CN112725899A - Preparation method of 0-dimensional antimonide single crystal with optical waveguide property - Google Patents

Preparation method of 0-dimensional antimonide single crystal with optical waveguide property Download PDF

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CN112725899A
CN112725899A CN202011543230.4A CN202011543230A CN112725899A CN 112725899 A CN112725899 A CN 112725899A CN 202011543230 A CN202011543230 A CN 202011543230A CN 112725899 A CN112725899 A CN 112725899A
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optical waveguide
dimensional
single crystal
precursor solution
crystal
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CN112725899B (en
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解仁国
刘峰
汪大洋
杨文胜
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Jilin University
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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
    • C30B29/54—Organic compounds
    • 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
    • C30B29/60—Single crystals or homogeneous polycrystalline material with defined structure characterised by the material or by their shape characterised by shape
    • 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 invention relates to a preparation method of a 0-dimensional antimonide single crystal with optical waveguide properties, which belongs to the technical field of semiconductor material preparation, and the preparation method comprises the steps of firstly dissolving antimony chloride and dodecyl trimethyl ammonium chloride in a dimethyl formamide solution, carrying out strong ultrasonic dispersion and filtration to obtain a precursor solution, slowly diffusing a nonpolar solvent into the precursor solution in a sealed system, and precipitating a rod-shaped crystal after 24 hours to obtain the 0-dimensional antimonide single crystal with optical waveguide properties. The method has the advantages of simple operation, fixed crystal morphology, high fluorescence yield and the like, and the prepared crystal has excellent optical waveguide property and linear polarization property and shows double-optical property under high-energy excitation.

Description

Preparation method of 0-dimensional antimonide single crystal with optical waveguide property
Technical Field
The invention belongs to the technical field of semiconductor material preparation, and particularly relates to a synthesis method of a 0-dimensional organic-inorganic hybrid antimonide rod-shaped crystal with optical waveguide properties.
Background
Organic-inorganic hybrid metal halides are a class of materials with excellent photoelectric properties formed by self-assembly of organic cations and inorganic anions, and have become a hot spot of research in recent years. The organic-inorganic hybrid metal halide provides the possibility of integrating organic and inorganic characteristics into a single crystalline molecular composite material, and has a very wide application prospect in the optical fields of photovoltaic devices, light emitting diodes, optical pumping lasers and the like. One-and zero-dimensional structures with self-trapped excited state emission are relatively less studied than well-developed three-dimensional (3D) and two-dimensional (2D) metal halides with small stokes shift narrow-band emission.
Therefore, the selection of proper transition metal and organic matter hybridization in a visible light range has excellent optical properties, which is particularly important, and compared with the traditional lead-based perovskite, the transition metal halide has higher stability, can avoid the introduction of toxic heavy metals, and is a more green and environment-friendly fluorescent material.
Recently, more organic-inorganic hybrid antimony-based halides are reported, have higher fluorescence quantum yield and stability and few double-light properties, and can be used as a potential material of a white light LED. It is well known that the optical properties of a compound are influenced by the external shape, including shape and size. For example, a nano/micron crystal with a specific morphology can have the properties of an optical waveguide, and can be widely applied to optical devices. To date, relatively little research has been conducted into optical waveguides having organic-inorganic hybrid metal halide crystals of specific morphologies. Although organic-inorganic hybrid antimony-based halides have outstanding optical properties, for most hybrid metal halides, only irregular crystals are obtained after crystal growth, which limits their application in the optical field.
In summary, further improvements are needed in the current methods for preparing organic-inorganic hybrid antimony-based halide crystals.
Disclosure of Invention
The technical problem to be solved by the invention is to overcome the problems in the background technology and provide a method for synthesizing 0-dimensional organic-inorganic hybrid antimonide rod-shaped crystal with optical waveguide property.
The technical problem of the invention is solved by the following technical scheme:
a preparation method of a 0-dimensional antimonide single crystal with optical waveguide properties comprises the steps of firstly dissolving antimony chloride and dodecyl trimethyl ammonium chloride in a dimethyl formamide solution according to a molar ratio of 1: 1-6, carrying out strong ultrasonic dispersion by using an ultrasonic crusher, filtering by using a 0.22-micron organic microporous filter membrane to obtain a precursor solution, slowly diffusing diethyl ether or isopropyl ether serving as a nonpolar solvent into the precursor solution under a sealed system, wherein the volume ratio of the nonpolar solvent to the precursor solution is 1.5-3: 1, and precipitating a rod-shaped crystal after 24 hours, namely the 0-dimensional antimonide single crystal with optical waveguide properties.
In the method for producing a 0-dimensional antimonide single crystal having optical waveguide properties of the present invention, it is preferable to dissolve 11ml of dimethylformamide per millimole of antimony chloride.
In the method for preparing a 0-dimensional antimonide single crystal having optical waveguide properties according to the present invention, the molar ratio of antimony chloride to dodecyltrimethylammonium chloride is preferably 1: 2.
In the method for preparing a 0-dimensional antimonide single crystal having optical waveguide properties of the present invention, the volume ratio of the nonpolar solvent to the precursor solution is preferably 2: 1.
Has the advantages that:
the invention provides a synthesis method of an anti-solvent by using dodecyl trimethyl quaternary ammonium salt and antimony chloride, and finally synthesizing an organic-inorganic hybrid halogen antimonide crystal, wherein the organic-inorganic hybrid halogen antimonide crystal is rod-shaped, has excellent optical waveguide property and linear polarization property, has the fluorescence yield of 78 percent, and shows double-optical property under high-energy excitation.
The method has the advantages of simple operation, fixed crystal morphology, high fluorescence yield and the like.
Drawings
FIG. 1 is an absorption spectrum of the rod-like crystalline powder of organic-inorganic hybrid antimonide prepared in example 1.
FIG. 2 is a fluorescence emission spectrum of the organic-inorganic hybrid antimonide rod-shaped crystal prepared in example 1 under excitation of 360nm and 320 nm.
FIG. 3 is an XRD spectrum of the rod-shaped crystalline powder of organic-inorganic hybrid antimonide prepared in example 1.
FIG. 4 is an optical waveguide spectrum of the organic-inorganic hybrid antimonide rod crystal prepared in example 1.
FIG. 5 is a linear polarization spectrum of the organic-inorganic hybrid antimonide rod-shaped crystal prepared in example 1.
Detailed Description
Example 1:
firstly, 0.5mmol of antimony chloride and 1mmol of dodecyl trimethyl ammonium chloride are dissolved in 5.5ml of dimethylformamide solution, strong ultrasonic dispersion is carried out by using a sonic ultrasonicator vcx750, the power is 50 percent, the solution is treated for 10 minutes in a cold water bath, and the solution is filtered by a 0.22um organic microporous filter membrane to obtain a precursor solution. Under a sealed system, 11ml of diethyl ether as a nonpolar solvent was slowly diffused into a container containing 5.5ml of the precursor solution, and rod-shaped crystals slowly precipitated after 24 hours. The product was subjected to solid absorption analysis and fluorescence emission test, the absorption spectrum is shown in fig. 1, the emission spectrum under excitation of 360nm and 320nm is shown in fig. 2, the fluorescence yield is 78%, the XRD spectrum of the product is shown in fig. 3, the optical waveguide of the product under excitation of a laser (350nm) is shown in fig. 4, and the linear polarization is shown in fig. 5.
Example 2:
the dosage of the dodecyl trimethyl quaternary ammonium salt in the embodiment 1 is changed from 1mmol to 1.5mmol, 2mmol and 2.5mmol respectively, and the rod-shaped crystal can be obtained without changing other conditions and steps, and the fluorescence property is not changed.
Example 3:
the dosage of the ether in the example 1 is changed from 11ml to 8.25ml and 16.5ml respectively, and the rod-shaped crystal can be obtained without changing other conditions and steps, and the fluorescence property is not changed.
Example 4:
the ether in example 1 is changed into isopropyl ether as a reverse polarity diffusion solvent, and other conditions and steps are not changed, so that rod-shaped crystals can be obtained, and the fluorescence property is not changed.
It should be understood that the above-described embodiments of the present invention are merely examples for clearly illustrating the present invention, and are not intended to limit the embodiments of the present invention. Other variations and modifications will be apparent to persons skilled in the art in light of the above description. And are neither required nor exhaustive of all embodiments. Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention should be included in the protection scope of the claims of the present invention.

Claims (4)

1. A preparation method of a 0-dimensional antimonide single crystal with optical waveguide properties comprises the steps of firstly dissolving antimony chloride and dodecyl trimethyl ammonium chloride in a dimethyl formamide solution according to a molar ratio of 1: 1-6, carrying out strong ultrasonic dispersion by using an ultrasonic crusher, filtering by using a 0.22-micron organic microporous filter membrane to obtain a precursor solution, slowly diffusing diethyl ether or isopropyl ether serving as a nonpolar solvent into the precursor solution under a sealed system, wherein the volume ratio of the nonpolar solvent to the precursor solution is 1.5-3: 1, and precipitating a rod-shaped crystal after 24 hours, namely the 0-dimensional antimonide single crystal with optical waveguide properties.
2. The method for producing a 0-dimensional antimonide single crystal having optical waveguide properties according to claim 1, wherein 11ml of dimethylformamide is used for dissolving antimony chloride per mmol of antimony chloride.
3. The method of claim 1, wherein the molar ratio of antimony chloride to dodecyltrimethylammonium chloride is 1: 2.
4. The method of claim 1, wherein the volume ratio of the nonpolar solvent to the precursor solution is 2: 1.
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Cited By (3)

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Publication number Priority date Publication date Assignee Title
CN114716324A (en) * 2022-04-26 2022-07-08 福州大学 Organic-inorganic hybrid metal halide perovskite compound, preparation method and application
CN114736127A (en) * 2022-04-02 2022-07-12 中山大学 Antimony pentachloride fluorescent compound, crystal, preparation method and application thereof
CN114907835A (en) * 2022-04-29 2022-08-16 北京理工大学 Zero-dimensional organic-inorganic hybrid metal halide single crystal material, preparation method and application thereof

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CN105789465A (en) * 2016-04-05 2016-07-20 南昌航空大学 Method of preparing antimony-containing organic-inorganic perovskite quantum dot electroluminescent diode
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CN108329912A (en) * 2018-01-18 2018-07-27 华中科技大学 A method of improving the fluorescent yield and stability of non-lead halogen perovskite material
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Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114736127A (en) * 2022-04-02 2022-07-12 中山大学 Antimony pentachloride fluorescent compound, crystal, preparation method and application thereof
CN114716324A (en) * 2022-04-26 2022-07-08 福州大学 Organic-inorganic hybrid metal halide perovskite compound, preparation method and application
CN114907835A (en) * 2022-04-29 2022-08-16 北京理工大学 Zero-dimensional organic-inorganic hybrid metal halide single crystal material, preparation method and application thereof
CN114907835B (en) * 2022-04-29 2023-11-21 北京理工大学 Zero-dimensional organic-inorganic hybrid metal halide single crystal material, preparation method and application thereof

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