CN106842807A - Chemical sensitization method of silver halide emulsion - Google Patents
Chemical sensitization method of silver halide emulsion Download PDFInfo
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- CN106842807A CN106842807A CN201510888466.4A CN201510888466A CN106842807A CN 106842807 A CN106842807 A CN 106842807A CN 201510888466 A CN201510888466 A CN 201510888466A CN 106842807 A CN106842807 A CN 106842807A
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- Prior art keywords
- silver
- chemical sensitization
- halogen
- gelatin solution
- barium fluoride
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- 229910052709 silver Inorganic materials 0.000 title claims abstract description 59
- 239000004332 silver Substances 0.000 title claims abstract description 59
- 206010070834 Sensitisation Diseases 0.000 title claims abstract description 52
- 230000008313 sensitization Effects 0.000 title claims abstract description 52
- 239000000839 emulsion Substances 0.000 title claims abstract description 51
- 239000000126 substance Substances 0.000 title claims abstract description 51
- 238000000034 method Methods 0.000 title claims abstract description 31
- -1 silver halide Chemical class 0.000 title claims abstract description 30
- 108010010803 Gelatin Proteins 0.000 claims abstract description 48
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims abstract description 48
- 229920000159 gelatin Polymers 0.000 claims abstract description 48
- 239000008273 gelatin Substances 0.000 claims abstract description 48
- 235000019322 gelatine Nutrition 0.000 claims abstract description 48
- 235000011852 gelatine desserts Nutrition 0.000 claims abstract description 48
- 229910052736 halogen Inorganic materials 0.000 claims abstract description 28
- 239000002245 particle Substances 0.000 claims abstract description 27
- 238000000498 ball milling Methods 0.000 claims abstract description 26
- 229910001632 barium fluoride Inorganic materials 0.000 claims abstract description 15
- 238000003756 stirring Methods 0.000 claims abstract description 8
- 229910052794 bromium Inorganic materials 0.000 claims abstract description 7
- 229910052801 chlorine Inorganic materials 0.000 claims abstract description 5
- 229910052740 iodine Inorganic materials 0.000 claims abstract description 4
- 150000002367 halogens Chemical class 0.000 claims description 12
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 claims description 11
- ADZWSOLPGZMUMY-UHFFFAOYSA-M silver bromide Chemical compound [Ag]Br ADZWSOLPGZMUMY-UHFFFAOYSA-M 0.000 claims description 9
- 239000000843 powder Substances 0.000 claims description 7
- 230000008859 change Effects 0.000 claims description 5
- 239000000460 chlorine Substances 0.000 claims description 5
- 238000003682 fluorination reaction Methods 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims description 5
- CBEQRNSPHCCXSH-UHFFFAOYSA-N iodine monobromide Chemical compound IBr CBEQRNSPHCCXSH-UHFFFAOYSA-N 0.000 claims description 2
- SDLBJIZEEMKQKY-UHFFFAOYSA-M silver chlorate Chemical compound [Ag+].[O-]Cl(=O)=O SDLBJIZEEMKQKY-UHFFFAOYSA-M 0.000 claims description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 2
- CSYKLDTVFRFMIT-UHFFFAOYSA-M [Ag]Br.[Cl] Chemical compound [Ag]Br.[Cl] CSYKLDTVFRFMIT-UHFFFAOYSA-M 0.000 claims 1
- OAAKZKGKPMPJIF-UHFFFAOYSA-N [Cl].[I] Chemical compound [Cl].[I] OAAKZKGKPMPJIF-UHFFFAOYSA-N 0.000 claims 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 abstract description 20
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 abstract description 18
- 229910052737 gold Inorganic materials 0.000 abstract description 18
- 239000010931 gold Substances 0.000 abstract description 18
- 229910052717 sulfur Inorganic materials 0.000 abstract description 18
- 239000011593 sulfur Substances 0.000 abstract description 18
- 229910052761 rare earth metal Inorganic materials 0.000 abstract description 5
- OYLGJCQECKOTOL-UHFFFAOYSA-L barium fluoride Chemical class [F-].[F-].[Ba+2] OYLGJCQECKOTOL-UHFFFAOYSA-L 0.000 abstract description 3
- 239000002019 doping agent Substances 0.000 abstract description 2
- 206010034960 Photophobia Diseases 0.000 abstract 1
- SOHDHMRBRGSXMV-UHFFFAOYSA-N [Ba].FOF Chemical compound [Ba].FOF SOHDHMRBRGSXMV-UHFFFAOYSA-N 0.000 abstract 1
- 230000008014 freezing Effects 0.000 abstract 1
- 238000007710 freezing Methods 0.000 abstract 1
- 208000013469 light sensitivity Diseases 0.000 abstract 1
- AYUUVHOACZVCBF-UHFFFAOYSA-K [F-].[Ba+2].[Br+].[F-].[F-] Chemical compound [F-].[Ba+2].[Br+].[F-].[F-] AYUUVHOACZVCBF-UHFFFAOYSA-K 0.000 description 25
- 230000001235 sensitizing effect Effects 0.000 description 16
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 description 13
- 229910052788 barium Inorganic materials 0.000 description 12
- FHOMZPIQIJQCHD-UHFFFAOYSA-K [I+].[F-].[Ba+2].[F-].[F-] Chemical compound [I+].[F-].[Ba+2].[F-].[F-] FHOMZPIQIJQCHD-UHFFFAOYSA-K 0.000 description 9
- 238000003384 imaging method Methods 0.000 description 7
- 239000000463 material Substances 0.000 description 7
- MCMNRKCIXSYSNV-UHFFFAOYSA-N ZrO2 Inorganic materials O=[Zr]=O MCMNRKCIXSYSNV-UHFFFAOYSA-N 0.000 description 5
- 230000010198 maturation time Effects 0.000 description 5
- 230000003287 optical effect Effects 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 230000009467 reduction Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000006185 dispersion Substances 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- 239000003795 chemical substances by application Substances 0.000 description 3
- 150000004820 halides Chemical class 0.000 description 3
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 2
- KRHYYFGTRYWZRS-UHFFFAOYSA-M Fluoride anion Chemical compound [F-] KRHYYFGTRYWZRS-UHFFFAOYSA-M 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 2
- 239000005864 Sulphur Substances 0.000 description 2
- 230000015572 biosynthetic process Effects 0.000 description 2
- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 2
- 229910001634 calcium fluoride Inorganic materials 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 238000004020 luminiscence type Methods 0.000 description 2
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 1
- 229910021607 Silver chloride Inorganic materials 0.000 description 1
- XEIPQVVAVOUIOP-UHFFFAOYSA-N [Au]=S Chemical compound [Au]=S XEIPQVVAVOUIOP-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000090 biomarker Substances 0.000 description 1
- WUKWITHWXAAZEY-UHFFFAOYSA-L calcium difluoride Chemical compound [F-].[F-].[Ca+2] WUKWITHWXAAZEY-UHFFFAOYSA-L 0.000 description 1
- 150000001735 carboxylic acids Chemical class 0.000 description 1
- 238000005957 chlorosulfonylation reaction Methods 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000000539 dimer Substances 0.000 description 1
- 239000003937 drug carrier Substances 0.000 description 1
- 238000000799 fluorescence microscopy Methods 0.000 description 1
- 239000012634 fragment Substances 0.000 description 1
- 238000011835 investigation Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000005259 measurement Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000005424 photoluminescence Methods 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 238000002601 radiography Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 150000003378 silver Chemical class 0.000 description 1
- HKZLPVFGJNLROG-UHFFFAOYSA-M silver monochloride Chemical compound [Cl-].[Ag+] HKZLPVFGJNLROG-UHFFFAOYSA-M 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 230000003595 spectral effect Effects 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
Classifications
-
- G—PHYSICS
- G03—PHOTOGRAPHY; CINEMATOGRAPHY; ANALOGOUS TECHNIQUES USING WAVES OTHER THAN OPTICAL WAVES; ELECTROGRAPHY; HOLOGRAPHY
- G03C—PHOTOSENSITIVE MATERIALS FOR PHOTOGRAPHIC PURPOSES; PHOTOGRAPHIC PROCESSES, e.g. CINE, X-RAY, COLOUR, STEREO-PHOTOGRAPHIC PROCESSES; AUXILIARY PROCESSES IN PHOTOGRAPHY
- G03C1/00—Photosensitive materials
- G03C1/005—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein
- G03C1/06—Silver halide emulsions; Preparation thereof; Physical treatment thereof; Incorporation of additives therein with non-macromolecular additives
- G03C1/08—Sensitivity-increasing substances
Landscapes
- Physics & Mathematics (AREA)
- Chemical & Material Sciences (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Engineering & Computer Science (AREA)
- Materials Engineering (AREA)
- General Physics & Mathematics (AREA)
- Silver Salt Photography Or Processing Solution Therefor (AREA)
- Conversion Of X-Rays Into Visible Images (AREA)
- Non-Silver Salt Photosensitive Materials And Non-Silver Salt Photography (AREA)
Abstract
the invention discloses a chemical sensitization method of a silver halide emulsion, which is characterized in that gelatin solution containing halogenated barium fluoride particles after ball milling is added into the silver halide emulsion at the constant temperature of 45-55 ℃, and the addition amount is 1 multiplied by 10 according to the addition amount of each mole of silver in the silver halide emulsion-3～1×10-6And (3) stirring for 20-80 minutes according to the molar halogenated barium fluoride, and then quickly freezing and storing. The invention discloses a fluoride-halogen barium fluoride (BaFX: Eu) doped with rare earth ions for the first time2+) (X ═ Cl, Br, I) as a dopant, was introduced into a silver halide emulsion to prepare a barium oxyfluoride (BaFX: eu (Eu)2+) Compared with the conventional chemical sensitization of the sulfur and gold, the chemical sensitization of the silver halide emulsion after chemical sensitization can improve the light sensitivity by 2 times, and the fog is not increased.
Description
Technical field
The present invention relates to photosensitive material technical field.More particularly, to a kind of the efficient of silver emulsion
Chemical sensitization method.
Background technology
Although developing through nearly 20 years, camera maximum pixel used has even reached more than one hundred million in digital technology, has had
Standby at a relatively high speed and fabulous image quality, have replaced silver halide photography and have occupied commercial market
Main status, but in special imaging field, digital photographic technology can't obtain clear enough so far
Its definition can become worse after clear visible image, and the amplified treatment of image.And ISO halogen
Changing silver-colored emulsion free and relaxed can then obtain the observed image that the quality of image is high, exquisiteness is soft.Further investigation and
Preparation and the sensibilization technology of extraordinary ray photosensitive silve halide material are improved, to improve its speed and imaging matter
Amount etc. will be the groundwork that image department educational circles must do at present.
Current reported in literature, the sensitizing means of photosensitive silve halide material include conventional chemical sensitization (such as sulphur
Sensitizing, golden sensitizing and sulphur gold joint sensitizing etc.), spectral sensitization (such as feels green sensitizing, the blue sensitizing of sense and feels red
Sensitizing etc.), hole-electron converter sensibilization technology is (such as silver-colored dimer conversion agent, carboxylic acids hole conversion agent
With the bielectron donor compound conversion agent that can split into molecule fragment etc.) (Xia Peijie, state is red, Yao Linhui,
Zhao Wenfang, hole and its conversion in formation process of latent image, photographic science and photochemistry, 2002,20 (1):
46-59) and hydrogen cross sensitizing (Hailstone R K, Liebert N B, Levy M, McCleary R T,
Girolmo S R,Jeanmaire D L,Boda C R.Achieving High Quantum Sensitivities
with Hydrogen Hypersensitization 1.Measurement.J.Imaging Sci.,1988,32:
113-124) etc..
Rare earth ion doped fluoride is subject to very big concern (Facile micro-nano luminescent material recent years
and controllable synthesis of monodisperse CaF2and CaF2:Ce3+/Tb3+hollow
spheres as efficient luminescent materials and smart drug carriers[J].Chem.Eur.
J., 2010,16 (19):5672-5680.) it is had the following advantages that as emission peak is narrow, photoluminescence quantum yield
High, stable luminescence persistently etc., shows at aspects such as laser, display, fluorescence imaging, biomarkers
Go out good application prospect.Such as there is excellent optical stimulated luminescence property BaFX：Eu2+(X=Cl, Br
And I), it is best X-ray storage phosphor, can be used for X-ray intensifying screen and radiated from computer imaging
(Imaging Plates, IPs) (Physics and current in (Computed Radiography, CR) imaging plate
Understanding of X-ray storage phosphors [J] .Phys.Status.Solid.A, 2001,187
(2):335-393)。
By improving preparation and the sensibilization technology of photosensitive silve halide material, to improve its speed and imaging matter
Amount, it is desirable to provide a kind of chemical sensitization method of silver emulsion.
The content of the invention
It is an object of the present invention to provide a kind of chemical sensitization method of silver emulsion.It is fluorinated through halogen
Silver emulsion after barium chemical sensitization, and by the silver emulsion after conventional sulfur plus gold chemical sensitization
Compare, speed can improve 2 times, and photographic fog does not increase.
To reach above-mentioned purpose, the present invention uses following technical proposals：
A kind of chemical sensitization method of silver emulsion, under 45~55 DEG C of constant temperature, in silver emulsion
Add by the gelatin solution that titanate particle is fluorinated containing halogen after ball milling, addition is according in silver emulsion
1 × 10 is added per moles of silver-3~1 × 10-6Mole halogen barium fluoride is calculated, and stirring maturation time is 20~80
Minute, then quick freeze is stored.The molecular formula of the halogen barium fluoride is expressed as BaFX：Eu2+(X=Cl,
Br、I)。
Preferably, the preparation method of the gelatin solution containing halogen fluorination titanate particle by after ball milling is：
1) halogen barium fluoride powder is dispersed in aqueous gelatin solution and is carried out ultrasonically treated；
2) pouring into finely dispersed halogen barium fluoride aqueous gelatin solution carries out ball milling in ball grinder, contained
Halogen is fluorinated the gelatin solution of titanate particle.
Preferably, step 1) in, mass percentage concentration of the halogen barium fluoride in aqueous gelatin solution be 1~
10%.
Preferably, step 1) in, the mass percentage concentration of institute's gelatin water solution is 1~6%.
Preferably, step 2) in, rotational speed of ball-mill is 200~600 revs/min, a length of 15~30 during ball milling
Individual hour.
Preferably, halogen is fluorinated the particle diameter of titanate particle in the gelatin solution containing halogen fluorination titanate particle after ball milling
Scope is 1.0-10.0 microns, and particle diameter distribution is narrow.
Preferably, the silver halide pattern in the silver emulsion is cube, octahedron, spherical and T-
One or more in particle.
Preferably, the silver halide in the silver emulsion is silver chlorate, silver bromide, bromo-iodide, chlorine
One or more in silver bromide and chlorosulfonylation silver.
So far, also cross and rare earth ion doped fluoride micro Nano material can be answered without document report
In for the research and development of silver halide material in photographic chemistry field, the particularly preparation of silver emulsion and sensitizing.
Applicant of the present invention is fluorinated by numerous studies by by a kind of rare earth ion doped fluoride-halogen
Barium is dispersed in gelatin solution, recycles ball milling by its size controlling at 1.0-10.0 microns, and
Present invention provide that addition under be doped (addition according to silver emulsion in per moles of silver add 1
×10-3~1 × 10-6Mole halogen barium fluoride is calculated), prepare through halogen barium fluoride (BaFX：Eu2+) change
The silver emulsion after sensitizing is learned, through the silver emulsion after this chemical sensitization, than conventional sulfur plus gold
Sensitizing is learned, speed can improve 2 times, and photographic fog does not increase.
Beneficial effects of the present invention are as follows：
Present invention firstly discloses using a kind of rare earth ion doped fluoride-halogen barium fluoride (BaFX：
Eu2+) (X=Cl, Br, I) as dopant, be introduced into silver emulsion, prepare through halogen be fluorinated
Silver emulsion after barium chemical sensitization, through the silver emulsion after this chemical sensitization, adds than conventional sulphur
Golden chemical sensitization, speed can improve 2 times, and photographic fog does not increase.
Specific embodiment
In order to illustrate more clearly of the present invention, the present invention is done further with reference to preferred embodiment
It is bright.It will be appreciated by those skilled in the art that specifically described content is illustrative rather than limitation below
Property, should not be limited the scope of the invention with this.
Embodiment 1
(1) first by 4 grams of bromine barium fluoride (BaFBr：Eu2+) powder dispersed with stirring is at 200 milliliters
Mass percentage concentration be 7% aqueous gelatin solution, it is then ultrasonically treated at normal temperatures so that bromine is fluorinated
Barium (BaBrF：Eu2+) even particulate dispersion is in aqueous gelatin solution；Wherein bromine barium fluoride (BaBrF：
Eu2+) aqueous gelatin solution mass percentage concentration be 2%.
(2) by finely dispersed bromine barium fluoride (BaBrF：Eu2+) aqueous gelatin solution poured into ball grinder
Ball milling is carried out, using 100500Zirconia ball carry out ball milling, rotating speed is every point
200 turns of clock, the time is 15 hours, obtains narrow containing a diameter of 10 microns and particle diameter distribution
The aqueous gelatin solution of bromine barium fluoride；
(3) at 45 DEG C, to the above-mentioned process that 10 milliliters are added in 100 grams of cubic silver bromide emulsion
The bromine barium fluoride aqueous gelatin solution narrow containing a diameter of 10 microns and particle diameter distribution obtained after ball milling,
Addition is according to the addition 1 × 10 per moles of silver in silver emulsion-3Mole bromine barium fluoride is calculated, maturation time
It is 20 minutes, smear, exposure, aobvious fixing processing, test optical density is then carried out under dark room conditions,
Ask for photosensitive degrees of data as follows.The Data Comparison of the present embodiment method and conventional sulfur plus gold chemical sensitization method
As shown in table 1.
Table 1
| Sensitizing mode | Conventional sulfur plus gold chemical sensitization | Bromine barium fluoride chemical sensitization |
| Speed | 75 | 150 |
| Photographic fog | 0.08 | 0.08 |
| Contrast factor | 0.65 | 0.5 |
Data display in table：Through bromine barium fluoride (BaBrF：Eu2+) silver emulsion after chemical sensitization,
Than conventional sulfur plus gold chemical sensitization, emulsion speed can improve 1 times, and photographic fog does not increase, instead
Difference coefficient slightly has reduction.
Embodiment 2
(1) first by 8 grams of chlorofluorination barium (BaFCl：Eu2+) powder dispersed with stirring is at 200 milliliters
Mass percentage concentration be 7% aqueous gelatin solution, it is then ultrasonically treated at normal temperatures so that chlorofluorination
Titanate particle is dispersed in aqueous gelatin solution；Wherein chlorofluorination barium is dense in the quality percentage of aqueous gelatin solution
Spend is 4%.
(2) pouring into finely dispersed chlorofluorination barium aqueous gelatin solution carries out ball milling in ball grinder, using 100
It is individual500Zirconia ball carry out ball milling, rotating speed is 300 turns per minute, and the time is 20
Hour, obtain the aqueous gelatin solution containing the narrow chlorofluorination barium of a diameter of 8 microns and particle diameter distribution；
(3) at 48 DEG C, to the above-mentioned warp that 10 milliliters are added in 100 grams of octahedra chlorofluorination barium emulsion
The gelatin for crossing the chlorofluorination barium narrow containing a diameter of 8 microns and particle diameter distribution obtained after ball milling is water-soluble
Liquid, addition is according to the addition 1 × 10 per moles of silver in silver bromide emulsion-4Mole chlorofluorination barium is calculated, into
The ripe time is 40 minutes, and smear, exposure, aobvious fixing processing, test light are then carried out under dark room conditions
Density, asks for photosensitive degrees of data as follows.The number of the present embodiment method and conventional sulfur plus gold chemical sensitization method
It is as shown in table 2 according to contrast.
Table 2
| Sensitizing mode | Conventional sulfur plus gold chemical sensitization | Chlorofluorination barium chemical sensitization |
| Speed | 75 | 200 |
| Photographic fog | 0.08 | 0.08 |
| Contrast factor | 0.65 | 0.55 |
Data display in table：Through chlorofluorination barium (BaFCl：Eu2+) silver emulsion after chemical sensitization,
Than conventional sulfur plus gold chemical sensitization, emulsion speed can improve nearly 2 times, and photographic fog does not increase,
Contrast factor slightly has reduction.
Embodiment 3
(1) mass percentage concentration first by 12 grams of bromine barium fluoride powder dispersed with stirring at 200 milliliters
It is then ultrasonically treated at normal temperatures in for 7% aqueous gelatin solution so that bromine barium fluoride even particulate dispersion
In aqueous gelatin solution；Wherein bromine barium fluoride is 6% in the mass percentage concentration of aqueous gelatin solution.
(2) by finely dispersed bromine barium fluoride (BaBrF：Eu2+) aqueous gelatin solution poured into ball grinder
Ball milling is carried out, using 100500Zirconia ball carry out ball milling, rotating speed is every point
400 turns of clock, the time is 25 hours, obtains containing a diameter of 7 microns and the narrow bromine of particle diameter distribution
The aqueous gelatin solution of barium fluoride；
(3) at 52 DEG C, to the above-mentioned process that 10 milliliters are added in 100 grams of spherical silver bromide emulsions
The bromine barium fluoride aqueous gelatin solution narrow containing a diameter of 7 microns and particle diameter distribution obtained after ball milling,
Addition is according to the addition 1 × 10 per moles of silver in silver emulsion-5Mole bromine barium fluoride is calculated, maturation time
It is 60 minutes, smear, exposure, aobvious fixing processing, test optical density is then carried out under dark room conditions,
Ask for photosensitive degrees of data as follows.The Data Comparison of the present embodiment method and conventional sulfur plus gold chemical sensitization method
As shown in table 3.
Table 3
| Sensitizing mode | Conventional sulfur plus gold chemical sensitization | Bromine barium fluoride chemical sensitization |
| Speed | 75 | 220 |
| Photographic fog | 0.08 | 0.08 |
| Contrast factor | 0.65 | 0.53 |
Data display in table：Through bromine barium fluoride (BaBrF：Eu2+) silver emulsion after chemical sensitization,
Than conventional sulfur plus gold chemical sensitization, emulsion speed can improve 2 times, and photographic fog does not increase, instead
Difference coefficient slightly has reduction.
Embodiment 4
(1) mass percentage concentration first by 16 grams of iodine barium fluoride powder dispersed with stirring at 200 milliliters
It is then ultrasonically treated at normal temperatures in for 7% aqueous gelatin solution so that iodine barium fluoride even particulate dispersion
In aqueous gelatin solution；Wherein iodine barium fluoride is 8% in the mass percentage concentration of aqueous gelatin solution.
(2) pouring into finely dispersed iodine barium fluoride aqueous gelatin solution carries out ball milling in ball grinder, using 100
It is individual500Zirconia ball carry out ball milling, rotating speed is 500 turns per minute, and the time is 30
Individual hour, obtain the aqueous gelatin solution containing the narrow iodine barium fluoride of a diameter of 4 microns and particle diameter distribution；
(3) at 55 DEG C, to adding 10 milliliters above-mentioned by ball in 100 grams of T-shaped silver bromide emulsions
The iodine barium fluoride aqueous gelatin solution narrow containing a diameter of 4 microns and particle diameter distribution obtained after mill, plus
Enter amount according to the addition 1 × 10 per moles of silver in silver bromide emulsion-5Mole iodine barium fluoride is calculated, and maturation time is
60 minutes, smear, exposure, aobvious fixing processing, test optical density are then carried out under dark room conditions, asked
Take photosensitive degrees of data as follows.The Data Comparison of the present embodiment method and conventional sulfur plus gold chemical sensitization method is such as
Shown in table 4.
Table 4
| Sensitizing mode | Conventional sulfur plus gold chemical sensitization | Iodine barium fluoride chemical sensitization |
| Speed | 75 | 240 |
| Photographic fog | 0.08 | 0.08 |
| Contrast factor | 0.65 | 0.50 |
Data display in table：Through iodine barium fluoride (BaFI：Eu2+) silver emulsion after chemical sensitization, than
Conventional sulfur plus gold chemical sensitization, emulsion speed can be improved more than 2 times, and photographic fog does not increase.Instead
Difference coefficient slightly has reduction.
Embodiment 5
(1) mass percentage concentration first by 20 grams of bromine barium fluoride powder dispersed with stirring at 200 milliliters
It is then ultrasonically treated at normal temperatures in for 7% aqueous gelatin solution so that bromine barium fluoride even particulate dispersion
In aqueous gelatin solution；Wherein bromine barium fluoride is 10% in the mass percentage concentration of aqueous gelatin solution.
(2) pouring into finely dispersed bromine barium fluoride aqueous gelatin solution carries out ball milling in ball grinder, using 100
It is individual500Zirconia ball carry out ball milling, rotating speed is 600 turns per minute, and the time is 30
Individual hour, obtain the aqueous gelatin solution containing the narrow bromine barium fluoride of a diameter of 1 microns and particle diameter distribution；
(3) at 55 DEG C, to the above-mentioned process that 10 milliliters are added in 100 grams of cube silver chloride emulsions
The bromine barium fluoride aqueous gelatin solution narrow containing a diameter of 2 microns and particle diameter distribution obtained after ball milling,
Addition is according to the addition 1 × 10 per moles of silver in silver bromide emulsion-6Mole bromine barium fluoride is calculated, maturation time
It is 80 minutes, smear, exposure, aobvious fixing processing, test optical density is then carried out under dark room conditions,
Ask for photosensitive degrees of data as follows.The Data Comparison of the present embodiment method and conventional sulfur plus gold chemical sensitization method
As shown in table 5.
Table 5
| Sensitizing mode | Conventional sulfur plus gold chemical sensitization | Bromine barium fluoride chemical sensitization |
| Speed | 75 | 250 |
| Photographic fog | 0.08 | 0.08 |
| Contrast factor | 0.65 | 0.50 |
Data display in table：Through bromine barium fluoride (BaBrF：Eu2+) silver emulsion after chemical sensitization,
Than conventional sulfur plus gold chemical sensitization, emulsion speed can be improved more than 2 times, and photographic fog does not increase.
Contrast factor slightly has reduction.
Obviously, the above embodiment of the present invention is only intended to clearly illustrate example of the present invention, and
It is not the restriction to embodiments of the present invention, for those of ordinary skill in the field,
Can also be made other changes in different forms on the basis of described above, here cannot be to all
Implementation method be exhaustive, it is every to belong to the obvious change that technical scheme is extended out
Change or change the row still in protection scope of the present invention.
Claims (9)
1. a kind of chemical sensitization method of silver emulsion, it is characterised in that：Under 45~55 DEG C of constant temperature,
To being added in silver emulsion by the gelatin solution that titanate particle is fluorinated containing halogen after ball milling, addition is pressed
According to the addition 1 × 10 per moles of silver in silver emulsion-3~1 × 10-6Mole halogen barium fluoride is calculated, and stirring is ripe
Time is 20~80 minutes, then quick freeze storage.
2. the chemical sensitization method of a kind of silver emulsion according to claim 1, it is characterised in that
The preparation method of the gelatin solution by containing halogen fluorination titanate particle after ball milling is：
1) halogen barium fluoride powder is dispersed in aqueous gelatin solution and is carried out ultrasonically treated；
2) pouring into finely dispersed halogen barium fluoride aqueous gelatin solution carries out ball milling in ball grinder, contained
Halogen is fluorinated the gelatin solution of titanate particle.
3. the chemical sensitization method of a kind of silver emulsion according to claim 2, it is characterised in that：
Step 1) in, mass percentage concentration of the halogen barium fluoride in aqueous gelatin solution is 1~10%.
4. the chemical sensitization method of a kind of silver emulsion according to claim 2, it is characterised in that：
Step 1) in, the mass percentage concentration of institute's gelatin water solution is 1~6%.
5. the chemical sensitization method of a kind of silver emulsion according to claim 2, it is characterised in that：
Step 2) in, rotational speed of ball-mill is 200~600 revs/min, a length of 15~30 hours during ball milling.
6. a kind of chemical sensitization method of silver emulsion according to claim 1 and 2, its feature
It is：The particle size range of halogen fluorination titanate particle is in the gelatin solution containing halogen fluorination titanate particle after ball milling
1.0-10.0 microns.
7. a kind of chemical sensitization method of silver emulsion according to claim 1 and 2, its feature
It is：The halogen barium fluoride is BaFX：Eu2+, wherein X is the one kind in Cl, Br, I.
8. the chemical sensitization method of a kind of silver emulsion according to claim 1, it is characterised in that：
Silver halide pattern in the silver emulsion is the one kind in cube, octahedron, spherical and T- particles
Or it is various.
9. the chemical sensitization method of a kind of silver emulsion according to claim 1, it is characterised in that：
Silver halide in the silver emulsion is silver chlorate, silver bromide, bromo-iodide, chlorine silver bromide and chlorine iodine
Change one or more in silver.
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| CN112558406A (en) * | 2020-12-17 | 2021-03-26 | 合肥菲力姆科技有限公司 | Preparation method of thermosensitive film photosensitive emulsion |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000275771A (en) * | 1999-03-24 | 2000-10-06 | Fuji Photo Film Co Ltd | Silver halide photographic emulsion and photosensitive material containing the same, and image forming method by using it |
| CN1438541A (en) * | 2002-01-25 | 2003-08-27 | 富士胶片株式会社 | Photography treatment composition and image formation method using same |
| US6682868B1 (en) * | 2003-03-26 | 2004-01-27 | Eastman Kodak Company | Radiographic imaging assembly with blue-sensitive film |
| CN101434841A (en) * | 2008-12-18 | 2009-05-20 | 北京交通大学 | Functional material for X ray image storage and preparation thereof |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2000275771A (en) * | 1999-03-24 | 2000-10-06 | Fuji Photo Film Co Ltd | Silver halide photographic emulsion and photosensitive material containing the same, and image forming method by using it |
| CN1438541A (en) * | 2002-01-25 | 2003-08-27 | 富士胶片株式会社 | Photography treatment composition and image formation method using same |
| US6682868B1 (en) * | 2003-03-26 | 2004-01-27 | Eastman Kodak Company | Radiographic imaging assembly with blue-sensitive film |
| CN101434841A (en) * | 2008-12-18 | 2009-05-20 | 北京交通大学 | Functional material for X ray image storage and preparation thereof |
Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112558406A (en) * | 2020-12-17 | 2021-03-26 | 合肥菲力姆科技有限公司 | Preparation method of thermosensitive film photosensitive emulsion |
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