Method for synthesizing rod-like and echinoid molybdena-based nano-material

A sea urchin-shaped, molybdenum oxide technology, applied in the directions of molybdenum oxide/molybdenum hydroxide, nanotechnology, nanotechnology, etc., can solve the problems of long synthesis time and difficult preservation, and achieve controllable reaction conditions, short hydrothermal time, and product good repeatability

Inactive Publication Date: 2009-04-22
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Application Information

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Problems solved by technology

Using hydrated molybdenum oxide to solvothermally treat under acidic or near-neutral conditions can synthesize submicron fibers in one step, but the solid precursor dihydrate molybdenum trioxide, which is not easy to store, must be prepared before the reaction (Chem.Mater.2004, 16, 1126)
The latter two methods require a long (about 1 month) synthesis time

Method used

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  • Method for synthesizing rod-like and echinoid molybdena-based nano-material
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  • Method for synthesizing rod-like and echinoid molybdena-based nano-material

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Experimental program
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Effect test

Embodiment 1

[0041] The preparation of α-molybdenum trioxide nanorod, its specific steps are:

[0042] A) Add 1.44 g of molybdenum trioxide (10 mmol) into 10 ml of 30% hydrogen peroxide aqueous solution, keep the external temperature at 30° C., and stir. After reacting for 6 hours, the molybdenum trioxide was completely dissolved to obtain a clear yellow-green aqueous solution of molybdic acid peroxide (wherein the concentration of molybdenum was 1.0 mol / L).

[0043] B) Using aqueous molybdic acid peroxide as a precursor solution. The solution was transferred into a Teflon-lined stainless steel hydrothermal synthesis kettle. Seal the hydrothermal synthesis kettle, place it at 180°C, and heat it in an electric furnace for 48 hours. After the heating, the hydrothermal synthesis kettle was taken out, and the kettle body was placed in the laboratory, and cooled naturally at room temperature. The solid product was separated by centrifugation, washed repeatedly and thoroughly with deionized w...

Embodiment 2

[0046] The preparation of α-molybdenum trioxide nanorod, its specific steps are:

[0047] A) with embodiment 1A)

[0048] B) Dilute the molybdenum peroxide aqueous solution with deionized water to a molybdenum concentration of 0.2 mol / L, as a precursor solution. The solution was transferred into a Teflon-lined stainless steel hydrothermal synthesis kettle. Seal the hydrothermal synthesis kettle, place it at 180°C, and heat it in an electric furnace for 48 hours. After the heating, the hydrothermal synthesis kettle was taken out, and the kettle body was placed in the laboratory, and cooled naturally at room temperature. The solid product was separated by centrifugation, washed repeatedly and thoroughly with deionized water, and the solid product was dried at room temperature to obtain α-molybdenum trioxide nanorods.

[0049] Depend on Figure 4 It can be seen that the length of α-molybdenum trioxide nanorods is 5.5-7.5 μm, the width is 200-330 nm, most of them are about 250...

Embodiment 3

[0051] The preparation of α-molybdenum trioxide nanorod, its specific steps are:

[0052] A) with embodiment 1A)

[0053] B) Using aqueous molybdic acid peroxide as a precursor solution. The solution was transferred into a Teflon-lined stainless steel hydrothermal synthesis kettle. Seal the hydrothermal synthesis kettle, place it at 80° C., and heat it in an electric furnace for 48 hours. After the heating, the hydrothermal synthesis kettle was taken out, and the kettle body was placed in the laboratory, and cooled naturally at room temperature. The solid product was separated by centrifugation, washed repeatedly and thoroughly with deionized water, and the solid product was dried at room temperature to obtain α-molybdenum trioxide nanorods.

[0054] Depend on Figure 5 It can be seen that the length of α-molybdenum trioxide nanorods is 1-3 μm, the width is 200-300 nm, most of them are about 250 nm. The generated nanorods have small thickness and relatively uniform scale....

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Abstract

The invention relates to a quick and efficient non-template agent hydro-thermal synthesizing method. The system can synthesize an alpha-molybdenum trioxide nanometer rod and a high-density echinoid molybdenum oxide based nanometer materials. Molybdenum peroxide acid prepared from molybdenum trioxide and aqueous hydrogen peroxide solution is used as a precursor, is produced into scattered alpha-molybdenum trioxide nanometer rod by hydro-thermal synthesis at a temperature of between 80 and 180 DEG C, and is produced into the peroxide modified molybdenum oxide hydrate by hydro-thermal synthesis at a temperature of between 65 and 75 DEG C. The hydrate is a multiscale structure; a nanometer thin slice, a micron prism and a nanometer rod-shaped structure unit are divergently assembled into a micron-size high-density echinoid structure. The hydrate is roasted to obtain high-density echinoid alpha-molybdenum trioxide. Modulation of the synthesizing condition can realize fine adjustment for appearance of the nanometer rod, the micron-size echinoid structure and the structure unit thereof. The method uses raw materials with low cost, has the advantages of simple technical process, controllable conditions and the like, and can promote research and application of the molybdenum oxide in the fields of sensors, field transmission, electrode materials and so on.

Description

technical field [0001] The invention relates to a hydrothermal preparation method of α-molybdenum trioxide nanorods and high-density sea urchin-like molybdenum oxide-based nanomaterials, specifically a template-free method for rapidly and effectively synthesizing rod-shaped and high-density sea urchin-like molybdenum oxide-based nanomaterials A method for rapidly and efficiently preparing α-molybdenum trioxide nanorods and high-density sea urchin-like molybdenum oxide-based nanomaterials through a template-free hydrothermal process. Background technique [0002] In recent years, morphology-anisotropic nanostructured materials (including nanotubes, nanowires, nanorods, and nanoribbons) and their multiscale assemblies have received more and more attention in the field of materials research. On the one hand, nanoscale materials themselves can exhibit completely different physical and chemical properties from corresponding bulk-level materials; on the other hand, the anisotropy ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G39/02B82B3/00
Inventor 方亮张涛王爱琴
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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