Preparation method for nanometer composite metal oxide

A nano-composite and composite metal technology, which is applied in the preparation of oxides/hydroxides, rare earth metal oxides/hydroxides, rare earth metal compounds, etc. Commercial application of the system, complex preparation equipment or process flow, etc., to avoid impure components and difficult to control microstructure, reduce pollutant emissions and production costs, reduce equipment costs and operational difficulties

Active Publication Date: 2018-05-18
深圳市大擎科技有限公司
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  • Description
  • Claims
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Problems solved by technology

Although the stability of the precursor can be improved through some improvement measures (such as the use of solvents such as ethylene glycol or methyl ether), this problem has not been fundamentally solved, and the commercial application of similar precursor systems has been greatly limited.
[0014] Niobium pentachloride or niobium pentoxide dissolved in hydrofluoric acid can also be used as the precursor of niobium. Although the price of halogen salts is cheaper than alkoxides and the stability is improved, however, because the precursor liquid contains halogen group elements, so it is inevitable that there will be halogen residues in the final material, which may deteriorate the relevant properties of the material
[0018] 1. Although the solid-phase method is simple and cheap, it cannot achieve precise control of product composition and microstructure
[0019] 2. Although the wet chemical method can obtain products with good purity and microstructure, the preparation equipment or process is complicated, and expensive organic precursors or a large amount of organic complexing agents need to be used

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  • Preparation method for nanometer composite metal oxide
  • Preparation method for nanometer composite metal oxide
  • Preparation method for nanometer composite metal oxide

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preparation example Construction

[0049] One embodiment of the present invention provides a method for preparing a nano-composite metal oxide, comprising: using nano-metal oxide, one of the main metal components of the composite metal oxide, as a nano-template, and uniformly dispersing the nano-template in In the aqueous solution of water-soluble salts of other metal components in the composite metal oxide to obtain a mixed dispersion, the main metal component refers to a metal component whose molar content accounts for more than 30% of the molar content of all metal components; Dry the mixed dispersion by spray drying or vacuum drying to obtain a powder mixture; heat-treat the powder mixture so that the oxides generated by the decomposition of the water-soluble salt combine with the nano-metal oxides to form The nanocomposite metal oxide.

[0050] The scheme of the present invention uses nano-oxides of main metal elements as templates, and soluble salts (such as inorganic salts) added to the aqueous solution ...

Embodiment 1

[0068] SrTiO 3±δ preparation of

[0069] 1. Weigh 0.2 mol of TiO with a particle size of about 15 nm 2 Put the particles in a beaker, add 100mL deionized water and stir to form a suspension, set as A;

[0070] 2. Weigh 0.2mol Sr(NO 3 ) 2 , add 800mL deionized water to dissolve, set as B;

[0071] 3. Slowly pour B into A, stir and mix evenly; add a small amount of surfactant (P123, PVP, Triton-100 or PEG400-2000) to form a stable suspension.

[0072] 4. Transfer the suspension in step 3 to a spray dryer for spray drying. The inlet air temperature is set to 150-180°C, the air flow is 120-200L / min, and the residence time is 1-4s;

[0073]5. After drying the powder at 120°C in a blast drying oven for 2 hours, take out the powder and pour it into a crucible, place the crucible in a muffle furnace, raise the temperature to 350°C at a heating rate of 1°C / min and keep it warm After cooling for 1 hour, place the crucible in the middle of the tube furnace, seal it and feed nitroge...

Embodiment 2

[0076] Sr 0.95 Ti 0.9 Nb 0.1 o 3±δ preparation of

[0077] 1. Weigh 0.18 mol of TiO with a particle size of 60 nm 2 Put the particles in a beaker, add 700mL deionized water and stir to form a suspension, set as A;

[0078] 2. Weigh 0.19mol Sr(NO 3 ) 2 Add 800mL deionized water to dissolve and set it as B; slowly pour B into A, stir and mix evenly to form solution C;

[0079] 3. Weigh 0.02mol C 4 h 4 NbO 9 , into C, stir rapidly, and add a small amount of surfactant (P123, PVP, Triton-100 or PEG400-2000) to form a stable suspension.

[0080] 4. Transfer the suspension in step 3 to a vacuum freeze dryer, quickly freeze it into a solid state at -10 to -50°C, and then directly sublimate the water into a gaseous state under a vacuum of 1.3 to 13Pa to remove it.

[0081] 5. Put the powder in the muffle furnace, raise the temperature to 350°C at a heating rate of 1°C / min and keep it warm for 1 hour. After cooling, place the crucible in the middle of the tube furnace, and a...

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Abstract

The invention discloses a preparation method for a nanometer composite metal oxide. The preparation method comprises the following steps: with a nanometer metal oxide, which is one of the main metal components of the composite metal oxide, as a nanometer template, evenly dispersing the nanometer template in aqueous solutions of water-soluble salts of other metal components in the composite metal oxide so as to obtain mixed dispersion liquid, wherein the main metal component refers to a metal component with a molar content accounting for more than 30% of the molar content of all metal components; drying the mixed dispersion liquid through spray drying or vacuum freeze drying so as to obtain a powder mixture; and subjecting the powder mixture to heat treatment to allow oxides formed by the decomposition of the water-soluble salts to be compounded with the nanometer metal oxide so as to form the nanometer composite metal oxide. The preparation method of the invention significantly reducescost and operation difficulties, avoids the large-scale use of organic compounds, and prevents the problems of impure composition and difficultly-controllable microstructure caused by nonuniform mixing and the introduction of ball milling impurities.

Description

technical field [0001] The invention relates to the technical field of preparation of nanomaterials, in particular to a preparation method of nanocomposite metal oxides. Background technique [0002] The existing methods for preparing nanocomposite metal oxides mainly include two categories, one is liquid phase method, or wet chemical method, including co-precipitation method, hydrothermal method, sol-gel method, and the other is solid phase method. Law. The above method is briefly introduced as follows: [0003] 1. Co-precipitation method: dissolve the compound containing metal elements in the liquid (deionized water or absolute ethanol, etc., determine the type of solvent according to the nature of the compound), add a precipitant and stir, so that several metal ions are mixed in proportion A precipitate is generated, and the precipitate is washed and calcined to obtain the target product. [0004] 2. Hydrothermal method: a modification of the co-precipitation method, t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B13/14C01G23/00C01G33/00C01F17/00C01G53/00B82Y30/00B82Y40/00
CPCB82Y30/00B82Y40/00C01B13/14C01G23/006C01G25/02C01G33/006C01G53/50C01P2002/34C01P2002/72C01P2004/03C01P2004/64C01F17/206
Inventor 陶有堃邵静
Owner 深圳市大擎科技有限公司
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