CN109411327B - All-inorganic perovskite nanowire CsPbX2Y and preparation method and application thereof - Google Patents

All-inorganic perovskite nanowire CsPbX2Y and preparation method and application thereof Download PDF

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CN109411327B
CN109411327B CN201811075229.6A CN201811075229A CN109411327B CN 109411327 B CN109411327 B CN 109411327B CN 201811075229 A CN201811075229 A CN 201811075229A CN 109411327 B CN109411327 B CN 109411327B
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inorganic perovskite
cspbx
perovskite nanowire
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CN109411327A (en
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周张凯
蒋丽
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National Sun Yat Sen University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01L—SEMICONDUCTOR DEVICES NOT COVERED BY CLASS H10
    • H01L21/00—Processes or apparatus adapted for the manufacture or treatment of semiconductor or solid state devices or of parts thereof
    • H01L21/02—Manufacture or treatment of semiconductor devices or of parts thereof
    • H01L21/02104—Forming layers
    • H01L21/02365—Forming inorganic semiconducting materials on a substrate
    • H01L21/02518—Deposited layers
    • H01L21/02587—Structure
    • H01L21/0259—Microstructure
    • H01L21/02603—Nanowires
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B82—NANOTECHNOLOGY
    • B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
    • B82Y40/00—Manufacture or treatment of nanostructures

Abstract

The invention relates to an all-inorganic perovskite nanowire CsPbX2Y and a preparation method and application thereof. The preparation method comprises the following steps: s1: mixing PbX2And CsY is dissolved in the solvent A to form a mixed solution; wherein X, Y are all halogens; the solvent A is one or two of dimethyl sulfoxide or dimethylformamide; s2: coating the mixed solution S1 on a substrate, and standing the substrate in a closed environment with a solvent B volatilization atmosphere at 17-25 ℃ for 12-24 h to obtain the fully inorganic perovskite nanowire CsPbX with good dispersibility2Y; the solvent B is one or more of isopropanol, n-propanol, n-butanol or cyclohexane. The preparation method provided by the invention has the advantages of low cost, simple process and easily-controlled conditions, and the obtained all-inorganic perovskite nanowire CsPbX2The Y has uniform appearance, good dispersibility and high crystal quality, and can be used as a potential laser material to be applied to a photoelectric detector or a laser.

Description

All-inorganic perovskite nanowire CsPbX2Y and preparation method and application thereof
Technical Field
The invention belongs to the field of inorganic nanowire preparation, and particularly relates to an all-inorganic perovskite nanowire CsPbX2Y and a preparation method and application thereof.
Background
The perovskite material has great application value due to excellent and unique optical and electrical properties, and can be applied to photoelectric detectors, lasers and the like as a photoelectric material. Most perovskite materials synthesized by the prior art are synthesized by a chemical vapor deposition method or a high-temperature pyrolysis method, and the synthesis equipment is expensive, the synthesis process is complex, the controllability of process conditions is not strong, the morphology and the structure are not uniform, so that the further application of a sample is limited.
Therefore, it is necessary to develop a perovskite material with low cost, simple preparation process and controllable structural morphology to promote further application of the perovskite material.
Disclosure of Invention
The invention aims to overcome the defects of high cost, complex preparation process, low controllability of process conditions, uneven morphology and structure and the like of perovskite materials in the prior art, and provides the CsPbX full-inorganic perovskite nanowire2A method for preparing Y. The preparation method has the advantages of low cost, simple preparation process and easily controlled process conditions, and the prepared all-inorganic perovskite nanowire CsPbX is prepared2The shape of Y is uniform, the dispersity is good, and the crystal quality is high.
Another purpose of the invention is to provide the fully inorganic perovskite nanowire CsPbX prepared by the method2Y。
Another object of the present invention is to provide the above-mentioned all-inorganic perovskite nanowireCsPbX2The use of Y in a photodetector or a laser.
In order to achieve the purpose, the invention adopts the following technical scheme:
all-inorganic perovskite nanowire CsPbX2The preparation method of Y comprises the following steps:
s1: mixing PbX2And CsY is dissolved in the solvent A to form a mixed solution; wherein X, Y are all halogens; the solvent A is one or two of dimethyl sulfoxide or dimethylformamide;
s2: coating the mixed solution S1 on a substrate, and standing the substrate in a closed environment with a solvent B volatilization atmosphere at 17-25 ℃ for 12-24 h to obtain the fully inorganic perovskite nanowire CsPbX with good dispersibility2Y; the solvent B is one or more of isopropanol, n-propanol, n-butanol or cyclohexane.
Controlling PbX2The volatilization rate of the solvent in the mixed solution of CsY and CsPbX is that the prepared all-inorganic perovskite nanowire CsPbX has uniform appearance, good dispersibility and high crystal quality2Key step of Y. Through multiple researches, the inventor of the invention discovers that when one or two of dimethyl sulfoxide and dimethylformamide is selected as a dissolving solvent, the dissolving solvent can be slowly volatilized at a lower temperature of 17-25 ℃ under the volatilization atmosphere of one or more of isopropanol, normal propanol, normal butanol or cyclohexane, the crystallization speed in the solution is reduced, and the all-inorganic perovskite nanowire CsPbX obtained through the reaction can be obtained2The Y shape is uniform, the dispersibility is good, the crystal quality is high, and the all-inorganic perovskite nanowire CsPbX2The Y can be used as a potential laser material in a photoelectric detector or a laser.
In addition, the preparation method has low cost, simple preparation process and easily controlled process conditions.
Preferably, each of said X, Y is independently selected from Cl, Br or I; and X, Y where one is Cl, the other is not I.
All-inorganic perovskite nanowire CsPbX prepared by using lead halide and cesium halide as raw materials2The morphology of Y is relatively uniform.
More preferably, both X and Y are Cl, Br or I.
When X and Y are Cl, Br or I, the prepared all-inorganic perovskite nanowire CsPbX2The purity of Y is high and the appearance is uniform.
Preferably, PbX is contained in the mixed solution S12The concentration of (b) is 0.001-0.25 mol/L, and the molar ratio of Pb ions to Cs ions is 1: 1.
The fully inorganic perovskite nano-wire CsPbX prepared in the concentration range2The length of Y is moderate, and the quality is high.
Preferably, the solvent a in S1 is dimethylformamide.
All-inorganic perovskite nanowire CsPbX prepared by using dimethylformamide as solvent A2The Y dispersibility is better.
Preferably, the solvent B in S2 is isopropanol.
The atmosphere formed by the volatilization of the isopropanol has the best effect of slowing down the volatilization of the mixed solution, and the prepared all-inorganic perovskite nanowire CsPbX2The morphology of Y is more uniform.
Preferably, the substrate in S2 is a silicon wafer, a quartz wafer, or ITO.
The surface of the material as a substrate is smooth, and the prepared all-inorganic perovskite nanowire CsPbX2The morphology of Y is relatively uniform.
The invention also provides the fully inorganic perovskite nanowire CsPbX2Y, obtained by the above preparation method.
Preferably, the all-inorganic perovskite nanowire CsPbX2The length of Y is 1.5 to 12 μm.
The length of the fully inorganic perovskite nanowire CsPbX is in the range2The Y has higher application value in a photoelectric detector or a laser.
The above-mentioned all-inorganic perovskite nanowire CsPbX2The use of Y in photodetectors or lasers is also within the scope of the present invention.
Compared with the prior art, the invention has the following beneficial effects:
the invention provides a medicineOrganic perovskite nanowire CsPbX2The preparation method of Y has low cost, simple preparation process and easily controlled process conditions, and the prepared all-inorganic perovskite nanowire CsPbX is2The shape of Y is uniform, the dispersity is good, and the crystal quality is high; the all-inorganic perovskite nanowire CsPbX2The Y can be used as a potential laser material in a photoelectric detector or a laser.
Drawings
FIG. 1 shows the CsPbX full-inorganic perovskite nanowire provided in example 12SEM picture of Y;
FIG. 2 shows the CsPbX full-inorganic perovskite nanowire provided in example 22SEM picture of Y;
FIG. 3 shows the CsPbX full-inorganic perovskite nanowire provided in example 12Experimental setup diagram of Y;
wherein, 1 is a beaker; 2 is a sealant; 3 is a platform; 4 is a substrate; 5 is isopropanol; 6 is a mixed solution.
Detailed Description
The invention is further illustrated by the following examples. These examples are intended to illustrate the invention and are not intended to limit the scope of the invention. Experimental procedures without specific conditions noted in the examples below, generally according to conditions conventional in the art or as suggested by the manufacturer; the raw materials, reagents and the like used are, unless otherwise specified, those commercially available from the conventional markets and the like. Any insubstantial changes and substitutions made by those skilled in the art based on the present invention are intended to be covered by the claims.
Example 1
This example provides an all-inorganic perovskite nanowire CsPbBr3. The preparation method comprises the following steps:
0.02mmol of lead halide (PbBr) was added to a small beaker (10 mL) in that order2) And 0.02mmol cesium halide (CsBr) and 2.0mL DMF, stirred to complete dissolution. Dropping 2 μ L of the mixed solution on a silicon substrate suspended on a platform above the isopropanol liquid level, sealing a beaker (100 mL) as shown in FIG. 3, placing in an environment of 22 deg.C, and standing for 12 hr to obtain the final product with good dispersibilityAll-inorganic perovskite nanowire (CsPbBr)3）。
As shown in FIG. 1, the all-inorganic perovskite nanowire prepared by the embodiment has good dispersibility and uniform morphology, and the length of the all-inorganic perovskite nanowire is 1.5-2.0 μm.
Example 2
This example provides an all-inorganic perovskite nanowire CsPbBr3. The preparation method comprises the following steps:
0.1mmol of lead halide (PbBr) was added to a small beaker (10 mL) in that order2) And 0.1mmol cesium halide (CsBr) and 2.0mL DMF, stirred to complete dissolution. Dropping 2 μ L of the mixed solution on a silicon substrate suspended on a platform above the isopropanol liquid level, sealing a beaker (100 mL), placing in an environment of 20 ℃, and obtaining the fully inorganic perovskite nanowire (CsPbBr) with good dispersibility after 12h3）。
As shown in FIG. 2, the all-inorganic perovskite nanowire prepared by the embodiment has good dispersibility and uniform morphology, and the length of the all-inorganic perovskite nanowire is 6.0-12.0 μm.
Example 3
This example provides an all-inorganic perovskite nanowire CsPbBr2I. In the preparation method, 0.002mmol of PbBr is selected as lead halide2The cesium halide was chosen for CsI of 0.002mmol, and the rest of the procedure was the same as in example 1.
The fully inorganic perovskite nanowire (CsPbBr) prepared in this example2I) The dispersibility, morphology and length are similar to those of example 1.
Example 4
This example provides an all-inorganic perovskite nanowire CsPbBr3. In the preparation method, the adding amount of the lead halide and the adding amount of the cesium halide are both 0.5mmol, and the rest steps are the same as the steps in the example 1.
The fully inorganic perovskite nanowire (CsPbBr) prepared in this example3) The dispersibility, morphology and length are similar to those of example 2.
Example 5
This example provides an all-inorganic perovskite nanowire CsPbBr3. In the preparation method, DMF is changed into dimethyl sulfoxide, isopropanol is changed into normal propanol, and the reaction is carried outThe temperature was 17 ℃ and the reaction time was 24h, the rest of the procedure being identical to that of example 1.
The fully inorganic perovskite nanowire (CsPbBr) prepared in this example3) The dispersibility, morphology and length are similar to those of example 1.
Example 6
This example provides an all-inorganic perovskite nanowire CsPbBr3. In the preparation method, isopropanol is changed into n-butanol, the reaction temperature is 25 ℃, the substrate is quartz plate, and the rest steps are the same as those in the example 1.
The fully inorganic perovskite nanowire (CsPbBr) prepared in this example3) The dispersibility, morphology and length are similar to those of example 1.
Example 7
This example provides an all-inorganic perovskite nanowire CsPbBr3. In the preparation method, isopropanol is changed into cyclohexane, the substrate is ITO, and the rest steps are the same as those in the embodiment 1.
The fully inorganic perovskite nanowire (CsPbBr) prepared in this example3) The dispersibility, morphology and length are similar to those of example 1.
It will be appreciated by those of ordinary skill in the art that the examples provided herein are intended to assist the reader in understanding the principles of the invention and are to be construed as being without limitation to such specifically recited examples and embodiments. Those skilled in the art can make various other specific changes and combinations based on the teachings of the present invention without departing from the spirit of the invention, and these changes and combinations are within the scope of the invention.

Claims (10)

1. All-inorganic perovskite nanowire CsPbX2The preparation method of Y is characterized by comprising the following steps:
s1: mixing PbX2And CsY is dissolved in the solvent A to form a mixed solution; wherein X, Y are all halogens; the solvent A is one or two of dimethyl sulfoxide or dimethylformamide;
s2: coating the mixed solution S1 on a substrate, and placing the substrate onStanding the mixture for 12-24 hours at 17-25 ℃ in a closed environment with a solvent B volatilization atmosphere to obtain the fully inorganic perovskite nanowire CsPbX with good dispersibility2Y; the solvent B is one or more of isopropanol, n-propanol, n-butanol or cyclohexane.
2. The all-inorganic perovskite nanowire CsPbX of claim 12A process for the preparation of Y, wherein each of said X, Y is independently selected from Cl, Br or I; and X, Y where one is Cl, the other is not I.
3. The all-inorganic perovskite nanowire CsPbX of claim 22The preparation method of Y is characterized in that X and Y are Cl, Br or I.
4. The all-inorganic perovskite nanowire CsPbX of claim 12The preparation method of Y is characterized in that PbX is contained in the mixed solution of S12The concentration of (b) is 0.001-0.25 mol/L, and the molar ratio of Pb ions to Cs ions is 1: 1.
5. The all-inorganic perovskite nanowire CsPbX of claim 12A method for producing Y, wherein the solvent a in S1 is dimethylformamide.
6. The all-inorganic perovskite nanowire CsPbX of claim 12The process for producing Y is characterized in that the solvent B in S2 is isopropyl alcohol.
7. The all-inorganic perovskite nanowire CsPbX of claim 12The preparation method of Y is characterized in that the substrate in S2 is a silicon wafer, a quartz wafer or ITO.
8. All-inorganic perovskite nanowire CsPbX2Y, which is obtained by the production method according to any one of claims 1 to 7.
9. According toThe all-inorganic perovskite nanowire CsPbX of claim 82Y, characterized in that the all-inorganic perovskite nanowire CsPbX2The length of Y is 1.5 to 12 μm.
10. The fully inorganic perovskite nanowire CsPbX of claim 8 or 92The use of Y in a photodetector or a laser.
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CN111139518A (en) * 2019-12-23 2020-05-12 大连理工大学 Preparation method of air-stable all-inorganic mixed halogen perovskite nanowire
CN113186600A (en) * 2021-04-27 2021-07-30 上海大学 All-photon password primitive preparation method based on high-flux perovskite micro-single crystal array
CN113594396B (en) * 2021-07-08 2022-08-05 浙江大学 Solvent atmosphere controlled perovskite in-situ film forming method and product and application thereof
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