CN108531987A - A kind of preparation method that halogen perovskite is nanocrystalline - Google Patents
A kind of preparation method that halogen perovskite is nanocrystalline Download PDFInfo
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- CN108531987A CN108531987A CN201810297662.8A CN201810297662A CN108531987A CN 108531987 A CN108531987 A CN 108531987A CN 201810297662 A CN201810297662 A CN 201810297662A CN 108531987 A CN108531987 A CN 108531987A
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B29/00—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape
- C30B29/10—Inorganic compounds or compositions
- C30B29/12—Halides
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- 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
- C09K11/67—Luminescent, e.g. electroluminescent, chemiluminescent materials containing inorganic luminescent materials containing refractory metals
- C09K11/674—Halogenides
- C09K11/675—Halogenides with alkali or alkaline earth metals
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- C—CHEMISTRY; METALLURGY
- C30—CRYSTAL GROWTH
- C30B—SINGLE-CRYSTAL GROWTH; UNIDIRECTIONAL SOLIDIFICATION OF EUTECTIC MATERIAL OR UNIDIRECTIONAL DEMIXING OF EUTECTOID MATERIAL; REFINING BY ZONE-MELTING OF MATERIAL; PRODUCTION OF A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; SINGLE CRYSTALS OR HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; AFTER-TREATMENT OF SINGLE CRYSTALS OR A HOMOGENEOUS POLYCRYSTALLINE MATERIAL WITH DEFINED STRUCTURE; APPARATUS THEREFOR
- C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
- C30B7/14—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions the crystallising materials being formed by chemical reactions in the solution
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Abstract
The present invention is a kind of preparation method that halogen perovskite is nanocrystalline, is included the following steps：1), silicon dioxide microsphere, lead halide, cesium carbonate and octadecylene are mixed, and surfactant and surface passivator is added, obtains mixture；2), the mixture that step 1) obtains is stirred to react 5 10min in 150 300 DEG C, is then down to room temperature, obtained nanocrystalline.The nanocrystalline preparation method of halogen perovskite of the present invention does not need protective gas by the way that presoma and ligand to be all blended in octadecylene solution, equipment and easy to operate, is produced on a large scale.This method is a kind of pervasive, general synthetic method, and the synthesis of a variety of cations and halogen may be implemented.By selecting halogen and adjusting its ratio, shining for total visible light wave band can be obtained.
Description
Technical field
The invention belongs to photoelectron material preparation fields, and in particular to a kind of preparation method that halogen perovskite is nanocrystalline.
Background technology
Ca-Ti ore type is nanocrystalline or nano particle, such as Ca-Ti ore type Organic leadP halogen compound (CH3NH3PbX3, X=F,
Cl, Br, I) or full-inorganic Ca-Ti ore type lead halide (CsPbX3, X=F, Cl, Br, I) and since its synthesis cost is low, fluorescence is imitated
The advantages such as rate is up to 90%, and luminous half-peak width and energy gap are adjustable, in solar cell, laser, optical detection
There is potential application value (Nature2013,499,316) in the fields such as device, light emitting diode.At the beginning of 2015, Nanjing science and engineering is big
The Zeng Haibo team initiative development QLED devices of full-inorganic perovskite quantum dot in the world are learned, and illustrates and is conducive to flexibility
The wide colour gamut three primary colours electroluminescent (Adv.Mater.2015,27,7162) that high definition is shown.In laser application aspect, Zeng Haibo
Team and the Nanyang Technolohy University east Sun Han, which cooperate to be found that the new system is nanocrystalline, also has Laser emission performance very outstanding,
It is expected the nanocrystalline laser display (Adv.Mater.2015,27,7101, Nano Lett.2016,16,448) for future.Together
When, between short several years, the photoelectric conversion efficiency highest of perovskite solar cell has reached 20% or more
(ChemSusChem,2016,9:252)。
However, inorganic halogen perovskite is mainly synthesized using hot injection method, i.e., lead halide is dissolved in octadecylene and surface is lived
Property agent oleic acid and oleyl amine in, argon gas protection and hot conditions under inject oleic acid caesium, obtain CsPbX3。(Advanced
Materials,2015,27,7101、Nano Letters 2015,6,3692).But because its harsh preparation requires, such as high temperature,
Inert ambient environment etc., not only considerably increases synthesis cost, reduces materials synthesis efficiency, and carry polar solvent is added
The aggregation that perovskite can be caused nanocrystalline in pure process, so that fluorescence efficiency drastically reduces.In addition, this method is big
There are also problems for scale preparation, and when carrying out high-volume synthesis, nanocrystalline quality and monodispersity will substantially reduce.
Therefore, it is necessary to a kind of preparation methods that halogen perovskite is nanocrystalline to solve the above problems.
Invention content
In view of the problems of the existing technology the present invention, provides a kind of preparation method that halogen perovskite is nanocrystalline.
A kind of preparation method that halogen perovskite is nanocrystalline, which is characterized in that include the following steps：
1), silicon dioxide microsphere, lead halide, cesium carbonate and octadecylene are mixed, and surfactant is added and surface is blunt
Agent obtains mixture；
2), the mixture that step 1) obtains is stirred to react 5-10min in 150-300 DEG C, is then down to room temperature, obtained
It is nanocrystalline.
Further, the amount ratio of the silicon dioxide microsphere, lead halide, cesium carbonate and octadecylene is：0.3g：
0.0967g-0.1284g：0.0326g：15ml.
Further, surfactant described in step 1) is oleyl amine and/or oleic acid.
Further, surface passivator described in step 1) is didodecyldimethylammbromide bromide, methyl trioctylphosphine
Ammonium chloride or double dodecyl dimethyl iodate amine.
Further, lead halide described in step 1) replaces with lead oxide.
Further, the amount ratio of the silicon dioxide microsphere, lead oxide, cesium carbonate and octadecylene is：0.3g：
0.0967g-0.1284g：0.0326g：15ml.
Further, cesium carbonate described in step 1) replaces with bromination methylamine or formamidine acetate.
Further, all components of step 1) are mixed at normal temperatures.
Further, it is to be down to room temperature by ice bath that room temperature is down in step 2).
Further, lead halide described in step 1) is any one in lead chloride, lead bromide and lead iodide or the two
Mixture.
Inventive principle：The nanocrystalline structure being prepared is perovskite structure, and Cl contents are higher in raw material, and shine wave
Length is shorter；I contents are higher in raw material, and emission wavelength is longer；When halogen is pure Br, shine in green range, and can obtain
To the half-peak breadth of 15-42nm wide, it is higher than 90% luminous efficiency.
Advantageous effect：The nanocrystalline preparation method of halogen perovskite of the invention is by all mixing presoma and ligand
In octadecylene solution, protective gas is not needed, equipment and easy to operate is produced on a large scale.This method be it is a kind of it is pervasive,
The synthesis of a variety of cations and halogen may be implemented in general synthetic method.By selecting halogen and adjusting its ratio, can obtain
To shining for total visible light wave band.
Description of the drawings
Fig. 1 is the nanocrystalline fluorescence spectrum and absorption figure prepared by embodiment 1-3.
Fig. 2 is the nanocrystalline fluorescence spectra prepared by embodiment 1,4 and 5.
Fig. 3 is the nanocrystalline fluorescence spectrum and absorption figure of other kind of cationoid prepared by embodiment 6 and 7.
Specific implementation mode
In the following with reference to the drawings and specific embodiments, the present invention is furture elucidated, it should be understood that these embodiments are merely to illustrate
It the present invention rather than limits the scope of the invention, after having read the present invention, those skilled in the art are to of the invention each
The modification of kind equivalent form falls within the application range as defined in the appended claims.
Embodiment 1
0.0326g cesium carbonates, 0.3g silicon dioxide microspheres, 0.1101g lead bromides are weighed, 15 milliliters of octadecylenes, 0.5 are measured
Milliliter oleyl amine, 0.5 milliliter of oleic acid and 0.0231gDDAB.It is fitted into flask after above-mentioned raw materials are mixed, at 200 degrees celsius
Reaction is cooled down with ice-water bath after five minutes.The luminous maximum luminous wavelength of the composite phosphor of preparation is 510nm, and halfwidth is
15nm, fluorescence quantum efficiency 90%.
Table 1 is the nanocrystalline fluorescence parameter prepared by embodiment 1
Embodiment 2
0.0326g cesium carbonates, 0.3g silicon dioxide microspheres, 0.055g lead bromides and 0.0417g lead chlorides are weighed, measures 15
Milliliter octadecylene, 0.5 milliliter of oleyl amine, 0.5 milliliter of oleic acid and 0.0231gDDAB.Flask is packed into after above-mentioned raw materials are mixed
In, it is stirred to react is cooled down after five minutes with ice-water bath at 200 degrees celsius.The luminous maximum luminous wave of the composite phosphor of preparation
A length of 461nm, halfwidth 18nm, fluorescence quantum efficiency 76%.
Embodiment 3
0.0326g cesium carbonates, 0.3g silicon dioxide microspheres, 0.0362g lead bromides and 0.0922g lead iodides are weighed, is measured
15 milliliters of octadecylenes, 0.5 milliliter of oleyl amine, 0.5 milliliter of oleic acid and 0.0231gDDAB.Flask is packed into after above-mentioned raw materials are mixed
In, it is stirred to react is cooled down after five minutes with ice-water bath at 200 degrees celsius.The luminous maximum luminous wave of the composite phosphor of preparation
A length of 644nm, halfwidth 42nm, fluorescence quantum efficiency 80%.
Embodiment 4
0.0326g cesium carbonates, 0.3g silicon dioxide microspheres, 0.1101g lead bromides are weighed, 15 milliliters of octadecylenes, 0.5 are measured
Milliliter oleyl amine and 0.5 milliliter of oleic acid.It is fitted into flask, is stirred to react at 200 degrees celsius 5 minutes after above-mentioned raw materials are mixed
It is cooled down afterwards with ice-water bath.The luminous maximum luminous wavelength of the composite phosphor of preparation is 510nm, halfwidth 20nm, fluorescence volume
Sub- efficiency is 82%.
Embodiment 5
Weigh 0.0326g cesium carbonates, 0.3g silicon dioxide microspheres and 0.1101g lead bromides, measure 15 milliliters of octadecylenes,
0.5 milliliter of oleyl amine and 0.5 milliliter of oleic acid.It is fitted into flask after above-mentioned raw materials are mixed, is stirred to react 5 points at 200 degrees celsius
Zhong Houyong ice-water baths cool down.The luminous maximum luminous wavelength of the composite phosphor of preparation is 510nm, halfwidth 24nm, fluorescence
Quantum efficiency is 60%.
Embodiment 6
Weigh 0.0832g tumers miaow, 0.3g silicon dioxide microspheres, 0.0446g lead oxide, measure 15 milliliters of octadecylenes,
1.5 milliliters of oleic acid and 0.0231gDDAB.It is fitted into flask after above-mentioned raw materials are mixed, is stirred to react 5 at 200 degrees celsius
It is cooled down with ice-water bath after minute.The luminous maximum luminous wavelength of the composite phosphor of preparation is 527nm, halfwidth 28nm, glimmering
Photo-quantum efficiency is 69%.
Embodiment 7
Weigh 0.0896g brominations methylamine, 0.3g silicon dioxide microspheres, 0.0446g lead oxide, measure 15 milliliters of octadecylenes,
1.5 milliliters of oleic acid and 0.0231g DDAB.It is fitted into flask after above-mentioned raw materials are mixed, 10 points is reacted under 160 degrees Celsius
Zhong Houyong ice-water baths cool down.The luminous maximum luminous wavelength of the composite phosphor of preparation is 503nm, halfwidth 27nm, fluorescence
Quantum efficiency is 74%.
Embodiment 8
0.0326g cesium carbonates, 0.3g silicon dioxide microspheres, 0.0551g lead bromides and 0.0417g lead chlorides are weighed, is measured
15 milliliters of octadecylenes, 0.5 milliliter of oleyl amine, 0.5 milliliter of oleic acid and 0.0179gMTAC.Flask is packed into after above-mentioned raw materials are mixed
In, it is stirred to react is cooled down after five minutes with ice-water bath at 200 degrees celsius.The luminous maximum luminous wave of the composite phosphor of preparation
A length of 461nm, halfwidth 18nm, fluorescence quantum efficiency 76%.
Nanocrystalline structure prepared by the present invention is perovskite structure, by the way that presoma and ligand are all blended in ten
In eight alkene solution, protective gas is not needed, equipment and easy to operate is produced on a large scale.This method is a kind of pervasive, general
Synthetic method, may be implemented it is a variety of cation and halogen synthesis.By selecting halogen and adjusting its ratio, can obtain complete
Visible light wave range shines.Cl contents are higher in raw material, and emission wavelength is shorter；I contents are higher in raw material, and emission wavelength is longer；
When halogen is pure Br, shine in green range.And the half-peak breadth of 15-42nm wide can be obtained, 90% luminous effect is higher than
Rate.
Nanocrystalline luminescent properties prepared by the present invention are excellent, can be used for electroluminance display, and luminescence generated by light illuminates and it
His photoelectric field.
Claims (9)
1. a kind of preparation method that halogen perovskite is nanocrystalline, which is characterized in that include the following steps：
1), silicon dioxide microsphere, lead halide, cesium carbonate and octadecylene are mixed, and surfactant and surface passivator is added,
Obtain mixture；
2), the mixture that step 1) obtains is stirred to react 5-10min in 150-300 DEG C, is then down to room temperature, obtain nanometer
It is brilliant.
2. the nanocrystalline preparation method of halogen perovskite according to claim 1, it is characterised in that：The silica is micro-
Ball, lead halide, cesium carbonate and octadecylene amount ratio be：0.3g：0.0967g-0.1284g：0.0326g：15ml.
3. the nanocrystalline preparation method of halogen perovskite according to claim 1, it is characterised in that：Surface described in step 1)
Activating agent is oleyl amine and/or oleic acid.
4. the nanocrystalline preparation method of halogen perovskite according to claim 1, it is characterised in that：Surface described in step 1)
Passivator is didodecyldimethylammbromide bromide, methyl tricapryl ammonium chloride or double dodecyl dimethyl iodate amine.
5. the nanocrystalline preparation method of halogen perovskite according to claim 1, it is characterised in that：Halogenation described in step 1)
Lead replaces with lead oxide.
6. the nanocrystalline preparation method of halogen perovskite according to claim 1, it is characterised in that：The silica is micro-
Ball, lead oxide, cesium carbonate and octadecylene amount ratio be：0.3g：0.0967g-0.1284g：0.0326g：15ml.
7. the nanocrystalline preparation method of halogen perovskite according to claim 1, it is characterised in that：Carbonic acid described in step 1)
Caesium replaces with bromination methylamine or formamidine acetate.
8. the nanocrystalline preparation method of halogen perovskite according to claim 1, it is characterised in that：Room temperature is down in step 2)
To be down to room temperature by ice bath.
9. the nanocrystalline preparation method of halogen perovskite according to claim 1, it is characterised in that：Halogenation described in step 1)
Lead is the mixture of any one or the two in lead chloride, lead bromide and lead iodide.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109456763A (en) * | 2018-10-15 | 2019-03-12 | 厦门大学 | A kind of synthetic method of lead iodine perovskite quantum dot |
| CN111808609A (en) * | 2020-05-29 | 2020-10-23 | 苏州星烁纳米科技有限公司 | Perovskite nanocrystal composites |
| CN113683513A (en) * | 2021-09-18 | 2021-11-23 | 厦门大学 | Double-bromine quaternary ammonium salt ligand and synthesis method for lead-halogen perovskite nanocrystalline solution |
| CN116925742A (en) * | 2023-07-26 | 2023-10-24 | 桑若(厦门)光伏产业有限公司 | Preparation method of ligand self-coated perovskite quantum dot |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107523296A (en) * | 2017-08-14 | 2017-12-29 | 南京理工大学 | The one-step method for synthesizing of big yield halogen perovskite/silicon dioxide microsphere composite phosphor |
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2018
- 2018-03-30 CN CN201810297662.8A patent/CN108531987A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN107523296A (en) * | 2017-08-14 | 2017-12-29 | 南京理工大学 | The one-step method for synthesizing of big yield halogen perovskite/silicon dioxide microsphere composite phosphor |
Non-Patent Citations (2)
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| JUN PAN ET AL.: "Highly Efficient Perovskite-Quantum-Dot Light-Emitting Diodes by Surface Engineering", 《ADV. MATER.》 * |
| JUN PAN, ET AL: "Bidentate Ligand-Passivated CsPbI3 Perovskite Nanocrystals for Stable Near-Unity Photoluminescence Quantum Yield and Efficient Red Light-Emitting Diodes", 《JOURNAL OF THE AMERICAN CHEMICAL SOCIETY》 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109456763A (en) * | 2018-10-15 | 2019-03-12 | 厦门大学 | A kind of synthetic method of lead iodine perovskite quantum dot |
| CN109456763B (en) * | 2018-10-15 | 2020-11-24 | 厦门大学 | Synthesis method of lead-iodine perovskite quantum dots |
| CN111808609A (en) * | 2020-05-29 | 2020-10-23 | 苏州星烁纳米科技有限公司 | Perovskite nanocrystal composites |
| CN113683513A (en) * | 2021-09-18 | 2021-11-23 | 厦门大学 | Double-bromine quaternary ammonium salt ligand and synthesis method for lead-halogen perovskite nanocrystalline solution |
| CN116925742A (en) * | 2023-07-26 | 2023-10-24 | 桑若(厦门)光伏产业有限公司 | Preparation method of ligand self-coated perovskite quantum dot |
| CN116925742B (en) * | 2023-07-26 | 2024-01-30 | 桑若(厦门)光伏产业有限公司 | Preparation method of ligand self-coated perovskite quantum dot |
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