CN110515113A - Core-shell structure halogen perovskite X-ray scintillation body and preparation method thereof - Google Patents
Core-shell structure halogen perovskite X-ray scintillation body and preparation method thereof Download PDFInfo
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- CN110515113A CN110515113A CN201910709406.XA CN201910709406A CN110515113A CN 110515113 A CN110515113 A CN 110515113A CN 201910709406 A CN201910709406 A CN 201910709406A CN 110515113 A CN110515113 A CN 110515113A
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- 239000011258 core-shell material Substances 0.000 title claims abstract description 28
- 229910052736 halogen Inorganic materials 0.000 title claims abstract description 27
- 150000002367 halogens Chemical class 0.000 title claims abstract description 27
- 238000002360 preparation method Methods 0.000 title claims abstract description 13
- ZASWJUOMEGBQCQ-UHFFFAOYSA-L dibromolead Chemical compound Br[Pb]Br ZASWJUOMEGBQCQ-UHFFFAOYSA-L 0.000 claims abstract description 8
- LYQFWZFBNBDLEO-UHFFFAOYSA-M caesium bromide Chemical compound [Br-].[Cs+] LYQFWZFBNBDLEO-UHFFFAOYSA-M 0.000 claims abstract description 7
- 239000000047 product Substances 0.000 claims description 17
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 13
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 12
- 238000000034 method Methods 0.000 claims description 11
- 239000012296 anti-solvent Substances 0.000 claims description 9
- 238000006243 chemical reaction Methods 0.000 claims description 9
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 4
- VLKZOEOYAKHREP-UHFFFAOYSA-N n-Hexane Chemical group CCCCCC VLKZOEOYAKHREP-UHFFFAOYSA-N 0.000 claims description 4
- 238000003756 stirring Methods 0.000 claims description 4
- 238000005119 centrifugation Methods 0.000 claims description 3
- 235000019441 ethanol Nutrition 0.000 claims description 2
- 239000012467 final product Substances 0.000 claims description 2
- 238000001291 vacuum drying Methods 0.000 claims description 2
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 claims 3
- YXFVVABEGXRONW-UHFFFAOYSA-N Toluene Chemical compound CC1=CC=CC=C1 YXFVVABEGXRONW-UHFFFAOYSA-N 0.000 description 24
- 238000003384 imaging method Methods 0.000 description 14
- 238000001514 detection method Methods 0.000 description 13
- 239000000463 material Substances 0.000 description 8
- 239000000523 sample Substances 0.000 description 7
- 238000005516 engineering process Methods 0.000 description 5
- 238000002189 fluorescence spectrum Methods 0.000 description 5
- 239000000843 powder Substances 0.000 description 5
- 239000002775 capsule Substances 0.000 description 4
- 230000000052 comparative effect Effects 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 230000005284 excitation Effects 0.000 description 4
- 230000003287 optical effect Effects 0.000 description 4
- 238000004140 cleaning Methods 0.000 description 3
- 239000013078 crystal Substances 0.000 description 3
- 239000002244 precipitate Substances 0.000 description 3
- 238000000862 absorption spectrum Methods 0.000 description 2
- -1 dimethyl methyl Chemical group 0.000 description 2
- 229910001385 heavy metal Inorganic materials 0.000 description 2
- 238000004519 manufacturing process Methods 0.000 description 2
- 230000008569 process Effects 0.000 description 2
- 238000004445 quantitative analysis Methods 0.000 description 2
- 239000002904 solvent Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 229910052797 bismuth Inorganic materials 0.000 description 1
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 description 1
- SDUQQTUFOHZBMY-UHFFFAOYSA-K cesium lead(2+) tribromide Chemical compound [Br-].[Br-].[Br-].[Cs+].[Pb++] SDUQQTUFOHZBMY-UHFFFAOYSA-K 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 238000012512 characterization method Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000004090 dissolution Methods 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000005855 radiation Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 239000004065 semiconductor Substances 0.000 description 1
- 238000001228 spectrum Methods 0.000 description 1
- 239000006228 supernatant Substances 0.000 description 1
- 230000002463 transducing effect Effects 0.000 description 1
- 230000001052 transient effect Effects 0.000 description 1
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 1
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N23/00—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00
- G01N23/22—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material
- G01N23/223—Investigating or analysing materials by the use of wave or particle radiation, e.g. X-rays or neutrons, not covered by groups G01N3/00 – G01N17/00, G01N21/00 or G01N22/00 by measuring secondary emission from the material by irradiating the sample with X-rays or gamma-rays and by measuring X-ray fluorescence
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01T—MEASUREMENT OF NUCLEAR OR X-RADIATION
- G01T1/00—Measuring X-radiation, gamma radiation, corpuscular radiation, or cosmic radiation
- G01T1/16—Measuring radiation intensity
- G01T1/20—Measuring radiation intensity with scintillation detectors
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/07—Investigating materials by wave or particle radiation secondary emission
- G01N2223/076—X-ray fluorescence
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/10—Different kinds of radiation or particles
- G01N2223/101—Different kinds of radiation or particles electromagnetic radiation
- G01N2223/1016—X-ray
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N2223/00—Investigating materials by wave or particle radiation
- G01N2223/30—Accessories, mechanical or electrical features
- G01N2223/312—Accessories, mechanical or electrical features powder preparation
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- Physics & Mathematics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Physics & Mathematics (AREA)
- High Energy & Nuclear Physics (AREA)
- Molecular Biology (AREA)
- Spectroscopy & Molecular Physics (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Luminescent Compositions (AREA)
Abstract
The invention discloses a kind of core-shell structure halogen perovskite X-ray scintillation bodies and preparation method thereof.The scintillator is CsPbBr3@Cs4PbBr6, there is core-shell structure to heat and recrystallize at a certain temperature after dissolving lead bromide and cesium bromide according to stoichiometric ratio, the core-shell structure halogen perovskite scintillator of high quality can be prepared on a large scale.Scintillator of the present invention is had excellent performance, and especially has the light decay deceleration being exceedingly fast, and is conducive to reduce the X-ray exposure period, is improved image quality.
Description
Technical field
The present invention relates to a kind of X-ray detection scintillator materials, more particularly to a kind of core-shell structure perovskite scintillator
X-ray scintillation body material and preparation method thereof, belong to technical field of nano material application.
Background technique
X-ray is a kind of High energy electromagnetic wave.Its wavelength is very short (0.01 ~ 100), therefore penetrates energy with very strong
The substance that light element content is higher in power, especially component, density is less big.X-ray have in numerous major areas and
Its important application, including military field, medical field and civil field.X-ray detection technology refers to for X-ray being converted to
Detectable optical signal either electric signal, to carry out a kind of technology that is quantitative or qualitatively analyzing to X-ray.At present
Some X-ray detection technologies can be divided into detection of gas technology, scintillator Detection Techniques and semiconductor probe technology.Wherein flash
Body Detection Techniques are using the radiative recombination process in excitation of X-rays scintillator, to X-ray is converted to visible to infrared waves
The light of section.Scintillator material refers to the material that fluorescence can be issued under the action of the high-energy ray including X-ray.Pass through
X-ray imaging is may be implemented into scintillator in conjunction with visible light detector array, combining with photomultiplier tube may be implemented X and penetrate
The quantitative analysis of line.
Ideal scintillator material should have the spies such as average atomic number is big, density is big, light conversion efficiency is high, sunset glow is short
Property.Existing frequently-used X-ray scintillation body mainly includes the NaI crystal of NaI:Tl(Tl element doping), ZnWO4、BGO
(Bi4Ge3O12), CsI(Tl), CdWO4Deng.These scintillators more or less have some shortcomings, and wherein NaI:Tl sunset glow is very
It is long, and easily deliquesce and be unfavorable for storing, the small absorption for being unfavorable for X-ray of density；ZnWO4Poor with the light output ability of BGO, signal turns
Transducing power is weak；CsI(Tl sunset glow) is longer；CdWO4In Cd be hypertoxic element.In addition, preparing for these scintillation crystals is most
Using Czochralski czochralski method, required temperature is more than 1700 DEG C, and not only at high cost and operation difficulty is big.
Summary of the invention
The present invention is directed to propose a kind of core-shell structure halogen perovskite scintillator and its preparation side for detecting X-ray
Method.Using the optical property that core-shell structure halogen perovskite is excellent, sigmatron can be converted to detectable visible light letter
Number, to realize imaging and the quantitative analysis tech of X-ray.
The technical solution for realizing the aim of the invention is as follows: the core-shell structure halogen perovskite for detecting X-ray flashes
Body, the scintillator are CsPbBr3@Cs4PbBr6。
For detecting the preparation method of the core-shell structure halogen perovskite scintillator of X-ray, include the following steps:
Step 1: cesium bromide and lead bromide are dissolved in dimethyl sulfoxide or dimethylformamide, and forming concentration is 0.2
The precursor solution of mol/ml；
Step 2: the precursor solution is placed in anti-solvent, is heated to certain temperature, stirs sufficiently reaction；
Step 3: after reaction terminate, the precipitated product of generation being centrifuged and is extracted, after cleaned with anti-solvent, repeated centrifugation-
Product repeatedly, until completely removing dimethyl sulfoxide or dimethylformamide, is then carried out low-temperature vacuum drying, obtained by cleaning
Obtain final product.
Preferably, in step 1, the molar ratio of cesium bromide and lead bromide is 2:1 ~ 10:1.
Preferably, in step 2 and step 3, anti-solvent uses the solvent to lead bromide and cesium bromide solubility very little, packet
Include any one in n-hexane, toluene, ethyl alcohol, isopropanol etc..
Preferably, in step 2, the volume ratio of anti-solvent and precursor solution is not less than 2:1.
Preferably, in step 2,60 ~ 400 DEG C are heated to, stirs sufficiently reaction.
Preferably, in step 2, the time sufficiently reacted is not less than 5 min.
Compared with prior art, the invention has the advantages that
(1) preparation means are convenient and quick, can at low temperature with all preparation process are completed in open environment, and can manufacture；
(2) CsPbBr3@Cs4PbBr6Scintillator is had excellent performance, and especially has the light decay deceleration being exceedingly fast, and is conducive to reduction X and is penetrated
The line exposing period improves image quality.
Detailed description of the invention
Fig. 1 is the scanning electron microscopic picture of core-shell structure halogen perovskite prepared by embodiment 1.
Fig. 2 is the fluorescence spectrum and absorption spectrum of core-shell structure halogen perovskite prepared by embodiment 1.
Fig. 3 is the XRD spectrum of core-shell structure halogen perovskite prepared by embodiment 1.
Fig. 4 is fluorescence spectrum of the core-shell structure halogen perovskite of the preparation of embodiment 1 under varying strength excitation of X-rays.
Fig. 5 is the device figure that core-shell structure halogen perovskite is used for x-ray imaging.
Fig. 6 is X-ray target sample, i.e., containing the capsule for including spring.
Fig. 7 is the result figure for carrying out x-ray imaging to capsule containing spring using core-shell structure halogen perovskite.
Fig. 8 is the transient radiation fluorescence spectrum of core-shell structure halogen perovskite prepared by embodiment 1.
Specific embodiment
Below with reference to embodiment and attached drawing, the invention will be further described.
The core-shell structure halogen perovskite that the present invention uses contains heavy metal element lead, and lead is that quality is only secondary in stable element
In the heavy metal element of bismuth, therefore interception collection effectively can be carried out to X-ray signal.Meanwhile core-shell structure halogen calcium titanium
The excellent luminescent properties of mine also in that lead presence, the electronic structure of lead directly determines that core-shell structure halogen perovskite is excellent
Optical property.Core-shell structure halogen perovskite mentioned here actually refers to CsPbBr3@Cs4PbBr6Material, really
That with fluorescent effect is internal CsPbBr3It is nanocrystalline.CsPbBr3Perovskite is nanocrystalline to be embedded in Cs4PbBr6In block.
Cs4PbBr6Without fluorescent effect, and to CsPbBr3 Nanocrystalline sent out fluorescent optics is transparent.It is flashed compared to others
Body, core-shell structure halogen perovskite do not need to be prepared into crystal habit, and powder morphology shows very excellent optical property.
The core-shell structure halogen perovskite preparation process of powder morphology is very easy, can be into low temperature (< 120 DEG C) and open environment
Row preparation, and it is low to the purity requirement of raw material, cost of material is cheap, and fluorescence efficiency can achieve 80% or more.
Embodiment 1
Step 1, by 4.2562(20 mmol) grams of cesium bromide lead and 1.83505(5 mmol) gram lead bromide (amount of substance it
Than being dissolved into the dimethyl sulfoxide of 100 ml for 4:1), dissolution is sufficiently stirred.
Step 2, above-mentioned 100 ml presoma is all added in toluene, the volume of toluene is 400 ml.It can be precipitated at this time
White precipitate.120 DEG C are heated to, 2 h of reaction are sufficiently stirred, white precipitate can be gradually transformed into green precipitate in the process.
Step 3, above-mentioned precipitated product is extracted by way of centrifugation, is centrifuged 1 under conditions of revolving speed is 6000 rpm
min.Supernatant is outwelled after centrifugation, then cleans the precipitated product with toluene.The centrifugation-cleaning operation repeated several times,
Sufficiently to remove dimethyl sulfoxide.
Step 4, the product that above-mentioned eccentric cleaning obtains is dried in vacuo at room temperature, until toluene is completely removed,
Until obtaining dried powder sample.Core-shell structure halogen perovskite obtained shows very strong green under ultraviolet source excitation
Fluorescence.Pattern that scanning electron microscope is shown is as shown in Figure 1, the oblique pattern and CsPbBr of quadrangular3@Cs4PbBr6Shapes kiss
It closes, illustrates that the product crystallinity of this method preparation is good.Its corresponding fluorescence spectrum and absorption spectrum are as shown in Figure 2.Fig. 3 is it
XRD diagram, it can be seen that product obtained is pure phase product, and there is no other impurity to occur.
Step 5, x-ray imaging device is integrated into using above-mentioned core-shell structure halogen perovskite product as scintillator material
In, imaging detection is carried out to the capsule containing spring.Fig. 4 is that core-shell structure halogen perovskite scintillator is strong in different x-ray
The lower fluorescence spectrum of degree, it can be seen that under different excitation of X-rays intensity, spent before corresponding fluorescence also can sounding change, this
It is the basis for carrying out aerial image to X-ray using core-shell structure halogen perovskite scintillator.By halogen perovskite scintillator collection
At into device shown in fig. 5, x-ray imaging detection is carried out to target sample, Fig. 6 is sample photo, and sample is to include metal
The capsule of spring can obtain the sample interior structure that naked eyes cannot be shown in, as shown in fig. 7, to realize that the imaging of X-ray is visited
It surveys.CsPbBr3@Cs4PbBr6The radiofluorescence decaying characterization of pulsed X-rays is as shown in figure 8, die-away time is 3 as the result is shown
Time needed for ns(, that is, radiofluorescence strength retrogression to 1/e), this ultrafast rate of decay is to obtain high quality imaging picture
Key.
Embodiment 2
The present embodiment is substantially the same manner as Example 1, unique the difference is that the solvent used is changed to dimethyl methyl by dimethyl sulfoxide
Amide, product obtained and X-ray detection/imaging results are essentially identical.
Embodiment 3
The present embodiment is substantially the same manner as Example 1, unique the difference is that the stoichiometric ratio of cesium bromide and lead bromide is 5:1, matter
Amount is respectively 5.32025 g and 1.83505 g, and product obtained and X-ray detection/imaging results are essentially identical.
Embodiment 4
The present embodiment is substantially the same manner as Example 1, it is unique unlike reaction temperature by 120 DEG C be changed to 90 DEG C, it is obtained
Product and X-ray detection/imaging results are essentially identical.
Embodiment 5
The present embodiment is substantially the same manner as Example 1, unique the difference is that anti-solvent has been changed to isopropanol, production obtained by toluene
Object and X-ray detection/imaging results are essentially identical.
Embodiment 6
The present embodiment is substantially the same manner as Example 1, uniquely the difference is that the volume of toluene becomes 800 ml by 400 ml, is obtained
The product and X-ray detection/imaging results obtained is essentially identical.
Comparative example 1
This comparative example is substantially the same manner as Example 1, unique the difference is that toluene has changed water into.Product obtained is white powder
End does not have fluorescent effect.
Comparative example 2
This comparative example is substantially the same manner as Example 1, unique the difference is that reaction temperature has been changed to room temperature (20 degree of left sides by 120 degree
It is right).Product obtained is white powder, does not have fluorescent effect.
Claims (7)
1. the halogen perovskite scintillator for detecting X-ray, which is characterized in that the scintillator is CsPbBr3@
Cs4PbBr6, there is core-shell structure.
2. the preparation method of scintillator as described in claim 1, which comprises the steps of:
Step 1: cesium bromide and lead bromide are dissolved in dimethyl sulfoxide or dimethylformamide, and forming concentration is 0.2
The precursor solution of mol/ml；
Step 2: the precursor solution is placed in anti-solvent, is heated to certain temperature, stirs sufficiently reaction；
Step 3: after reaction terminate, the precipitated product of generation being centrifuged and is extracted, is cleaned with anti-solvent, repeated centrifugation, clear
It washes repeatedly, until completely removing dimethyl sulfoxide or dimethylformamide, product is then subjected to low-temperature vacuum drying, obtain
Final product.
3. method according to claim 2, which is characterized in that in step 1, the molar ratio of cesium bromide and lead bromide is 2:1
~10:1。
4. method according to claim 2, which is characterized in that in step 2 and step 3, anti-solvent is selected from n-hexane, first
Benzene, ethyl alcohol, any one in isopropanol.
5. method according to claim 2, which is characterized in that in step 2, the volume ratio of anti-solvent and precursor solution is not
Less than 2:1.
6. method according to claim 2, which is characterized in that in step 2, be heated to 60 ~ 400 DEG C, stirring is sufficiently anti-
It answers.
7. method according to claim 2, which is characterized in that in step 2, the time sufficiently reacted is not less than 5 min.
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| CN113066809A (en) * | 2021-03-05 | 2021-07-02 | 兰州大学 | Preparation method of flexible X-ray scintillator detector |
| CN113845908A (en) * | 2021-09-22 | 2021-12-28 | 天津理工大学 | Cs (volatile organic Compounds)4PbX6/CsPbX3Preparation method of composite microcrystal |
| CN115703967A (en) * | 2021-08-14 | 2023-02-17 | 兰州大学 | Preparation method of perovskite nanocrystalline luminescent material |
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