CN107902691A - A kind of inorganic perovskite material and preparation method thereof - Google Patents
A kind of inorganic perovskite material and preparation method thereof Download PDFInfo
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- CN107902691A CN107902691A CN201611207467.9A CN201611207467A CN107902691A CN 107902691 A CN107902691 A CN 107902691A CN 201611207467 A CN201611207467 A CN 201611207467A CN 107902691 A CN107902691 A CN 107902691A
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- 239000000463 material Substances 0.000 title claims abstract description 38
- 238000002360 preparation method Methods 0.000 title claims abstract description 14
- 239000000126 substance Substances 0.000 claims abstract description 5
- 150000001449 anionic compounds Chemical class 0.000 claims abstract description 4
- 150000001767 cationic compounds Chemical class 0.000 claims abstract description 4
- 229910001412 inorganic anion Inorganic materials 0.000 claims abstract description 4
- 229910001411 inorganic cation Inorganic materials 0.000 claims abstract description 4
- 229910052751 metal Inorganic materials 0.000 claims abstract description 4
- 239000002184 metal Substances 0.000 claims abstract description 4
- 150000003839 salts Chemical class 0.000 claims description 14
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 9
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 8
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 claims description 8
- TWRXJAOTZQYOKJ-UHFFFAOYSA-L Magnesium chloride Chemical compound [Mg+2].[Cl-].[Cl-] TWRXJAOTZQYOKJ-UHFFFAOYSA-L 0.000 claims description 6
- MUBZPKHOEPUJKR-UHFFFAOYSA-N Oxalic acid Chemical compound OC(=O)C(O)=O MUBZPKHOEPUJKR-UHFFFAOYSA-N 0.000 claims description 6
- WCUXLLCKKVVCTQ-UHFFFAOYSA-M Potassium chloride Chemical compound [Cl-].[K+] WCUXLLCKKVVCTQ-UHFFFAOYSA-M 0.000 claims description 6
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 claims description 6
- LWBPNIJBHRISSS-UHFFFAOYSA-L beryllium dichloride Chemical compound Cl[Be]Cl LWBPNIJBHRISSS-UHFFFAOYSA-L 0.000 claims description 6
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims description 6
- 239000011259 mixed solution Substances 0.000 claims description 6
- FGDZQCVHDSGLHJ-UHFFFAOYSA-M rubidium chloride Chemical compound [Cl-].[Rb+] FGDZQCVHDSGLHJ-UHFFFAOYSA-M 0.000 claims description 6
- 229910052712 strontium Inorganic materials 0.000 claims description 6
- CIOAGBVUUVVLOB-UHFFFAOYSA-N strontium atom Chemical compound [Sr] CIOAGBVUUVVLOB-UHFFFAOYSA-N 0.000 claims description 6
- WDIHJSXYQDMJHN-UHFFFAOYSA-L barium chloride Chemical compound [Cl-].[Cl-].[Ba+2] WDIHJSXYQDMJHN-UHFFFAOYSA-L 0.000 claims description 5
- 239000000243 solution Substances 0.000 claims description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 4
- CDBYLPFSWZWCQE-UHFFFAOYSA-L Sodium Carbonate Chemical compound [Na+].[Na+].[O-]C([O-])=O CDBYLPFSWZWCQE-UHFFFAOYSA-L 0.000 claims description 4
- 229910001626 barium chloride Inorganic materials 0.000 claims description 4
- 239000000460 chlorine Substances 0.000 claims description 4
- 229910052801 chlorine Inorganic materials 0.000 claims description 4
- 238000004140 cleaning Methods 0.000 claims description 4
- 239000008367 deionised water Substances 0.000 claims description 4
- 229910021641 deionized water Inorganic materials 0.000 claims description 4
- 238000010438 heat treatment Methods 0.000 claims description 4
- 239000013049 sediment Substances 0.000 claims description 4
- OYPRJOBELJOOCE-UHFFFAOYSA-N Calcium Chemical compound [Ca] OYPRJOBELJOOCE-UHFFFAOYSA-N 0.000 claims description 3
- UXVMQQNJUSDDNG-UHFFFAOYSA-L Calcium chloride Chemical compound [Cl-].[Cl-].[Ca+2] UXVMQQNJUSDDNG-UHFFFAOYSA-L 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 3
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 claims description 3
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 claims description 3
- FYYHWMGAXLPEAU-UHFFFAOYSA-N Magnesium Chemical compound [Mg] FYYHWMGAXLPEAU-UHFFFAOYSA-N 0.000 claims description 3
- ZLMJMSJWJFRBEC-UHFFFAOYSA-N Potassium Chemical compound [K] ZLMJMSJWJFRBEC-UHFFFAOYSA-N 0.000 claims description 3
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims description 3
- 229910052788 barium Inorganic materials 0.000 claims description 3
- DSAJWYNOEDNPEQ-UHFFFAOYSA-N barium atom Chemical compound [Ba] DSAJWYNOEDNPEQ-UHFFFAOYSA-N 0.000 claims description 3
- 229910052790 beryllium Inorganic materials 0.000 claims description 3
- ATBAMAFKBVZNFJ-UHFFFAOYSA-N beryllium atom Chemical compound [Be] ATBAMAFKBVZNFJ-UHFFFAOYSA-N 0.000 claims description 3
- 229910001627 beryllium chloride Inorganic materials 0.000 claims description 3
- 229910052792 caesium Inorganic materials 0.000 claims description 3
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims description 3
- AIYUHDOJVYHVIT-UHFFFAOYSA-M caesium chloride Chemical compound [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 claims description 3
- 229910052791 calcium Inorganic materials 0.000 claims description 3
- 239000011575 calcium Substances 0.000 claims description 3
- 239000001110 calcium chloride Substances 0.000 claims description 3
- 229910001628 calcium chloride Inorganic materials 0.000 claims description 3
- 239000010949 copper Substances 0.000 claims description 3
- 229910052802 copper Inorganic materials 0.000 claims description 3
- 229910052732 germanium Inorganic materials 0.000 claims description 3
- GNPVGFCGXDBREM-UHFFFAOYSA-N germanium atom Chemical compound [Ge] GNPVGFCGXDBREM-UHFFFAOYSA-N 0.000 claims description 3
- 229910052744 lithium Inorganic materials 0.000 claims description 3
- 229910052749 magnesium Inorganic materials 0.000 claims description 3
- 239000011777 magnesium Substances 0.000 claims description 3
- 229910001629 magnesium chloride Inorganic materials 0.000 claims description 3
- 229910052700 potassium Inorganic materials 0.000 claims description 3
- 239000011591 potassium Substances 0.000 claims description 3
- 239000001103 potassium chloride Substances 0.000 claims description 3
- 235000011164 potassium chloride Nutrition 0.000 claims description 3
- 229910052701 rubidium Inorganic materials 0.000 claims description 3
- IGLNJRXAVVLDKE-UHFFFAOYSA-N rubidium atom Chemical compound [Rb] IGLNJRXAVVLDKE-UHFFFAOYSA-N 0.000 claims description 3
- 229940102127 rubidium chloride Drugs 0.000 claims description 3
- 239000011734 sodium Substances 0.000 claims description 3
- 229910052708 sodium Inorganic materials 0.000 claims description 3
- 239000011780 sodium chloride Substances 0.000 claims description 3
- 229910052718 tin Inorganic materials 0.000 claims description 3
- BMYNFMYTOJXKLE-UHFFFAOYSA-N 3-azaniumyl-2-hydroxypropanoate Chemical compound NCC(O)C(O)=O BMYNFMYTOJXKLE-UHFFFAOYSA-N 0.000 claims description 2
- VHUUQVKOLVNVRT-UHFFFAOYSA-N Ammonium hydroxide Chemical compound [NH4+].[OH-] VHUUQVKOLVNVRT-UHFFFAOYSA-N 0.000 claims description 2
- UIIMBOGNXHQVGW-UHFFFAOYSA-M Sodium bicarbonate Chemical compound [Na+].OC([O-])=O UIIMBOGNXHQVGW-UHFFFAOYSA-M 0.000 claims description 2
- 240000008866 Ziziphus nummularia Species 0.000 claims description 2
- 239000000908 ammonium hydroxide Substances 0.000 claims description 2
- 238000005660 chlorination reaction Methods 0.000 claims description 2
- 235000006408 oxalic acid Nutrition 0.000 claims description 2
- 229910000029 sodium carbonate Inorganic materials 0.000 claims description 2
- 238000002604 ultrasonography Methods 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims 1
- 150000001768 cations Chemical class 0.000 claims 1
- 235000011167 hydrochloric acid Nutrition 0.000 claims 1
- 239000000052 vinegar Substances 0.000 claims 1
- 235000021419 vinegar Nutrition 0.000 claims 1
- 238000001514 detection method Methods 0.000 abstract description 13
- 230000005251 gamma ray Effects 0.000 abstract description 7
- 230000035945 sensitivity Effects 0.000 abstract description 7
- 238000009792 diffusion process Methods 0.000 abstract description 4
- 230000001737 promoting effect Effects 0.000 abstract 1
- 239000000047 product Substances 0.000 description 6
- 238000000034 method Methods 0.000 description 4
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- 239000002994 raw material Substances 0.000 description 3
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 description 2
- 230000000052 comparative effect Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 238000001027 hydrothermal synthesis Methods 0.000 description 2
- 230000005855 radiation Effects 0.000 description 2
- 229910004613 CdTe Inorganic materials 0.000 description 1
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 description 1
- JTCFNJXQEFODHE-UHFFFAOYSA-N [Ca].[Ti] Chemical compound [Ca].[Ti] JTCFNJXQEFODHE-UHFFFAOYSA-N 0.000 description 1
- 229910021529 ammonia Inorganic materials 0.000 description 1
- 230000003796 beauty Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 150000001805 chlorine compounds Chemical class 0.000 description 1
- 239000003814 drug Substances 0.000 description 1
- 239000010408 film Substances 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000009396 hybridization Methods 0.000 description 1
- HWSZZLVAJGOAAY-UHFFFAOYSA-L lead(II) chloride Chemical group Cl[Pb]Cl HWSZZLVAJGOAAY-UHFFFAOYSA-L 0.000 description 1
- 229910000069 nitrogen hydride Inorganic materials 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000005498 polishing Methods 0.000 description 1
- 239000010409 thin film Substances 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G21/00—Compounds of lead
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01C—AMMONIA; CYANOGEN; COMPOUNDS THEREOF
- C01C3/00—Cyanogen; Compounds thereof
- C01C3/20—Thiocyanic acid; Salts thereof
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G17/00—Compounds of germanium
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G17/00—Compounds of germanium
- C01G17/006—Compounds containing germanium, with or without oxygen or hydrogen, and containing two or more other elements
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G19/00—Compounds of tin
- C01G19/006—Compounds containing tin, with or without oxygen or hydrogen, and containing two or more other elements
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G21/00—Compounds of lead
- C01G21/006—Compounds containing lead, with or without oxygen or hydrogen, and containing two or more other elements
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G3/00—Compounds of copper
- C01G3/006—Compounds containing copper, with or without oxygen or hydrogen, and containing two or more other elements
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01V—GEOPHYSICS; GRAVITATIONAL MEASUREMENTS; DETECTING MASSES OR OBJECTS; TAGS
- G01V5/00—Prospecting or detecting by the use of ionising radiation, e.g. of natural or induced radioactivity
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- High Energy & Nuclear Physics (AREA)
- Life Sciences & Earth Sciences (AREA)
- General Life Sciences & Earth Sciences (AREA)
- General Physics & Mathematics (AREA)
- Geophysics (AREA)
- Compositions Of Oxide Ceramics (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention discloses a kind of inorganic perovskite material, the chemical formula of the inorganic perovskite material is (A1)x(A2)1‑x(B1)y(B2)1‑y(X1)z(X2)3‑z, wherein 0≤x≤1,0≤y≤1,0≤z≤3, A1, A2 are inorganic cation, B1, B2 are divalent metal, and X1, X2 are the inorganic anion of not boracic, during and x=0, y=0.The present invention still further there is provided the preparation method of the perovskite material.The present invention is used as X/ gamma-ray detection materials, can be obviously improved carrier mobility and exciton diffusion length, realize to the gamma-ray high sensitivity detections of X/；Meanwhile preparation process of the present invention is simple, of low cost, therefore, the present invention is suitable for promoting and applying.
Description
Technical field
The present invention relates to radiation detection technology field, and in particular to be a kind of inorganic perovskite material and its preparation side
Method.
Background technology
Perovskite structural material is by its adjustable energy gap, high carrier mobility, good the two poles of the earth electric charge transmission
Characteristic, long exciton diffusion length and simple preparation process, in field of electronic devices such as solar cell, optical detectors
It is extensively studied and applies.
A kind of nearest emerging new organic inorganic hybridization perovskite material has very excellent physicochemical characteristics,
Its energy gap is adjustable, carrier mobility is very high, exciton diffusion length more than 1 μm, be a kind of very potential application
In the material of detector.A kind of perovskite monocrystalline CH grown up to using solwution method3NH3PbI3(MAPbI3) it has been used successfully as γ
Ray detector (50keV-10MeV), its sensitivity can match in excellence or beauty with response speed with commercialized CdTe.(Nature photonics,2016(10)585).This perovskite material is except as gamma ray detector, it can be applied equally to X and penetrates
The detection of line[33] (Nature photonics,2016(9)444), this by solwution method preparation is based on perovskite thin film
X-ray photodetector, preparation process is simple, high sensitivity（25 μC mGyair −1 cm−3）, response is rapid, in medicine and
Great application prospect in military affairs.
However, the perovskite material environmental stability mentioned by such scheme is poor, its application range is limited.Therefore,
Need to find suitable perovskite system, while its high sensitivity detection is ensured, significantly improve its environmental stability.This is right
In the practical application of perovskite-based detector it is particularly important that.
The content of the invention
In view of the above shortcomings of the prior art, the present invention provides a kind of inorganic perovskite material and preparation method thereof, its
Inorganic perovskite is prepared with reference to hydro-thermal method by being co-precipitated, its stability in the environment is improved, ensures its carrier concentration, hole
Mobility, electrical conductivity, are realized to the gamma-ray radiation detections of X/.
To achieve the above object, the technical solution adopted by the present invention is as follows：
A kind of inorganic perovskite material, the chemical formula of the perovskite material is (A1)x(A2)1-x(B1)y(B2)1-y(X1)z
(X2)3-z, wherein 0≤x≤1,0≤y≤1,0≤z≤3, A1, A2 are inorganic cation, B1, B2 be divalent metal sun from
Son, X1, X2 are inorganic anion.
Preferably, the A1 and A2 are any one in lithium, sodium, potassium, rubidium, caesium, beryllium, magnesium, calcium, strontium, barium.
Preferably, the B1 and B2 are any one in lead, tin, copper, germanium.
Preferably, described X1, X2 are O, S, I, Br, Cl, PF6, any one in SCN.
Based on above-mentioned material, present invention also offers the preparation method of the inorganic perovskite material, comprise the following steps：
（1）A salt is mixed with B salt for 1: 1 ratio in molar ratio, and is added in 30% hydrogen peroxide and dissolves, is uniformly mixed；
The A salt and B salt are lithium chloride, sodium chloride, potassium chloride, rubidium chloride, cesium chloride, beryllium chloride, magnesium chloride, calcium chloride, chlorination
One or more in strontium, barium chloride；
（2）The pH value for adjusting mixed solution is 2~11；
（3）Above-mentioned solution is transferred in water heating kettle, and at 60~200 DEG C, heats 3~80h, obtains head product；
（4）The thing that will dispatch from the factory uses deionized water and ethanol eccentric cleaning three times respectively, and sediment is freeze-dried；
（5）Dry jujube product is calcined into 1~4h at 300~900 DEG C, obtains inorganic perovskite material.
Preferably, the step（2）In, using hydrochloric acid, oxalic acid, acetic acid, hydrobromic acid, sodium carbonate, sodium acid carbonate and ammonia
One or more in water etc. adjust the pH value of mixed solution.
Preferably, the step（3）In, heated by the way of water-bath, oil bath, microwave or ultrasound.
Compared with prior art, the invention has the advantages that：
（1）Inorganic perovskite material is prepared with reference to hydro-thermal method by being co-precipitated in the present invention（Chemical formula：(A1)x(A2)1-x
(B1)y(B2)1-y(X1)z(X2)3-z）, the concentration of perovskite material carrier, hole mobility, electrical conductivity has been effectively ensured and has swashed
Carrier diffusion length, realizes the high sensitivity detection to X/ gamma-ray detection materials.
（2）Raw material of the present invention and equipment cost is cheap, raw material sources are extensive, it is convenient to prepare, can with whole soln working process,
Therefore, the present invention is with a wide range of applications.
Embodiment
With reference to embodiment, the invention will be further described, and mode of the invention includes but are not limited to following implementation
Example.
The present invention provides a kind of inorganic perovskite material, can be used as X/ gamma-ray detection materials, its chemical formula is (A1)x
(A2)1-x(B1)y(B2)1-y(X1)z(X2)3-z, wherein 0≤x≤1,0≤y≤1,0≤z≤3, A1, A2 are inorganic cation
（Such as lithium, sodium, potassium, rubidium, caesium, beryllium, magnesium, calcium, strontium or barium）, B1, B2 are divalent metal（Such as lead, tin, copper or
Germanium）, X1, X2 are inorganic anion（Such as O, S, I, Br, Cl, PF6Or SCN）.Inorganic perovskite material of the present invention
Preparation process it is as follows：
（1）A salt is mixed with B salt for 1: 1 ratio in molar ratio, and is added in 30% hydrogen peroxide and dissolves, is uniformly mixed；
The A salt and B salt is lithium chloride, sodium chloride, potassium chloride, rubidium chloride, cesium chloride, beryllium chloride, magnesium chloride, calcium chloride, chlorine
Change the one or more in strontium, barium chloride；
（2）The pH value for adjusting mixed solution is 2~11；
（3）Above-mentioned solution is transferred in water heating kettle, and at 60~200 DEG C, heats 3~80h, obtains head product；
（4）Hydrothermal product is used into deionized water and ethanol eccentric cleaning three times respectively, sediment is freeze-dried；
（5）Desciccate is calcined into 1~4h at 300~900 DEG C, obtains inorganic perovskite material.
The present invention is illustrated as one example with row below.
In perovskite-based material, the A salt is barium chloride, and B salt is lead chloride, the specific implementation step which prepares
It is as follows：
（1）Take 10mmol lead chlorides to be mixed with 10mmol barium chlorides, be added in 30% hydrogen peroxide and dissolve, be uniformly mixed；
（2）The pH value that mixed solution is adjusted with ammonium hydroxide is 10；
（3）Above-mentioned solution is transferred in water heating kettle, and at 150 DEG C, heats 12h, obtains head product；
（4）Hydrothermal product is used into deionized water and ethanol eccentric cleaning three times respectively, sediment is freeze-dried；
（5）Desciccate is calcined into 2h at 800 DEG C, obtains the inorganic perovskite material of final product.
The inorganic perovskite material film of 2 μ m-thicks is tested to Cu K α X-rays (8 keV) and Cs137The gamma-rays (600 in source
KeV detectivity performance).
Change presoma component, on the premise of other conditions are constant, obtained (A1)x(A2)1-x(B1)y(B2)1-y(X1)z
(X2)3-zDetection performance is as shown in table 1 below.
(A1) that the different presoma components of table 1 obtainx(A2)1-x(B1)y(B2)1-y(X1)z(X2)3-zResult of detection
The wherein sample comparative example of 1 numbering 5 of table.As can be seen that the detection of inorganic perovskite-based material prepared by the present invention
Sensitivity is with comparative example in an order of magnitude.
The present invention is selected by rational raw material and Proportionality design has prepared inorganic perovskite material, this kind of inorganic calcium titanium
Pit wood material can carry out high sensitivity detection and good stability to X/ gamma-rays.Therefore, compared with prior art,
The technology of the present invention progress is fairly obvious, it has prominent substantive distinguishing features and significant progress.
Above-described embodiment is only one of the preferred embodiment of the present invention, should not be taken to limit the protection model of the present invention
Enclose, all body design thought in the present invention and that mentally makes have no the change of essential meaning or polishing, what it was solved
Technical problem is still consistent with the present invention, should be included within protection scope of the present invention.
Claims (7)
1. a kind of inorganic perovskite material, it is characterised in that the chemical formula of the perovskite material is (A1)x(A2)1-x(B1)y
(B2)1-y(X1)z(X2)3-z, wherein 0≤x≤1,0≤y≤1,0≤z≤3, A1, A2 are inorganic cation, B1, B2 are two
Valency metal cation, X1, X2 are the inorganic anion of not boracic, during and x=0, y=0.
A kind of 2. inorganic perovskite material according to claim 1, it is characterised in that the A1 and A2 be lithium, sodium,
Any one in potassium, rubidium, caesium, beryllium, magnesium, calcium, strontium, barium.
A kind of 3. inorganic perovskite material according to claim 2, it is characterised in that the B1 and B2 be lead, tin,
Any one in copper, germanium.
A kind of 4. inorganic perovskite material according to claim 3, it is characterised in that described X1, X2 be O, S, I, Br,
Cl、PF6, any one in SCN.
5. the preparation method of the inorganic perovskite material described in Claims 1 to 4 any one, it is characterised in that including following
Step：
（1）A salt is mixed with B salt for 1: 1 ratio in molar ratio, and is added in 30% hydrogen peroxide and dissolves, is uniformly mixed；
The A salt and B salt are lithium chloride, sodium chloride, potassium chloride, rubidium chloride, cesium chloride, beryllium chloride, magnesium chloride, calcium chloride, chlorination
One or more in strontium, barium chloride；
（2）The pH value for adjusting mixed solution is 2~11；
（3）Above-mentioned solution is transferred in water heating kettle, and at 60~200 DEG C, heats 3~80h, obtains head product；
（4）The thing that will dispatch from the factory uses deionized water and ethanol eccentric cleaning three times respectively, and sediment is freeze-dried；
（5）Dry jujube product is calcined into 1~4h at 300~900 DEG C, obtains inorganic perovskite material.
6. preparation method according to claim 5, it is characterised in that the step（2）In, using hydrochloric acid, oxalic acid, vinegar
One or more in acid, hydrobromic acid, sodium carbonate, sodium acid carbonate and ammonium hydroxide etc. adjust the pH value of mixed solution.
7. preparation method according to claim 6, it is characterised in that the step（3）In, using water-bath, oil bath, microwave
Or the mode of ultrasound is heated.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611207467.9A CN107902691A (en) | 2016-12-23 | 2016-12-23 | A kind of inorganic perovskite material and preparation method thereof |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201611207467.9A CN107902691A (en) | 2016-12-23 | 2016-12-23 | A kind of inorganic perovskite material and preparation method thereof |
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| Publication Number | Publication Date |
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| CN107902691A true CN107902691A (en) | 2018-04-13 |
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| CN201611207467.9A Pending CN107902691A (en) | 2016-12-23 | 2016-12-23 | A kind of inorganic perovskite material and preparation method thereof |
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Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1524792A (en) * | 2003-02-28 | 2004-09-01 | 新加坡纳米材料科技有限公司 | A method for preparing various crystalline perovskite compound powders |
| CN1683278A (en) * | 2005-03-13 | 2005-10-19 | 中国科学院青海盐湖研究所 | Process for hydro-thermally synthesizing strontium titanate ceramic powder at normal atmosphere |
| CN101014538A (en) * | 2004-08-13 | 2007-08-08 | 堺化学工业株式会社 | Method for producing perovskite compound powder |
| CN101717261A (en) * | 2009-11-18 | 2010-06-02 | 广东风华高新科技股份有限公司 | Method for preparing perovskite powder and obtained substance |
-
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1524792A (en) * | 2003-02-28 | 2004-09-01 | 新加坡纳米材料科技有限公司 | A method for preparing various crystalline perovskite compound powders |
| CN101014538A (en) * | 2004-08-13 | 2007-08-08 | 堺化学工业株式会社 | Method for producing perovskite compound powder |
| CN1683278A (en) * | 2005-03-13 | 2005-10-19 | 中国科学院青海盐湖研究所 | Process for hydro-thermally synthesizing strontium titanate ceramic powder at normal atmosphere |
| CN101717261A (en) * | 2009-11-18 | 2010-06-02 | 广东风华高新科技股份有限公司 | Method for preparing perovskite powder and obtained substance |
Non-Patent Citations (1)
| Title |
|---|
| 陈良尧: "《凝聚态光学研究前沿》", 30 September 2014 * |
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