CN111574727A - Radiation photoluminescence material, preparation method and application - Google Patents
Radiation photoluminescence material, preparation method and application Download PDFInfo
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Abstract
The invention discloses a radiation photoluminescence material, a preparation method and application thereof, wherein the preparation method of the radiation photoluminescence material comprises the following steps: mixing soluble metal salt, a ligand and a solvent to obtain a mixed solution, synthesizing a metal organic framework crystal by adopting a solvothermal method for the mixed solution, cleaning and drying the metal organic framework crystal to obtain the radiation photoluminescence material, wherein the molar ratio of the soluble metal salt to the ligand is 1:10-10:1, a benzene ring of the ligand is connected with a methyl group, and the valence state of the soluble metal salt is divalent and/or trivalent. The radiation photoluminescence material prepared by the preparation method has wider radiation detection limit, namely the upper limit of detectable radiation is 3700Gy, while the upper limit of detectable radiation of the preparation material of the traditional silver glass dosimeter is only 10 Gy.
Description
Technical Field
The invention relates to the technical field of nuclear radiation, in particular to a radiation photoluminescence material, a preparation method and application thereof.
Background
With the development of nuclear science and technology, the demand for accurate dosimeters in the fields of radiotherapy, radiodiagnosis, radiation protection and the like is increasing. Compared with real-time radiation detection equipment such as an ionization chamber, a scintillator and a semiconductor, the solid dosimeter has the characteristics of small volume, continuous monitoring, separation of test and read signals and the like, and has an irreplaceable effect in radiation dosage testing.
At present, the field of solid radiation dosimeters mainly comprises three dosimeters, namely thermoluminescent dosimeters, photoluminescent dosimeters and thermoluminescent dosimeters. The thermoluminescent dosimeter and the photoluminescent dosimeter are thermally excited or optically excited, so that fluorescence is induced by recombination of electron holes generated by radiation, and the limitation of poor signal stability under the condition of photo-thermal exists. The radiation photoluminescence dosimeter reads signals by ultraviolet excitation by using new energy levels generated by radiation defects, and the new energy levels do not disappear after being excited, so that the radiation photoluminescence dosimeter has the capability of repeated reading, and the signals are not obviously attenuated in the reading process. The traditional radiation photoluminescence material mainly uses silver-doped phosphate glass and Al2O3: related researches mostly surround doping modification of materials to strengthen partial radiation detection performance, and few new materials are found to be suitable for radiation photoluminescence detection, so that the problems of limited selectable materials, low upper limit of radiation dose test, limited application scenes and the like exist. Therefore, there is a need to develop a new material possessing radiation photoluminescence properties.
The Metal Organic Framework (MOF) material is used as a metal organic hybrid with high crystallinity, and organic ligands can modify various groups and have high designability. Due to the unique framework structure, the properties of gas adsorption, separation, catalysis, fluorescence and the like are widely researched. The metal part can have higher radiation retardation capability, and the radiation detection efficiency can be obviously improved. The organic part is proved to be beneficial to designing MOF materials with high quantum yield by selecting luminescent components, and the organic part has good application prospect in the field of radiation detection, but the current application is still less.
Disclosure of Invention
The invention aims to provide a novel radiation photoluminescence material capable of improving the upper limit of detection of radiation dose, a preparation method and application thereof.
In order to solve the above technical problems, the present invention provides a method for preparing a radiation photoluminescent material, comprising the steps of:
mixing soluble metal salt, a ligand and a solvent to obtain a mixed solution, synthesizing a metal organic framework crystal by adopting a solvothermal method for the mixed solution, cleaning and drying the metal organic framework crystal to obtain the radiation photoluminescence material, wherein the molar ratio of the soluble metal salt to the ligand is 1:10-10:1, a benzene ring of the ligand is connected with a methyl group, and the valence state of the soluble metal salt is divalent and/or trivalent.
The preparation method of the radiation photoluminescence material is simple, and the radiation photoluminescence material is obtained by mixing soluble metal salt, the ligand with methyl connected on a benzene ring and a solvent, synthesizing by adopting a solvothermal method to obtain a metal organic framework crystal, cleaning and drying the metal organic framework crystal.
Experiments prove that the radiation photoluminescence material has higher density and radiation stopping capability due to the synthesis of highly-crystallized metal organic framework crystals (MOF), the methyl connected to the benzene ring of the ligand can enable the radiation photoluminescence material to accumulate fluorescence signals generated by free radicals after irradiation, and therefore the radiation photoluminescence material has good radiation photoluminescence properties, wherein the ligand connected with the methyl on the benzene ring can accumulate and maintain the fluorescence signals generated by the free radicals compared with the ligand connected with other groups (such as carboxyl) on the benzene ring. In addition, the material also has certain light transmittance, excellent luminous efficiency and good mechanical strength. The fluorescent signal may be maintained for a period of several days to several weeks.
Compared with the traditional silver glass dosimeter material, the radiation detection limit of the radiation photoluminescence material is larger, namely the detectable radiation detection upper limit is 3700Gy, and the detection upper limit of the traditional silver glass dosimeter material is 10 Gy.
In one embodiment, the soluble metal salt is selected from at least one of lead nitrate, lead chloride, barium nitrate, bismuth nitrate, calcium nitrate, gadolinium nitrate, zinc nitrate, europium nitrate, and terbium nitrate.
In one embodiment, the ligand is selected from at least one of 2-methyl terephthalic acid, 2, 5-dimethyl terephthalic acid, 2, 6-dimethyl terephthalic acid, tetramethyl terephthalic acid, and 4-methyl-2, 6-naphthalene dicarboxylic acid. The fluorescence signal generated by free radicals can be accumulated and maintained by the methyl groups connected to the benzene rings of the ligands compared with the ligands connected with other groups (such as carboxyl groups) on the benzene rings.
In one embodiment, the solvent is selected from at least one of N, N-dimethylformamide, dimethylsulfoxide, N-dimethylacetamide, ethanol, and water.
In one embodiment, in the step of synthesizing the metal organic framework crystal by using a solvothermal method, the solvothermal temperature is 60-140 ℃.
In one embodiment, the synthesis is performed for a period of 3 to 7 days.
In one embodiment, in the step of mixing the soluble metal salt, the ligand and the solvent to obtain the mixed solution, the ultrasonic treatment of the mixed solution is further included.
In one embodiment, the frequency of the sonication is 33-40 kHz.
The invention also provides a radiation photoluminescence material prepared by the preparation method of the radiation photoluminescence.
The invention also provides the application of the radiation photoluminescence material in the preparation of the radiation photoluminescence dosimeter.
Drawings
FIG. 1 is a graph of the measurement of the radiation of a radiation photoluminescent material in example 1 of the present invention;
FIG. 2 is a graph of the measurement of the radiation photoluminescent material in comparative example 2 of the present invention;
fig. 3 is a graph of the measurement of the radiation photoluminescent material in comparative example 3 of the present invention.
Detailed Description
In order to make the aforementioned objects, features and advantages of the present invention comprehensible, embodiments accompanied with figures are described in detail below. In the following description, numerous specific details are set forth in order to provide a thorough understanding of the present invention. This invention may, however, be embodied in many different forms and should not be construed as limited to the embodiments set forth herein.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
Example 1
A preparation method of a radiation photoluminescence material comprises the following steps:
0.01mmol of lead nitrate and 0.1mmol of 2-methyl terephthalic acid were mixed in a 5mL scintillation vial, after which 2mL of N, N-dimethylformamide was added. The powder is dissolved and dispersed evenly by ultrasonic, and the ultrasonic frequency is 33 kHz. And (3) screwing the cover of the scintillation vial, putting the scintillation vial into an oven at 140 ℃, and standing for 3 days to generate a metal organic framework crystal. And taking out the metal organic framework crystal, cleaning the surface of the metal organic framework crystal for 3 times by using N, N-dimethylformamide and ethanol, and drying at room temperature to obtain the product, namely the radiation photoluminescence material.
Example 2
A preparation method of a radiation photoluminescence material comprises the following steps:
0.05mmol of lead chloride, 0.05mmol of barium nitrate and 0.01mmol of 2, 5-dimethylterephthalic acid were mixed in a 10mL scintillation vial, and 1mL of N, N-dimethylformamide and 1mL of water were added. The powder is dissolved and dispersed evenly by ultrasonic, and the ultrasonic frequency is 35 kHz. And screwing the cover of the scintillation vial, putting the scintillation vial into an oven at 80 ℃, and standing for 3 days to generate a metal organic framework crystal. And taking out the metal organic framework crystal, cleaning the surface of the metal organic framework crystal for 3 times by using N, N-dimethylformamide and ethanol, and drying at room temperature to obtain the product, namely the radiation photoluminescence material.
Example 3
A preparation method of a radiation photoluminescence material comprises the following steps:
0.05mmol of bismuth nitrate, 0.05mmol of calcium nitrate and 0.1mmol of 2, 5-dimethylterephthalic acid, 0.1mmol of 4-methyl-2, 6-naphthalenedicarboxylic acid were mixed in a 5mL scintillation vial, and 0.5mL of N, N-dimethylformamide and 1mL of dimethyl sulfoxide were added. The powder is dissolved and dispersed evenly by ultrasonic, and the ultrasonic frequency is 40 kHz. And screwing the cover of the scintillation vial, putting the scintillation vial into an oven at 60 ℃, and standing for 3 days to generate a metal organic framework crystal. And taking out the metal organic framework crystal, cleaning the surface of the metal organic framework crystal for 3 times by using N, N-dimethylformamide and ethanol, and drying at room temperature to obtain the product, namely the radiation photoluminescence material.
Example 4
A preparation method of a radiation photoluminescence material comprises the following steps:
0.05mmol of barium nitrate, 0.05mmol of zinc nitrate, 0.05mmol of europium nitrate and 0.05mmol of 2, 6-dimethylterephthalic acid, 0.05mmol of 2, 5-dimethylterephthalic acid were mixed in a 5mL scintillation vial, and 1.5mL of N, N-dimethylformamide and 1mL of ethanol were added. The powder is dissolved and dispersed evenly by ultrasonic, and the ultrasonic frequency is 33 kHz. And screwing the cover of the scintillation vial, putting the scintillation vial into an oven at 80 ℃, and standing for 5 days to generate the metal organic framework crystal. And taking out the metal organic framework crystal, cleaning the surface of the crystal for 3 times by using N, N-dimethylformamide and ethanol, and drying at room temperature to obtain the product, namely the radiation photoluminescence material.
Example 5
A preparation method of a radiation photoluminescence material comprises the following steps:
0.05mmol of gadolinium nitrate, 0.05mmol of terbium nitrate, 0.1mmol of 4-methyl-2, 6-naphthalenedicarboxylic acid and 0.05mmol of tetramethylterephthalic acid were mixed in a 20mL scintillation vial, and 5mL of N, N-dimethylformamide and 5mL of water were added. The powder is dissolved and dispersed evenly by ultrasonic, and the ultrasonic frequency is 33 kHz. And screwing the cover of the scintillation vial, putting the scintillation vial into an oven at 80 ℃, and standing for 7 days to generate the metal organic framework crystal. And taking out the metal organic framework crystal, cleaning the surface of the metal organic framework crystal for 3 times by using N, N-dimethylformamide and ethanol, and drying at room temperature to obtain the product, namely the radiation photoluminescence material.
Comparative example 1
Silver glass dosimeter materials are available from CHIYADA.
Comparative example 2
A method of making a radiation photoluminescent material, substantially as described in example 1, except that the ligand is selected from 2, 5-dihydroxyterephthalic acid, which was tested to be free of radiation photoluminescence.
Comparative example 3
A method of making a radiation photoluminescent material, substantially as described in example 1, except that the ligand is selected from terephthalic acid, which was tested to be free of radiation photoluminescence.
Effect verification
The solid state spectrometer of CRAIC was used to perform the radiation photoluminescence detection of the synthesized radiation photoluminescence materials in the examples of the invention, and the detection results are shown in Table 1 below.
TABLE 1
| Group of | Upper limit of radiation measurement (Gy) |
| Example 1 | 3657 |
| Example 2 | 1007 |
| Example 4 | 477 |
| COMPARATIVE EXAMPLE 1 (silver glass dosimeter Material) | 10 |
| Comparative example 2 | No signal response |
| Comparative example 3 | No signal response |
It can be seen from fig. 1 and table 1 that the upper limit of the detected radiation value of the synthetic radiation photoluminescent material in the example group of the present invention is much larger than that of the comparative example group 1 (silver glass dosimeter material), and when the synthetic radiation photoluminescent materials in the comparative example groups 2 and 3 have no signal response, which indicates that the radiation photoluminescent materials in the comparative example groups 2 and 3 have no radiation photoluminescence phenomenon.
The technical features of the embodiments described above may be arbitrarily combined, and for the sake of brevity, all possible combinations of the technical features in the embodiments described above are not described, but should be considered as being within the scope of the present specification as long as there is no contradiction between the combinations of the technical features.
The above-mentioned embodiments only express several embodiments of the present invention, and the description thereof is more specific and detailed, but not construed as limiting the scope of the invention. It should be noted that, for a person skilled in the art, several variations and modifications can be made without departing from the inventive concept, which falls within the scope of the present invention. Therefore, the protection scope of the present patent shall be subject to the appended claims.
Claims (10)
1. A preparation method of a radiation photoluminescence material is characterized by comprising the following steps:
mixing soluble metal salt, a ligand and a solvent to obtain a mixed solution, synthesizing a metal organic framework crystal by adopting a solvothermal method for the mixed solution, cleaning and drying the metal organic framework crystal to obtain the radiation photoluminescence material, wherein the molar ratio of the soluble metal salt to the ligand is 1:10-10:1, a benzene ring of the ligand is connected with a methyl group, and the valence state of the soluble metal salt is divalent and/or trivalent.
2. The method of claim 1, wherein the soluble metal salt is at least one selected from the group consisting of lead nitrate, lead chloride, barium nitrate, bismuth nitrate, calcium nitrate, gadolinium nitrate, zinc nitrate, europium nitrate, and terbium nitrate.
3. The method of claim 1, wherein the ligand is at least one selected from the group consisting of 2-methyl terephthalic acid, 2, 5-dimethyl terephthalic acid, 2, 6-dimethyl terephthalic acid, tetramethyl terephthalic acid, and 4-methyl-2, 6-naphthalene dicarboxylic acid.
4. The method for producing a radiation photoluminescent material according to any one of claims 1 to 3, wherein the solvent is selected from at least one of N, N-dimethylformamide, dimethyl sulfoxide, N-dimethylacetamide, ethanol and water.
5. The method for producing a radiation photoluminescent material according to any one of claims 1 to 3, wherein in the step of synthesizing the metal organic framework crystal by a solvothermal method, the solvothermal temperature is 60 to 140 ℃.
6. A method of preparing a radiation photoluminescent material according to any one of claims 1 to 3, wherein the time of synthesis is from 3 to 7 days.
7. The method for producing a radiation photoluminescent material according to any one of claims 1 to 3, wherein in the step of mixing a soluble metal salt, a ligand and a solvent to obtain a mixed solution, the method further comprises subjecting the mixed solution to ultrasonic treatment.
8. The method of claim 7, wherein the sonication frequency is 33-40 kHz.
9. A radiation photoluminescent material prepared by the method for preparing radiation photoluminescence as recited in any one of claims 1 to 8.
10. Use of a radiation photoluminescent material according to claim 9 in the manufacture of a radiation photoluminescent dosimeter.
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| PCT/CN2020/137814 WO2021253774A1 (en) | 2020-06-18 | 2020-12-19 | Radiophotoluminescent material and preparation method and use |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112877714A (en) * | 2021-01-27 | 2021-06-01 | 浙江大学衢州研究院 | Double-defect ultrathin metal organic framework nanosheet catalyst and preparation method and application thereof |
| WO2021253774A1 (en) * | 2020-06-18 | 2021-12-23 | 苏州大学 | Radiophotoluminescent material and preparation method and use |
| CN115308786A (en) * | 2022-07-28 | 2022-11-08 | 李明皓 | Production process of latest LiF thermoluminescent material detector |
| CN115926179A (en) * | 2022-09-29 | 2023-04-07 | 苏州大学 | Thermoluminescent material based on metal organic framework and preparation method and application thereof |
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| CN116425989B (en) * | 2023-04-12 | 2024-06-21 | 苏州大学 | EPR radiation dosimeter material based on metal-organic framework and application thereof |
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| CN110128674B (en) * | 2019-05-31 | 2021-05-07 | 聊城大学 | Water-stable rare earth metal organic framework material for fluorescence detection of sulfonamide antibiotics and preparation method thereof |
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| CN103748064A (en) * | 2011-08-17 | 2014-04-23 | 株式会社可乐丽 | Metal complex and adsorbent material, storage material, and separating material comprising same |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021253774A1 (en) * | 2020-06-18 | 2021-12-23 | 苏州大学 | Radiophotoluminescent material and preparation method and use |
| CN112877714A (en) * | 2021-01-27 | 2021-06-01 | 浙江大学衢州研究院 | Double-defect ultrathin metal organic framework nanosheet catalyst and preparation method and application thereof |
| CN115308786A (en) * | 2022-07-28 | 2022-11-08 | 李明皓 | Production process of latest LiF thermoluminescent material detector |
| CN115926179A (en) * | 2022-09-29 | 2023-04-07 | 苏州大学 | Thermoluminescent material based on metal organic framework and preparation method and application thereof |
| CN115926179B (en) * | 2022-09-29 | 2023-10-27 | 苏州大学 | Thermoluminescent material based on metal organic frame and preparation method and application thereof |
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