CN110526824A - Beta scintillator and preparation method thereof based on additive Mn two dimension halogen perovskite - Google Patents
Beta scintillator and preparation method thereof based on additive Mn two dimension halogen perovskite Download PDFInfo
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- CN110526824A CN110526824A CN201910709403.6A CN201910709403A CN110526824A CN 110526824 A CN110526824 A CN 110526824A CN 201910709403 A CN201910709403 A CN 201910709403A CN 110526824 A CN110526824 A CN 110526824A
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- C07C209/00—Preparation of compounds containing amino groups bound to a carbon skeleton
- C07C209/68—Preparation of compounds containing amino groups bound to a carbon skeleton from amines, by reactions not involving amino groups, e.g. reduction of unsaturated amines, aromatisation, or substitution of the carbon skeleton
- C07C209/74—Preparation of compounds containing amino groups bound to a carbon skeleton from amines, by reactions not involving amino groups, e.g. reduction of unsaturated amines, aromatisation, or substitution of the carbon skeleton by halogenation, hydrohalogenation, dehalogenation, or dehydrohalogenation
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Abstract
The present invention relates to a kind of beta scintillator and preparation method thereof based on additive Mn two dimension halogen perovskite, the beta scintillator is the two-dimentional halogen perovskite XA of additive Mn2PbBr4: Mn, wherein, XA represents halogenation organic amine, and by low temperature liquid phase reaction, centrifugal drying, grinding, annealing, the high-volume synthesis of the material can be realized, the beta scintillator of preparation is had excellent performance, it is strong to the tolerance of high-power electron beam, there is stronger hydrophobicity, be not easy to deliquesce, it is easily stored, and its fluorescence efficiency can reach 60%.
Description
Technical field
The present invention relates to a kind of scintillator materials for beta-ray detection, more particularly, to one kind based on additive Mn two dimension
The beta scintillator and preparation method thereof of halogen perovskite, belongs to nano material technology application field.
Background technique
β particle refers to when β decay, the high energy electron emitted occur for radioactive substance.In β decay, radioactive atom
Core is changed into another seed nucleus by launching electronics and neutrino, and the electronics in product is thus referred to as β particle.β ray is exactly by β
Molecular high-energy ray.β radial energy penetrates skin, the change for causing cytochemistry to balance, so as to cause canceration.Therefore, β is penetrated
The detection of line and protection are most important.
Ideal beta scintillator should have following speciality: 1) photoelectric effect ratio is big, has high light extraction efficiency；2)
Density is big, prevents ability strong on β ray；3) strong to Beta-ray tolerance.Common scintillation crystal can be divided into two classes: inorganic
Scintillator and organic scintillator.Wherein, inorganic scintillator includes NaI (Tl), CsI (Tl), CsI (Na), ZnS (Ag), bismuth germanium oxide
(Bi4Ge3O12, BGO) etc.；Organic scintillator can be divided into organic crystal scintillator, liquid scintillator and plastic scintillant again.Its
In, NaI (Tl), CsI (Tl), CsI (Na) are easily deliquesced, and ZnS (Ag) is long placed in humid air, can gradually be oxidized to zinc sulfate；
The price of bismuth germanium oxide is very expensive；Organic scintillator non-refractory, and volume is not allowed to be easy to do greatly, use condition is limited.Therefore, it opens
It is significant to send out beta scintillator novel.
Halogen perovskite is a kind of material with excellent photoelectric characteristic of new development in recent years, one of them draws very much
The advantage that people gazes at is exactly that the cost of halogen perovskite is very low, and prepares simple.Some researches show that three-dimensional halogen perovskite exists
Cathode-luminescence can be issued under high-power electron beam effect, however, since the bonding of three-dimensional halogen perovskite is poor, to high energy electron
The tolerance of beam is very poor, easily decomposes under long duration of action, so being not appropriate for for doing beta-ray detection.Two-dimentional halogen calcium titanium
Mine is one of three-dimensional halogen perovskite variant, and organic component, this organic component energy are introduced in two-dimentional halogen perovskite
It is enough to realize stronger chemical bonding in two-dimentional halogen perovskite, improve its chemical stability.Meanwhile organic component is hydrophobic in
Group can be realized its self assembly in two-dimentional halogen perovskite, form one layer of fine and close hydrophobic layer on surface, protection is internal
Photoelectric functional structure not by the injury of steam.Importantly, organic component is mainly by three kinds of carbon, hydrogen, nitrogen light element groups
At they and Beta-ray interact can reduce rapidly Beta-ray energy compared to heavy element, so that it be made to reach internal
Stronger fluorescence signal is inspired when photoelectric functional layer, improves capacity switching signal.But intrinsic two-dimentional halogen perovskite is glimmering
Light efficiency is generally weaker, and commercial scintillator preparation requires the temperature more than 1700 DEG C, and complicated for operation, controllably
Property is poor.
Summary of the invention
The present invention is directed to propose a kind of beta scintillator and preparation method thereof based on additive Mn two dimension halogen perovskite,
β ray signal can be converted to visible light signal, to carry out quantitative analysis to β ray.
Realize technical solution of the invention are as follows: the beta scintillator based on additive Mn two dimension halogen perovskite, it is described
Beta scintillator be additive Mn two-dimentional halogen perovskite XA2PbBr4: Mn, wherein XA represents halogenation organic amine.
The preparation method of beta scintillator based on additive Mn two dimension halogen perovskite, includes the following steps:
Step 1: lead bromide and bromination halogen amine are dissolved into dimethyl sulfoxide or dimethylformamide, form a certain concentration
Presoma；
Step 2: above-mentioned presoma being placed in the toluene solution of excessive preheating, stirs sufficiently reaction a period of time；
Step 3: gained precipitating is extracted by way of centrifugation, is then cleaned with toluene, repeated centrifugation-cleaning
Operation is multiple, until dimethyl sulfoxide or dimethylformamide are cleaned up；
Step 4: the precipitated product after cleaning is dried in such a way that room temperature in vacuo is dry, toluene solvant is removed, obtains
Desciccate；
Step 5: above-mentioned desciccate and manganese salt are subjected to mixed grinding, places it in protective gas and moves back after being fully ground
Fire processing, obtains final product.
Preferably, in step 1, bromination halogen amine includes that bromination butylamine, bromination octylame, bromination lauryl amine, bromination octadecylamine exist
A series of interior bromination halogen amine.
Preferably, in step 1, lead bromide and bromination halogen amine are dissolved into dimethyl sulfoxide or dimethylformamide,
Form the presoma of the M concentration of 0.05 M ~ 1.
Preferably, in step 2, excessive toluene refers to that volume is no less than 2 times of presoma of toluene.
Preferably, in step 2, the toluene solution of preheating refers to 60 ~ 400 DEG C of toluene solution.
Preferably, in step 2, sufficiently reaction refers to that the reaction time is no less than 2 min.
Preferably, in step 5, common manganese salt of the manganese salt including manganous bromide, manganese acetate.
Preferably, it in step 5, is fully ground and refers to that milling time is no less than 5 min.
Preferably, in step 5, annealing temperature is not less than 60 DEG C, and annealing time is no less than 5 min.
Compared with prior art, the invention has the advantages that
(1) synthetic method of the present invention is simple, at low cost, and all synthetic operations can carry out under room temperature environment.
(2) beta scintillator of the present invention is had excellent performance, and strong to the tolerance of high-power electron beam, high reliablity.
Detailed description of the invention
Fig. 1 is the SEM picture of exemplary two dimensional halogen perovskite.
Fig. 2 is the XRD spectrum of typical additive Mn and pure phase two dimension halogen perovskite.
Fig. 3 is the Fluorescent Characterization map of exemplary two dimensional halogen perovskite.
Fig. 4 is spectrum of the exemplary two dimensional halogen perovskite under β actinism.
Fig. 5 is two-dimentional halogen perovskite in the spectral response long lasting for β actinism.
Fig. 6 is the paper-cut exposure mask for β radial imaging.
Fig. 7 is β imaging test image obtained.
Fig. 8 is the heat of the two-dimentional halogen perovskite beta scintillator described in embodiment 1 based on additive Mn bromination octadecylamine
Resurvey test result.
Fig. 9 is the XRD spectrum of the two-dimentional halogen perovskite described in embodiment 3 based on bromination butylamine.
Specific embodiment
Below with reference to embodiment and attached drawing, the invention will be further described.
The invention proposes a kind of additive Mn two dimension halogen perovskite materials to be used for efficient beta-ray detection.Manganese ion is two
It ties up as the new centre of luminescence in halogen perovskite, so that the electron hole pair lost originally by non-radiative recombination, it can
It is recycled by the manganese centre of luminescence and is converted into optical signal.Its fluorescence efficiency can achieve 60%.
Manganese element serves as the centre of luminescence in two-dimentional halogen perovskite main body, and β ray excites the electron-hole in main body
Right, electron hole pair is then transferred to manganese centre of luminescence site, and radiation recombination occurs to generate fluorescence signal.Fluorescence signal it is strong
Degree enhances with the increase of Beta-ray intensity, it is possible to carry out quantitative detection to β ray as scintillator using the material
And imaging.
Example 1
Step 1, the bromination octadecylamine of 0.1442 g and 0.7340 g lead bromide are dissolved in the dimethyl sulfoxide of 10 ml, shape
The precursor solution for being 0.2 M at concentration；
Step 2, above-mentioned precursor solution is added in the 100 ml toluene solutions heated at 100 DEG C in advance, stirring is anti-
It answers, has a large amount of white precipitates in solution at this time and be precipitated.Sufficiently 30 min of reaction；
Step 3, above-mentioned precipitating is extracted by way of centrifugation, centrifugal rotational speed is 6000 rpm, centrifugation time 1
min.Above-mentioned precipitating is cleaned with toluene later.Repeated centrifugation-cleaning operation is three times；
Step 4, above-mentioned precipitated product is placed in a vacuum drying oven and is dried in vacuo, remove toluene solvant；
Step 5, it by the above-mentioned drying precipitated manganous bromide mixed grinding with 0.0043 g, is fully ground after 30 min, by product
It is placed on the warm table in glove box and is made annealing treatment, annealing temperature is 100 DEG C.
Fig. 1 is the SEM photograph of final product, it can be seen that synthesized two-dimentional halogen perovskite has apparent two dimension
Layer structure is consistent with its crystal structure, illustrates it with good crystallinity.Fig. 2 be doping manganese element before with doping manganese
The XRD spectrum of product after element, it can be seen that additive Mn and the crystal structure that two-dimentional halogen perovskite is not significantly changed.Fig. 3 and
Fig. 4 is emission spectrum of the two-dimentional halogen perovskite of doping manganese under ultraviolet light and β actinism respectively, it can be seen that β is penetrated
Line can effectively inspire the fluorescence signal of additive Mn two dimension halogen perovskite as ultraviolet light.In long-time β actinism
Under, the spectral response for adulterating the two-dimentional halogen perovskite of manganese is highly stable, as shown in figure 5, it is good to illustrate that the scintillator has
Electronics tolerance.Using the scintillation properties that the scintillator is excellent to β ray, beta-ray detection can be not only carried out, can also be carried out
β radial imaging application.About β radial imaging, we cut out tri- monograms conducts of NJ, JU, ST by paper-cut and cover first
Film controls Beta-ray spatial distribution as shown in fig. 6, then the exposure mask is placed between beta ray source and scintillator material.Fig. 7
The β radial imaging that obtains as a result, can be clearly seen that the shape of paper-cut, illustrate the scintillator have good β ray at
As ability.Fig. 8 is the thermal gravimetric analysis results of product, it can be seen that the product will not be thermally decomposed at 300 DEG C or less, and heat is steady
It is qualitative good.
Example 2
The present embodiment is substantially the same manner as Example 1, unique the difference is that the dimethyl sulfoxide in step 1 has changed dimethyl formyl into
Amine, product obtained and example 1 are essentially identical.
Example 3
The present embodiment is substantially the same manner as Example 1, uniquely the difference is that the bromination octadecylamine in step 1 has changed bromination butylamine into,
Product obtained and the product obtained of example 1 have similar optical property, and XRD spectrum is as shown in Figure 9.
Example 4
The present embodiment is substantially the same manner as Example 1, uniquely the difference is that the heating temperature in step 2 has been changed to 150 DEG C, is obtained
The product and example 1 obtained is essentially identical.
Example 5
The present embodiment is substantially the same manner as Example 1, uniquely the difference is that the reaction time in step 2 has been changed to 60 min, is obtained
The product and example 1 obtained is essentially identical.
Example 6
The present embodiment is substantially the same manner as Example 1, uniquely the difference is that the manganous bromide in step 5 has been changed to manganese acetate, is obtained
Product and example 1 it is essentially identical.
Example 7
The present embodiment is substantially the same manner as Example 1, uniquely the difference is that the milling time in step 5 has been changed to 60 min, is obtained
The product and example 1 obtained is essentially identical.
Comparative example 1
This comparative example is substantially the same manner as Example 1, unique the difference is that the toluene in step 2 has changed hexane, production obtained into
Object does not have fluorescent effect.
Comparative example 2
This comparative example is substantially the same manner as Example 1, unique the difference is that not making annealing treatment to doped products, obtained product
Do not have the fluorescence signal of manganese after milling.
Claims (10)
1. the beta scintillator based on additive Mn two dimension halogen perovskite, which is characterized in that the beta scintillator is manganese
The two-dimentional halogen perovskite XA of doping2PbBr4: Mn, wherein XA represents halogenation organic amine.
2. the preparation method of the beta scintillator based on additive Mn two dimension halogen perovskite, includes the following steps:
Lead bromide and bromination halogen amine are dissolved into dimethyl sulfoxide or dimethylformamide by step 1, form presoma；
Above-mentioned presoma is placed in the toluene solution excessively preheated by step 2, is stirred and is sufficiently reacted；
Gained precipitating is extracted by way of centrifugation, is then cleaned with toluene, repeated centrifugation, cleaning by step 3
Operation is multiple, until dimethyl sulfoxide or dimethylformamide are cleaned up；
Precipitated product after cleaning is dried in such a way that room temperature in vacuo is dry, removes toluene solvant, obtain by step 4
Desciccate；
Step 5: above-mentioned desciccate and manganese salt are subjected to mixed grinding, places it in protective gas and moves back after being fully ground
Fire processing, obtains final product.
3. method according to claim 2, which is characterized in that in step 1, bromination halogen amine includes that bromination butylamine, bromination are pungent
Amine, bromination lauryl amine, bromination octadecylamine.
4. method according to claim 2, which is characterized in that in step 1, lead bromide and bromination halogen amine are dissolved into diformazan
In base sulfoxide or dimethylformamide, the presoma that concentration is the M of 0.05 M ~ 1 is formed.
5. method according to claim 2, which is characterized in that in step 2, excess toluene refers to that volume is no less than presoma 2
Toluene again.
6. method according to claim 2, which is characterized in that in step 2, the toluene solution of preheating refers to 60 ~ 400 DEG C
Toluene solution.
7. method according to claim 2, which is characterized in that in step 2, sufficiently reaction refers to that the reaction time is no less than 2
min。
8. method according to claim 2, which is characterized in that in step 5, manganese salt includes manganous bromide, manganese acetate.
9. method according to claim 2, which is characterized in that in step 5, be fully ground and refer to that milling time is no less than 5
min。
10. method according to claim 2, which is characterized in that in step 5, annealing temperature is not less than 60 DEG C, when annealing
Between no less than 5 min.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113943225A (en) * | 2021-09-26 | 2022-01-18 | 华中科技大学 | Zero-dimensional organic manganese-based metal halide beta-ray scintillator and preparation method thereof |
| CN115074116A (en) * | 2021-03-16 | 2022-09-20 | 中国科学院理化技术研究所 | Hydrogen-rich two-dimensional perovskite fast neutron scintillator material and preparation method and application thereof |
| CN115975633A (en) * | 2022-12-29 | 2023-04-18 | 北京工业大学 | Mn doped Cs 2 CdCl 4 Scintillator |
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| CN108192605A (en) * | 2018-01-22 | 2018-06-22 | 汕头大学 | A kind of additive Mn two dimension lead halogen perovskite material of high photoluminescence quantum yield and its preparation |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115074116A (en) * | 2021-03-16 | 2022-09-20 | 中国科学院理化技术研究所 | Hydrogen-rich two-dimensional perovskite fast neutron scintillator material and preparation method and application thereof |
| CN113943225A (en) * | 2021-09-26 | 2022-01-18 | 华中科技大学 | Zero-dimensional organic manganese-based metal halide beta-ray scintillator and preparation method thereof |
| CN113943225B (en) * | 2021-09-26 | 2022-11-11 | 华中科技大学 | Zero-dimensional organic manganese-based metal halide beta-ray scintillator and preparation method thereof |
| CN115975633A (en) * | 2022-12-29 | 2023-04-18 | 北京工业大学 | Mn doped Cs 2 CdCl 4 Scintillator |
| CN115975633B (en) * | 2022-12-29 | 2024-01-02 | 北京工业大学 | Mn-doped Cs 2 CdCl 4 Scintillator |
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