CN111270310A - Pure inorganic narrow-spectrum blue-violet light emitting two-dimensional perovskite single crystal material and growth method - Google Patents

Pure inorganic narrow-spectrum blue-violet light emitting two-dimensional perovskite single crystal material and growth method Download PDF

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CN111270310A
CN111270310A CN202010181827.2A CN202010181827A CN111270310A CN 111270310 A CN111270310 A CN 111270310A CN 202010181827 A CN202010181827 A CN 202010181827A CN 111270310 A CN111270310 A CN 111270310A
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single crystal
pbcl
solution
growth
temperature
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丁建旭
井琳
姚青
张�杰
王开宇
袁野
孙海清
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Shandong University of Science and Technology
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Shandong University of Science and Technology
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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
    • 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
    • C30B7/02—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by evaporation of the solvent
    • C30B7/04—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by evaporation of the solvent using aqueous solvents
    • 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
    • C30B7/08—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by cooling of the solution
    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01S—DEVICES USING THE PROCESS OF LIGHT AMPLIFICATION BY STIMULATED EMISSION OF RADIATION [LASER] TO AMPLIFY OR GENERATE LIGHT; DEVICES USING STIMULATED EMISSION OF ELECTROMAGNETIC RADIATION IN WAVE RANGES OTHER THAN OPTICAL
    • H01S3/00—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range
    • H01S3/14—Lasers, i.e. devices using stimulated emission of electromagnetic radiation in the infrared, visible or ultraviolet wave range characterised by the material used as the active medium
    • H01S3/16—Solid materials
    • H01S3/163—Solid materials characterised by a crystal matrix
    • H01S3/1645—Solid materials characterised by a crystal matrix halide

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  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Metallurgy (AREA)
  • Materials Engineering (AREA)
  • Organic Chemistry (AREA)
  • Electromagnetism (AREA)
  • Physics & Mathematics (AREA)
  • Plasma & Fusion (AREA)
  • Optics & Photonics (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)
  • Luminescent Compositions (AREA)

Abstract

The invention provides a pure inorganic, large-size and two-dimensional perovskite narrow-spectrum bluish violet light emitting single crystal material and a growth method thereof, wherein the method utilizes a method of slowly cooling or volatilizing a solvent from the solvent to obtain a large-size single crystal; wherein the chemical formula of the large-size two-dimensional perovskite luminescent single crystal is CsPb2Cl5. The single crystal has a two-dimensional crystal structure; the half-peak width of the luminescence peak is narrow, the position of the luminescence peak is 417nm, the half-height width is less than 18nm, and the size of the single crystal is large.

Description

Pure inorganic narrow-spectrum blue-violet light emitting two-dimensional perovskite single crystal material and growth method
Technical Field
The invention relates to a pure inorganic and two-dimensional perovskite single crystal material, which consists of Cs2PbCl5. The material can be excited by ultraviolet light to generate blue-violet luminescence with a strong main peak at 417nm and a spectral width of 18 nm.
Background
Lead halide perovskite material CsPb with two-dimensional structure2X5(X ═ Cl, Br, I) is [ PbX ] formed from Pb ion and halogen ion]6 4-The octahedron is connected through halogen ions to form a two-dimensional periodic structure. The material belongs to a pure inorganic perovskite material. Compared with organic-inorganic hybrid perovskite materials, on one hand, the material has higher stability; on the other hand, compared with the three-dimensional perovskite material, the two-dimensional perovskite has high luminescent color purity, adjustable luminescent color, longer carrier service life, higher luminescent efficiency and larger defect tolerance space, thereby having important application value in the fields of optoelectronic devices such as high-performance solar cells, photodetectors, transistors, memories and the like.
When the Cs-Pb-X system is adopted to synthesize the material, the Cs can be synthesized simultaneously4PbX6、CsPbX3、CsPb2X5Materials with various structures and easy interconversion between the materials, so that pure-phase CsPb is synthesized2X5It is difficult to control the solution concentration, temperature and pressure strictly; and the synthesized powder material is easy to be converted into CsPbX3Problems such as color impurities occur in light emitting and illuminating devices. Based on the above consideration, CsPb is obtained2X5And a photovoltaic device is prepared by using the single crystal.
The perovskite material is synthesized by adopting a Cs-Pb-X system, and CsPb is common2Br5A material. The material is a direct semiconductor with wide forbidden band, but the luminous activity is extremely low, so that the application in the field of photoelectric devices is limited. CsPb of its congeneric material2Cl5Accept [ PbX ]]6 4-The octahedron has small volume influence and good luminescence activity. But aim atUntil now, CsPb has not existed2Cl5Study of single crystal materials and growth methods.
Therefore, the invention provides a pure inorganic two-dimensional perovskite single crystal material capable of emitting narrow-bandwidth blue-violet light and a growth method thereof. The single crystal material and the growth method thereof are used for expanding CsPb2Cl5The application of the single crystal in semiconductor lasers and LEDs has important significance.
Disclosure of Invention
The invention aims to provide a pure inorganic two-dimensional perovskite crystal material emitting narrow-spectrum blue-violet light and a growth method thereof. The method is simple and feasible, and the obtained luminescent material has blue-violet luminescence with narrow band spectrum.
The chemical component of the crystal is CsPb2Cl5The crystal structure is a two-dimensional structure, [ PbCl ]]6 4-Octahedron connected in the layer.
The CsPb2Cl5The band gap of the crystal is-3.8 eV, and under the excitation of ultraviolet light, the crystal can emit narrow-spectrum blue-violet light with a main peak near 417nm, and the full width at half maximum of an emission spectrum is about 18 nm.
The blue-violet luminescent two-dimensional perovskite CsPb2Cl5The crystal growth method is a low-temperature slow cooling or slow volatilization solvent growth technology, and comprises the following growth steps:
mixing lead chloride (PbCl)2) And cesium chloride (CsCl) are mixed and dissolved in deionized water or concentrated hydrochloric acid according to a certain molar ratio, and the mixture is fully stirred and dissolved at the temperature of 40-80 ℃ to obtain a precursor solution. Obtaining a colorless and transparent Cs by slowly volatilizing to room temperature at a certain cooling rate2PbCl5A two-dimensional perovskite single crystal.
Further, the concentration of the growth system is 0.01-0.05 mol/L.
Further, for dissolving PbCl2The CsCl and CsCl solvent is pure deionized water, concentrated hydrochloric acid or the mixture of the concentrated hydrochloric acid and the deionized water according to a proportion, and the dissolving fixed concentration is taken as the standard: high concentration solution hydrochloric acid ratio increaseThe low concentration solution reduces the hydrochloric acid ratio.
Further, PbCl2The molar ratio of the CsCl raw material to the PbCl raw material is PbCl2：CsCl＝1：1～1:3。
Further, the temperature of the solution is higher than 60 ℃, and the solution can be naturally cooled.
Further, the solution temperature is below 60 ℃ and a lower cooling rate, such as 0.1 ℃/h, is used.
Further, the temperature of the solution is reduced to room temperature, and the solvent is slowly volatilized, so that the crystal continues to grow.
The growth method adopts the cooling according to 0.1 ℃/h, the crystallization time is 10-15 days, and the size of the obtained crystal is about 3 mm.
The invention provides a two-dimensional structure and large-size bluish violet CsPb2Cl5Single crystal material and method of growing the same. The crystal material is a two-dimensional structure material, can emit narrow-spectrum blue-violet light with a main peak at 417nm under the excitation of ultraviolet light, and has high luminous intensity, and the full width at half maximum of an emission spectrum is about 18 nm; the size of the single crystal obtained by the growth method is 2-4 mm, and the thickness of the single crystal is about 1 mm. The adopted crystal growth method is green and environment-friendly in the growth process; and has low requirements on equipment and reaction conditions; the growth method is controllable and has strong practical value.
Drawings
Embodiments of the invention are described in detail below with reference to the attached drawing figures, wherein:
FIG. 1 is a photograph of a single crystal obtained in example 1 of the present invention: the crystal is a slightly white transparent crystal;
FIG. 2 is an X-ray diffraction pattern of a single crystal obtained in example 1 of the present invention; wherein XRD adopts D/Max2500PC X-ray diffractometer to analyze the phase of the sample, CuKαAnd (3) radiation (lambda is 0.154nm), and the measurement range is 10-60.
FIG. 3 is a photograph of a single crystal obtained in example 2 of the present invention: the crystals were colorless transparent crystals.
FIG. 4 shows Cs obtained in example 2 of the present invention2PbCl5Crystal structure diagram obtained by single crystal X-ray diffraction of single crystal.
FIG. 5 shows Cs obtained in example 2 of the present invention2PbCl5Comparison of powder XRD obtained for single crystals and single crystal diffraction calculations.
FIG. 6 shows Cs obtained in example 2 of the present invention2PbCl5Uv-visible absorption spectrum of single crystal: an Shimadzu UV-2550 ultraviolet-visible spectrophotometer is adopted, a small integrating sphere accessory is adopted, barium sulfate powder is used as a reference, a test sample is powder particles, and the scanning wavelength range is 270-450 nm.
FIG. 7 shows Cs obtained in example 2 of the present invention2PbCl5Fluorescence spectrum of single crystal: 365nm is used as an excitation light source, and an FLS-980 fluorescence spectrometer is adopted to test the fluorescence spectrum of the sample; the material emits blue-violet light, the full width at half maximum of an emission spectrum is about 18nm, and the luminous intensity is high.
FIG. 8 shows Cs obtained in example 2 of the present invention2PbCl5Luminescence photograph of single crystal: the material emits blue-violet light with high intensity and pure chroma visible to naked eyes.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. The experimental procedures, in which specific conditions are not noted in the following examples, are generally carried out according to conventional conditions or according to conditions recommended by the manufacturers.
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art. In addition, any methods and materials similar or equivalent to those described herein can be used in the methods of the present invention. The preferred embodiments and materials described herein are intended to be exemplary only.
It should be understood that the invention provides a pure inorganic blue-violet light emitting two-dimensional perovskite single crystal material with narrow bandwidth and a growth method thereof, and the material is a two-dimensional layered structure and large-size blue-violet light emitting Cs2PbCl5Single crystal with which Cs can be grown2PbCl5And (3) single crystal.
It is to be understood that the invention is not intended to be exhaustiveFor growing Cs2PbCl5A solution system of single crystal (containing an organic solvent), in order to exhibit the effect of the present invention, only a part of the growth example and the light emission result are shown in the following examples.
The reagents used in the following comparative examples and examples are all commercially available.
Example 1:
0.001 mol of PbCl was weighed2And 0.001 mol of CsCl into 25 ml of deionized water, sealing, magnetically stirring at the constant temperature of 40-60 ℃, adding less than or equal to 15 ml of concentrated hydrochloric acid until the solution is completely dissolved, and then, heating to 60 ℃ and then cooling at the speed of 0.1 ℃/hour. When the temperature is reduced to 40-55 ℃, a transparent crystal is found to be separated out, the temperature is reduced to room temperature at the same speed, and the solvent is volatilized until the crystal grows up.
FIG. 1 is a photograph of a real object of a single crystal obtained in example 1.
FIG. 2 shows the results of X-ray diffraction on Cs obtained in example 12PbCl5The material was subjected to XRD for structural analysis.
Example 2:
0.001 mol of PbCl was weighed2And 0.001 mol of CsCl in 30 ml of concentrated hydrochloric acid, sealed and magnetically stirred at a constant temperature of 60 ℃ until the solution is completely dissolved. Then heating to 80 deg.C, stirring thoroughly to make solute fully dissolved and uniform. Then slowly cooling to 60 ℃, starting to generate crystals, then cooling to room temperature at the speed of 0.1 ℃/hour, and realizing the simultaneous growth of a plurality of transparent cubic Cs2PbCl5Single crystal, transparent crystal with size of about 4 × 1.5 mm.
FIG. 3 is a photograph of a real object of a single crystal obtained in example 2;
FIG. 4 shows Cs obtained in example 22PbCl5A crystal structure diagram obtained by single crystal X-ray diffraction performed on a single crystal;
FIG. 5 shows Cs obtained in example 22PbCl5Comparing the calculation results of powder XRD and single crystal diffraction obtained by single crystal;
FIG. 6 shows Cs obtained in example 22PbCl5Ultraviolet-visible absorption spectrum of single crystal;
FIG. 7 Cs obtained in example 22PbCl5Fluorescence spectrum of single crystal: the material emits blue-violet light, the full width at half maximum of an emission spectrum is about 18nm, and the luminous intensity is high;
FIG. 8 Cs obtained in example 22PbCl5Luminescence photograph of single crystal: the material glows with blue and violet light.

Claims (9)

1. A growth method of a pure inorganic narrow-spectrum blue-violet light two-dimensional perovskite single crystal is characterized by comprising the following steps: the method adopts a method of reducing the temperature of the solution or volatilizing the solvent for growth; the chemical component of the two-dimensional perovskite single crystal obtained by the method is Cs2PbCl5。
2. The growing method according to claim 1, wherein: cs obtained by the method2PbCl5Under the excitation of ultraviolet light, the two-dimensional perovskite single crystal can emit narrow-spectrum blue-violet light with a main peak near 417nm, and the full width at half maximum of an emission spectrum is about 18 nm.
3. The growing method according to claim 1, wherein: the method specifically comprises the step of mixing lead chloride (PbCl)2) Mixing with cesium chloride (CsCl) in proportion, and dissolving in deionized water or concentrated hydrochloric acid, wherein the raw material molar ratio is PbCl2: CsCl ═ 1: 1-1: 3; the concentration of the growth system is 0.01-0.05mol/L, the growth system is fully stirred and dissolved at the temperature of 40-80 ℃ to obtain a light yellow transparent precursor solution, and the light yellow transparent precursor solution is obtained by slowly volatilizing to room temperature at a certain cooling rate to obtain colorless transparent Cs2PbCl5A two-dimensional perovskite single crystal.
4. The growing method according to claim 3, wherein: the deionized water and the concentrated hydrochloric acid can be used as growth solutions in any proportion.
5. The growing method according to claim 3, wherein: the PbCl2: the molar ratio of CsCl was: 1: 1-1: 3.
6. The growing method according to claim 3, wherein: the temperature of the solution is higher than 60 ℃, and the solution is cooled to room temperature by adopting a natural cooling mode.
7. The growing method according to claim 3, wherein: the temperature of the solution is lower than 60 ℃, and a lower cooling rate of 0.1 ℃/h is adopted.
8. The growing method according to claim 3, wherein: after the temperature of the solution is reduced to room temperature, the solvent is slowly volatilized, so that the crystal continues to grow.
9. A two-dimensional structure, large-size, blue-violet light emitting perovskite single crystal material obtained by the growth method according to any one of claims 1 to 8.
CN202010181827.2A 2020-03-16 2020-03-16 Pure inorganic narrow-spectrum blue-violet light emitting two-dimensional perovskite single crystal material and growth method Withdrawn CN111270310A (en)

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Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112195516A (en) * 2020-10-10 2021-01-08 东南大学 Mn-doped CsPb2Br5Method for preparing bulk crystals
CN113060762A (en) * 2021-03-25 2021-07-02 昆明理工大学 Perovskite X-ray scintillator and preparation method thereof
CN113620339A (en) * 2021-08-16 2021-11-09 浙江大学 Large-size ultrathin all-inorganic lead-halogen perovskite nanosheet and preparation method and application thereof

Cited By (6)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112195516A (en) * 2020-10-10 2021-01-08 东南大学 Mn-doped CsPb2Br5Method for preparing bulk crystals
CN112195516B (en) * 2020-10-10 2021-12-21 东南大学 Mn-doped CsPb2Br5Method for preparing bulk crystals
CN113060762A (en) * 2021-03-25 2021-07-02 昆明理工大学 Perovskite X-ray scintillator and preparation method thereof
CN113060762B (en) * 2021-03-25 2022-01-25 昆明理工大学 Perovskite X-ray scintillator and preparation method thereof
CN113620339A (en) * 2021-08-16 2021-11-09 浙江大学 Large-size ultrathin all-inorganic lead-halogen perovskite nanosheet and preparation method and application thereof
CN113620339B (en) * 2021-08-16 2022-06-07 浙江大学 Large-size ultrathin all-inorganic lead-halogen perovskite nanosheet and preparation method and application thereof

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Application publication date: 20200612