Preparation method and application of a pure organic high-resolution glass scintillator

Abstract

The present application discloses a preparation method and application of a pure organic high-resolution glass scintillator, belonging to the technical fields of optical functional materials and detection technologies. The pure organic high-resolution glass scintillator is composed of any one of the following structural formulas: , or . The pure organic high-resolution glass scintillator of the present invention is a single-component light-emitting source, with a simple preparation method, a short preparation period, and no environmentally unfriendly elements such as lead, which is convenient for popularization and use. At the same time, the luminescence lifetimes of the pure organic high-resolution glass scintillators are all below 10 ns. The short luminescence lifetimes significantly avoid imaging afterimages caused by radiation afterglow, realizing an improvement in resolution and providing a new tool for the field of X-ray detection.

Description

Technical Field

[0001] The present invention relates to the field of optical functional materials and detection technologies, and particularly to a preparation method and application of a pure organic high-resolution glass scintillator. Background Art

[0002] Scintillators have a wide range of applications in fields such as medical imaging, industrial non-destructive testing, and security inspections. When exposed to ionizing radiation, scintillators have the ability to convert the absorbed radiation energy into visible light. The converted visible light can be easily detected and measured by detectors (such as photomultiplier tubes or solid-state photodetectors), thereby realizing the positioning and quantification of radiation sources.

[0003] The current scintillator technology mainly has the following defects: 1. The preparation process of traditional single-crystal scintillators is cumbersome, and the preparation process usually requires a high-temperature environment. 2. Inorganic scintillators and emerging perovskite scintillators usually use heavy metals to enhance the ability to absorb rays, and the presence of heavy metals often has an impact on the environment and human health. 3. In pure organic scintillators, their imaging usually relies on doping a polymer matrix to form a film for imaging. The limited doping concentration and low-density distribution of luminescent centers often result in poor imaging effects and low resolution.

[0004] In order to meet the diversification of social functions and the progress of science and technology, scintillators need to be continuously iterated and updated in terms of performance and quality. Therefore, the present invention is committed to developing a scintillator that has both the advantages of the above-mentioned materials and overcomes their disadvantages. Summary of the Invention

[0005] The purpose of the present invention is to overcome the deficiencies of the prior art and provide a preparation method and application of a pure organic high-resolution glass scintillator.

[0006] According to one aspect of the present invention, a pure organic high-resolution glass scintillator is provided, which is composed of any one of the following structural formulas:

[0007] 、 or 。

[0008] According to the second aspect of the present invention, a preparation method of the pure organic high-resolution glass scintillator is provided, and the preparation method is as follows:

[0009] S1. Using Dpbp as the luminescent center, modifying different halogen atoms Cl, Br, or I to obtain a luminescent molecule Dpbp-Cl, a luminescent molecule Dpbp-Br, or a luminescent molecule Dpbp-I;

[0010] S2. Weigh the luminescent molecule and place it in a glass groove. Heat the heating table until the temperature is stable, and then place the glass groove on the heating table;

[0011] S3. When the luminescent molecules start to melt into a melt, use a needle to stir to evenly spread the melt in the glass groove;

[0012] S4. Turn off the power of the heating stage, and the melt in S3 slowly cools to room temperature with the heating stage, and stand still to obtain a uniform and transparent pure organic high-resolution glass scintillator.

[0013] Further, the heating stage in S2 is heated to 145°C to 155°C, and the standing time in S4 is 4 to 6 minutes.

[0014] Further, the preparation method of the luminescent molecule Dpbp-Cl in S1 is as follows:

[0015] 。

[0016] Further, the preparation method of the luminescent molecule Dpbp-Br in S1 is as follows:

[0017] 。

[0018] Further, the preparation method of the luminescent molecule Dpbp-I in S1 is as follows:

[0019] 。

[0020] Further, the acquisition of the luminescent molecule Dpbp-Cl, the luminescent molecule Dpbp-Br or the luminescent molecule Dpbp-I in S1 also requires a purification step, and the purification step includes extraction, rotary evaporation, column chromatography and recrystallization.

[0021] Further, the extraction is liquid-liquid extraction using dichloromethane as the organic phase and water as the aqueous phase.

[0022] Further, the column chromatography uses a mixed system of petroleum ether and dichloromethane as the mobile phase and silica gel as the stationary phase.

[0023] According to the third aspect of the present invention, an application of the above-mentioned pure organic high-resolution glass scintillator in the field of X-ray detection is proposed.

[0024] Advantages of the present invention:

[0025] The scintillator provided by the present invention has low preparation cost, simple preparation method and short preparation cycle. The scintillator does not contain environmentally unfriendly elements such as lead, and has no special requirements for recycling and treatment, which is convenient for popularization and use.

[0026] Second, the scintillator provided by the present invention is a single-component light-emitting source, and its preparation method is to form a transparent glass state by low-temperature hot melting in a glass matrix and then cooling to room temperature.

[0027] Third, the luminescence lifetimes of the scintillators provided by the present invention are all below 10 ns. The relatively short luminescence lifetimes significantly avoid imaging afterimages caused by radiation afterglow, which helps to improve the resolution. BRIEF DESCRIPTION OF THE DRAWINGS

[0028] Figure 1 It is a state diagram of the pure organic high-resolution glass scintillator provided by the present invention under natural light;

[0029] Figure 2 It is an XRD diagram of the pure organic high-resolution glass scintillator provided by the present invention;

[0030] Figure 3 It is a transmittance diagram of the pure organic high-resolution glass scintillator provided by the present invention in the visible light region;

[0031] Figure 4 It is a photoluminescence spectrum diagram of the pure organic high-resolution glass scintillator provided by the present invention;

[0032] Figure 5 It is a photoluminescence lifetime decay diagram of the pure organic high-resolution glass scintillator provided by the present invention;

[0033] Figure 6 It is an X-ray luminescence spectrum diagram of the pure organic high-resolution glass scintillator provided by the present invention;

[0034] Figure 7 It is a stability diagram of the pure organic high-resolution glass scintillator provided by the present invention under X-rays. DETAILED DESCRIPTION OF THE EMBODIMENTS

[0035] The following further describes the present application in detail with reference to the drawings and embodiments. It can be understood that the specific embodiments described herein are only used to explain the related invention, rather than limiting the invention. Additionally, it should be noted that for the sake of description, only parts related to the relevant invention are shown in the drawings.

[0036] It should be noted that, without conflict, the embodiments in the present application and the features in the embodiments can be combined with each other. The following will describe the present application in detail with reference to the drawings and embodiments.

[0037] In view of the disadvantages of the current scintillator technology, such as the cumbersome preparation process, the participation of heavy metals, and the poor imaging effect, the first object of the present invention is to propose a pure organic high-resolution glass scintillator.

[0038] The second objective of the present invention is to propose a preparation method of the pure organic high-resolution glass scintillator, and the preparation method is simple and has a short cycle.

[0039] The third objective of the present invention is to propose an application of the pure organic high-resolution glass scintillator in the field of X-ray detection. The luminescence lifetimes of the scintillators are all below 10 ns. The short luminescence lifetimes significantly avoid imaging afterimages caused by radiation afterglow, which helps to improve the resolution.

[0040] Example 1: Preparation of the pure organic high-resolution glass scintillator

[0041] The preparation of the pure organic high-resolution glass scintillator is based on the luminescent molecule Dpbp-Cl, the luminescent molecule Dpbp-Br, or the luminescent molecule Dpbp-I. The luminescent molecule uses Dpbp as the luminescence center and modifies different halogen atoms Cl, Br, or I.

[0042] The specific preparation method of the luminescent molecule Dpbp-Cl is as follows:

[0043] 。

[0044] The specific preparation method of the luminescent molecule Dpbp-Br is as follows:

[0045] 。

[0046] The specific preparation method of the luminescent molecule Dpbp-I is as follows:

[0047] 。

[0048] After the above reaction, the obtained product is washed with dichloromethane and water to remove inorganic substances. After drying the solvent by evaporation, the product is purified by column chromatography (petroleum ether, dichloromethane system). Finally, the luminescent molecule Dpbp-Cl, the luminescent molecule Dpbp-Br, or the luminescent molecule Dpbp-I is obtained by recrystallization with a dichloromethane and petroleum ether system. Then, the pure organic high-resolution glass scintillator is prepared respectively according to the following steps, namely the scintillator of formula (I), the scintillator of formula (II), and the scintillator of formula (III) (corresponding to scintillator Dpbp-Cl, scintillator Dpbp-Br, and scintillator Dpbp-I in sequence):

[0049] (1) Weigh 100 mg of the luminescent molecule and place it in a glass groove of 1 cm * 1 cm * 0.3 cm;

[0050] (2) Heat the heating table to 150 °C. After the temperature is stable, place the glass groove containing the luminescent molecule in step (1) on the heating table;

[0051] (3) After placing the glass groove containing the luminescent molecules on the hot stage for several seconds in step (2), it is observed that the luminescent molecules start to melt, and a needle is used to stir the melt to spread it evenly on the glass groove;

[0052] (4) Turn off the power of the heating stage, and slowly cool the uniform melt obtained in S3 with the heating stage to room temperature;

[0053] (5) Place it at room temperature for 5 min to obtain the corresponding scintillator of the luminescent molecules.

[0054] The physical object of the prepared pure organic high-resolution glass scintillator is as Figure 1 shown. At the same time, the structural formula of the pure organic high-resolution glass scintillator is composed as follows:

[0055] .

[0056] Example 2: Performance test of pure organic high-resolution glass scintillator

[0057] To explore whether the pure organic high-resolution glass scintillator obtained in Test Example 1 forms an amorphous vitreous body after melting, XRD testing is carried out. As Figure 2 shown, the pure organic high-resolution glass scintillator has no obvious crystal structure after melting and forms an amorphous vitreous body. At the same time, as Figure 3 shown, the transmittance of the pure organic high-resolution glass scintillator remains at 80% in the range of 550 nm - 2500 nm, all showing good transparency.

[0058] Further test the luminescence performance of the pure organic high-resolution glass scintillator, Figure 4 and Figure 5 are respectively the photoluminescence spectrum diagram and the photoluminescence lifetime decay diagram of the pure organic high-resolution glass scintillator. From this, it can be obtained that the fluorescence emission peaks of the pure organic high-resolution glass scintillator are all located at 480 nm, the fluorescence lifetime of the scintillator of formula (Ⅰ) (i.e., scintillator Dpbp-Cl) is 4.5 ns; since the atomic number of Br is larger than that of Cl, resulting in a larger spin-coupling constant, therefore the fluorescence lifetime of the scintillator of formula (Ⅱ) (i.e., scintillator Dpbp-Br) is 2.4 ns; similarly, since a heavier I atom is introduced, resulting in a larger spin-coupling constant, therefore the fluorescence lifetime of the scintillator of formula (Ⅲ) (i.e., scintillator Dpbp-I) is 0.9 ns; the fluorescence lifetimes of the pure organic high-resolution glass scintillators are all below 10 ns, and the shorter luminescence lifetime significantly avoids the imaging afterimage caused by radiation afterglow, thereby improving the resolution.

[0059] Figure 6 This is the X-ray luminescence spectrum diagram of the pure organic high-resolution glass scintillator. The results show that the characteristic emission peaks of the radiation luminescence of the pure organic high-resolution glass scintillator are basically consistent with those of photoluminescence. And as Figure 7 shown, the pure organic high-resolution glass scintillator has good stability under X-rays.

[0060] The specific implementation manners of the present application have been described above, but the protection scope of the present application is not limited thereto. Any person skilled in the art within the technical scope disclosed by the present application can easily think of changes or substitutions, which should all be covered within the protection scope of the present application. Therefore, the protection scope of the present application shall be subject to the protection scope of the claims.

Claims

1. A pure organic high-resolution glass scintillator, characterized in that: It is composed of any of the following structural formulas:

2. A method for preparing a pure organic high-resolution glass scintillator as claimed in claim 1, characterized in that: The preparation method is as follows: S1. Using Dpbp as the luminescent center, modify different halogen atoms Cl or I to obtain the luminescent molecule Dpbp-Cl or the luminescent molecule Dpbp-I; S2, weighing the luminescent molecule and placing it in a glass groove, heating the heating platform until the temperature is stable, and then placing the glass groove on the heating platform; S3, when the luminescent molecules begin to melt into a melt, stirring with a needle to make the melt spread evenly in the glass groove; S4, turning off the power of the heating platform, and the melt in S3 is slowly cooled to room temperature along with the heating platform, and is left to stand to obtain a uniform and transparent pure organic high-resolution glass scintillator.

3. The method for preparing a pure organic high-resolution glass scintillator according to claim 2, characterized in that: The heating stage in S2 is heated to 145° C. to 155° C., and the standing time in S4 is 4 to 6 minutes.

4. The method for preparing a pure organic high-resolution glass scintillator according to claim 2, characterized in that: The preparation method of the luminescent molecule Dpbp-Cl in S1 is as follows:

5. The method for preparing a pure organic high-resolution glass scintillator according to claim 2, characterized in that: The preparation method of the luminescent molecule Dpbp-I in S1 is as follows:

6. The method for preparing a pure organic high-resolution glass scintillator according to claim 2, characterized in that: The acquisition of the luminescent molecule Dpbp-Cl or the luminescent molecule Dpbp-I in S1 further requires a purification step, which includes extraction, rotary evaporation, column chromatography and recrystallization.

7. The method for preparing a pure organic high-resolution glass scintillator according to claim 6, characterized in that: The extraction is performed by using dichloromethane as an organic phase and water as an aqueous phase to perform liquid-liquid extraction.

8. The method for preparing a pure organic high-resolution glass scintillator according to claim 6, characterized in that: The column chromatography uses a mixed system of petroleum ether and dichloromethane as a mobile phase and silica gel as a stationary phase.

9. An application of the pure organic high-resolution glass scintillator as claimed in claim 1 in the field of X-ray detection.

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