CN112898961B - Organic-inorganic hybrid scintillator and preparation method and application thereof - Google Patents
Organic-inorganic hybrid scintillator and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses an organic-inorganic hybrid scintillator and a preparation method and application thereof, wherein the molecular formula of the organic-inorganic hybrid scintillator is C 10 H 22 The preparation method of the NCuBrI comprises the following steps: dissolving N-methyl-N-butyl piperidine bromide and cuprous iodide in N, N-dimethylformamide to obtain a mixed solution; dripping an anti-solvent into the mixed solution under the condition of stirring to obtain a mixture; and washing and drying the mixture to obtain the organic-inorganic hybrid scintillator. The preparation method is simple and low in cost, the substrates used in the preparation method are commercially available and low-cost raw materials, the prepared organic-inorganic hybrid scintillator has the characteristics of high brightness and high stability, the copper element is completely non-toxic, the organic-inorganic hybrid scintillator has excellent luminous performance under X-ray excitation, the emission waveband range is wide, the photon yield is 25000photons/MeV, the commercial standard is reached, and the organic-inorganic hybrid scintillator can be applied to X-ray fluorescence imaging.
Description
Technical Field
The invention relates to the technical field of scintillating materials, in particular to an organic-inorganic hybrid scintillator and a preparation method and application thereof.
Background
The scintillator can absorb high-energy rays and convert the high-energy rays into visible photons with lower energy, and has important application in a plurality of fields such as X-ray imaging, radiation monitoring, safety inspection, nuclear physics and the like.
The traditional scintillators are divided into two categories of inorganic scintillators and organic scintillators, the inorganic scintillators are mostly synthesized by a high-temperature melting method, the energy required by high temperature is large, and the cost is high; most organic scintillators are easily soluble in solvents such as alcohols, ketones, dilute acid and alkali, and have low luminous intensity, so that the application of the scintillators in the imaging field is limited.
Accordingly, the prior art is yet to be improved and developed.
Disclosure of Invention
The invention aims to solve the technical problems that the existing scintillator is high in preparation cost and low in luminous intensity and cannot be applied to the field of imaging.
The technical method adopted by the invention for solving the technical problemThe scheme is as follows: an organic-inorganic hybrid scintillator, wherein the chemical formula of the scintillator is C 10 H 22 NCuBrI。
The organic-inorganic hybrid scintillator, wherein the photon yield of the scintillator is 25000photons/MeV.
A preparation method of an organic-inorganic hybrid scintillator comprises the following steps:
dissolving N-methyl-N-butyl piperidine bromide and cuprous iodide in N, N-dimethylformamide to obtain a mixed solution;
dripping an anti-solvent into the mixed solution under the condition of stirring to obtain a mixture;
and washing and drying the mixture to obtain the organic-inorganic hybrid scintillator.
The preparation method of the organic-inorganic hybrid scintillator comprises the following steps of 1-1.2 molar ratio of N-methyl-N-butyl piperidine bromide to cuprous iodide.
The preparation method of the organic-inorganic hybrid scintillator comprises the following steps of (1-1.5mL).
The preparation method of the organic-inorganic hybrid scintillator comprises the step of dissolving the organic-inorganic hybrid scintillator in an organic solvent.
The preparation method of the organic-inorganic hybrid scintillator comprises the following steps of (1) enabling the volume ratio of diethyl ether to N, N-dimethylformamide to be 5-10: 1.
the preparation method of the organic-inorganic hybrid scintillator comprises the following steps: washing with ether for 3-5 times.
The preparation method of the organic-inorganic hybrid scintillator comprises the following steps of drying at the temperature of 50-70 ℃ for 5-10 min.
The application of the organic-inorganic hybrid scintillator in X-ray fluorescence imaging.
Has the advantages that: the preparation method is simple and low in cost, the substrates used in the preparation method are all raw materials which are commercially available and low in cost, the prepared organic-inorganic hybrid scintillator has the characteristics of high brightness and high stability, copper element is completely non-toxic, the organic-inorganic hybrid scintillator has excellent luminous performance under X-ray excitation, the emission waveband range is wide, the photon yield is 25000photons/MeV, the commercial standard is reached, and the organic-inorganic hybrid scintillator can be applied to X-ray fluorescence imaging.
Drawings
FIG. 1 is a chemical synthesis equation of an organic-inorganic hybrid scintillator according to an embodiment of the present invention;
FIG. 2 is a single crystal analysis structural diagram of an organic-inorganic hybrid scintillator prepared in an example of the present invention;
FIG. 3 is a powder XRD pattern of an organic-inorganic hybrid scintillator prepared according to an example of the present invention;
FIG. 4 is a fluorescence spectrum of an organic-inorganic hybrid scintillator prepared according to an embodiment of the present invention;
FIG. 5 is an X-ray excitation spectrum of an organic-inorganic hybrid scintillator prepared according to an example of the present invention;
FIG. 6 is an X-ray excitation spectrum of comparative CsI (Tl) of the organic-inorganic hybrid scintillator prepared in the example of the present invention;
FIG. 7 is a graph of the radiation stability of organic-inorganic hybrid scintillators prepared in accordance with embodiments of the invention under X-ray irradiation.
Detailed Description
The invention provides an organic-inorganic hybrid scintillator, and a preparation method and application thereof, and the invention is further described in detail below in order to make the purpose, technical scheme and advantages of the invention clearer and clearer. It should be understood that the specific embodiments described herein are merely illustrative of the invention and do not limit the invention.
The traditional scintillators are divided into two categories of inorganic scintillators and organic scintillators, the inorganic scintillators are mostly synthesized by a high-temperature melting method, the energy required at high temperature is large, and the cost is high; most organic scintillators are easily soluble in solvents such as alcohols, ketones, dilute acid and alkali, and have low luminous intensity, so that the application of the scintillators in the imaging field is limited.
Perovskite scintillators developed recently can be prepared by a solution method at low temperature, have high luminous performance and well solve the problems of the traditional inorganic scintillators and organic scintillators. However, pb in perovskite is a toxic element, and perovskite itself has poor stability, so that it cannot be applied to commercial production.
In order to solve the above problems, the present invention provides an organic-inorganic hybrid scintillator, wherein the organic-inorganic hybrid scintillator has a chemical formula of C 10 H 22 The organic component of NCuBrI is N-methyl-N-butyl piperidine bromide, the inorganic component is cuprous iodide, the organic-inorganic hybrid scintillator has the characteristics of high brightness and high stability, and the copper element is non-toxic, so that the organic-inorganic hybrid scintillator can be applied to the fields of X-ray imaging, radiation imaging, safety inspection, petroleum exploration, nuclear physics and the like.
Furthermore, the organic-inorganic hybrid scintillator has excellent luminescence property under the excitation of X-rays, the emission peak position is 465nm, the emission waveband range is wide, the photon yield is 25000photons/MeV, the commercial standard is reached, so that clear images can be formed under the X-rays, and an X-ray imaging fluorescent screen can be prepared.
The invention also provides a preparation method of the organic-inorganic hybrid scintillator, which comprises the following steps:
s1, dissolving N-methyl-N-butyl piperidine bromide and cuprous iodide in N, N-dimethylformamide to obtain a mixed solution.
The solid inorganic scintillator generally refers to an inorganic salt crystal containing a small amount of a mixture, wherein a cuprous iodide crystal is used as a semiconductor material, has a large forbidden band width, is opposite to spin-orbit splitting, has good diamagnetism and fast ion conductivity, is considered to be an inorganic scintillator material with the fastest time response, and most of organic scintillators belong to aromatic hydrocarbon compounds with benzene ring structures. In the embodiment, N-methyl-N-butyl piperidine bromide is used as an organic component, cuprous iodide is used as an inorganic component to prepare the organic-inorganic hybrid scintillator, substrates used in the preparation process are all commercially available raw materials with low cost, and the preparation cost is low. In the specific preparation process, N-methyl-N-butyl piperidine bromide and cuprous iodide are dissolved in an organic solvent N, N-dimethylformamide to obtain a mixed solution, N, N-dimethylformamide is used as a good solvent with wide application, and the N-methyl-N-butyl piperidine bromide and cuprous iodide have good solubility and chemical stability, so that the N-methyl-N-butyl piperidine bromide and the cuprous iodide can be uniformly dispersed in the mixed solution.
And S2, dropwise adding the anti-solvent into the mixed solution under the stirring condition to obtain a mixture.
Specifically, in the method for precipitating solute by using the antisolvent in this embodiment, after dissolving N-methyl-N-butylpiperidinium bromide and cuprous iodide in N, N-dimethylformamide, stirring the obtained mixed solution, and dropwise adding the antisolvent into the mixed solution under the stirring condition at normal temperature, cu is formed by the cuprous iodide and N-methyl-N-butylpiperidinium bromide in the N, N-dimethylformamide 2 Br 2 I 2 2- The coordination ions form a tetragonal structure, and organic ammonium ions in the N-methyl-N-butyl piperidinium bromide fill in gaps of the coordination ions and are separated out under the action of an anti-solvent to form a precipitate. In the embodiment, the organic-inorganic hybrid scintillator is formed by the anti-solvent at normal temperature, the synthesis step is simple, energy-consuming operations such as high-temperature heating are not needed, the preparation cost is low, and the copper element in the prepared organic-inorganic hybrid scintillator is completely non-toxic.
In one embodiment, the anti-solvent is diethyl ether, and the reaction formula of N-methyl-N-butyl piperidinium bromide and cuprous iodide with diethyl ether as the anti-solvent is shown in FIG. 1, wherein cuprous iodide and N-methyl-N-butyl piperidinium bromide form Cu in N, N-dimethylformamide 2 Br 2 I 2 2- Coordination ion, organic ammonium ion in N-methyl-N-butyl piperidine bromide filled in Cu 2 Br 2 I 2 2- In the complex ions, precipitates are separated out under the action of diethyl ether to form precipitates.
Too much N-methyl-N-butyl piperidine bromide or cuprous iodide is added, which wastes raw materials, and too little N-methyl-N-butyl piperidine bromide or cuprous iodide is added, which cannot react sufficiently to form coordination ions. In a specific embodiment, the molar ratio of the N-methyl-N-butyl piperidine onium bromide to the cuprous iodide is 1-1.2, the volume-to-mass ratio of the N, N-dimethylformamide to the cuprous iodide is 1-1.5 mL.
The ether used as an anti-solvent of the reaction can influence the precipitation speed of the N-methyl-N-butyl piperidine bromide and cuprous iodide, and further influence the performance of the generated organic-inorganic hybrid scintillator. In one embodiment, the volume ratio of diethyl ether to N, N-dimethylformamide is 5 to 10:1, the organic-inorganic hybrid scintillator prepared in the proportion has the characteristics of high brightness and high stability.
And S3, washing and drying the mixture to obtain the organic-inorganic hybrid scintillator.
Considering that the surface of the formed precipitate can be attached with raw materials, solvents and the like which are not completely reacted after the reaction is finished, after the mixture is obtained in the embodiment, the solvent is removed from the mixture, then the mixture is washed for 3 to 5 times by using ether, and then the mixture is dried for 5 to 10min at the temperature of between 50 and 70 ℃ to obtain the organic-inorganic hybrid scintillator.
The invention also provides an application of the organic-inorganic hybrid scintillator in X-ray fluorescence imaging. The organic-inorganic hybrid scintillator prepared by the invention has the characteristics of high brightness and high stability, has excellent luminous performance under the excitation of X-rays, has an emission peak position of 465nm, a wide emission waveband range and a photon yield of 25000photons/MeV, reaches the commercial standard, and can be applied to X-ray fluorescence imaging. The X-ray fluorescence imaging principle of the organic-inorganic hybrid scintillator prepared by the invention is as follows: different substances have different absorption degrees for X-rays at different positions due to uneven density, thickness and substance distribution. Correspondingly, the attenuation degree of the X-ray after penetrating the object is different, and an image formed by points with different brightness can be obtained on the fluorescent screen by utilizing the principle, which is called X-ray imaging. Under the condition of a certain projection thickness, a dark area in the image shows that the area has strong absorption to X-rays; on the contrary, the bright area in the image indicates that the area has weak absorption of X-rays, and the observer can determine the property of the object by combining the image with the density, thickness and other factors of the object.
The invention is further illustrated by the following specific examples.
Example 1
(1) Dissolving N-methyl-N-butyl piperidine bromide and cuprous iodide in a molar ratio of 1;
(2) And dropwise adding diethyl ether into the mixed solution under stirring to obtain a mixture, wherein the volume ratio of the diethyl ether to the N, N-dimethylformamide is 6:1;
(3) And filtering the mixture, washing the mixture for 3 times by using diethyl ether, and drying the washed mixture at 60 ℃ for 10min to obtain the organic-inorganic hybrid scintillator.
Example 2
(1) Dissolving N-methyl-N-butyl piperidine bromide and cuprous iodide in a molar ratio of 1.1 in N, N-dimethylformamide to obtain a mixed solution;
(2) And dropwise adding diethyl ether into the mixed solution under the stirring condition to obtain a mixture, wherein the volume ratio of the diethyl ether to the N, N-dimethylformamide is 8:1;
(3) And filtering the mixture, washing the mixture for 3 times by using diethyl ether, and drying the washed precipitate at the temperature of 60 ℃ for 10min to obtain the organic-inorganic hybrid scintillator.
Example 3
(1) Dissolving N-methyl-N-butyl piperidine bromide and cuprous iodide in a molar ratio of 1.2 in N, N-dimethylformamide to obtain a mixed solution;
(2) And dropwise adding diethyl ether into the mixed solution under stirring to obtain a mixture, wherein the volume ratio of the diethyl ether to the N, N-dimethylformamide is 10:1;
(3) And filtering the precipitate, washing the precipitate with diethyl ether for 3 times, and drying the washed precipitate at 60 ℃ for 10min to obtain the organic-inorganic hybrid scintillator.
FIG. 2 is a single crystal analysis structure diagram of an organic-inorganic hybrid scintillator prepared in an example of the present invention, and it can be seen from FIG. 2 that Cu (I) forms Cu with a halogen in N-methyl-N-butylpiperidinium bromide 2 Br 2 I 2 2- Complex ions ofThe ions form a tetragonal structure, and organic ammonium ions fill in the gaps of the coordination ions.
Fig. 3 is a powder XRD pattern of the organic-inorganic hybrid scintillator prepared in the example of the present invention, and fig. 3 is very similar to the XRD pattern obtained by fitting the single crystal structure, which shows that the organic-inorganic hybrid scintillator prepared in this example is pure phase and does not need further purification.
Fig. 4 is a fluorescence spectrum of the organic-inorganic hybrid scintillator prepared in the embodiment of the present invention, and as can be seen from fig. 4, the main fluorescence emission peak of the organic-inorganic hybrid scintillator prepared in the embodiment of the present invention is located at 465nm, another weaker peak is located at 630nm, the emission band is 380-800 nm, the emission range is very wide, the fluorescence quantum yield of the organic-inorganic hybrid scintillator is 99.5%, and the fluorescence color is bluish white.
Fig. 5 is an X-ray excitation spectrum of the organic-inorganic hybrid scintillator prepared in the example of the present invention, and it can be seen from fig. 5 that the position of the X-ray excitation spectrum peak of the organic-inorganic hybrid scintillator is 465nm, which is consistent with the position of the main peak of the fluorescence spectrum, indicating that the intrinsic mechanisms of light emission of the two are likely to be consistent, and no obvious X-ray excitation emission peak is observed at 630 nm.
Fig. 6 is an X-ray excitation spectrum of a comparative CsI (Tl) of the organic-inorganic hybrid scintillator prepared in the example of the present invention, the CsI (Tl) is a general reference substance for measuring photon yield, and the photon yield of the measured substance can be estimated by comparing the integrated value of the excitation spectrum of the measured substance and the CsI (Tl) under the same conditions. Through calculation, the fluorescence quantum yield of the organic-inorganic hybrid scintillator prepared by the embodiment of the invention reaches 99%, the photon yield is 25000photons/MeV, and the value reaches the standard of commercial inorganic scintillators, so that the organic-inorganic hybrid scintillator has commercial potential.
FIG. 7 is a graph showing the radiation stability of the organic-inorganic hybrid scintillator prepared in the example of the present invention under the irradiation of X-rays, and it can be seen from FIG. 7 that the organic-inorganic hybrid scintillator prepared in the example of the present invention has no significant attenuation of the emission intensity within 20 minutes under the continuous irradiation of X-rays, which indicates that the radiation stability is good, and the organic-inorganic hybrid scintillator can be applied to practical applications
In summary, the invention discloses an organic-inorganic hybrid scintillator, a preparation method and an application thereof, wherein the molecular formula of the organic-inorganic hybrid scintillator is C 10 H 22 NCuBrI, and the preparation method comprises the following steps: dissolving N-methyl-N-butyl piperidine bromide and cuprous iodide in N, N-dimethylformamide to obtain a mixed solution; dripping an anti-solvent into the mixed solution under the condition of stirring to obtain a mixture; and washing and drying the mixture to obtain the organic-inorganic hybrid scintillator. The preparation method is simple and low in cost, the substrates used in the preparation method are all commercially available and low-cost raw materials, the prepared organic-inorganic hybrid scintillator has the characteristics of high brightness and high stability, the copper element is completely non-toxic, the organic-inorganic hybrid scintillator has excellent luminous performance under the excitation of X rays, the emission waveband range is wide, the photon yield is 25000photons/MeV, the commercial standard is reached, and the organic-inorganic hybrid scintillator can be applied to X-ray fluorescence imaging.
It is to be understood that the invention is not limited to the examples described above, but that modifications and variations may be effected thereto by those of ordinary skill in the art in light of the foregoing description, and that all such modifications and variations are intended to be within the scope of the invention as defined by the appended claims.
Claims (9)
1. An organic-inorganic hybrid scintillator, wherein the chemical formula of the scintillator is C 10 H 22 NCuBrI; the organic component in the organic-inorganic hybrid scintillator is N-methyl-N-butyl piperidine bromide, and the inorganic component is cuprous iodide; the emission peak position of the scintillator is 465nm; the photon yield of the scintillator was 25000photons/MeV.
2. A preparation method of an organic-inorganic hybrid scintillator is characterized by comprising the following steps:
dissolving N-methyl-N-butyl piperidine bromide and cuprous iodide in N, N-dimethylformamide to obtain a mixed solution;
dripping an anti-solvent into the mixed solution under the condition of stirring to obtain a mixture;
and washing and drying the mixture to obtain the organic-inorganic hybrid scintillator.
3. The method for preparing an organic-inorganic hybrid scintillator according to claim 2, wherein the molar ratio of N-methyl-N-butylpiperidinium bromide to cuprous iodide is 1 to 1.2.
4. The method for preparing an organic-inorganic hybrid scintillator according to claim 2, wherein the volume-to-mass ratio of N, N-dimethylformamide to cuprous iodide is 1 to 1.5ml.
5. The method of preparing an organic-inorganic hybrid scintillator according to claim 2, wherein the anti-solvent is diethyl ether.
6. The method for preparing an organic-inorganic hybrid scintillator according to claim 5, wherein the volume ratio of the diethyl ether to the N, N-dimethylformamide is 5 to 10:1.
7. the method for preparing an organic-inorganic hybrid scintillator according to claim 2, wherein the washing conditions are: washing with ether for 3-5 times.
8. The method for preparing an organic-inorganic hybrid scintillator according to claim 2, wherein the drying temperature is 50 to 70 ℃ and the drying time is 5 to 10min.
9. Use of the organic-inorganic hybrid scintillator of claim 1 in X-ray fluorescence imaging.
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