Method for preparing transition metal oxide microspheres with controllable morphology

A transition metal and transition metal salt technology, applied in the field of materials science, can solve the problems of complex and tedious operation steps of transition metal oxides, easy agglomeration of nanoparticles, lack of active sites, etc., and achieves controllable morphology and adjustable morphology. , the effect of simple steps

Active Publication Date: 2015-07-01
SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI
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Problems solved by technology

In recent years, the synthesis of transition metal oxides with different morphologies has become a research hotspot (J.Am.Chem.Soc.2011, 133, 19314), but some shortcomings still need to be solved, for example: the synthesis of fine nanoparticles is used When it is easy to agglomerate, it leads to the loss of active sites and the decrease of activity; however, the synthesis of transition metal oxides with complex structures often requires complex and tedious steps, and the yield is low

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  • Method for preparing transition metal oxide microspheres with controllable morphology
  • Method for preparing transition metal oxide microspheres with controllable morphology
  • Method for preparing transition metal oxide microspheres with controllable morphology

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[0029] In one embodiment of the present invention, a method for preparing transition metal oxide microspheres with controllable morphology may include: taking 1-5 mmol of transition metal salt and 0.1-3 mmol of catechol compound in water After 1-24 hours of reaction in the thermal reaction system, the transition metal oxide microspheres are prepared. If an additional 0-3 mmol of other morphology control agents are added to the hydrothermal system, the morphology of the transition metal oxide microspheres can be regulated.

[0030] In a more specific embodiment, the preparation method may include the following steps:

[0031] Ⅰ. Mix polar solvent and alcohol solvent, and add 0.1-3mmol catechol compound to the mixed solution, and then disperse evenly by ultrasonic;

[0032] Ⅱ. Add 1 to 5 mmol of transition metal salt and 0 to 3 mmol of morphology control agent to the mixed solution treated in step I, mix and disperse evenly, and react at 160 to 200°C for 1 to 24 hours;

[0033]...

Embodiment 1

[0040] Example 1 Dissolve 1mmol of dopamine and 1mmol of iron acetylacetonate in a mixed solution of 20mL of ethanol and 20mL of acetic acid, and disperse evenly by ultrasonication. Then, add 3mmol of tetraisopropyl titanate, continue stirring for 30 minutes, and transfer the solution to 50mL In the reaction kettle, react at 200°C for 12 hours. After cooling down, the product is collected by centrifugation. After washing and drying, hollow titanium dioxide microspheres can be obtained. For the morphology, please refer to Figure 1a-Figure 1b, it can be seen that the hollow titanium dioxide microspheres are uniform in size, with a diameter of about 1 μm.

Embodiment 2

[0041] Example 2 Dissolve 1mmol of catechol and 1mmol of 1,10-phenanthroline in a mixed solution of 10mL of water and 30mL of formic acid, ultrasonically disperse evenly, then add 1mmol of titanium tetrachloride, and continue to stir for 30 minutes. The solution was transferred to a 50mL reactor and reacted at 180°C for 18h. After cooling down, the product was collected by centrifugation, washed and dried to obtain titanium dioxide microspheres assembled from nanosheets.

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Abstract

The invention discloses a method for preparing transition metal oxide microspheres with controllable morphology. According to the method for preparing the transition metal oxide microspheres, the transition metal oxide microspheres are produced according to the steps of introducing catechol compounds into a reaction system and then performing simple hydrothermal reaction, and preferably, a morphology control agent can also be added in the hydrothermal reaction system to control the morphology of the transition metal oxide microspheres. According to the method for preparing the transition metal oxide microspheres with controllable morphology disclosed by the invention, the transition metal oxide microspheres with controllable morphology are produced by adding a special morphology control agent into the hydrothermal reaction system to control the anisotropic growth of the material, not only the technology is simple, the controllability is good and the yield is high, but also the product produced according to the method has uniform size, larger specific surface area and high reaction activity and is suitable for large-scale preparation.

Description

technical field [0001] The invention relates to a preparation method of nanomaterials, in particular to a preparation method of monodisperse transition metal oxide microspheres, belonging to the technical field of material science. Background technique [0002] Compared with individual nanoparticles or bulk materials, the three-dimensional nanostructures formed by the assembly of nano-units have been proved to have good performance. Transition metal oxides have been widely used in lithium-ion batteries, supercapacitors, photocatalytic degradation, and gas detection due to their abundant reserves, environmental friendliness, and low price. It is generally believed that the morphology and surface properties of transition metal oxides have an important impact on the physical and chemical properties of materials, and the structure of transition metal oxide materials has important significance for their applications. In recent years, the synthesis of transition metal oxides with...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G23/053C01G45/02B82Y30/00
Inventor 王强斌李德鲁李轮
Owner SUZHOU INST OF NANO TECH & NANO BIONICS CHINESE ACEDEMY OF SCI
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