CN112624978B - Benzimidazole cation <100> type two-dimensional perovskite material, preparation method and application thereof - Google Patents

Benzimidazole cation <100> type two-dimensional perovskite material, preparation method and application thereof Download PDF

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CN112624978B
CN112624978B CN202011416643.6A CN202011416643A CN112624978B CN 112624978 B CN112624978 B CN 112624978B CN 202011416643 A CN202011416643 A CN 202011416643A CN 112624978 B CN112624978 B CN 112624978B
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benzimidazole
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CN112624978A (en
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崔彬彬
韩颖
曹广岳
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Beijing Institute of Technology BIT
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    • C07D235/02—Heterocyclic compounds containing 1,3-diazole or hydrogenated 1,3-diazole rings, condensed with other rings condensed with carbocyclic rings or ring systems
    • C07D235/04—Benzimidazoles; Hydrogenated benzimidazoles
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Abstract

The invention relates toBenzimidazole cation<100>A two-dimensional perovskite material, a preparation method and application thereof belong to the technical field of luminescent materials. The chemical formula of the material is (C) 7 H 7 N 2 ) 2 BX 4 B is a metal ion Pb 2+ 、Sn 2+ Or Ge 2+ X is a halogen ion Cl ‑ Or Br ‑ . The material has high stability, wherein<100>Type 2D perovskite material (C) 7 H 7 N 2 ) 2 PbBr 4 Exhibits bright deep blue emission; the structure is regular<100>Type 2D perovskite material (C) 7 H 7 N 2 ) 2 PbCl 4 Is a single-component white light luminescent material. Compared with an anti-solvent method and a volatilization method, the crystal material prepared by the cooling method has larger size, the obtained crystal is transparent, has no obvious crystal boundary, has less crystal defect states, and is a near-perfect single crystal material with regular structure and long-range order.

Description

Benzimidazole cation <100> type two-dimensional perovskite material, preparation method and application thereof
Technical Field
The invention relates to a benzimidazole cation <100> type two-dimensional perovskite material, a preparation method and application thereof, belonging to the technical field of luminescent materials.
Background
Over the past decade, Solid State Lighting (SSL) has emerged in the corner of the automotive lighting, architectural lighting, and general lighting markets. Compared with the traditional incandescent lamp and fluorescent lamp, the LED lamp has the advantages of low energy consumption, high efficiency, long service life and the like. Typical SSL devices include a single phosphor coated Light Emitting Diode (LED) (e.g., a yellow phosphor coated blue LED) or a mixed phosphor coated LED (e.g., a blue and yellow phosphor coated ultraviolet LED). Despite significant advances in the down-conversion technology of white leds, there are still many problems and challenges that limit their development, for example, monochromaticity tends to be poor due to the discontinuity of the emission spectrum. On the other hand, mixed phosphors can reduce efficiency due to self-absorption effects. Meanwhile, due to different attenuation degrees, the light emitting color of the fluorescent powder can change along with the change of time. To solve these problems, a desirable solution for a single-component white light-emitting phosphor was developed. Such materials are currently relatively rare. Most of them are inorganic materials doped with rare earth elements. These inorganic phosphors have generally low luminous efficiency, complex manufacturing process and high manufacturing cost. Therefore, the development of novel single-component white light materials is of great significance. At present, the <110> type structure distorted corrugated two-dimensional material is widely noticed due to the characteristic of single-component broad-peak white light emission, but the distorted corrugated configuration of the <110> type two-dimensional (2D) material is mainly stabilized by the hydrogen bonding force formed between the hydrogen atom on the A-site cationic amine group and the halogen atom of the lead halogen octahedron, so the structural stability of the <100> type two-dimensional perovskite material is poor. No <100> type two-dimensional perovskite with a single component white light with regular and non-distorted structure has been found so far. Furthermore, solid state lighting requires the generation of red, green and blue light sources across the full color gamut and white light, and blue light emitting materials have proven to be the most challenging, and finding a <100> type two-dimensional perovskite material with efficient narrow-band pure blue light emission characteristics is crucial.
Disclosure of Invention
In view of the above, the present invention aims to provide a benzimidazole cation <100> type two-dimensional perovskite material, a preparation method and applications thereof.
In order to achieve the purpose, the technical scheme of the invention is as follows:
benzimidazole cation<100>A type two-dimensional perovskite material having the chemical formula (C) 7 H 7 N 2 ) 2 BX 4 B is a metal ion Pb 2+ 、Sn 2+ Or Ge 2+ X is a halogen ion Cl - Or Br - 。
Preferably, the material has the chemical formula (C) 7 H 7 N 2 ) 2 PbCl 4 (BM-Cl for short).
Preferably, the material has the chemical formula (C) 7 H 7 N 2 ) 2 PbBr 4 (BM-Br for short).
A preparation method of benzimidazole cation <100> type two-dimensional perovskite single crystal material comprises the following steps:
adding benzimidazole and B-site metal oxide or B-site metal halide into halogen acid, heating to completely dissolve, then cooling to room temperature at the speed of 1-5 ℃/h, taking out crystals, and washing to obtain a benzimidazole cation <100> type two-dimensional perovskite material;
wherein the B-site metal oxide is PbO, SnO or GeO;
the B-site metal halide is chloride, bromide or iodide of Pb, Sn or Ge;
the halogen acid is hydrochloric acid or bromine hydrogen acid.
Preferably, the amount ratio of the B-site metal oxide or B-site metal halide to the halogen acid is 0.05mol to 0.5 mol: 1L of the compound.
Preferably, the heating temperature is 70-150 ℃, and the heat preservation time is 0.5-2 h.
Preferably, the benzimidazole and the B-site metal oxide or the B-site metal halide are added into a mixture of a halogen acid and an organic solvent, wherein the organic solvent is dimethyl formamide (DMF) or dimethyl sulfoxide (DMSO), and the volume ratio of the halogen acid to the organic solvent is 1:4-4: 1.
Application of benzimidazole cation <100> type two-dimensional perovskite single crystal material, wherein the material is used as a luminescent material.
Preferably, the material is (C) 7 H 7 N 2 ) 2 PbCl 4 When used as a single-component white light emitting material.
Preferably, the material is (C) 7 H 7 N 2 ) 2 PbBr 4 When used as a single-component blue light emitting material.
Advantageous effects
The material of the invention takes benzimidazole as cation<100>A two-dimensional perovskite structure of the type in which the material stability is high, wherein<100>Type 2D perovskite material (C) 7 H 7 N 2 ) 2 PbBr 4 Exhibits bright deep blue emission; the structure is regular<100>Type 2D perovskite material (C) 7 H 7 N 2 ) 2 PbCl 4 Is a single-component white light luminescent material. Compared with an anti-solvent method and a volatilization method, the crystal material prepared by the cooling method has larger size, the obtained crystal is transparent, has no obvious crystal boundary, has less crystal defect states, and is a nearly perfect single crystal material with regular structure and long-range order.
Drawings
FIG. 1 is a single crystal diffraction structure diagram of the material described in example 1;
FIG. 2 is a single crystal diffraction structure of the material described in example 2;
FIG. 3 is a powder X-ray diffraction (PXRD) pattern of the material described in example 1;
FIG. 4 is a PXRD pattern of the material described in example 2;
FIG. 5 is a photograph of the morphology and luminescence under UV light of the material of example 1;
FIG. 6 is a photograph of the morphology and luminescence of the material of example 2 under UV lamp illumination;
FIG. 7 is a photograph of a UV-LED lamp coated with the material described in example 2 in the off and on states;
FIG. 8 is a graph of the UV-VIS absorption spectra of the materials of examples 1 and 2;
FIG. 9 is a plot of the fluorescence emission spectra (PL) of the materials described in examples 1 and 2;
FIG. 10 is a time resolved photoluminescence spectrum (TRPL) plot of the materials described in examples 1 and 2;
FIG. 11 is a graph of temperature change PL for the material described in example 1;
FIG. 12 is a graph of temperature change PL for the material described in example 2;
fig. 13 is a Thermogravimetric (TG) plot of the mass as a function of temperature for the materials described in examples 1 and 2.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
In the following examples:
(1) PXRD test: d8ADVANCE X-ray diffractometer was used to scan the diffraction over a range of 5-60 degrees at room temperature in 5 deg./min steps using copper X-ray tube (standard) radiation at 40kV and 40mA current.
(2) Ultraviolet visible absorption spectrum: UV-3600 ultraviolet-visible-near infrared spectrophotometer.
(3) Fluorescence emission spectrum: FLS980 fluorescence spectrometer (edinburg instruments).
(4) Time resolved photoluminescence spectroscopy: FLS980 fluorescence spectrometer (edinburg instruments).
(5) Temperature-variable fluorescence emission spectrum: FLS980 fluorescence spectrometer (edinburg instruments).
(6) Thermogravimetric analysis: STA449F5 thermogravimetric analyzer.
Example 1
Mixing solid PbO (0.225mmol, 50mg) and benzimidazole (0.45mmol, 52.9mg) with 2mL hydrobromic acid with mass fraction of 48% in a glass tube at room temperature, heating to 95 ℃, keeping the temperature for 2h until the solid is dissolved, then slowly cooling to room temperature at the speed of 1 ℃/h to obtain crystals, and washing the crystals from the mother liquor by using acetone to obtain a light yellow flaky monocrystal (C) 7 H 7 N 2 ) 2 PbBr 4 (BM-Br)。
As can be seen from the single crystal diffraction pattern of FIG. 1, the crystal structure of BM-Br is<100>Type two-dimensional perovskite configuration, 2D PbBr 4 2- The inorganic layers are separated by benzimidazole cations.
As shown in fig. 3, the PXRD pattern of the final product sample after ball milling was consistent with the single crystal simulated PXRD pattern, further confirming the structure of BM-Br.
As shown in FIG. 5, the color of BM-Br plate crystal is light yellow (FIG. 5 left), and BM-Br emits deep blue light at room temperature by irradiation with a 325nm UV lamp (FIG. 5 right).
From the absorption spectrum of BM-Br in FIG. 8, a band gap of 2.27eV can be calculated.
As shown by the PL spectrum of FIG. 9, BM-Br showed two distinct blue emissions at 442nm and 468nm, respectively, due to the emission of surface and internal bulk crystals, respectively.
As shown in FIG. 10, the luminescence decay times of BM-Br at 468nm and 442nm were 1.25ns and 1.18ns, respectively.
FIG. 11 is a temperature-variable spectrum of BM-Br, which shows a broad peak of self-trapping state in a low energy region when the temperature is decreased to 230K, and gradually increases with decreasing temperature.
As shown in FIG. 13, <100> type two-dimensional perovskite BM-Br was excellent in thermal stability and did not decompose at about 260 ℃.
Example 2
Mixing solid PbO (0.225mmol, 50mg) and benzimidazole (0.45mmol, 52.9mg) with 2mL hydrochloric acid with mass fraction of 37% at room temperature in a glass tube, heating to 95 deg.C, maintaining the temperature for 2h to dissolve the solid, slowly cooling to room temperature at 1 deg.C/h to obtain crystals, and washing with acetone to obtain almost transparent needle-like crystals (C) 7 H 7 N 2 ) 2 PbCl 4 (BM-Cl)。
As can be seen from the single crystal diffraction pattern of FIG. 2, the crystal structure of BM-Cl is<100>Type two-dimensional perovskite configuration, 2D PbCl 4 2- The inorganic layers are separated by benzimidazole cations.
As shown in fig. 4, the PXRD pattern of the final product after ball milling was consistent with the single crystal simulated PXRD pattern, further confirming the structure of BM-Cl.
As shown in FIG. 6, the color of the needle-shaped crystals of BM-Cl was transparent (left in FIG. 6), and BM-Cl emitted bright white light at room temperature under irradiation with a 325nm UV lamp (right in FIG. 6).
As shown in FIG. 7, a UV-LED lamp with a thin BM-Cl layer adhered thereto can emit bright white light.
From the absorption spectrum of BM-Cl shown in FIG. 8, a band gap of 3.13eV can be calculated.
As shown in the PL spectrum of FIG. 9, the BM-Cl crystal dominated a broadband emission of 500nm with a full width at half maximum (FWHM) of 245nm at room temperature.
As shown in FIG. 10, the emission decay time of the broad peak of BM-Cl was 11.9 ns.
FIG. 12 is a temperature-varying spectrum of BM-Cl with narrow peak emission in the high-energy region increasing with decreasing temperature.
As shown in FIG. 13, the <100> type two-dimensional perovskite BM-Cl has excellent thermal stability and does not undergo decomposition at about 240 ℃.
Example 3
Preparation of (C) by anti-solvent method 7 H 7 N 2 ) 2 PbBr 4 The single crystal steps are as follows:
dissolving PbO (0.225mmol, 50mg) and benzimidazole (0.45mmol, 52.9mg) in 4mL of 48% hydrobromic acid to obtain clear precursor solution, placing the precursor solution in a small bottle, using acetone or diethyl ether as an anti-solvent, and diffusing the acetone or diethyl ether in the system for 24h to obtain light yellow flaky crystals (C) 7 H 7 N 2 ) 2 PbBr 4 。
The sheet material was smaller in size than the material described in example 1, with individual distinct grain boundaries.
Example 4
Preparation of (C) by anti-solvent method 7 H 7 N 2 ) 2 PbCl 4 The single crystal steps are as follows:
dissolving PbO (0.225mmol, 50mg) and benzimidazole (0.45mmol, 52.9mg) in 4mL hydrochloric acid solution with mass fraction of 37% to obtain clear precursor solution, placing the precursor solution in a small bottle, using acetone or diethyl ether as anti-solvent, and obtaining almost transparent needle crystal (C) after acetone or diethyl ether diffuses in the system for 24h 7 H 7 N 2 ) 2 PbCl 4 。
The needle-like material was smaller in size than the material described in example 2.
Example 5
Preparation of (C) by slow volatilization 7 H 7 N 2 ) 2 PbBr 4 The single crystal steps are as follows:
mixing benzimidazole bromide salt and PbBr 2 And (3) adding the following components in percentage by weight of 2: 1 molar ratio in a small beaker, PbBr was dissolved in DMF solvent 2 And benzimidazole bromide. Then slowly evaporating by DMF solution in a vacuum oven (or heating-assisted evaporation) to obtain (C) 7 H 7 N 2 ) 2 PbBr 4 And (3) single crystal.
The sheet material was smaller in size than the material described in example 1, with small particle crystals packed together with distinct grain boundaries.
Example 6
Preparation of (C) by slow volatilization 7 H 7 N 2 ) 2 PbCl 4 The single crystal steps are as follows:
mixing benzimidazole chloride salt and PbCl 2 And (3) adding the following components in percentage by weight of 2: 1 molar ratio in a vial, PbCl was dissolved with DMF solvent 2 And benzimidazole chloride. Then slowly evaporating by DMF solution in a vacuum oven (or heating-assisted evaporation) to obtain (C) 7 H 7 N 2 ) 2 PbCl 4 And (3) single crystal.
The needle-like material was smaller in size than the material described in example 2.
In summary, the invention includes but is not limited to the above embodiments, and any equivalent replacement or local modification made under the spirit and principle of the invention should be considered as being within the protection scope of the invention.

Claims (5)

1. Benzimidazole cation<100>A two-dimensional perovskite material characterized by: the chemical formula of the material is (C) 7 H 7 N 2 ) 2 BX 4 ，(C 7 H 7 N 2 ) + Is a benzimidazole cation, B is a metal ion Pb 2+ X is a halogen ion Br - (ii) a The material is of a single-crystal and double-peak emission structure and is prepared by the following method, and the method comprises the following steps:
adding benzimidazole and B-site metal oxide or B-site metal halide into halogen acid, heating until the benzimidazole and the B-site metal oxide or the B-site metal halide are completely dissolved, then cooling to room temperature at the speed of 1-5 ℃/h, taking out crystals, and washing to obtain a benzimidazole cation <100> type two-dimensional perovskite material;
wherein the B-site metal oxide is PbO;
the B-site metal halide is a bromide of Pb;
the halogen acid is hydrogen bromide acid;
the heating temperature is 70-150 ℃.
2. A benzimidazole cation <100> type two-dimensional perovskite material as claimed in claim 1, wherein: the dosage ratio of the B-site metal oxide or the B-site metal halide to the halogen acid is 0.05mol-0.5 mol: 1L of the compound.
3. A benzimidazole cation <100> type two-dimensional perovskite material as claimed in claim 1, wherein: the heat preservation time is 0.5-2h when heating.
4. A benzimidazole cation <100> type two-dimensional perovskite material as claimed in claim 1, wherein: adding benzimidazole and B-site metal oxide or B-site metal halide into a mixture of halogen acid and an organic solvent, wherein the organic solvent is DMF or DMSO, and the volume ratio of the halogen acid to the organic solvent is 1:4-4: 1.
5. Use of a benzimidazole cation <100> type two-dimensional perovskite material according to claim 1, wherein: the material is used as a single-component blue light emitting material.
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