Method for preparing large batch of binary superlattice emulsion balls

A superlattice and emulsion technology, which is applied in nanostructure manufacturing, nanotechnology for materials and surface science, formation of specific nanostructures, etc., can solve problems such as unfavorable material application value, multi-phase coexistence, material limitations, etc., to achieve Overcome the effects of inability to scale up large-scale preparation, simple assembly method, and controllable size

Inactive Publication Date: 2019-10-11
FUDAN UNIV
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Problems solved by technology

[0003] At present, the solvent evaporation method and the gas-liquid interface assembly method are relatively common methods for preparing binary superlattices, but they all have their limitations.
The binary superlattice prepared by the solvent evaporation method is generally deposited on the base material, and it is difficult to separate from the base material to obtain a separate binary superlattice material; although the binary superlattice prepared by the gas-liquid interface assembly method can be transferred, However, the prepared materials are limited to the shape of two-dimensional thin films, which is not conducive to the potential application value of subsequent research materials.
At the same time, the binary superlattice materials prepared by these two methods often have multiple phases coexisting, and it is impossible to separate the binary superlattice materials of a single phase.
The more serious challenge is that these two assembly methods cannot prepare binary superlattice materials in large quantities, which seriously hinders the subsequent research on material properties.

Method used

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  • Method for preparing large batch of binary superlattice emulsion balls
  • Method for preparing large batch of binary superlattice emulsion balls
  • Method for preparing large batch of binary superlattice emulsion balls

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Embodiment 1

[0031] (1) Add 36 g iron oleate, 8 g oleic acid, 200 g 1-octadecene into a 500 ml three-necked bottle, and add a high-temperature magnet. After evacuating at 120° C. under the condition of stirring, the temperature was raised to 320° C. under an argon atmosphere, and kept at a constant temperature for 60 minutes, and then naturally cooled to obtain a brown or black reaction product. Next, add n-hexane, isopropanol and ethanol to the product, mix thoroughly, collect the precipitate by centrifugation, and dissolve it with n-hexane. After a uniform solution is formed, add isopropanol and methanol in turn, mix thoroughly, and The precipitate was collected and dispersed with n-hexane again to obtain 40 ml of oleic acid molecules as a ligand-protected uniform solution of 17 nm ferric oxide colloidal nanocrystals.

[0032] (2) Add 5.6 g of iron acetylacetonate, 2.0 g of cobalt acetylacetonate, 4.5 g of oleic acid, 21.0 g of oleylamine, and 25 ml of benzyl ether into a 250 ml three-ne...

Embodiment 2

[0041] According to the basic steps of particle synthesis given in Example 1, by changing different synthesis conditions (reaction temperature, heating rate, reactant feed ratio), the particle size can be adjusted in the range of 2-20nm, excellent monodispersity and stable dispersion Inorganic nanoparticles in nonpolar solvents. The assembly method is the same as in Example 1, wherein the inorganic colloidal crystal nanoparticles are dispersed with chloroform, and 11nm iron ferric oxide particles and 4.5nm cobalt ferrite particles with a concentration of 10mg / mL are selected and mixed according to the ratio of the number of particles of 1:2. Take 10mL chloroform solution of particles, add 10mL sodium lauryl sulfate concentration to 100g / L deionized aqueous solution (volume ratio of oil phase to water phase is 1:1), emulsification rate is 12000rmp, homogenize for 5 minutes, And reacted under argon atmosphere at 20°C for 60 minutes, washed and separated to obtain 2 Morphology o...

Embodiment 3

[0043] The method is the same as in Example 1-2, the inorganic colloidal crystal nanoparticles are dispersed with toluene solvent, 7nm iron ferric oxide particles and 5nm cobalt ferrite particles with a concentration of 200mg / mL are selected, and mixed according to the ratio of the number of particles of 1:5, taking Add 1mL of particle chloroform solution to 100mL polyethylene glycol octylphenyl ether concentration of 2g / L deionized aqueous solution (volume ratio of oil phase to water phase is 1:100), emulsification rate is 2000rmp, homogeneity is 30 Minutes, and react under nitrogen atmosphere at 70°C for 30 minutes, wash and separate to obtain 5 Morphology of binary superlattice materials. After mixing particles of different types and sizes according to a certain concentration ratio, this method can be used to synthesize a series of binary superlattice materials with spherical emulsion shapes, including type AB, AB 2 Type, AB 3 Type, AB 4 Type, AB 5 Type, AB 6 Type, AB ...

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Abstract

The invention provides a method for preparing a large batch of binary superlattice emulsion balls. The method includes: by pyrolysis, preparing a series of monodisperse and size-adjustable inorganic colloid nanocrystalline particles with organic molecular ligands on surfaces, and by an emulsion assembling method, directly preparing a large batch of the binary superlattice emulsion balls which areordered in height and are provided with single structures. The method is simple and high in repeatability, conditions for the method are easy to control, large-scale production can be realized, the problem of multiphase coexistence during binary superlattice preparation can be solved effectively, and the method also can be applied to assemblies of various inorganic nanometer particles and is highin universality. The prepared binary superlattice material is widely applied to energy storage and transformation, biological marking and imaging, photoelectric devices and the like.

Description

technical field [0001] The invention belongs to the technical field of inorganic materials, and in particular relates to a method for preparing binary superlattice emulsion balls in large quantities. Background technique [0002] The co-assembly of multi-component inorganic colloidal nanocrystalline particles can prepare superstructure materials with new morphology and new properties, which have a wide range of applications in biomarking and imaging, energy conversion and storage, and optoelectronic devices. Among them, the binary superlattice material has a rich and adjustable morphology, and can combine a variety of nano-components with different functions, which is a composite material with great application prospects. [0003] At present, the solvent evaporation method and the gas-liquid interface assembly method are relatively common methods for preparing binary superlattices, but both have their limitations. The binary superlattice prepared by the solvent evaporation ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B82B3/00B82Y30/00B82Y40/00
CPCB82B3/0019B82Y30/00B82Y40/00
Inventor 董安钢杨于驰杨东韩文茜李明重宁静刘梓涵邓雨薇邹金祥
Owner FUDAN UNIV
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