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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 The effect of high stability, short synthesis time and simple method

Inactive Publication Date: 2012-08-01
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] Embodiment 1 The process of synthesizing nano cadmium oxide

[0038] Put 0.128g (1mmol) cadmium oxide powder, 1ml oleic acid and 5ml oleylamine into the 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 it from one side of the three-neck bottle (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 continuing to heat to 260°C, the color of the transparent solution gradually turns yellow and turbid, that is, nano-cadmium oxide is formed, which is the starting point for the growth of nano-cadmium oxide.

[0039] Samples were extracted for sample characterization at 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, which is a nano-cluster, and the size of the ...

Embodiment 2

[0042] Embodiment 2 The process of 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 need to replace 0.128g (1mmol) cadmium oxide powder with 0.081g (1mmol) zinc oxide powder. Zinc oxide dissolves completely when heated to 180°C. Continue heating, and when the temperature reaches 240°C, the color of the transparent solution gradually changes to light yellow and turbid, that is, nano-zinc oxide is formed.

[0044] The transmission electron microscope pictures of nano-zinc oxide samples are as follows: Figure 9 , 10 as shown, Figure 9 is the morphology of the sample when reacted for 1 minute, Figure 10 is the sample morphology when reacted for 10 minutes, and the morphology and size of the two samples have little change. The X-ray diffraction pattern of nano-zinc oxide is as follows: Figure 11 As shown, it is a wurtzite hexagonal structure (JCPDS No.79-205), whic...

Embodiment 3

[0045] Embodiment 3 The process of synthesizing nano gallium oxide

[0046] Put 0.0469g (0.25mmol) of gallium oxide powder, 1ml of oleic acid and 5ml of oleylamine into a three-necked bottle, connect it to a Schlenk system, stir and heat. When heated to 240°C, the color of the solution gradually turns orange-red and turbid, that is, nano-gallium oxide is formed.

[0047] Figure 14 It is a transmission electron microscope picture of a nano-gallium oxide sample, which is a morphology similar to a porous structure. Figure 15 It is the X-ray diffraction pattern of the nano-gallium oxide sample, which completely corresponds to the standard card of gallium oxide (JCPDS No. 43-1012), and the structure is consistent with the structure of the reaction raw material bulk gallium oxide.

[0048] Figures 16-18 It is the scanning electron microscope picture of bulk cadmium oxide, zinc oxide and gallium oxide that this method adopts respectively, from Figures 16-18 It can be seen tha...

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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 solutionrecrystallization 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 preparationmethod 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 preparation of nanometer materials, and relates to a method for preparing nanometer metal oxides from bulk metal oxides. Background technique [0002] Among numerous functional materials, metal oxides have attracted extensive attention due to their applications in many fields such as catalysis, sensing, optics, energy storage and conversion. Due to their unique properties different from bulk materials and wide application potential, the synthesis and properties of metal nanooxides 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 the particle size distribution of the obtained nanoparticles Uneven etc. Among these methods, the py...

Claims

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Application Information

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Patent Type & Authority Applications(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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