CN114132954B - Preparation method of chain-shaped interlocking nanocrystalline super-structure material - Google Patents
Preparation method of chain-shaped interlocking nanocrystalline super-structure material Download PDFInfo
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- CN114132954B CN114132954B CN202111384286.4A CN202111384286A CN114132954B CN 114132954 B CN114132954 B CN 114132954B CN 202111384286 A CN202111384286 A CN 202111384286A CN 114132954 B CN114132954 B CN 114132954B
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- C01F17/00—Compounds of rare earth metals
- C01F17/10—Preparation or treatment, e.g. separation or purification
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- 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
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01F—COMPOUNDS OF THE METALS BERYLLIUM, MAGNESIUM, ALUMINIUM, CALCIUM, STRONTIUM, BARIUM, RADIUM, THORIUM, OR OF THE RARE-EARTH METALS
- 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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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
- C01P2004/16—Nanowires or nanorods, i.e. solid nanofibres with two nearly equal dimensions between 1-100 nanometer
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/80—Particles consisting of a mixture of two or more inorganic phases
- C01P2004/82—Particles consisting of a mixture of two or more inorganic phases two phases having the same anion, e.g. both oxidic phases
Abstract
The invention provides a preparation method of a chain-shaped interlocking nanocrystalline super-structure material, which comprises the following steps: soaking the double-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-shaped nanocrystalline n-hexane solution, immersing the film in the solution, packaging the glass container, and heating to volatilize n-hexane; and (3) carrying out high-temperature treatment on the obtained film, and etching the aluminum oxide by using a sodium hydroxide solution to obtain the chain-shaped interlocking nanocrystalline super-structure material. The invention overcomes the defects that the nanocrystals in the material obtained by the prior assembly technology tend to be the closest-packed, have single structure and can not ensure the long-range order of crystal orientation, develops a chain-shaped interlocking structure obtained by finite field assembly based on anisotropic nanocrystals, and expands the diversity of the super structure and the adjustability of the optical performance.
Description
Technical Field
The invention belongs to the fields of materials and inorganic chemistry, and particularly relates to a preparation method of a chain-shaped interlocking nanocrystalline super-structure material.
Background
The nanocrystalline self-assembly technology utilizes van der Waals force, electrostatic acting force, magnetic interaction force and the like among nanocrystalline to form an ordered structure, and is an effective means for constructing a complex functional metamaterial from bottom to top. When the nanocrystals are self-assembled into an ordered array, the coupling effect between the nanocrystals can drive the nanocrystals to generate new overall integration performance, and the performance is closely related to the symmetry, coordination, inter-particle distance, order and macroscopic orientation of the super structure, so that the method has wide application prospect in the fields of film electronics, photoelectrons, energy storage, conversion and the like. The shape and the arrangement orientation of the nanocrystals are critical to optimizing the material performance, and the anisotropic construction element is assembled to prepare the super structure with adjustable orientation, symmetry and periodicity, so that the research on the unique characteristic depending on the shape and the orientation is significant. Although some liquid crystal phase superstructures assembled from rod-shaped rare earth nanocrystals have been developed to achieve modulation of their optical properties, the diversity of superstructures and adjustability of optical properties are greatly limited due to the simpler shape of rod-shaped nanocrystals.
The nanocrystalline 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, a gas-liquid phase interface self-assembly method and the like. The above assembling method can obtain ordered super-structure materials, but under entropy driving, nanocrystals tend to be in the closest packing 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 limit, the nanocrystalline can rearrange according to the principle of lowest energy, so that a novel super structure is hopefully obtained and is used as a brand new performance research object. Therefore, it is necessary 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 nanocrystalline super-structure material.
The invention provides a preparation method of a chain-shaped interlocking nanocrystalline super-structure material, which specifically comprises the following steps:
(1) Soaking the double-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-shaped nanocrystalline n-hexane solution, immersing the film in the solution, packaging the glass container, and heating to volatilize n-hexane;
(3) Carrying out high-temperature treatment on the film obtained in the step (2), and etching aluminum oxide by using a sodium hydroxide solution to obtain a chain-shaped interlocking nanocrystalline super-structure material;
wherein the dumbbell-shaped nanocrystalline component in the step (2) is NaYF 4 ：Yb/Er@NaGdF 4 @NaNdF 4 。
In the invention, in the step (1), the center-to-center distance of the holes of the double-pass anodic aluminum oxide film is 65-200 nm, the aperture is 50-70 nm, and the film thickness is 40-60 mu m.
In the present invention, the concentration of the ethanol solution of n-tetradecylphosphonic acid in step (1) was 0.05 mol/L.
In the invention, the concentration of the dumbbell type nanocrystalline in the step (2) is 30 mg/mL.
In the invention, the specific condition of heating in the step (2) is heating for 4-8 hours at 60-80 ℃ in an air atmosphere.
In the invention, the high temperature treatment condition in the step (3) is N 2 Treating at 350-450 deg.C for 2-4 hr under atmosphere.
In the present invention, the concentration of the 1 mol/L sodium hydroxide solution in the step (3) is 1 mol/L.
The invention modifies n-tetradecylphosphonic acid on the surface of a bi-pass anodized aluminum film, immerses the film in normal hexane solution of dumbbell-shaped nanocrystalline, heats and volatilizes the solvent, the nanocrystalline completes assembly in pore channels of the bi-pass anodized aluminum film, then carries out high-temperature treatment on the film, and etches aluminum oxide by sodium hydroxide solution to obtain the ordered interlocking structure.
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 the closest-packed, have single structure and can not ensure the long-range order of crystal orientation, develops a chain-shaped interlocking structure obtained by finite field assembly based on anisotropic nanocrystals, and expands the diversity of the super structure and the adjustability of the optical performance.
Drawings
FIG. 1 is an infrared spectrum of a front-to-back bi-pass anodized aluminum film modified with n-tetradecylphosphonic acid of 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) Immersing a double-pass anodic aluminum oxide film (aperture center distance 65 nm, aperture 50 nm, film thickness 40 μm) with an area of 1cm×1cm in 5 mL of 0.05 mol/L ethanol solution of n-tetradecylphosphonic acid, standing for 24 hours, and drying;
(2) To the n-tetradecylphosphonic acid modified thin obtained in step (1)The membrane was placed in a glass bottle, and 2 mL of 30 mg/mL dumbbell-shaped nanocrystals (NaYF as a component) were slowly added 4 ：Yb/Er@NaGdF 4 @NaNdF 4 In YCl 3 、YbCl 3 、ErCl 3 、GdCl 3 、NdCl 3 As a precursor, oleic acid as a ligand and 1-octadecene as a solvent, and is prepared 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 the n-hexane;
(3) The film obtained in the step (2) is coated on N 2 And (3) under the atmosphere, after the treatment for 2 hours at 350 ℃, etching the film for 6 hours by using 1 mol/L sodium hydroxide solution to obtain the chain-shaped interlocking nanocrystalline super-structure material.
FIG. 1 is an infrared spectrum of a double pass anodized aluminum film before and after modification of n-tetradecylphosphonic acid in example 1, demonstrating that n-tetradecylphosphonic acid was successfully modified on the surface of the double pass anodized aluminum film.
Fig. 2 is a scanning electron microscope image of the chain-shaped interlocking type nanocrystalline super structure material prepared in example 1, which proves that the method can realize batch preparation of high-quality ordered interlocking structures.
Example 2
(1) Immersing a double-pass anodic aluminum oxide film (aperture center distance 200 nm, aperture 70 nm, film thickness 60 μm) with an area of 1cm×1cm in 5 mL of 0.05 mol/L ethanol solution of n-tetradecylphosphonic acid, standing for 20 hours, and drying;
(2) Placing the film modified by the n-tetradecylphosphonic acid obtained in the step (1) into a glass bottle, slowly adding 2 mL of dumbbell-shaped nanocrystalline (with the component of NaYF) of 30 mg/mL 4 ：Yb/Er@NaGdF 4 @NaNdF 4 In YCl 3 、YbCl 3 、ErCl 3 、GdCl 3 、NdCl 3 As a precursor, oleic acid as a ligand and 1-octadecene as a solvent, and is prepared 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 the n-hexane;
(3) The film obtained in the step (2) is coated on N 2 450 ℃ under the atmosphereAfter 4 hours of treatment, etching the film for 6 hours by using 1 mol/L sodium hydroxide solution, thus obtaining the chain-shaped interlocking nanocrystalline super-structure material.
Claims (7)
1. The preparation method of the chain-shaped interlocking nanocrystalline super-structure material is characterized by comprising the following steps of:
(1) Soaking the double-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-shaped nanocrystalline n-hexane solution, immersing the film in the solution, packaging the glass container, and heating to volatilize n-hexane;
(3) Carrying out high-temperature treatment on the film obtained in the step (2), and etching aluminum oxide by using a sodium hydroxide solution to obtain a chain-shaped interlocking nanocrystalline super-structure material;
wherein the dumbbell-shaped nanocrystalline component in the step (2) is NaYF 4 ：Yb/Er@NaGdF 4 @NaNdF 4 。
2. The method according to claim 1, wherein the center-to-center spacing of the holes of the double-pass anodized aluminum film in the step (1) is 65-200 nm, the pore 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 dumbbell nanocrystals in step (2) is 30 mg/mL.
5. The method according to claim 1, wherein the specific condition of heating in the step (2) is heating at 60-80 ℃ for 4-8 hours under an air atmosphere.
6. The method according to claim 1, characterized in that the steps of3) The medium-high temperature treatment condition is N 2 Treating at 350-450 deg.C for 2-4 hr under atmosphere.
7. The process according to claim 1, wherein the concentration of sodium hydroxide solution in step (3) is 1 mol/L.
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| 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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| EP1534631A1 (en) * | 2002-09-07 | 2005-06-01 | Schott Glas | Method for the production of highly organized crystals by means of sol-gel methods |
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| 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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