CN112794362B - Inorganic perovskite material, preparation method thereof and LED device - Google Patents
Inorganic perovskite material, preparation method thereof and LED device Download PDFInfo
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- 238000002360 preparation method Methods 0.000 title claims abstract description 21
- 238000006243 chemical reaction Methods 0.000 claims abstract description 33
- 239000002904 solvent Substances 0.000 claims abstract description 21
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 20
- TVFDJXOCXUVLDH-UHFFFAOYSA-N caesium atom Chemical compound [Cs] TVFDJXOCXUVLDH-UHFFFAOYSA-N 0.000 claims abstract description 20
- 238000010438 heat treatment Methods 0.000 claims abstract description 20
- 229910052792 caesium Inorganic materials 0.000 claims abstract description 19
- 229910052797 bismuth Inorganic materials 0.000 claims abstract description 15
- JCXGWMGPZLAOME-UHFFFAOYSA-N bismuth atom Chemical compound [Bi] JCXGWMGPZLAOME-UHFFFAOYSA-N 0.000 claims abstract description 14
- 238000003756 stirring Methods 0.000 claims abstract description 10
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- JHXKRIRFYBPWGE-UHFFFAOYSA-K bismuth chloride Chemical group Cl[Bi](Cl)Cl JHXKRIRFYBPWGE-UHFFFAOYSA-K 0.000 claims description 10
- AIYUHDOJVYHVIT-UHFFFAOYSA-M caesium chloride Chemical group [Cl-].[Cs+] AIYUHDOJVYHVIT-UHFFFAOYSA-M 0.000 claims description 9
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical group C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 3
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 3
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- 150000001875 compounds Chemical class 0.000 abstract description 4
- 125000000962 organic group Chemical group 0.000 abstract description 4
- ZAMOUSCENKQFHK-UHFFFAOYSA-N Chlorine atom Chemical compound [Cl] ZAMOUSCENKQFHK-UHFFFAOYSA-N 0.000 abstract description 3
- 239000000460 chlorine Substances 0.000 abstract description 3
- 229910052801 chlorine Inorganic materials 0.000 abstract description 3
- 239000011521 glass Substances 0.000 description 26
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 24
- 239000000047 product Substances 0.000 description 22
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- OQBLGYCUQGDOOR-UHFFFAOYSA-L 1,3,2$l^{2}-dioxastannolane-4,5-dione Chemical compound O=C1O[Sn]OC1=O OQBLGYCUQGDOOR-UHFFFAOYSA-L 0.000 description 6
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- ORFSSYGWXNGVFB-UHFFFAOYSA-N sodium 4-amino-6-[[4-[4-[(8-amino-1-hydroxy-5,7-disulfonaphthalen-2-yl)diazenyl]-3-methoxyphenyl]-2-methoxyphenyl]diazenyl]-5-hydroxynaphthalene-1,3-disulfonic acid Chemical compound COC1=C(C=CC(=C1)C2=CC(=C(C=C2)N=NC3=C(C4=C(C=C3)C(=CC(=C4N)S(=O)(=O)O)S(=O)(=O)O)O)OC)N=NC5=C(C6=C(C=C5)C(=CC(=C6N)S(=O)(=O)O)S(=O)(=O)O)O.[Na+] ORFSSYGWXNGVFB-UHFFFAOYSA-N 0.000 description 4
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- 238000002441 X-ray diffraction Methods 0.000 description 2
- 239000007864 aqueous solution Substances 0.000 description 2
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- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 231100000956 nontoxicity Toxicity 0.000 description 2
- BWOROQSFKKODDR-UHFFFAOYSA-N oxobismuth;hydrochloride Chemical compound Cl.[Bi]=O BWOROQSFKKODDR-UHFFFAOYSA-N 0.000 description 2
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- JTDNNCYXCFHBGG-UHFFFAOYSA-L tin(ii) iodide Chemical compound I[Sn]I JTDNNCYXCFHBGG-UHFFFAOYSA-L 0.000 description 2
- QHGNHLZPVBIIPX-UHFFFAOYSA-N tin(ii) oxide Chemical compound [Sn]=O QHGNHLZPVBIIPX-UHFFFAOYSA-N 0.000 description 2
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 2
- MFGOFGRYDNHJTA-UHFFFAOYSA-N 2-amino-1-(2-fluorophenyl)ethanol Chemical compound NCC(O)C1=CC=CC=C1F MFGOFGRYDNHJTA-UHFFFAOYSA-N 0.000 description 1
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- NIPNSKYNPDTRPC-UHFFFAOYSA-N N-[2-oxo-2-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)ethyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 NIPNSKYNPDTRPC-UHFFFAOYSA-N 0.000 description 1
- AFCARXCZXQIEQB-UHFFFAOYSA-N N-[3-oxo-3-(2,4,6,7-tetrahydrotriazolo[4,5-c]pyridin-5-yl)propyl]-2-[[3-(trifluoromethoxy)phenyl]methylamino]pyrimidine-5-carboxamide Chemical compound O=C(CCNC(=O)C=1C=NC(=NC=1)NCC1=CC(=CC=C1)OC(F)(F)F)N1CC2=C(CC1)NN=N2 AFCARXCZXQIEQB-UHFFFAOYSA-N 0.000 description 1
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- 241000083879 Polyommatus icarus Species 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910000416 bismuth oxide Inorganic materials 0.000 description 1
- 229940073609 bismuth oxychloride Drugs 0.000 description 1
- 229910000380 bismuth sulfate Inorganic materials 0.000 description 1
- TXKAQZRUJUNDHI-UHFFFAOYSA-K bismuth tribromide Chemical compound Br[Bi](Br)Br TXKAQZRUJUNDHI-UHFFFAOYSA-K 0.000 description 1
- LYQFWZFBNBDLEO-UHFFFAOYSA-M caesium bromide Chemical compound [Br-].[Cs+] LYQFWZFBNBDLEO-UHFFFAOYSA-M 0.000 description 1
- ATZQZZAXOPPAAQ-UHFFFAOYSA-M caesium formate Chemical compound [Cs+].[O-]C=O ATZQZZAXOPPAAQ-UHFFFAOYSA-M 0.000 description 1
- HUCVOHYBFXVBRW-UHFFFAOYSA-M caesium hydroxide Inorganic materials [OH-].[Cs+] HUCVOHYBFXVBRW-UHFFFAOYSA-M 0.000 description 1
- XQPRBTXUXXVTKB-UHFFFAOYSA-M caesium iodide Chemical compound [I-].[Cs+] XQPRBTXUXXVTKB-UHFFFAOYSA-M 0.000 description 1
- KOPBYBDAPCDYFK-UHFFFAOYSA-N caesium oxide Chemical compound [O-2].[Cs+].[Cs+] KOPBYBDAPCDYFK-UHFFFAOYSA-N 0.000 description 1
- 229910001942 caesium oxide Inorganic materials 0.000 description 1
- 239000001569 carbon dioxide Substances 0.000 description 1
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- 238000010276 construction Methods 0.000 description 1
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- PNOXNTGLSKTMQO-UHFFFAOYSA-L diacetyloxytin Chemical compound CC(=O)O[Sn]OC(C)=O PNOXNTGLSKTMQO-UHFFFAOYSA-L 0.000 description 1
- TYIXMATWDRGMPF-UHFFFAOYSA-N dibismuth;oxygen(2-) Chemical compound [O-2].[O-2].[O-2].[Bi+3].[Bi+3] TYIXMATWDRGMPF-UHFFFAOYSA-N 0.000 description 1
- BEQZMQXCOWIHRY-UHFFFAOYSA-H dibismuth;trisulfate Chemical compound [Bi+3].[Bi+3].[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O.[O-]S([O-])(=O)=O BEQZMQXCOWIHRY-UHFFFAOYSA-H 0.000 description 1
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- 235000019253 formic acid Nutrition 0.000 description 1
- 150000004820 halides Chemical class 0.000 description 1
- RXPAJWPEYBDXOG-UHFFFAOYSA-N hydron;methyl 4-methoxypyridine-2-carboxylate;chloride Chemical compound Cl.COC(=O)C1=CC(OC)=CC=N1 RXPAJWPEYBDXOG-UHFFFAOYSA-N 0.000 description 1
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- PNYYBUOBTVHFDN-UHFFFAOYSA-N sodium bismuthate Chemical compound [Na+].[O-][Bi](=O)=O PNYYBUOBTVHFDN-UHFFFAOYSA-N 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 238000004528 spin coating Methods 0.000 description 1
- 229940108184 stannous iodide Drugs 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- IUTCEZPPWBHGIX-UHFFFAOYSA-N tin(2+) Chemical compound [Sn+2] IUTCEZPPWBHGIX-UHFFFAOYSA-N 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- KOECRLKKXSXCPB-UHFFFAOYSA-K triiodobismuthane Chemical compound I[Bi](I)I KOECRLKKXSXCPB-UHFFFAOYSA-K 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G29/00—Compounds of bismuth
- C01G29/006—Compounds containing, besides bismuth, two or more other elements, with the exception of oxygen or hydrogen
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
- C09K11/00—Luminescent, e.g. electroluminescent, chemiluminescent materials
- C09K11/08—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials
- C09K11/74—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing arsenic, antimony or bismuth
- C09K11/7428—Halogenides
- C09K11/7435—Halogenides with alkali or alkaline earth metals
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
- H01L33/00—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof
- H01L33/48—Semiconductor devices having potential barriers specially adapted for light emission; Processes or apparatus specially adapted for the manufacture or treatment thereof or of parts thereof; Details thereof characterised by the semiconductor body packages
- H01L33/50—Wavelength conversion elements
- H01L33/501—Wavelength conversion elements characterised by the materials, e.g. binder
- H01L33/502—Wavelength conversion materials
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
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- C01P2004/01—Particle morphology depicted by an image
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- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02B—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO BUILDINGS, e.g. HOUSING, HOUSE APPLIANCES OR RELATED END-USER APPLICATIONS
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Abstract
The invention discloses an inorganic perovskite material, a preparation method thereof and an LED device, wherein the preparation method comprises the following steps: s1, dissolving a tin source and a bismuth source in a first solvent to obtain a first solution; dissolving a cesium source in a second solvent to obtain a second solution; the tin source is a stannous compound; and the cesium source, the tin source and the bismuth source are chlorine sources, and/or the first solvent and the second solvent are chlorine sources; and S2, mixing the first solution and the second solution, stirring, heating, reacting, performing solid-liquid separation, washing and drying. The preparation raw materials of the invention have low cost, safety and innocuity, the synthesis operation is simple, the crystal can be obtained by heating reaction, the equipment requirement is low, the reaction condition requirement is loose, the product has good crystallinity and uniform particles, the fluorescence yield is high, the inorganic perovskite material of the product has no organic group, the light stability and the thermal stability are strong, and the invention has the potential application value of preparing the blue-light fluorescent powder with high fluorescence yield, and can be further applied to preparing LED devices.
Description
Technical Field
The invention relates to the technical field of photoelectric materials, in particular to an inorganic perovskite material, a preparation method thereof and an LED device.
Background
In the existing perovskite materials, two-dimensional hybrid organic-inorganic perovskites (2D-HOIPs) are more typical, and the most common synthetic method is a solution cooling method, which specifically comprises the steps of dissolving reaction raw materials in a same solution according to a certain proportion, heating to a certain temperature to completely dissolve the reaction raw materials, and then cooling and crystallizing; when the temperature is reduced, the solubility of the 2D-HOIPs is reduced and the 2D-HOIPs are separated out from the solution, and in order to control the crystallization speed to obtain crystals with good crystallinity, a constant cooling rate needs to be kept, so that the key of crystal acquisition depends on a controlled cooling program, and the synthesis method has high requirements on equipment. In addition, the 2D-HOIPs contain organic groups, so that the material has poor light stability and is easy to decompose under illumination; furthermore, the organic group in the perovskite causes poor conductivity of the perovskite, and current is difficult to inject, so that deep blue light is difficult to obtain, and the efficiency and the brightness of the device are influenced. It is reported that 2D-HOIPs can be applied to the preparation of electroluminescent devices, but in the application process, it is necessary to dissolve it in an organic solvent first, and then prepare a luminescent film by spin coating or evaporation, so the application is complicated, and its solubility is generally poor, crystallization is too fast, and then an uneven discrete film can be formed, and it is difficult to satisfy the emission of pure blue light.
In addition, most of the existing common blue light powders are mixed with Eu 2+ As the activated central ion, the high temperature solid phase method is a common synthetic method, but the method has high reaction temperature and large energy consumption, and the reaction at high temperature is easy to generate impure phases, such as Eu 2+ The impurities are oxidized to cause impurity phases, and the quality of the product is further influenced. In addition, the synthesis conditions are harsh, the equipment requirements are high, and if raw materials which are easy to oxidize are involved, the reaction needs to be carried out under a protective atmosphere. For example, eu is added 2+ The raw materials are generally Eu, which is relatively easy to store, when being introduced into the fluorescent powder 3+ Oxide Eu of 2 O 3 Therefore, the reaction is carried out in a reducing gas H 2 Under the protection of (1), but the construction of a reduction system is not easy due to Eu introduced into the phosphor 2+ The Eu is not much originally contained in the system as long as the system contains very little oxidizing agent (such as water and oxygen) 2+ The oxidation will cause the product to fail, and therefore, the reaction conditions are very severe.
Cesium tin chloride (Cs) 2 SnCl 6 ) The double perovskite structure is an inorganic non-metallic material and is also a direct band gap semiconductor material. Into which Bi is doped 3+ Produced Cs 2 SnCl 6 :Bi 3+ Can emit fluorescence in visible light band under external excitation of light, electricity and the like,the luminous efficiency is higher, and the LED has potential value in white light LEDs. Cesium tin chloride can be synthesized by a hydrothermal method, and CsSnCl is easily formed in the air due to the divalent Sn of the raw material of the product 3 Miscellaneous phases, which seriously affect the product crystallinity and fluorescence yield and phase purity. Therefore, a perovskite material preparation method which is simple in synthesis process, low in equipment requirement, good in product crystallinity and high in fluorescence yield is urgently needed.
Disclosure of Invention
The present invention is directed to solving at least one of the problems of the prior art. Therefore, the invention provides an inorganic perovskite material, a preparation method thereof and an LED device.
In a first aspect of the present invention, there is provided a method for preparing an inorganic perovskite material, comprising the steps of:
s1, dissolving a tin source and a bismuth source in a first solvent to obtain a first solution; dissolving a cesium source in a second solvent to obtain a second solvent; the tin source is a stannous compound;
additionally, the cesium source, the tin source, and the bismuth source are chlorides, and/or the first solvent and the second solvent are chlorine sources;
s2, mixing the first solution and the second solution, stirring and heating to react to generate Cs 2 SnCl 6 :Bi 3+ Precipitating, then carrying out solid-liquid separation, washing and drying.
The preparation method of the inorganic perovskite material provided by the embodiment of the invention has at least the following beneficial effects: the preparation method adopts liquid phase synthesis, wherein Bi is introduced 3+ Ion, bi 3+ Can maintain stability even when completely exposed to air or water at normal temperature, and Bi 3+ Introduction of ions, capable of being in situ with Cs 2 SnCl 6 The energy level of the blue light is introduced with a defect energy level, so that electron transition is easier, and strong 456nm blue light is caused; meanwhile, a protective layer of basic bismuth oxychloride BiOCl (non-toxic) can be covered on the surface of the material, so that the material is protected from the influence of external environment such as water and oxygen, and the stability of the material is improved. And the preparation method has the advantages of low cost of raw materials, safety, no toxicity, simple synthesis operation, and the addition ofThe crystal can be obtained through thermal reaction, the equipment requirement is low, the reaction condition requirement is loose, the product crystallinity is good, the particles are uniform, the fluorescence yield is high, the obtained inorganic perovskite material has no organic group, the light stability and the thermal stability are strong, the application value of potential blue-light fluorescent powder with high fluorescence yield can be realized, and the blue-light fluorescent powder can be further applied to the preparation of LED devices and has high display color saturation.
According to some embodiments of the invention, in step S1, the molar ratio of the cesium source, the tin source and the bismuth source is 2.
According to some embodiments of the invention, the first solvent and the second solvent are hydrochloric acid; the cesium source is selected from inorganic cesium compounds and/or organic cesium compounds; the tin source is selected from inorganic stannous compound and/or organic stannous compound; the bismuth source is selected from an inorganic bismuth compound and/or an organic bismuth compound.
According to some embodiments of the invention, the cesium source is selected from at least one of cesium halides (such as cesium chloride, cesium iodide and cesium bromide), cesium oxide, cesium hydroxide, cesium formate; the tin source is at least one selected from stannous oxalate, stannous acetate, stannous halide (such as stannous chloride, stannous iodide and stannous bromide), and stannous oxide; the bismuth source is at least one selected from bismuth oxide, bismuth halide (such as bismuth chloride, bismuth iodide and bismuth bromide), bismuth sulfate, bismuth nitrate and sodium bismuthate.
According to some embodiments of the invention, the hydrochloric acid is concentrated hydrochloric acid with a mass fraction of more than 20%.
According to some embodiments of the invention, the first solvent and the second solvent are polar organic solvents and the cesium source, the tin source and the bismuth source are chlorides.
According to some embodiments of the invention, the first solvent and the second solvent are selected from at least one of N, N-dimethylformamide, dimethyl sulfoxide, ethanol; the cesium source is selected from cesium chloride, the tin source is selected from stannous chloride, and the bismuth source is selected from bismuth chloride.
According to some embodiments of the invention, in step S2, the reaction temperature of the stirring heating reaction is 60 to 120 ℃.
In addition, to facilitate dissolution of the tin source, bismuth source, and cesium source, dissolving the tin source, bismuth source in the first solvent and dissolving the cesium source in the second solvent can be accelerated by heating.
In a second aspect of the present invention, there is provided an inorganic perovskite material, which is prepared by any one of the methods for preparing an inorganic perovskite material provided in the first aspect of the present invention; having a chemical formula of Cs 2 SnCl 6 :Bi 3+ 。
In a third aspect of the invention, an LED device is provided, which includes an LED chip and a coating applied on the surface of the LED chip, wherein the coating is prepared by mixing raw materials including any one of the inorganic perovskite materials provided by the second aspect of the invention and a binder and coating the raw materials on the surface of the LED chip.
Drawings
The invention is further described with reference to the following figures and examples, in which:
FIG. 1 is a reaction system employed in the preparation of an inorganic perovskite material of example 1;
FIG. 2 is an SEM image of an inorganic perovskite material of example 1;
FIG. 3 is an SEM image of an inorganic perovskite material of comparative example 1;
FIG. 4 is a PL diagram for the inorganic perovskite material of example 1;
FIG. 5 is a PL diagram for the inorganic perovskite materials of example 1 and comparative example 1;
FIG. 6 is a plot of PL relative intensity versus inorganic perovskite material of example 1 and comparative example 2;
FIG. 7 is a plot of PL relative strength comparison for the inorganic perovskite materials of example 1 and comparative example 3;
FIG. 8 is a PL profile of the inorganic perovskite material of example 1 before and after exposure to light;
FIG. 9 is an XRD pattern of the inorganic perovskite material of example 1 before and after being placed under light;
FIG. 10 is an XRD pattern of the inorganic perovskite material of comparative example 1;
FIG. 11 is a PL profile of the inorganic perovskite material of example 1 after storage at different temperatures;
FIG. 12 is a schematic view of an embodimentExample 1 inorganic perovskite Material Cs 2 SnCl 6 :Bi 3+ The blue light CIE coordinate diagram of (a).
Reference numerals: 11-double-mouth glass flask, 12-oil bath kettle, 13-condenser, 14-rubber tube, 15-funnel and 16-tail gas treatment container.
Detailed Description
The concept and technical effects of the present invention will be clearly and completely described below in conjunction with the embodiments to fully understand the objects, features and effects of the present invention. It is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all embodiments, and other embodiments obtained by those skilled in the art without inventive efforts are within the protection scope of the present invention based on the embodiments of the present invention.
Example 1
An inorganic perovskite material is prepared and synthesized in a reaction system shown in figure 1 by a liquid phase method, and the preparation method comprises the following steps:
s1, weighing 0.6734g of cesium chloride, 0.4010g of stannous oxalate and 0.0189g of bismuth chloride, putting the stannous oxalate and the bismuth chloride into a double-mouth glass flask 11, then injecting 5mL of concentrated hydrochloric acid into the double-mouth glass flask, and putting a rotary stirring magneton into the double-mouth glass flask; mixing cesium chloride and 11ml of concentrated hydrochloric acid in a small bottle, and heating the small bottle to 80 ℃ for about 30min by using a water bath to obtain a cesium chloride-concentrated hydrochloric acid mixed solution;
s2, putting the double-mouth glass flask 11 into an oil bath 12 with a heat-collecting constant-temperature heating magnetic stirrer, wherein the upper opening of the double-mouth glass flask 11 is connected with a condenser 13, the side opening of the double-mouth glass flask is connected with a funnel 15 through a rubber tube 14, and the opening of the funnel 15 is contacted with the surface of a potassium hydroxide aqueous solution contained in a tail gas treatment container 16 so as to be used for discharging concentrated hydrochloric acid volatilized in the double-mouth glass flask 11, carbon dioxide and formic acid generated by reaction into the potassium hydroxide aqueous solution contained in the tail gas treatment container, so that accidents caused by overlarge pressure in the flask are prevented; then starting a heat collection type constant temperature heating magnetic stirrer to stir the material in the double-mouth glass flask 11;
and S3, starting the condenser 13, raising the temperature of the oil bath 12 to 80 ℃, wherein the temperature raising rate is 5.7 ℃/min, opening the side opening when the temperature of the sample is raised to 80 ℃, and pouring the cesium chloride-concentrated hydrochloric acid mixed solution into a reaction glass bottle. Closing the side opening, and then preserving heat for 3 hours to carry out reaction;
s4, after the reaction is finished, closing the heat collection type heating magnetic stirrer and the oil bath pot 12, taking the double-opening glass bottle 11 out of the oil bath pot 12, and quickly taking down the condenser pipe 13 and the funnel 14 to prevent air from entering; cooling the temperature of the double-mouth glass flask 11 to room temperature, then pouring the solid-liquid phase product in the double-mouth glass flask 11 into a glass beaker, covering the mouth of the glass beaker with tinfoil paper, standing for 8 hours, pouring out a clear liquid after layering, cleaning the product particles with absolute ethyl alcohol, standing for 4 hours, repeating the operation for 3-4 times until the pH of the supernatant absolute ethyl alcohol liquid is neutral, and finishing cleaning;
s5, covering the mouth of the beaker filled with the cleaned solid product by using tin foil paper, then putting the beaker into a vacuum drying box, and drying the beaker for 6 hours at 70 ℃ in a vacuum environment; and putting the product into an agate mortar, grinding the product into powder, putting the powder into a small glass bottle, sealing, drying and storing.
Example 2
An inorganic perovskite material, which comprises the following steps:
s1, weighing 0.6734g of cesium chloride, 0.4514mg of stannous chloride dihydrate and 0.0189g of bismuth chloride, putting the stannous chloride dihydrate and the bismuth chloride into a reaction glass bottle, and then injecting 5mL of ethanol into the reaction glass bottle to obtain a first mixture; mixing cesium chloride and 11ml of ethanol in a small vial, and heating the small vial to 60 ℃ for about 30mins using a water bath to obtain a second mixture;
and S2, raising the temperature of the first mixture obtained in the step S1 to 80 ℃ under a stirring state, wherein the heating rate is 8 ℃/min, opening the side opening when the temperature of the sample is raised to 80 ℃, and pouring the second mixture into a reaction glass bottle. Closing the side opening, and then carrying out heat preservation reaction for 3 hours;
s3, after the reaction is finished, cooling the temperature of the material to room temperature, standing for layering to obtain a solid product, washing product particles with absolute ethyl alcohol, standing for 4 hours, then washing the product particles with absolute ethyl alcohol, standing for 4 hours, repeating the steps for 3-4 times until the pH value of the supernatant absolute ethyl alcohol liquid is neutral, and finishing washing; then placing the mixture in a vacuum drying oven, and drying the mixture for 6 hours at 70 ℃ in a vacuum environment; and putting the product into an agate mortar, grinding the product into powder, putting the powder into a small glass bottle, sealing, drying and storing.
Comparative example 1
The preparation method of the inorganic perovskite material is different from that of the inorganic perovskite material in the embodiment 1 in that: in this comparative example, a hydrothermal reactor was used in place of the conventional two-neck glass flask, and the operation was otherwise the same as in example 1. The specific mode is as follows:
s1, weighing 0.6734g of cesium chloride, 0.4010g of stannous oxalate and 0.0189g of bismuth chloride, putting the stannous oxalate and the bismuth chloride into a polytetrafluoroethylene lining of a hydrothermal kettle, then injecting 5mL of concentrated hydrochloric acid into the hydrothermal kettle, and putting a rotary stirring magneton into the hydrothermal kettle; mixing cesium chloride and 11ml of concentrated hydrochloric acid in a small bottle, and heating the small bottle to 80 ℃ for about 30min by using a water bath to obtain a cesium chloride-concentrated hydrochloric acid mixed solution;
s2, putting the polytetrafluoroethylene lining into a matched steel sleeve (body), putting the steel sleeve into an oil bath pan with a heat collection type constant temperature heating magnetic stirrer, starting the heat collection type constant temperature heating magnetic stirrer to stir materials in the polytetrafluoroethylene lining, and covering an upper opening of the lining with a cover of the matched polytetrafluoroethylene lining;
and S3, raising the temperature of the oil bath to 80 ℃, wherein the heating rate is 5.7 ℃/min, opening a cover on the polytetrafluoroethylene lining when the temperature of the sample is raised to 80 ℃, and pouring the cesium chloride-concentrated hydrochloric acid mixed solution into the lining. Closing the cover, tightly covering the whole lining cover with a steel sleeve cover, and then preserving heat for 3 hours to carry out reaction;
s4, after the reaction is finished, closing the heat collection type heating magnetic stirrer and the oil bath pot, taking the hydrothermal reaction kettle out of the oil bath pot, cooling the temperature of the hydrothermal reaction kettle to room temperature, taking out the polytetrafluoroethylene lining, pouring a solid-liquid phase product in the hydrothermal reaction kettle into a glass beaker, covering the mouth of the glass beaker with tin foil paper, standing for 8 hours, pouring out a clear liquid after layering, cleaning the product particles with absolute ethyl alcohol, standing for 4 hours, repeating the steps for 3-4 times until the pH of the supernatant absolute ethyl alcohol liquid is neutral, and finishing cleaning;
s5, covering the beaker with the cleaned solid product by using tinfoil paper, then putting the beaker into a vacuum drying box, and drying the beaker for 6 hours at 70 ℃ in a vacuum environment; and then putting the product into an agate mortar, grinding the product into powder, putting the powder into a small glass bottle, sealing, drying and storing.
Comparative example 2
The preparation method of the inorganic perovskite material is different from that of the inorganic perovskite material in the embodiment 1 in that: in this comparative example, tin tetrachloride was used instead of stannous oxalate, and the other operations were the same as in example 1.
Comparative example 3
The preparation method of the inorganic perovskite material is different from that of the inorganic perovskite material in the embodiment 1 in that: in this comparative example, bismuth chloride was not added, and the other operations were the same as in example 1.
The results of observing the inorganic perovskite materials prepared in example 1 and comparative example 1 by Scanning Electron Microscopy (SEM) are shown in fig. 2 and 3, respectively, and SEM detection times are all performed at nearly the same magnification, so that the particle size and crystallization of the sample can be detected at the same magnification. From fig. 2 and 3, the inorganic perovskite material of example 1 has good crystallinity and uniform particles, compared to comparative example 1. Photoluminescence spectroscopy (PL) measurements were performed on the inorganic perovskite materials prepared in example 1 and comparative examples 1 to 3, respectively, and the results are shown in fig. 4 to 7. As can be seen from FIG. 4, the peak position of the inorganic perovskite material of example 1 is 456nm; the 456nm emission peak position is fixed, the peak position of the excitation spectrum is detected to be 362nm, namely, under the 362nm excitation light source, the 456nm blue light can be obtained through photoluminescence. As can be seen from fig. 5, the inorganic perovskite material prepared by the liquid phase method in example 1 has a stronger luminous intensity than the inorganic perovskite material prepared by the hydrothermal method in comparative example 1. As can be seen from FIGS. 2 and 3, the larger particle size of the example and the stronger crystallinity than those of the crystal of comparative example 1 and the larger number of the smaller particles of the crystal of comparative example 1 indicate that the crystallinity of the product obtained by the reaction in the hydrothermal reactor is inferior to that obtained in the double-neck glass flask, which affects the luminous intensity of the product.
As can be seen from fig. 6, in comparative example 2, the Sn source was replaced by tin tetrachloride, and the emission intensity of the target product was not as high as that of the product obtained in example 1 using tin (ii) as the reaction material. As can be seen from FIG. 7, bi was doped in example 1 3+ Cs of (A) 2 SnCl 6 The luminous intensity of the material is far higher than that of the material of comparative example 3 which is not doped with Bi 3+ Cs of (A) 2 SnCl 6 The luminous intensity of the material.
In addition, the inorganic perovskite material prepared in example 1 was left to stand under light for 15 days, and the results of photoluminescence spectrum detection were performed on the inorganic perovskite material before and after the left to stand under light, respectively, as shown in fig. 8, and the results of photoluminescence spectrum detection were performed on the inorganic perovskite material before and after the left to stand under light in example 1 and the inorganic perovskite material prepared in comparative example 1, respectively, using an X-ray diffractometer (XRD), as shown in fig. 9 and 10. As can be seen from fig. 8 and 9, the inorganic perovskite material obtained in example 1 has high photostability. As is clear from fig. 9 and 10, XRD of the inorganic perovskite material of comparative example 1 is a pure phase, which is not different from XRD of the inorganic perovskite material of example 1, and it is demonstrated that the pure phase can be synthesized by the raw material addition method according to this synthesis scheme when the reaction vessel is replaced (double-neck glass flask, hydrothermal reaction vessel). The inorganic perovskite material prepared in example 1 was stored at different temperatures for 1 day, and then the inorganic perovskite material was subjected to photoluminescence spectrum detection, and the obtained results are shown in fig. 11. As can be seen from fig. 11, the inorganic perovskite material of example 1 has high thermal stability, and the emission peak position thereof is not changed after storage under different temperature conditions, and the emission intensity thereof is not significantly different, and no PL shift occurs.
FIG. 12 shows the inorganic perovskite Cs obtained in example 1 2 SnCl 6 :Bi 3+ The black point M is the powder CIE coordinate calculated from the PL data of the powder, it can be seen that the black point M is close to the edge of the color coordinate, and in fact, the closer the point is to the color coordinate edge tableThe purer the light of the powder. Calculated color coordinates (x, y) = (0.1400, 0.0850), x + y =0.2250<0.3, and judging whether the powder body is pure blue light or not is carried out by judging whether the color coordinate of the powder body is pure blue light or not<0.3, color coordinates of the powder<0.3, indicating that the blue light of the powder is pure blue light. The purer the light of the powder, the larger the color gamut which can be covered by the powder, the higher the color saturation applied to display, the closer the displayed light is to the light which is true to an object, the closer the display is to the reality, and the more distortion of the color caused by the light-emitting material is avoided. Further, the application of the inorganic perovskite material to the preparation of an LED device shows that the display color saturation is high. Meanwhile, the monochromatic light purity is calculated to be about 91.6% according to the following formula:
xi, yi CIE coordinates of the sample.
xd, yd: the CIE values of the emission peak positions of the samples are 456nm, (xd, yd) are about (0.1459, 0.0452).
x, y: the CIE coordinates of the standard white light are (0.3333 ).
It can be seen from the above that, in example 1, the inorganic perovskite material synthesized by the liquid phase method has good crystallinity, uniform particles, high fluorescence yield, strong light stability and thermal stability, low cost of the synthetic raw materials, safety, no toxicity, simple synthesis operation, low requirement on equipment, loose requirement on reaction conditions, and suitability for industrial production, and the raw materials are mixed and then subjected to heating reaction in the synthesis process to obtain crystals. The inorganic perovskite material has potential application value of preparing blue-light fluorescent powder with high fluorescence yield, and can be further applied to the preparation of LED devices, and the display color saturation is high.
Therefore, the invention also provides an LED device, which comprises an LED chip and a coating coated on the surface of the LED chip, wherein the coating is prepared by mixing the raw materials comprising the inorganic perovskite material and the binder of the invention and coating the raw materials on the surface of the LED chip. The composite material can be prepared by mixing an inorganic perovskite material with a binder and encapsulating the mixture on a chip, does not need to design the arrangement of a traditional hole transmission layer and an electron transmission layer, does not need to form a film first, and has simple structure and convenient operation; and other colors of phosphors can be added to prepare corresponding LED devices, for example, yellow phosphors can be added to prepare white LED devices. In addition, organic silica gel can be used as the binder, and the organic silica gel has good temperature tolerance, so that the thermal stability of the device can be ensured.
Claims (1)
1. A preparation method of an inorganic perovskite material is characterized by comprising the following steps:
s1, dissolving a tin source and a bismuth source in a first solvent to obtain a first solution; dissolving a cesium source in a second solvent to obtain a second solution; the tin source is stannous chloride, the cesium source is cesium chloride, and the bismuth source is bismuth chloride; the molar ratio of the cesium source to the tin source to the bismuth source is 2:1: 6; the first solvent and the second solvent are selected from ethanol;
s2, mixing the first solution and the second solution, stirring and heating to react to generate Cs 2 SnCl 6 :Bi 3+ Precipitating, then carrying out solid-liquid separation, washing and drying; the reaction temperature of the stirring and heating reaction is 60 to 120 ℃.
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