Method for preparing nanometer metallic oxide by bulk metallic oxide

A nano-metal and bulk metal technology, applied in the direction of oxide/hydroxide preparation, zinc oxide/zinc hydroxide, chemical instruments and methods, etc., can solve the problems of complex production process and high production cost, and achieve air stability High stability, short synthesis time, and good sample crystallinity

Inactive Publication Date: 2013-10-23
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the use of complex complex precursors, the production cost is expensive and the production process is complicated

Method used

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  • Method for preparing nanometer metallic oxide by bulk metallic oxide
  • Method for preparing nanometer metallic oxide by bulk metallic oxide
  • Method for preparing nanometer metallic oxide by bulk metallic oxide

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Example 1 Process for synthesizing nano-cadmium oxide

[0038] Put 0.128g (1mmol) of cadmium oxide powder, 1ml oleic acid and 5ml oleylamine into a three-necked bottle, then plug the two sides of the three-necked bottle with rubber stoppers, connect the middle port to the Schlenk system, and connect the thermocouple Insert the three-necked flask from one side (such as the right side) under the liquid surface, stir and heat, and when heated to 180°C, the cadmium oxide is completely dissolved to obtain a clear solution. When heating to 260°C, the color of the transparent solution gradually turns yellow and turbid, forming nano-cadmium oxide, which is the starting point of nano-cadmium oxide at this time.

[0039] Samples were taken for sample characterization in different growth times (1, 2, 10 minutes and longer). figure 1 It is a nano-cadmium oxide sample with a growth time of 1 minute. It is a nano-cluster with a cluster size of about 50 nanometers; figure 2 It is a nano-c...

Embodiment 2

[0042] Example 2 Process for synthesizing nano-zinc oxide

[0043] The process of synthesizing nano-zinc oxide is the same as the process of synthesizing cadmium oxide in Example 1, only 0.128g (1mmol) of cadmium oxide powder is replaced with 0.081g (1mmol) of zinc oxide powder. Zinc oxide is completely dissolved when heated to 180°C. Continue heating, when the temperature reaches 240°C, the color of the transparent solution gradually changes to light yellow and turbid, forming nanometer zinc oxide.

[0044] The TEM picture of the nano zinc oxide sample is as Picture 9 , 10 As shown, Picture 9 Is the morphology of the sample after 1 minute of reaction, Picture 10 It is the morphology of the sample after 10 minutes of reaction. The morphology and size of the two samples have little change. The X-ray diffraction pattern of nano-zinc oxide is as follows Picture 11 Shown is a wurtzite hexagonal structure (JCPDS No.79-205), which is consistent with the structure of the reacting raw...

Embodiment 3

[0045] Example 3 Process for synthesizing nano gallium oxide

[0046] 0.0469g (0.25mmol) of gallium oxide powder, 1ml of oleic acid and 5ml of oleylamine were put into a three-necked flask, connected to the Schlenk system, stirred and heated. When heated to 240°C, the color of the solution gradually becomes orange-red and turbid, forming nano-gallium oxide.

[0047] Figure 14 It is a transmission electron microscope picture of a nano gallium oxide sample, which is similar to a porous structure. Figure 15 It is the X-ray diffraction pattern of the nanometer gallium oxide sample, which corresponds exactly to the standard card of gallium oxide (JCPDSNo.43-1012). This structure is consistent with the structure of the bulk gallium oxide as the reaction raw material.

[0048] Figure 16-18 These are the scanning electron microscope pictures of bulk cadmium oxide, zinc oxide, and gallium oxide used in this method, from Figure 16-18 It can be seen that the morphology of the bulk metal o...

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Abstract

The invention relates to a method for preparing nanometer metallic oxide by bulk metallic oxide, which belongs to the technical field of preparation of nanometer materials. Cadmium oxide, zinc oxide and gallium oxide bulk materials are respectively used as raw materials, oleic acid and oleylamine are used as auxiliary materials, and corresponding nanometer metallic oxide is obtained by a solution recrystallization process. The shape and the size of the generated nanometer metallic oxide can be adjusted by means of controlling the concentration of an oxide source and reaction time, and the obtained nanometer metallic oxide still has the structure of the bulk materials. The bulk metallic oxide is directly converted into the nanometer metallic oxide, the raw materials used in the preparation method are common, cheap and relatively safe, and air stability is high. In addition, the preparation method has the advantages of simple synthetic process, high repeatability, fine sample crystallinity, uniform size distribution and the like, and has a potential of producing the nanometer metallic oxide on a large scale.

Description

Technical field [0001] The invention belongs to the technical field of nano material preparation, and relates to a method for preparing nano metal oxides from bulk metal oxides. Background technique [0002] Among the many functional materials, metal oxides have received widespread attention due to their applications in many fields such as catalysis, sensing, optics, energy storage and conversion. Due to its unique properties and wide application potentials that are different from bulk materials, the synthesis and properties of metal nano-oxides with controllable morphology and size have attracted extensive research interest. So far, metal oxide nanocrystals can be prepared by many technical methods, such as calcination, thermal decomposition, ion exchange, dehydration, etc., but these methods have some disadvantages, such as harsh preparation conditions, high cost, and particle size distribution of the obtained nanoparticles Uneven etc. Among these methods, the pyrolysis of or...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B13/14C01G11/00C01G9/02C01G15/00B82Y40/00
Inventor 邹勃王英楠张品华邹广田
Owner JILIN UNIV
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