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Preparation method for orthorhombic nanometer lead oxide and tetragonal-phase nanometer lead oxide

A technology of lead oxide and orthorhombic phase, which is applied in the field of preparation of nanomaterials to achieve the effects of short production cycle, high repeatability and high purity

Inactive Publication Date: 2012-08-01
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are few reports on the synthesis of pure PbO nanoparticles with these two different structures.

Method used

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  • Preparation method for orthorhombic nanometer lead oxide and tetragonal-phase nanometer lead oxide

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Experimental program
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Effect test

Embodiment 1

[0019] Embodiment 1 The process of synthesizing orthorhombic nano-lead oxide

[0020] Put 0.223g of orthorhombic bulk lead oxide powder, 1ml of oleic acid and 5ml of oleylamine into a 50mL three-necked bottle, then plug the two sides of the three-necked bottle with rubber stoppers, and connect the middle port to the Schlenk system , Insert a thermocouple from the side port of the three-necked bottle under the liquid surface, heat and stir, the heating rate is controlled at 25°C / min and when heated to 160°C, the lead oxide is completely dissolved to form a Pb-ligand complex solution. When the temperature continued to rise to 270°C, the color of the solution gradually turned yellow-green and turbid, and what was produced at this time was pure orthorhombic nano-lead oxide. After 10 minutes of reaction, a nano-lead oxide sample is obtained through nucleation and growth, and the sample is washed three times with a mixed solution of methanol and acetone at a volume ratio of 1:1 to o...

Embodiment 2

[0022] Embodiment 2 The process of synthesizing tetragonal phase nano lead oxide

[0023] Put 0.223g of orthorhombic bulk lead oxide powder, 1ml of oleic acid and 5ml of oleylamine into a 50mL three-necked bottle, then plug the two sides of the three-necked bottle with rubber stoppers, and connect the middle port to the Schlenk system , Insert a thermocouple from the side port of the three-necked bottle under the liquid surface, heat and stir, the heating rate is controlled at 18°C / min, when the lead oxide is heated to 140°C, the lead oxide is completely dissolved to form a Pb-ligand complex solution. When the temperature continued to rise to 220°C, the color of the solution gradually turned yellow and turbid, and what was produced at this time was pure tetragonal phase nano-lead oxide. After 10 minutes of reaction, a nano-lead oxide sample is obtained through nucleation and growth, and the sample is washed three times with a mixed solution of methanol and acetone with a volum...

Embodiment 3

[0025] Embodiment 3 The process of synthesizing orthorhombic phase and tetragonal phase nano lead oxide mixture

[0026] The process of synthesizing orthorhombic phase and tetragonal phase nano-lead oxide mixture is basically the same as the process of synthesizing orthorhombic phase nano-lead oxide in Example 1, except that the heating rate is controlled at 20°C / min, and the transparent Pb-ligand complex solution will be in At 230°C, it starts to turn yellow and turbid, and at this time, a mixture of orthorhombic and tetragonal nano-lead oxides is formed. React at 230-250°C for 10 minutes to obtain nano-lead oxide samples through nucleation and growth. Wash the samples three times with a mixed solution of methanol and acetone with a volume ratio of 1:1 to obtain orthorhombic and tetragonal phase nano-lead oxides. mixture.

[0027] Figure 6 It is the X-ray diffraction pattern of the mixture of orthorhombic and tetragonal nano-lead oxides, which completely corresponds to the...

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Abstract

The invention relates to a preparation method for an orthorhombic nanometer lead oxide and a tetragonal-phase nanometer oxide, which belongs to the technical field of preparation of nanometer materials. The preparation method includes using an orthorhombic bulk lead oxide as a raw materials and oleic acid and oleylamine as auxiliary materials; obtaining transparent Pb solution by means of heating and stirring; obtaining the orthorhombic nanometer lead oxide when the clear Pb solution becomes muddy at the temperature of 270 DEG C; obtaining pure tetragonal-phase lead oxide nanometer crystals when the Pb solution becomes muddy at the temperature of 220 DEG C; and obtaining mixture of the orthorhombic nanometer lead oxide and tetragonal-phase nanometer lead oxide when the reaction temperature ranging from 230 DEG C to 250 DEG C. The orthorhombic nanometer lead oxide and the tetragonal-phase nanometer oxide which are high in purity, uniform in shape and fine in monodispersity can be obtained. The raw material is simple and easy to obtain, is synthesized at one step and is low in cost. Besides, the preparation method has the advantages of short production period, high repeatability, fine sample crystallinity and the like, and has a potential of producing nanometer lead oxide on a large scale.

Description

technical field [0001] The invention relates to a method for directly preparing orthorhombic phase and tetragonal phase nanometer lead oxide from an orthorhombic phase bulk lead oxide, which belongs to the technical field of preparation of nanometer materials. Background technique [0002] Lead oxide is a traditional battery electrode material and is the material used to prepare lead-acid battery electrodes. In addition, reports have shown that lead oxide thin films can also be used as photoanode materials for solar cells. (References: VeluchamyP, Minoura H, Simple electrochemical method for the preparation of a highly oriented and highly photoactive α-PbO film. Appl. Phys. Lett., 1994, 65: 2431-2433.) Therefore, from the development of new energy From a perspective, it is necessary to study the preparation of nanostructured lead oxide materials for the development of super batteries and solar cells based on lead oxide nanostructures. Lead oxide has two crystal structures:...

Claims

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Application Information

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IPC IPC(8): C01G21/06B82Y40/00
Inventor 邹勃张品华王英楠邹广田
Owner JILIN UNIV
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