Table 1.
Embodiment 2
The plate shape silver halide emulsion preparation method is substantially the same manner as Example 1, and different is in emulsifying stage (during total silver amount 50% left and right sides), adds 5.0 * 10
-4-5.0 * 10
-7Mol (Srcl
2)/AgBrImol, 2.0 milliliters, other test is identical with comparative example, and gained photosensitive property test result sees Table 1.
Embodiment 3
Different is to add photographic gelatin, potassium bromide, 5%mol ammonium bromide, 5.0 * 10 in reaction pot for plate shape silver halide emulsion preparation method and embodiment 1
-4-5.0 * 10
-7Mol (Ircl
6)
-3/ molAgBrI, 2.0 milliliters.Other control and test condition are all identical with embodiment 1, and gained photosensitive property test result sees Table 1.
Table 1
Claims (10)
1. plate shape silver halide emulsion that is applicable to that radiography is used, it is characterized in that: contain iodine silver bromide emulsion in the described plate shape silver halide emulsion based on silver bromide, Br: I is 95～98%mol: 5～2%mol, and the weight ratio of take a picture lazy glue and silver is 0.7～1.5: 1; The concentration of iridium salt, rhodium salt or strontium salt is 10
-3～10
-6Mol/molAgBrI.
2. plate shape silver halide emulsion according to claim 1 is characterized in that: the size of described plate shape silver halide emulsion particle is at 1.5～2.0 μ m.
3. plate shape silver halide emulsion according to claim 1 is characterized in that: described iridium salt is ammonium chloroiridate, and rhodium salt is chlorine rhodium acid ammonium, and strontium salt is strontium chloride.
4. the preparation method according to each described plate shape silver halide emulsion of claim 1～3 is characterized in that, described method may further comprise the steps:
(1) add take a picture lazy glue, potassium iodide and ammonium bromide in reaction pot and obtain potpourri, wherein, the concentration expressed in percentage by weight of the lazy glue of taking a picture in the potpourri is 2～5%, and the concentration of potassium iodide is 0.018～0.03mol, and the concentration of ammonium bromide is 0.05～0.1mol;
(2) preparation 1～2mol liquor argenti nitratis ophthalmicus and 1～2mol ammonium bromide solution;
(3) according to two beam speed of setting, with two emulsification instruments of annotating the material that step (1) and step (2) obtain is mixed, the temperature range of emulsification is at 50 ℃～70 ℃, and PAg is controlled at 6.8～10.0, after emulsification finishes, sedimentation washing, the lazy glue remelt of adding photograph; Take a picture lazy glue with silver weight ratio be 0.7～1.5: 1;
Remelt emulsion is adjusted pH=6～6.8 with acetic acid or sodium carbonate under 40～50 ℃, adjust PAg=8.4～9, add sulphur aurification sensitizer and carry out chemical ripening, add stabilizing agent then and stop chemical ripening with potassium bromide; Be cooled to below 40 ℃, the emulsion cooling, standby; Add iridium salt, rhodium salt or strontium salt in the emulsion preparation process or in the chemical ripening process, iridium salt, rhodium salt or the concentration of strontium salt in plate shape silver halide emulsion are 10
-3～10
-6Mol/AgBrImol.
5. method according to claim 4 is characterized in that: described emulsification times 50～70 minutes.
6. method according to claim 4 is characterized in that: described stirring rate is～2500 rev/mins of 1500 commentaries on classics.
7. method according to claim 4 is characterized in that: the concentration of described acetic acid is 5～10wt%; The concentration of sodium carbonate is 5～10wt%; The concentration of potassium bromide is 2～10wt%.
8. method according to claim 4 is characterized in that: described sulphur aurification sensitizer is that sodium thiosulfate, gold chloride and ammonium thiocyanate mix the chemical sensitizer that forms complex compound; Sulphur gold volume ratio is 1: 2～5.
9. method according to claim 4 is characterized in that: described stabilizing agent is 5-methyl-7-hydroxyl-1,3,4-three nitrogen Yin Duo Li piperazines.
10. purposes according to each described plate shape silver halide emulsion of claim 1～3, it is characterized in that: described plate shape silver halide emulsion is applied to be coated with the ray film.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510086439 CN1932641A (en) | 2005-09-16 | 2005-09-16 | Plate shape silver halide emulsion adapted to ray photography, producing method and use thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200510086439 CN1932641A (en) | 2005-09-16 | 2005-09-16 | Plate shape silver halide emulsion adapted to ray photography, producing method and use thereof |
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| Publication Number | Publication Date |
|---|---|
| CN1932641A true CN1932641A (en) | 2007-03-21 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101256346B (en) * | 2008-02-04 | 2010-09-29 | 黄山银江科技有限公司 | Method for producing laser photo film |
| CN101900930A (en) * | 2010-02-26 | 2010-12-01 | 天津美迪亚影像材料有限公司 | Flocculating agent composition for preparing ray emulsion and desalination and concentration method |
| CN102087466A (en) * | 2010-12-29 | 2011-06-08 | 天津美迪亚影像材料有限公司 | Implementation method for improving photographic sensitivity of silver chloro-bromide emulsion |
| CN102338981A (en) * | 2010-07-23 | 2012-02-01 | 中国科学院理化技术研究所 | Efficient sensibilization method suitable for platy silver halides particle emulsion |
-
2005
- 2005-09-16 CN CN 200510086439 patent/CN1932641A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101256346B (en) * | 2008-02-04 | 2010-09-29 | 黄山银江科技有限公司 | Method for producing laser photo film |
| CN101900930A (en) * | 2010-02-26 | 2010-12-01 | 天津美迪亚影像材料有限公司 | Flocculating agent composition for preparing ray emulsion and desalination and concentration method |
| CN101900930B (en) * | 2010-02-26 | 2013-11-06 | 天津美迪亚影像材料有限公司 | Flocculating agent composition for preparing ray emulsion and desalination and concentration method |
| CN102338981A (en) * | 2010-07-23 | 2012-02-01 | 中国科学院理化技术研究所 | Efficient sensibilization method suitable for platy silver halides particle emulsion |
| CN102087466A (en) * | 2010-12-29 | 2011-06-08 | 天津美迪亚影像材料有限公司 | Implementation method for improving photographic sensitivity of silver chloro-bromide emulsion |
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Open date: 20070321 |