CN114132954A - Preparation method of chain-shaped interlocking type nanocrystalline superstructure material - Google Patents

Preparation method of chain-shaped interlocking type nanocrystalline superstructure material Download PDF

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CN114132954A
CN114132954A CN202111384286.4A CN202111384286A CN114132954A CN 114132954 A CN114132954 A CN 114132954A CN 202111384286 A CN202111384286 A CN 202111384286A CN 114132954 A CN114132954 A CN 114132954A
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chain
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superstructure
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CN114132954B (en
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董安钢
万思妤
杨东
宁静
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Fudan University
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    • C01F17/00—Compounds of rare earth metals
    • C01F17/30—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6
    • C01F17/36—Compounds containing rare earth metals and at least one element other than a rare earth metal, oxygen or hydrogen, e.g. La4S3Br6 halogen being the only anion, e.g. NaYF4
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Abstract

The invention provides a preparation method of a chain interlocking type nanocrystalline superstructure material, which comprises the following steps: soaking the bi-pass anodic aluminum oxide film in an ethanol solution of n-tetradecylphosphonic acid, standing for 20-24 hours, and drying; placing the obtained film in a glass container, adding a dumbbell type nanocrystalline n-hexane solution, sealing the glass container after the solution submerges the film, and heating to volatilize n-hexane; and (3) after the obtained film is subjected to high-temperature treatment, etching the aluminum oxide by using a sodium hydroxide solution to obtain the chain-like interlocking type nanocrystalline superstructure material. The invention overcomes the defects that the nanocrystals in the material obtained by the prior assembly technology tend to be densely packed, have single structure and cannot ensure long-range order of crystal orientation, develops the chain-shaped interlocking structure obtained by carrying out domain-limited assembly based on the anisotropic nanocrystals, and expands the diversity of the superstructure and the adjustability of optical performance.

Description

Preparation method of chain-shaped interlocking type nanocrystalline superstructure material
Technical Field
The invention belongs to the field of materials and inorganic chemistry, and particularly relates to a preparation method of a chain-shaped interlocking type nanocrystalline superstructure material.
Background
The nanocrystalline self-assembly technology utilizes Van der Waals force, electrostatic acting force, magnetic interaction acting force and the like among nanocrystals to form an ordered structure, and is an effective means for constructing a metamaterial with complex functions from bottom to top. When the nanocrystals are self-assembled into an ordered array, the coupling effect between the nanocrystals drives the nanocrystals to generate new overall integration performance, the performance is closely related to the symmetry, coordination, particle spacing, ordering and macroscopic orientation of a superstructure, and the nanocrystal has wide application prospect in the fields of thin film electronics, photoelectrons, energy storage and conversion and the like. The shape and the arrangement orientation of the nanocrystalline are crucial to optimizing the material performance, anisotropic construction elements are assembled to prepare a superstructure with adjustable orientation, symmetry and periodicity, so that the unique characteristic depending on the shape and the orientation is researched, and the method has important significance. Although some liquid crystal phase superstructures assembled from rod-shaped rare earth nanocrystals have been developed to achieve modulation of their optical properties, the versatility of superstructures and the tunability of optical properties are greatly limited due to the simpler shape of the rod-shaped nanocrystals.
The nano-crystal self-assembly technology developed in recent years mainly comprises a drop coating method, a blade coating method, a mixed benign and poor solvent method, a Langmuir-Blodgett method and a gas-liquid phase interface self-assembly method and the like. The above assembly method can obtain ordered superstructure materials, but under the drive of entropy, nanocrystals tend to the closest-packed assembly behavior, and the generation of new structures is limited, so that the structure-activity relationship of the materials cannot be deeply explored. Under the condition of extreme confinement, the nanocrystals can be rearranged according to the principle of energy minimization, so that a novel superstructure can be hopefully obtained and can be used as a brand-new performance research object. Therefore, there is a need to develop ordered structures based on domain-limited assembly of anisotropic nanocrystals.
Disclosure of Invention
The invention aims to provide a preparation method of a chain-shaped interlocking type nanocrystalline superstructure material.
The invention provides a preparation method of a chain-shaped interlocking type nanocrystalline superstructure material, which specifically comprises the following steps:
(1) soaking the bi-pass anodic aluminum oxide film in an ethanol solution of n-tetradecylphosphonic acid, standing for 20-24 hours, and drying;
(2) placing the film obtained in the step (1) in a glass container, adding a dumbbell type nanocrystalline n-hexane solution, sealing the glass container after the film is immersed in the solution, and heating to volatilize n-hexane;
(3) after the film obtained in the step (2) is subjected to high-temperature treatment, aluminum oxide is etched by using a sodium hydroxide solution to obtain a chain-like interlocking type nanocrystalline superstructure material;
wherein the dumbbell-shaped nanocrystalline component in the step (2) is NaYF4：Yb/Er@NaGdF4@NaNdF4。
In the invention, the hole center spacing of the two-way anodic alumina film in the step (1) is 65-200 nm, the hole diameter is 50-70 nm, and the film thickness is 40-60 μm.
In the present invention, the concentration of the ethanol solution of n-tetradecylphosphonic acid in step (1) is 0.05 mol/L.
In the invention, the concentration of the dumbbell-type nanocrystal in the step (2) is 30 mg/mL.
In the invention, the specific heating condition in the step (2) is heating for 4-8 hours at 60-80 ℃ in an air atmosphere.
In the present invention, the high-temperature treatment condition in the step (3) is N2Treating at 350-450 ℃ for 2-4 hours in an atmosphere.
In the present invention, the concentration of the 1 mol/L sodium hydroxide solution in the step (3) is 1 mol/L.
According to the invention, n-tetradecylphosphonic acid is modified on the surface of a bi-pass anodic aluminum oxide film, and is immersed in a normal hexane solution of dumbbell type nanocrystals, the solvent is heated and volatilized, the nanocrystals are assembled in a pore channel of the bi-pass anodic aluminum oxide film, then the film is subjected to high temperature treatment, and the aluminum oxide is etched by a sodium hydroxide solution, so that the ordered interlocking structure is obtained.
The invention has the beneficial effects that: the invention overcomes the defects that the nanocrystals in the material obtained by the prior assembly technology tend to be densely packed, have single structure and cannot ensure long-range order of crystal orientation, develops the chain-shaped interlocking structure obtained by carrying out domain-limited assembly based on the anisotropic nanocrystals, and expands the diversity of the superstructure and the adjustability of optical performance.
Drawings
FIG. 1 is an infrared spectrum of front and rear two-pass anodized aluminum films modified with n-tetradecylphosphonic acid in example 1;
fig. 2 is a scanning electron microscope image of the chain-like interlocking type nanocrystalline superstructure material prepared in example 1.
Detailed Description
Example 1
(1) Soaking a bi-pass anodic alumina film (with the hole center spacing of 65 nm, the hole diameter of 50 nm and the film thickness of 40 mu m) with the area of 1cm multiplied by 1cm in 5 mL of 0.05 mol/L ethanol solution of n-tetradecylphosphonic acid, standing for 24 hours and then drying;
(2) placing the n-tetradecylphosphonic acid modified film obtained in the step (1) into a glass bottle, and slowly adding 2 mL of 30 mg/mL dumbbell type nanocrystal (with the component of NaYF)4：Yb/Er@NaGdF4@NaNdF4By YCl3、YbCl3、ErCl3、GdCl3、NdCl3Is a precursor, oleic acid is a ligand, 1-octadecene is a solvent, and the preparation method comprises the steps of preparing) n-hexane solution by a thermal decomposition method, immersing a film in the solution, packaging a glass bottle, and heating at 60 ℃ for 8 hours in an air atmosphere to slowly volatilize n-hexane;
(3) the film obtained in the step (2) is placed in N2And (3) processing for 2 hours at 350 ℃ in the atmosphere, and etching the film for 6 hours by using 1 mol/L sodium hydroxide solution to obtain the chain interlocking type nanocrystalline superstructure material.
FIG. 1 is an infrared spectrum of two-pass anodized aluminum films before and after n-tetradecylphosphonic acid modification in example 1, which demonstrates that n-tetradecylphosphonic acid is successfully modified on the surface of the two-pass anodized aluminum film.
Fig. 2 is a scanning electron microscope image of the chain-like interlocking type nanocrystalline superstructure material prepared in example 1, which proves that the method can realize batch preparation of high-quality ordered interlocking structures.
Example 2
(1) Soaking a bi-pass anodic alumina film (with the hole center spacing of 200 nm, the hole diameter of 70 nm and the film thickness of 60 mu m) with the area of 1cm multiplied by 1cm in 5 mL of 0.05 mol/L ethanol solution of n-tetradecylphosphonic acid, standing for 20 hours and then drying;
(2) placing the n-tetradecylphosphonic acid modified film obtained in the step (1) into a glass bottle, and slowly adding 2 mL of 30 mg/mL dumbbell type nanocrystal (with the component of NaYF)4：Yb/Er@NaGdF4@NaNdF4By YCl3、YbCl3、ErCl3、GdCl3、NdCl3Is a precursor, oleic acid is a ligand, 1-octadecene is a solvent, and the preparation method comprises the steps of preparing) n-hexane solution by a thermal decomposition method, immersing a film in the solution, packaging a glass bottle, and heating at 80 ℃ for 4 hours in an air atmosphere to slowly volatilize n-hexane;
(3) the film obtained in the step (2) is placed in N2And (3) processing for 4 hours at 450 ℃ in the atmosphere, and etching the film for 6 hours by using 1 mol/L sodium hydroxide solution to obtain the chain interlocking type nanocrystalline superstructure material.

Claims (7)

1. A preparation method of chain-shaped interlocking type nanocrystalline superstructure materials is characterized by comprising the following steps:
(1) soaking the bi-pass anodic aluminum oxide film in an ethanol solution of n-tetradecylphosphonic acid, standing for 20-24 hours, and drying;
(2) placing the film obtained in the step (1) in a glass container, adding a dumbbell type nanocrystalline n-hexane solution, sealing the glass container after the film is immersed in the solution, and heating to volatilize n-hexane;
(3) after the film obtained in the step (2) is subjected to high-temperature treatment, aluminum oxide is etched by using a sodium hydroxide solution to obtain a chain-like interlocking type nanocrystalline superstructure material;
wherein the dumbbell-shaped nanocrystalline component in the step (2) is NaYF4：Yb/Er@NaGdF4@NaNdF4。
2. The method according to claim 1, wherein in the step (1), the hole center spacing of the two-pass anodic aluminum oxide film is 65-200 nm, the hole diameter is 50-70 nm, and the film thickness is 40-60 μm.
3. The process according to claim 1, wherein the concentration of the ethanol solution of n-tetradecylphosphonic acid in step (1) is 0.05 mol/L.
4. The method according to claim 1, wherein the concentration of the dumbbell-shaped nanocrystals in step (2) is 30 mg/mL.
5. The method according to claim 1, wherein the specific conditions for heating in the step (2) are 60 to 80 ℃ for 4 to 8 hours under an air atmosphere.
6. The method according to claim 1, wherein the high-temperature treatment condition in the step (3) is N2Treating at 350-450 ℃ for 2-4 hours in an atmosphere.
7. The process according to claim 1, wherein the concentration of the 1 mol/L sodium hydroxide solution in the step (3) is 1 mol/L.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040163758A1 (en) * 2000-04-21 2004-08-26 International Business Machines Corporation Patterning solution deposited thin films with self-assembled monolayers
US20050238561A1 (en) * 2002-09-07 2005-10-27 Schott Glass Process for the production of highly organized crystals by means of Sol-Gel methods
CN102011190A (en) * 2010-12-22 2011-04-13 南京工业大学 Method for preparing nanostructure barium strontium titanate ferroelectric film by utilizing nanocrystalline self assembly process

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
US20040163758A1 (en) * 2000-04-21 2004-08-26 International Business Machines Corporation Patterning solution deposited thin films with self-assembled monolayers
US20050238561A1 (en) * 2002-09-07 2005-10-27 Schott Glass Process for the production of highly organized crystals by means of Sol-Gel methods
CN102011190A (en) * 2010-12-22 2011-04-13 南京工业大学 Method for preparing nanostructure barium strontium titanate ferroelectric film by utilizing nanocrystalline self assembly process

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