CN109306523B - Preparation of single crystal Fe2O3Method for self-assembling cubic nanostructure by nanoparticles - Google Patents

Preparation of single crystal Fe2O3Method for self-assembling cubic nanostructure by nanoparticles Download PDF

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CN109306523B
CN109306523B CN201811016174.1A CN201811016174A CN109306523B CN 109306523 B CN109306523 B CN 109306523B CN 201811016174 A CN201811016174 A CN 201811016174A CN 109306523 B CN109306523 B CN 109306523B
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distilled water
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stirring
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CN109306523A (en
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董伟霞
包启富
顾幸勇
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Jingdezhen Ceramic Institute
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    • 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
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    • 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
    • C30B7/00—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions
    • C30B7/10—Single-crystal growth from solutions using solvents which are liquid at normal temperature, e.g. aqueous solutions by application of pressure, e.g. hydrothermal processes

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Abstract

The invention discloses a method for preparing single crystal Fe2O3A method for self-assembling cubic nanostructures with nanoparticles, comprising the steps of: dissolving an iron compound in distilled water, dropwise adding a NaOH solution to obtain a brownish red suspension, stirring for 15min, putting the suspension into a hydrothermal kettle for reaction, washing hydrothermal reaction products for 3 times by using distilled water and ethanol respectively, and filtering to obtain a precursor; secondly, mixing the precursor with distilled water and an organic solvent, and stirring the mixture uniformly to obtain a solution A; finally, dropwise adding KOH into the solution A, stirring, placing the mixture into a hydrothermal kettle for reaction, washing hydrothermal reaction products for 3 times by using distilled water and ethanol respectively, filtering and drying to obtain single crystal Fe2O3The nano particles are self-assembled into a cubic nano structure. The method has high yield, strong controllability, easy large-scale production and excellent photocatalytic performance under visible light, thereby having wide market prospect.

Description

Preparation of single crystal Fe2O3Method for self-assembling cubic nanostructure by nanoparticles
Technical Field
The invention belongs to the field of novel inorganic materials, and particularly relates to a method for preparing single crystal Fe2O3A method for self-assembling cubic nanostructures by nanoparticles.
Background
Recently Fe2O3The nano material has the advantages of good conductivity, narrow band gap energy, low preparation cost, corrosion resistance, good biocompatibility, no toxicity, environmental friendliness and the like, and is widely used in the fields of chemical sensors, catalysts, lithium ion batteries, magnetic devices and biomedicine. Fe2O3The properties of the nano material are closely related to the microstructure, such as size, appearance, dimension and structure. The solvothermal method has the advantages of low cost, no pollution, controllable appearance, environmental friendliness and the like, and is one of the existing preparation methods for effectively controlling the microstructure of the nano material. Some Fe is reported in the related literature2O3And (4) preparing a cube. For example, the preparation of quasi-cubic ferric oxide nano material and the research of photocatalysis performance are carried out by dissolving ferric nitrate and PVP in N, N-dimethyl formamide solventTo obtainQuasi-cubic Fe2O3And (3) nano materials. ' alpha-Fe2O3Controllable synthesis and mechanism research by FeCl3·6H2O and CTAB are used as main raw materials, and a hydrothermal method is adoptedPreparing spherical and cubic alpha-Fe2O3And (3) granules. ' alpha-Fe2O3Morphology control synthesis and Performance Studies "hydrothermal method with Zn2+Preparation of zinc-doped alpha-Fe for structure directing agent2O3A microcube. ' alpha-Fe2O3Research on controlled synthesis, growth mechanism and hydrogen storage property of micro/nano material2O3Micro/nano material. ' alpha-Fe2O3Preparation of cubes by hydrothermal method the hydrothermal method is carried out at 130 ℃ and ferric trichloride and urotropine are used as basic raw materials to react to obtain the cubes-like bodies. Quasi-cubic alpha-Fe2O3Research on ultraviolet and infrared spectra of nano-film2O3And (3) a nano film. ' alpha-Fe2O3Preparation and performance research of the nano material' the quasi-cubic iron oxide nano material is prepared by using ferric chloride as an iron source, using cetyl trimethyl ammonium bromide as a surfactant and adopting a hydrothermal method. Although these documents report cubic Fe2O3The patent discloses a method for preparing cubic ferric oxide single crystals, namely a method for preparing cubic ferric oxide single crystals, by utilizing ferric trichloride hexahydrate and anhydrous sodium carbonate to hydrothermally synthesize cubic ferric oxide, the prepared cubic size is not uniform and is distributed at 100 ~ 500nm, which is very unfavorable for performance.
Disclosure of Invention
The invention aims to overcome the defects in the prior art and provide a novel environment-friendly plastic bag which is low in cost, simple and convenient in process,Preparation of single crystal Fe with easy control, short preparation period and suitability for mass production2O3A method for self-assembling cubic nanostructures by nanoparticles.
In order to solve the technical problems, the technical scheme of the invention is as follows: preparation of single crystal Fe2O3The method for self-assembling cubic nano-structure by nano-particles is characterized by comprising the following steps:
dissolving an iron compound in distilled water, dropwise adding a 3M NaOH solution to obtain a brownish red suspension, stirring for 15min, placing the suspension in a hydrothermal kettle, keeping the temperature at 80 ~ 100 ℃ for 1 ~ 5min, respectively washing hydrothermal reaction products for 3 times by using distilled water and ethanol, and filtering to obtain Fe2O3A nanoparticle precursor;
step two: mixing Fe2O3Mixing the nanoparticle precursor with distilled water and an organic solvent, and stirring the mixture uniformly to obtain a solution A;
step three, dropwise adding 12 ~ 21ml of 3 ~ 8M KOH into the solution A, stirring for 5 ~ 10min, placing the mixture into a hydrothermal kettle, preserving the heat at 120 ~ 200 ℃ for 10 ~ 60min, washing the hydrothermal reaction product for 3 times by using distilled water and ethanol, respectively, filtering, placing the product into a vacuum drying oven, and drying for 24h at 60 ℃ to obtain single crystal Fe2O3The nano particles are self-assembled into a cubic nano structure.
In the first step, the iron compound is ferric chloride hexahydrate or ferric nitrate nonahydrate.
And in the second step, the organic solvent is one of ethanol, n-octanol, propanol, butanol, ethylene glycol, propylene glycol and tetrahydrofuran.
Fe in the second step2O3The molar ratio of nanoparticle precursor to distilled water to organic solvent was 1 ~ 1.15.15: 100 ~ 200:10 ~ 25.
The invention adopts cheap raw material iron compound to prepare pure Fe by a secondary solvothermal method2O3The monocrystal nano particle self-assembled cubic nano structure has simple process route, and the prepared monocrystal Fe2O3The nano-particle self-assembled cube nano-structure has high yield, strong controllability and easy large scaleThe product is produced by a mold, and has excellent photocatalytic performance under visible light, so the product has wide market prospect.
Drawings
FIG. 1 is Fe2O3TEM electron micrograph of nanoparticle precursor structure;
FIG. 2 is Fe2O3An X-ray diffraction pattern of a nanoparticle self-assembled cubic nanostructure;
FIG. 3 is Fe2O3SEM electron microscope photograph of nano particle self-assembled cubic nano structure;
FIG. 4 is Fe2O3TEM electron micrograph of the nanoparticle self-assembled cubic nanostructure;
FIG. 5 is Fe2O3SAED selective area diffraction analysis photo of nano particle self-assembled cube nano structure;
FIG. 6 is Fe2O3The photocatalytic performance of the nano particle self-assembled cubic nano structure under visible light.
Detailed Description
To further illustrate the technical means and effects of the present invention adopted to achieve the predetermined objects, the following preferred embodiments are combined to prepare single crystal Fe according to the present invention2O3The detailed description of the embodiments, methods, steps, features and effects of the method for self-assembly of cubic nanostructures by nanoparticles is as follows:
example 1:
preparation of single crystal Fe2O3A method for self-assembling cubic nanostructures with nanoparticles, comprising the steps of:
the method comprises the following steps: dissolving ferric chloride hexahydrate in distilled water, dropwise adding 3M NaOH solution to obtain brownish red suspension, stirring for 15min, placing the suspension in a hydrothermal kettle, keeping the temperature at 80 ℃ for 5min, washing hydrothermal reaction products with distilled water and ethanol for 3 times, and filtering to obtain Fe2O3An electron micrograph of the structure of the nanoparticle precursor is shown in fig. 1;
step two: mixing Fe2O3Mixing the nanoparticle precursor with distilled water and ethanol, and stirring uniformly to obtain solution A; said Fe2O3Nanoparticle precursor: distilled water: the molar ratio of ethanol is 1: 100: 10;
step three: dripping 21ml of 3M KOH into the solution A dropwise, stirring for 10min, placing in a hydrothermal kettle, keeping the temperature at 120 ℃ for 60min, washing the hydrothermal reaction product with distilled water and ethanol for 3 times, filtering, and drying the product in a vacuum drying oven at 60 ℃ for 24h to obtain single crystal Fe2O3The X-ray diffraction pattern of the nano-particle self-assembled cubic nano-structure is shown in figure 2, and the diffraction peak and Fe are2O3The phase standard maps (PDF: 89-0598) are consistent, which indicates that the obtained product is Fe2O3And (4) phase(s).
FIGS. 3 and 4 show Fe prepared in this example2O3Electron microscope photograph of nano-particle self-assembled cubic nano-structure. The high yield can be clearly seen from the electron microscope photo, the high yield is a cubic nanometer structure which is self-assembled by nanometer particles, and the side length average of the cubic is about 250-300 nm. The selected area diffraction analysis in FIG. 5 shows that Fe2O3Is a single crystal structure. Line 1 in FIG. 6 is Fe prepared in this example2O3The photocatalytic activity of the methyl orange solution is decomposed by the oval sphere micro-nano structure. The photocatalytic decolorization reaction of the methyl orange solution is expressed as a quasi first-order kinetic relationship, ln (C)0/C)=kt，C0And C is the concentration of methyl orange when the illumination time is 0 and t respectively; k is used as the apparent rate constant. And because ln (A)0/A) = ln(C0/C) =kt，A0And A is the absorbance value at 466nm at an illumination time of 0 and t, respectively. Therefore, the rate constant k is measured, and the larger the value, the better the photocatalytic performance is. From FIG. 6, it can be seen that Fe prepared in this example2O3The cubic nanostructure has excellent photocatalytic activity under visible light.
Example 2:
preparation of single crystal Fe2O3A method for self-assembling cubic nanostructures with nanoparticles, comprising the steps of:
the method comprises the following steps: dissolving ferric nitrate nonahydrate in distilled water, dropwise adding 3M NaOH solution to obtain brownish red suspension, stirring for 15min, placing the suspension in a hydrothermal kettle, keeping the temperature at 100 deg.C for 1min, washing hydrothermal reaction product with distilled water and ethanol for 3 times, and filtering to obtain Fe2O3A nanoparticle precursor;
step two: mixing Fe2O3Mixing the nanoparticle precursor with distilled water and n-octanol, and stirring uniformly to obtain a solution A; said Fe2O3Nanoparticle precursor: distilled water: the molar ratio of n-octanol was 1.15: 200: 15;
step three: dropwise adding 12ml of 7M KOH into the solution A, stirring for 5min, placing in a hydrothermal kettle, keeping the temperature at 200 ℃ for 10min, washing the hydrothermal reaction product with distilled water and ethanol for 3 times, filtering, and drying the product in a vacuum drying oven at 60 ℃ for 24h to obtain single crystal Fe2O3The nano particles are self-assembled into a cubic nano structure.
Example 3:
preparation of single crystal Fe2O3A method for self-assembling cubic nanostructures with nanoparticles, comprising the steps of:
the method comprises the following steps: dissolving ferric chloride hexahydrate in distilled water, dropwise adding 3M NaOH solution to obtain brownish red suspension, stirring for 15min, placing the suspension in a hydrothermal kettle, keeping the temperature at 90 ℃ for 3min, washing hydrothermal reaction products with distilled water and ethanol for 3 times respectively, and filtering to obtain Fe2O3A nanoparticle precursor;
step two: mixing Fe2O3Mixing the nanoparticle precursor with distilled water and butanol, and stirring uniformly to obtain a solution A; said Fe2O3Nanoparticle precursor: distilled water: the molar ratio of butanol was 1.1: 150: 25;
step three: dripping 18ml 5M KOH into solution A dropwise, stirring for 8min, placing in a hydrothermal kettle, keeping the temperature at 140 deg.C for 30min, washing the hydrothermal reaction product with distilled water and ethanol for 3 times, filtering, and drying at 60 deg.C in a vacuum drying ovenDrying for 24h to obtain single crystal Fe2O3The nano particles are self-assembled into a cubic nano structure.
Example 4:
preparation of single crystal Fe2O3A method for self-assembling cubic nanostructures with nanoparticles, comprising the steps of:
the method comprises the following steps: dissolving ferric nitrate nonahydrate in distilled water, dropwise adding 3M NaOH solution to obtain brownish red suspension, stirring for 15min, placing the suspension in a hydrothermal kettle, keeping the temperature at 80 deg.C for 4min, washing the hydrothermal reaction product with distilled water and ethanol for 3 times, and filtering to obtain Fe2O3A nanoparticle precursor;
step two: mixing Fe2O3Mixing the nanoparticle precursor with distilled water and propylene glycol, and stirring uniformly to obtain a solution A; said Fe2O3Nanoparticle precursor: distilled water: the molar ratio of propylene glycol is 1: 180: 20;
step three: dropwise adding 15ml of 8M KOH into the solution A, stirring for 7min, placing in a hydrothermal kettle, keeping the temperature at 160 ℃ for 45min, washing the hydrothermal reaction product with distilled water and ethanol for 3 times, filtering, and drying the product in a vacuum drying oven at 60 ℃ for 24h to obtain single crystal Fe2O3The nano particles are self-assembled into a cubic nano structure.

Claims (3)

1. Preparation of single crystal Fe2O3The method for self-assembling cubic nano-structure by nano-particles is characterized by comprising the following steps:
dissolving an iron compound in distilled water, dropwise adding a 3M NaOH solution to obtain a brownish red suspension, stirring for 15min, placing the suspension in a hydrothermal kettle, keeping the temperature at 80 ~ 100 ℃ for 1 ~ 5min, respectively washing hydrothermal reaction products for 3 times by using distilled water and ethanol, and filtering to obtain Fe2O3A nanoparticle precursor;
step two: mixing Fe2O3Mixing the nanoparticle precursor with distilled water and an organic solvent, and stirring the mixture uniformly to obtain a solution A;
step three, dropwise adding 12 ~ 21ml of 3 ~ 8M KOH into the solution A, stirring for 5 ~ 10min, placing the mixture into a hydrothermal kettle, preserving the heat at 120 ~ 200 ℃ for 10 ~ 60min, washing the hydrothermal reaction product for 3 times by using distilled water and ethanol, respectively, filtering, placing the product into a vacuum drying oven, and drying for 24h at 60 ℃ to obtain single crystal Fe2O3A nanoparticle self-assembled cubic nanostructure;
in the first step, the iron compound is ferric nitrate nonahydrate.
2. The method of claim 1, wherein: and in the second step, the organic solvent is one of ethanol, propanol, n-octanol, butanol, ethylene glycol, propylene glycol and tetrahydrofuran.
3. The method of claim 1, wherein: fe in the second step2O3The molar ratio of nanoparticle precursor to distilled water to organic solvent was 1 ~ 1.15.15: 100 ~ 200:10 ~ 25.
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