CN110592668A - Liquid phase synthesis method of hexagonal lead iodide micro-nano single crystal plate - Google Patents

Liquid phase synthesis method of hexagonal lead iodide micro-nano single crystal plate Download PDF

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CN110592668A
CN110592668A CN201910967468.0A CN201910967468A CN110592668A CN 110592668 A CN110592668 A CN 110592668A CN 201910967468 A CN201910967468 A CN 201910967468A CN 110592668 A CN110592668 A CN 110592668A
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single crystal
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hexagonal
crystal plate
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马德伟
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Zhejiang University of Technology ZJUT
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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
    • C30B19/00—Liquid-phase epitaxial-layer growth
    • C30B19/12—Liquid-phase epitaxial-layer growth characterised by the substrate
    • 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
    • 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
    • C30B29/64—Flat crystals, e.g. plates, strips or discs

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Materials Engineering (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Crystals, And After-Treatments Of Crystals (AREA)

Abstract

Hexagonal PbI2The liquid phase synthesis method of the micro-nano single crystal plate comprises the following steps: dissolving a Pb source in water, coating the obtained Pb source solution on a substrate, and drying to obtain a Pb source pre-deposited film; dissolving a source I in isopropanol to obtain a source I solution; immersing the Pb source pre-deposited film in the I source solution for 10-48 h, and taking out to generate hexagonal PbI on the substrate2Micro-nano single crystal plate; the preparation process can be carried out in the air at room temperature, the reaction condition is mild, the preparation process is simple, the operation is convenient, and the cost is low, so the invention provides the synthetic hexagonal PbI2An efficient method of micro-nano single crystal plate.

Description

Liquid phase synthesis method of hexagonal lead iodide micro-nano single crystal plate
Technical Field
The invention relates to the field of nano material preparation, in particular to hexagonal lead iodide (PbI) for a micro-nano laser and a photoelectric detector2) A liquid phase synthesis method of a micro-nano single crystal plate.
Background
The discovery of the graphene in 2004 opens a magical gate of two-dimensional material research for global researchers. Over the past 10 years, there has been a great deal of interest in unique crystal and electronic structures based on two-dimensional materials, excellent physical properties, and important applications in various electronic and photonic devices. PbI2Has a two-dimensional layered hexagonal structure, Pb in the layer is covalently bonded to I, and each Pb atom is bonded to 6Coordination of I atoms, each I atom being bonded to 3 Pb atoms, the layers being connected by weak van der Waals forces; the space group is P-3m1, unit cell parameterα＝β＝90°、γ＝120°。PbI2The bulk material has a direct band gap (2.4 eV), the single layer material has an indirect band gap of 2.64eV due to quantum confinement effect, and the material has excellent light absorption performance and high electron (4600 cm)2V-1s-1) Hole mobility (-3000 cm)2V-1s-1) So that the material has important application value in the aspects of solar cells, laser and luminescent materials, photoelectric detectors, X-ray and gamma-ray detection, nonlinear optics and the like.
According to the literature, PbI is reported2The synthesis method of the two-dimensional layered nanosheet mainly comprises a mechanical cleavage method, a Physical Vapor Deposition (PVD) method, a liquid phase growth method and the like. Compared with the traditional mechanical cleavage method and PVD method, the liquid phase growth method does not need vacuum, high temperature and complex equipment, is easy to operate and is suitable for various substrates, so the liquid phase method is an important nano material synthesis method.
Disclosure of Invention
The invention aims to provide a shape-controllable hexagonal PbI2A liquid phase synthesis method of a micro-nano single crystal plate.
The technical scheme of the invention is as follows:
hexagonal PbI2The liquid phase synthesis method of the micro-nano single crystal plate comprises the following steps:
(1) dissolving a Pb source in water, coating the obtained Pb source solution on a substrate, and drying (at 50 ℃) to obtain a Pb source pre-deposited film;
the Pb source is, for example: PbAc2Or Pb (NO)3)2；
The substrate is, for example: glass, silicon wafers, and the like;
the coating may be performed, for example, by a drop coating method;
the concentration of the Pb source solution is 50-150 mg/mL;
(2) dissolving a source I in isopropanol to obtain a source I solution;
the source of I is R-NH3I, wherein R ═ C3 to C6 chain hydrocarbons or C6 to C10 aromatic alkanes; specifically, the I source is, for example: c3H7NH3I、C6H13NH3I、C6H5CH2NH3I or C6H5C2H4NH3I；
The concentration of the source I solution is 2.5-7.5 mg/mL;
(3) immersing the Pb source pre-deposited film in the I source solution for 10-48 h, and taking out to generate hexagonal PbI on the substrate2A micro-nano single crystal plate.
The hexagonal PbI prepared by the invention2The micro-nano single crystal plate has controllable appearance, 2-10 mu m size and 20-100 nm thickness.
Compared with the prior art, the beneficial effects of this application lie in: the prior art mainly adopts a vapor phase method to grow hexagonal or triangular PbI2A micro-nano single crystal plate. Compared with the gas phase method, the liquid phase growth method does not need vacuum, high temperature and complex equipment, is easy to operate and is suitable for various substrates. In addition, a few reports employ liquid phase methods, but heating assistance is employed at the same time; and the precursor is Pb2+、I-The inorganic compound of (2) is different from the organic precursor of (I) used in the present invention. The preparation process can be carried out in the air at room temperature, and the reaction condition is mild. And the preparation process is simple, the operation is convenient, and the cost is low. Accordingly, the present invention provides a synthetic hexagonal PbI2An efficient method of micro-nano single crystal plate.
Drawings
FIG. 1 is the hexagonal PbI synthesized in example 12SEM picture of micro-nano single crystal plate;
FIG. 2 is the hexagonal PbI synthesized in example 22SEM picture of micro-nano single crystal plate;
FIG. 3 is the hexagonal PbI synthesized in example 32SEM picture of micro-nano single crystal plate;
FIG. 4 is the hexagonal PbI synthesized in example 42SEM picture of micro-nano single crystal plate;
FIG. 5 is the hexagonal PbI synthesized in example 52SEM picture of micro-nano single crystal plate;
FIG. 6 is the hexagonal PbI synthesized in example 62SEM picture of micro-nano single crystal plate;
FIG. 7 is the hexagonal PbI synthesized in example 72SEM image of micro-nano single crystal plate.
Detailed Description
The invention will be further described with reference to specific examples, but the scope of the invention is not limited thereto.
Example 1:
PbAc2preparing a pre-deposited film: weighing 100mg of PbAc2The powder was placed in a vial containing 1ml of water and dissolved thoroughly. Placing the glass sheet in alcohol, ultrasonic cleaning for 15min, taking out, and treating with N2And (5) drying. Dropping PbAc21-2 drops (about 0.05-0.1 mL) of the precursor solution are put on a glass substrate (area 25mm x 75mm), uniformly coated as much as possible and dried at 50 ℃ to obtain PbAc2And (5) pre-depositing a film.
C3H7NH3I, precursor solution preparation: weighing 5mg of C3H7NH3Placing the powder in a small bottle containing 1ml isopropanol, and dissolving with ultrasonic vibration to obtain brown clear C3H7NH3I precursor solution.
Hexagonal PbI2Preparing a micro-nano single crystal plate: pre-depositing PbAc2Glass sheets of film were cut to 1mm2Left and right small glass sheets immersed in C3H7NH3I precursor solution, and keeping the coating facing the bottom of the vial. After 10 hours, the glass sheet was taken out. Washing the glass sheet with an isopropanol solution to remove incompletely reacted precursor solution, and applying N2Blow-drying to obtain hexagonal PbI2Micro-nano single crystal plate (figure 1).
Example 2:
PbAc2preparing a pre-deposited film: weighing 100mg of PbAc2The powder was placed in a vial containing 1ml of water and dissolved thoroughly. Placing the glass sheet in alcoholCleaning with sound for 15min, taking out, and treating with N2And (5) drying. Dropping PbAc21-2 drops (about 0.05-0.1 mL) of the precursor solution are put on a glass substrate (area 25mm x 75mm), uniformly coated as much as possible and dried at 50 ℃ to obtain PbAc2And (5) pre-depositing a film.
C3H7NH3I, precursor solution preparation: weighing 2.5mg of C3H7NH3Placing the powder in a small bottle containing 1ml isopropanol, and dissolving with ultrasonic vibration to obtain brown clear C3H7NH3I precursor solution.
Hexagonal PbI2Preparing a micro-nano single crystal plate: pre-depositing PbAc2Glass sheets of film were cut to 1mm2Left and right small glass sheets immersed in C3H7NH3I precursor solution, and keeping the coating facing the bottom of the vial. After 10 hours, the glass sheet was taken out. Washing the glass sheet with an isopropanol solution to remove incompletely reacted precursor solution, and applying N2Blow-drying to obtain hexagonal PbI2Micro-nano single crystal plate (figure 2).
Example 3:
PbAc2preparing a pre-deposited film: weighing 100mg of PbAc2The powder was placed in a vial containing 1ml of water and dissolved thoroughly. Placing the glass sheet in alcohol, ultrasonic cleaning for 15min, taking out, and treating with N2And (5) drying. Dropping PbAc21-2 drops (about 0.05-0.1 mL) of the precursor solution are put on a glass substrate (area 25mm x 75mm), uniformly coated as much as possible and dried at 50 ℃ to obtain PbAc2And (5) pre-depositing a film.
C3H7NH3I, precursor solution preparation: weighing 7.5mg of C3H7NH3Placing the powder in a small bottle containing 1ml isopropanol, and dissolving with ultrasonic vibration to obtain brown clear C3H7NH3I precursor solution.
Hexagonal PbI2Preparing a micro-nano single crystal plate: pre-depositing PbAc2Glass sheets of film were cut to 1mm2Left and right small glass sheets immersed in C3H7NH3Small drug of precursor solutionIn the bottle, and the coating is kept facing the bottom of the bottle. After 10 hours, the glass sheet was taken out. Washing the glass sheet with an isopropanol solution to remove incompletely reacted precursor solution, and applying N2Blow-drying to obtain hexagonal PbI2Micro nano single crystal plate (figure 3).
Example 4:
PbAc2preparing a pre-deposited film: weighing 100mg of PbAc2The powder was placed in a vial containing 1ml of water and dissolved thoroughly. Placing the glass sheet in alcohol, ultrasonic cleaning for 15min, taking out, and treating with N2And (5) drying. Dropping PbAc21-2 drops (about 0.05-0.1 mL) of the precursor solution are put on a glass substrate (area 25mm x 75mm), uniformly coated as much as possible and dried at 50 ℃ to obtain PbAc2And (5) pre-depositing a film.
C6H13NH3I, precursor solution preparation: weighing 5mg of C6H13NH3Placing the powder in a small bottle containing 1ml isopropanol, and dissolving with ultrasonic vibration to obtain brown clear C6H13NH3I precursor solution.
Hexagonal PbI2Preparing a micro-nano single crystal plate: pre-depositing PbAc2Glass sheets of film were cut to 1mm2Left and right small glass sheets immersed in C6H13NH3I precursor solution, and keeping the coating facing the bottom of the vial. After 10 hours, the glass sheet was taken out. Washing the glass sheet with an isopropanol solution to remove incompletely reacted precursor solution, and applying N2Blow-drying to obtain hexagonal PbI2Micro nano single crystal plate (figure 4).
Example 5:
PbAc2preparing a pre-deposited film: weighing 100mg of PbAc2The powder was placed in a vial containing 1ml of water and dissolved thoroughly. Placing the glass sheet in alcohol, ultrasonic cleaning for 15min, taking out, and treating with N2And (5) drying. Dropping PbAc21-2 drops (about 0.05-0.1 mL) of the precursor solution are put on a glass substrate (area 25mm x 75mm), uniformly coated as much as possible and dried at 50 ℃ to obtain PbAc2And (5) pre-depositing a film.
C6H5CH2NH3I, precursor solution preparation: weighing 5mg of C6H5CH2NH3Placing the powder in a small bottle containing 1ml isopropanol, and dissolving with ultrasonic vibration to obtain brown clear C6H5CH2NH3I precursor solution.
Hexagonal PbI2Preparing a micro-nano single crystal plate: pre-depositing PbAc2Glass sheets of film were cut to 1mm2Left and right small glass sheets immersed in C6H5CH2NH3I precursor solution, and keeping the coating facing the bottom of the vial. After 48 hours, the glass sheet was taken out. Washing the glass sheet with an isopropanol solution to remove incompletely reacted precursor solution, and applying N2Blow-drying to obtain hexagonal PbI2Micro nano single crystal plate (figure 5).
Example 6:
PbAc2preparing a pre-deposited film: weighing 100mg of PbAc2The powder was placed in a vial containing 1ml of water and dissolved thoroughly. Placing the glass sheet in alcohol, ultrasonic cleaning for 15min, taking out, and treating with N2And (5) drying. Dropping PbAc21-2 drops (about 0.05-0.1 mL) of the precursor solution are put on a glass substrate (area 25mm x 75mm), uniformly coated as much as possible and dried at 50 ℃ to obtain PbAc2And (5) pre-depositing a film.
C6H5C2H4NH3I, precursor solution preparation: weighing 2.5mg of C6H5C2H4NH3Placing the powder in a small bottle containing 1ml isopropanol, and dissolving with ultrasonic vibration to obtain brown clear C6H5C2H4NH3I precursor solution.
Hexagonal PbI2Preparing a micro-nano single crystal plate: pre-depositing PbAc2Glass sheets of film were cut to 1mm2Left and right small glass sheets immersed in C6H5C2H4NH3I precursor solution, and keeping the coating facing the bottom of the vial. After 10 hours, the glass sheet was taken out. Washing the glass sheet with an isopropanol solution to remove incompletely reacted precursor solutionLiquid, in combination with N2Blow-drying to obtain hexagonal PbI2Micro nano single crystal plate (figure 6).
Example 7:
PbAc2preparing a pre-deposited film: weighing 100mg of PbAc2The powder was placed in a vial containing 1ml of water and dissolved thoroughly. Placing the glass sheet in alcohol, ultrasonic cleaning for 15min, taking out, and treating with N2And (5) drying. Dropping PbAc21-2 drops (about 0.05-0.1 mL) of the precursor solution are put on a glass substrate (area 25mm x 75mm), uniformly coated as much as possible and dried at 50 ℃ to obtain PbAc2And (5) pre-depositing a film.
C6H5C2H4NH3I, precursor solution preparation: weighing 5mg of C6H5C2H4NH3Placing the powder in a small bottle containing 1ml isopropanol, and dissolving with ultrasonic vibration to obtain brown clear C6H5C2H4NH3I precursor solution.
Hexagonal PbI2Preparing a micro-nano single crystal plate: pre-depositing PbAc2Glass sheets of film were cut to 1mm2Left and right small glass sheets immersed in C6H5C2H4NH3I precursor solution, and keeping the coating facing the bottom of the vial. After 22 hours, the glass sheet was removed. Washing the glass sheet with an isopropanol solution to remove incompletely reacted precursor solution, and applying N2Blow-drying to obtain hexagonal PbI2Micro nano single crystal plate (fig. 7).
While the preferred embodiments of the present invention have been illustrated and described, it will be apparent to those skilled in the art that various changes and modifications may be made therein without departing from the spirit and scope of the invention, and it is intended to cover all such modifications and variations as fall within the scope of the appended claims.

Claims (5)

1. Hexagonal PbI2The liquid phase synthesis method of the micro-nano single crystal plate is characterized by comprising the following steps:
(1) dissolving a Pb source in water, coating the obtained Pb source solution on a substrate, and drying to obtain a Pb source pre-deposited film;
the concentration of the Pb source solution is 50-150 mg/mL;
(2) dissolving a source I in isopropanol to obtain a source I solution;
the source of I is R-NH3I, wherein R ═ C3 to C6 chain hydrocarbons or C6 to C10 aromatic alkanes;
the concentration of the source I solution is 2.5-7.5 mg/mL;
(3) immersing the Pb source pre-deposited film in the I source solution for 10-48 h, and taking out to generate hexagonal PbI on the substrate2A micro-nano single crystal plate.
2. The hexagonal PbI of claim 12The liquid phase synthesis method of the micro-nano single crystal plate is characterized in that in the step (1), the Pb source is PbAc2Or Pb (NO)3)2。
3. The hexagonal PbI of claim 12The liquid phase synthesis method of the micro-nano single crystal plate is characterized in that in the step (1), the substrate is glass or a silicon wafer.
4. The hexagonal PbI of claim 12The liquid phase synthesis method of the micro-nano single crystal plate is characterized in that in the step (1), a dripping method is adopted for coating.
5. The hexagonal PbI of claim 12The liquid phase synthesis method of the micro-nano single crystal plate is characterized in that in the step (2), the source I is C3H7NH3I、C6H13NH3I、C6H5CH2NH3I or C6H5C2H4NH3I。
CN201910967468.0A 2019-10-12 2019-10-12 Liquid phase synthesis method of hexagonal lead iodide micro-nano single crystal plate Pending CN110592668A (en)

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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104851987A (en) * 2015-04-09 2015-08-19 中国科学院广州能源研究所 Perovskite structure organic-inorganic ternary alloy heterocomplex film photoanode with adjustable absorption spectrum and preparation method thereof
CN106757372A (en) * 2016-11-25 2017-05-31 太原理工大学 A kind of methylamine lead iodine perovskite monocrystalline microcavity and preparation method thereof
CN106796988A (en) * 2014-08-08 2017-05-31 牛津大学科技创新有限公司 The method of organic perovskite material layer that manufacture crystallinity improves

Patent Citations (3)

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Publication number Priority date Publication date Assignee Title
CN106796988A (en) * 2014-08-08 2017-05-31 牛津大学科技创新有限公司 The method of organic perovskite material layer that manufacture crystallinity improves
CN104851987A (en) * 2015-04-09 2015-08-19 中国科学院广州能源研究所 Perovskite structure organic-inorganic ternary alloy heterocomplex film photoanode with adjustable absorption spectrum and preparation method thereof
CN106757372A (en) * 2016-11-25 2017-05-31 太原理工大学 A kind of methylamine lead iodine perovskite monocrystalline microcavity and preparation method thereof

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Application publication date: 20191220