CN103048673A - Preparation method of radiochromic film - Google Patents
Preparation method of radiochromic film Download PDFInfo
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- CN103048673A CN103048673A CN2013100006588A CN201310000658A CN103048673A CN 103048673 A CN103048673 A CN 103048673A CN 2013100006588 A CN2013100006588 A CN 2013100006588A CN 201310000658 A CN201310000658 A CN 201310000658A CN 103048673 A CN103048673 A CN 103048673A
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Abstract
The invention discloses a preparation method of a radiochromic film. The preparation method comprises the following steps that (1) firstly, a film forming base material is completely dissolved in solvents; (2) halogen compounds and color change ingredients are added into a solution obtained in the step (1), and the uniform film forming solution is formed through stirring; and (3) the film forming solution is uniformly coated on a support body of a horizontal plane by a solution tape casting method, then, drying and curing are carried out, and the film is prepared. The invention provides the preparation method of the radiochromic film, which has the advantages that the 12kGy dosage threshold indication color change can be realized, the process is simple, the preparation process is safe, the environment is friendly, the thickness of the prepared film is uniform, and the color is uniform.
Description
Technical field
The present invention relates to the radiation checking technical field, particularly a kind of preparation method of the Radiochromic film for the RADIATION PROCESSING dose monitoring.
Background technology
Radiochromic film is a kind of organic solid film that change color can occur after being subject to certain ionizing radiation dose.Radiochromic film is usually used in measuring the dosage of the various radiation sources such as high energy proton, high energy electron, gamma-rays and X ray.Stablize, be subjected to behind simple, easy to use, the predose of preparation to change the advantages such as directly perceived according to rear color with dosage is different owing to possessing, Radiochromic film is widely used in the RADIATION PROCESSING field, such as radiation improvement of fresh-keeping or storage, insect sterilization, the modification of macromolecular material, semi-conductive modification or radiation hardening and " three wastes " of the sterilization of medical supplies and sterilization, food etc.
External research and report relevant for Radiochromic film, and form two class commercially available prod: Radiochromic film quantimeter and radiating color changing label.The former is generally transparent film, is subjected to change with the solid color depth behind the irradiation, has the characteristics of linear response absorbed dose, but accurate quantification absorbed dose, but the instruments such as needs use spectrophotometer are measured, and measure relative complex, are applicable to the quantitative test field; The latter is generally opaque adhesive type label, be subjected to become another kind of color from a kind of change color behind the irradiation, by this transformation dose indicating threshold value, can be used for visual observation and estimate dosage level, irradiation dose just can be determined in the scene, is applicable to the quantitative and semi-quantitative field.
Current, external research for the radiating color changing label, for example US Patent specification US3743846 and US4001587, usually adopt Polyvinylchloride or chlorine-containing copolymer to prepare the Radiochromic film of core main body, these materials are difficult selects suitable solvent, thereby does not usually adopt solution casting method, but adopts extrusion-blown modling method, rolling process etc., instrument requires high, complicated operation.
And domesticly focus mostly on Radiochromic film quantimeter direction for Radiochromic film research, and an example report is only arranged in the radiating color changing tag orientation: Shanghai Atomic Nucleus Inst., Chinese Academy of Sciences once developed the radiating color changing label of yellow and green two kinds of systems, be called " SN type dosage label " [Wu Zhili, Chen Xinwei. the performance study of the yellow dosage label of SN type system], but technology is in confidential state.In order to solve domestic RADIATION PROCESSING field to the heavy demand of radiating color changing label, therefore be badly in need of the preparation method of Radiochromic film.
Summary of the invention
The present invention has overcome deficiency of the prior art, provides a kind of and can realize 12kGy dosage threshold value discoloration indication, and technique is simple, safe preparation process, environmentally friendly, to make film thickness even, the preparation method of the uniform Radiochromic film of color.
In order to solve the problems of the technologies described above, the present invention is achieved by the following technical solutions:
A kind of preparation method of Radiochromic film, it may further comprise the steps, and (1) at first will become film base material to be dissolved in the solvent fully; (2) in the solution of step (1) acquisition, add halogen compounds and chromotropic dye, stir the film forming solution that forms homogeneous; (3) adopt solution casting method that film forming solution is uniformly coated on the horizontal plane support, then carry out dry solidification and make film.
The present invention is all right:
Described one-tenth film base material is selected polyvinyl alcohol (PVA) or polyvinyl butyral, and described solvent is selected a kind of in the mixed liquor of water, absolute ethyl alcohol or water and ethanol.
In described variable color Fuel Selection peacock green, methyl violet, cresol red (being o-cresol red), thymol blue (being bromothymol blue), methyl yellow (being dimethyl yellow), bromophenol blue, Congo red, methyl orange (being orange III), sodium alizarinsulfonate (being sodium alizarine sulphonate), bromcresol green, methyl red, bromcresol purple, bromthymol blue (being bromothymol blue), xylenol orange, aniline blue, the methylene blue any.
Described halogen compounds is selected one or more in chloral hydrate, trichloroacetic acid, carbon trichloride, carbon tetrabromide, the ethylene dibromide.
Described step (1) is dissolved in polyvinyl alcohol (PVA) in the water; (2) add chloral hydrate and methyl orange in the solution after the dissolving, stir the film forming solution that forms homogeneous; (3) adopt solution casting method prize film forming solution to be uniformly coated on the optical glass flat board, then carry out dry solidification and make film.
The quality proportioning 100:700 of described one-tenth film base material and dissolution with solvents～1000.
Described one-tenth film base material and variable color quality of fuel proportioning are 100:0.05～0.5.
The quality proportioning of described one-tenth film base material and halogen compounds is 100:5～50.
Described step (1) fully is dissolved in water according to the quality proportioning of 100:700～1000 polyvinyl alcohol (PVA), water; (2) add methyl orange and chloral hydrate according to the quality proportioning of 0.1～0.2:10～20 in the solution after the dissolving, stir the film forming solution that forms homogeneous; (3) adopt solution casting method prize film forming solution to be uniformly coated on the optical glass flat board of level, then under 10～50 ℃ temperature, 20%～70% humidity, carry out dry solidification and make film.
Described step (1) is dissolved polyvinyl alcohol (PVA), water fully according to the quality proportioning of 100:1000; (2) add methyl orange and chloral hydrate according to the quality proportioning of 0.1:10 in the solution after the dissolving, stir the film forming solution that forms homogeneous; (3) adopt solution casting method prize film forming solution to be uniformly coated on the optical glass flat board, then under 25 ℃ temperature, 30% humidity, carry out dry solidification and make film.
Compared with prior art, the invention has the beneficial effects as follows:
The present invention realizes a kind of Radiochromic film preparation method by the cooperation of basic process steps, and the method preparation technology is simple, and safe preparation process is environmentally friendly, makes film thickness even, and color is even.Use this method to prepare Radiochromic film, can select cheap material, preparation cost is low.
Simultaneously, the present invention is on the basis of basic process steps, the present invention has selected the cooperation that becomes film base material, chromotropic dye, halogen compounds, and special material and proportioning have been adopted, realized that by combination between material and the proportioning film irradiation color contrast behind predose of preparing is obvious, especially select the film of the prescription preparation of polyvinyl alcohol (PVA), methyl orange, chloral hydrate, be convenient to visual inspection, the transformation of color can realize this dosage threshold value indication of 12kGy, can be used for simultaneously visual observation and estimate dosage level, be applicable to make the radiating color changing label.
Description of drawings
The variable color situation that Fig. 1 Radiochromic film changes with radiation dose;
The uv-visible absorption spectra of Fig. 2 Radiochromic film;
The radiation dose response curve of Fig. 3 Radiochromic film.
Embodiment
Below in conjunction with accompanying drawing and embodiment the present invention is described in further detail:
The invention provides a kind of preparation method of Radiochromic film, it may further comprise the steps, and (1) at first will become film base material to be dissolved in the solvent fully; (2) in the solution of step (1) acquisition, add halogen compounds and chromotropic dye, stir the film forming solution that forms homogeneous; (3) adopt solution casting method that film forming solution is uniformly coated on the horizontal plane support, then carry out dry solidification and make film.
Described one-tenth film base material is selected polyvinyl alcohol (PVA) or polyvinyl butyral, and described solvent is selected a kind of in the mixed liquor of water, absolute ethyl alcohol or water and ethanol.
In variable color Fuel Selection peacock green, methyl violet, cresol red (being o-cresol red), thymol blue (being bromothymol blue), methyl yellow (being dimethyl yellow), bromophenol blue, Congo red, methyl orange (being orange III), sodium alizarinsulfonate (being sodium alizarine sulphonate), bromcresol green, methyl red, bromcresol purple, bromthymol blue (being bromothymol blue), xylenol orange, aniline blue, the methylene blue any.
Halogen compounds is selected one or more in chloral hydrate, trichloroacetic acid, carbon trichloride, carbon tetrabromide, the ethylene dibromide.
Film by the method preparation is subjected to become another kind of color from a kind of change color behind the irradiation, by dosage threshold value of this transformation indication.This Radiochromic film is used for making the radiating color changing label and sticks to and be subjected to irradiated material, and dosage level is estimated in visual observation.
Raw material umber described in this example is mass fraction, by weight.
Take by weighing 100 parts of polyvinyl alcohol (PVA), take 1000 parts of water as solvent, be mixed with the solution of homogeneous, take by weighing again 0.1 part of methyl orange and 10 parts of chloral hydrates, join in the mentioned solution, stirring and dissolving is made film forming solution fully, then with film forming solution curtain coating on the smooth optical glass flat board of level, keep stationary temperature (25 ℃) and Constant humidity (relative humidity 30%) natural drying 2 days, and made Radiochromic film.
Learn performance for the irradiation dose of investigating this Radiochromic film, in the cobalt-60 radiosterilize device, this Radiochromic film has been carried out irradiation experiment.After imposing the irradiation of various dose, the change color of observable Radiochromic film, as shown in Figure 1.
For the relation of Measurement accuracy change color and irradiation dose, adopt spectrophotometer that the absorbance of Radiochromic film under the different irradiation doses is changed and measure, the results are shown in Figure 2 and Fig. 3.As can be seen from Fig., this Radiochromic film becomes redness by yellow behind the radiation effects that is subject to this dosage threshold value of 12kGy.This characteristic can be used for visual observation and estimates dosage level.
The present embodiment is with embodiment 1, its difference is, take by weighing 100 parts of polyvinyl alcohol (PVA), take 700 parts of water as solvent, be mixed with the solution of homogeneous, take by weighing again 0.05 part of methyl orange and 5 parts of chloral hydrates, join in the mentioned solution, stirring and dissolving is made film forming solution fully, then with film forming solution curtain coating on the smooth optical glass flat board of level, keep stationary temperature (10 ℃) and Constant humidity (relative humidity 20%) natural drying 2 days, and made Radiochromic film.
This Radiochromic film becomes redness from yellow behind the radiation effects that is subject to the various dose level.
Embodiment 3
The present embodiment is with embodiment 1, its difference is, take by weighing 100 parts of polyvinyl alcohol (PVA), take 700 parts of water as solvent, be mixed with the solution of homogeneous, take by weighing again 0.2 part of methyl orange and 20 parts of chloral hydrates, join in the mentioned solution, stirring and dissolving is made film forming solution fully, then with film forming solution curtain coating on the smooth optical glass flat board of level, keep stationary temperature (25 ℃) and Constant humidity (relative humidity 30%) natural drying 2 days, and made Radiochromic film.
This Radiochromic film becomes redness from yellow behind the radiation effects that is subject to the various dose level.
Embodiment 4
The present embodiment is with embodiment 1, its difference is, take by weighing 100 parts of polyvinyl alcohol (PVA), take 900 parts of water as solvent, be mixed with the solution of homogeneous, take by weighing again 0.5 part of methyl orange and 50 parts of chloral hydrates, join in the mentioned solution, stirring and dissolving is made film forming solution fully, then with film forming solution curtain coating on the smooth optical glass flat board of level, keep stationary temperature (50 ℃) and Constant humidity (relative humidity 70%) natural drying 5 days, and made Radiochromic film.
This Radiochromic film becomes redness from yellow behind the radiation effects that is subject to the various dose level.
The present embodiment is with embodiment 1, its difference is, take by weighing 100 parts of polyvinyl butyrals, take 1000 parts of ethanol as solvent, be mixed with the solution of homogeneous, take by weighing again 0.5 part of cresol red and 35 parts of carbon tetrabromides, join in the mentioned solution, stirring and dissolving is made film forming solution fully, then with film forming solution curtain coating on the smooth optical glass flat board of level, the relative humidity that keeps stationary temperature (10 ℃～50 ℃) and relative humidity (20%～70%)) natural drying 1 day, make Radiochromic film.
This Radiochromic film becomes redness from yellow behind the radiation effects that is subject to the various dose level.
The present embodiment is with embodiment 1, its difference is, take by weighing 100 parts of polyvinyl alcohol (PVA), take 1000 parts of water as solvent, be mixed with the solution of homogeneous, take by weighing again 0.1 part of bromcresol green and 10 parts of chloral hydrates, join in the mentioned solution, stirring and dissolving is made film forming solution fully, then with film forming solution curtain coating on the smooth optical glass flat board of level, keep stationary temperature (25 ℃) and relative humidity (30%) natural drying 2 days, and made Radiochromic film.
This Radiochromic film is behind the radiation effects that is subject to the various dose level, from blue yellowing.
Claims (10)
1. the preparation method of a Radiochromic film is characterized in that, it may further comprise the steps, and (1) at first will become film base material to be dissolved in the solvent fully; (2) in the solution of step (1) acquisition, add halogen compounds and chromotropic dye, stir the film forming solution that forms homogeneous; (3) adopt solution casting method that film forming solution is uniformly coated on the horizontal plane support, then carry out dry solidification and make film.
2. the preparation method of a kind of Radiochromic film according to claim 1 is characterized in that, described one-tenth film base material is selected polyvinyl alcohol (PVA) or polyvinyl butyral, and described solvent is selected a kind of in the mixed liquor of water, absolute ethyl alcohol or water and ethanol.
3. the preparation method of a kind of Radiochromic film according to claim 1, it is characterized in that any in described variable color Fuel Selection peacock green, methyl violet, cresol red (being o-cresol red), thymol blue (being bromothymol blue), methyl yellow (being dimethyl yellow), bromophenol blue, Congo red, methyl orange (being orange III), sodium alizarinsulfonate (being sodium alizarine sulphonate), bromcresol green, methyl red, bromcresol purple, bromthymol blue (being bromothymol blue), xylenol orange, aniline blue, the methylene blue.
4. the preparation method of a kind of Radiochromic film according to claim 1 is characterized in that, described halogen compounds is selected one or more in chloral hydrate, trichloroacetic acid, carbon trichloride, carbon tetrabromide, the ethylene dibromide.
5. the preparation method of a kind of Radiochromic film according to claim 1 is characterized in that, described step (1) is dissolved in polyvinyl alcohol (PVA) in the water; (2) add chloral hydrate and methyl orange in the solution after the dissolving, stir the film forming solution that forms homogeneous; (3) adopt solution casting method prize film forming solution to be uniformly coated on the optical glass flat board, then carry out dry solidification and make film.
6. the preparation method of a kind of Radiochromic film according to claim 1 is characterized in that, the quality proportioning 100:700 of described one-tenth film base material and dissolution with solvents～1000.
7. the preparation method of a kind of Radiochromic film according to claim 1 is characterized in that, described one-tenth film base material and variable color quality of fuel proportioning are 100:0.05～0.5.
8. the preparation method of a kind of Radiochromic film according to claim 1 is characterized in that, the quality proportioning of described one-tenth film base material and halogen compounds is 100:5～50.
9. according to claim 5 to the preparation method of 8 each described a kind of Radiochromic films, it is characterized in that, described step (1) fully is dissolved in water according to the quality proportioning of 100:700～1000 polyvinyl alcohol (PVA), water; (2) add methyl orange and chloral hydrate according to the quality proportioning of 0.1～0.2:10～20 in the solution after the dissolving, stir the film forming solution that forms homogeneous; (3) adopt solution casting method prize film forming solution to be uniformly coated on the optical glass flat board of level, then under 10～50 ℃ temperature, 20%～70% humidity, carry out dry solidification and make film.
10. the preparation method of a kind of Radiochromic film according to claim 9 is characterized in that, described step (1) is dissolved polyvinyl alcohol (PVA), water fully according to the quality proportioning of 100:1000; (2) add methyl orange and chloral hydrate according to the quality proportioning of 0.1:10 in the solution after the dissolving, stir the film forming solution that forms homogeneous; (3) adopt solution casting method prize film forming solution to be uniformly coated on the optical glass flat board, then under 25 ℃ temperature, 30% relative humidity, carry out dry solidification and make film.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104361827A (en) * | 2014-11-17 | 2015-02-18 | 成都纽曼特科技有限公司 | Color changing label for marking radiation and preparation method thereof |
| CN104777503A (en) * | 2015-04-13 | 2015-07-15 | 中国原子能科学研究院 | Preparation technology of radiochromic film for dose monitoring |
| CN104777504A (en) * | 2015-04-13 | 2015-07-15 | 中国原子能科学研究院 | Preparation technology of radiation color changing film for monitoring dosage in radiation processing |
| CN105885718A (en) * | 2016-03-31 | 2016-08-24 | 中国原子能科学研究院 | Radiated discoloring label dosimeter and preparation process |
| CN114716872A (en) * | 2022-05-05 | 2022-07-08 | 天行智控(成都)科技有限公司 | Irradiation indication stamp-pad ink and preparation method and application thereof |
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| JPH02272383A (en) * | 1989-03-06 | 1990-11-07 | Minnesota Mining & Mfg Co <3M> | Color change posimeter and method of manufacturing the same |
| US6524763B1 (en) * | 2000-03-01 | 2003-02-25 | The Japan Atomic Power Company | Microcapsules containing a radiation sensitive composition and their use |
| CN101387706A (en) * | 2008-10-30 | 2009-03-18 | 上海大学 | Radiating color changing hydrogels three-dimensional monitor and method for making same |
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2013
- 2013-01-04 CN CN2013100006588A patent/CN103048673A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPH02272383A (en) * | 1989-03-06 | 1990-11-07 | Minnesota Mining & Mfg Co <3M> | Color change posimeter and method of manufacturing the same |
| US6524763B1 (en) * | 2000-03-01 | 2003-02-25 | The Japan Atomic Power Company | Microcapsules containing a radiation sensitive composition and their use |
| CN101387706A (en) * | 2008-10-30 | 2009-03-18 | 上海大学 | Radiating color changing hydrogels three-dimensional monitor and method for making same |
Non-Patent Citations (1)
| Title |
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| A.A.ABDEL-FATTAH: ""Development of a radiation-sensitive indicator"", 《RADIATION PHYSICS AND CHEMISTRY》 * |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104361827A (en) * | 2014-11-17 | 2015-02-18 | 成都纽曼特科技有限公司 | Color changing label for marking radiation and preparation method thereof |
| CN104777503A (en) * | 2015-04-13 | 2015-07-15 | 中国原子能科学研究院 | Preparation technology of radiochromic film for dose monitoring |
| CN104777504A (en) * | 2015-04-13 | 2015-07-15 | 中国原子能科学研究院 | Preparation technology of radiation color changing film for monitoring dosage in radiation processing |
| CN104777504B (en) * | 2015-04-13 | 2017-09-12 | 中国原子能科学研究院 | A kind of preparation technology of the Radiochromic film monitored for RADIATION PROCESSING middle dosage |
| CN105885718A (en) * | 2016-03-31 | 2016-08-24 | 中国原子能科学研究院 | Radiated discoloring label dosimeter and preparation process |
| CN105885718B (en) * | 2016-03-31 | 2019-08-06 | 中国原子能科学研究院 | A kind of preparation process of Radiochromic label dosimeter |
| CN114716872A (en) * | 2022-05-05 | 2022-07-08 | 天行智控(成都)科技有限公司 | Irradiation indication stamp-pad ink and preparation method and application thereof |
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Application publication date: 20130417 |