Method for solvent-thermally synthesizing nano bismuth oxide single-crystal chips

A technology of nano-bismuth oxide and single wafer, which is applied in chemical instruments and methods, single crystal growth, single crystal growth, etc. It can solve the problems of purity, low synthesis efficiency, difficult to control shape, and large one-time investment, etc., to achieve The effect of uniform product appearance, cheap raw materials, and easy operation

Active Publication Date: 2010-06-23
NANJING UNIV OF SCI & TECH
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  • Summary
  • Abstract
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  • Application Information

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Problems solved by technology

In the direct high-temperature synthesis of simple substances, it is easy to form oxides on the metal surface, which inhibits the further evaporation of metal bismuth, so the purity and synthesis efficiency are low (Surface & Coatings Technology 201 (2007): 5330-5332), which is greatly restricted in production and application. Restrictions; the synthesis of bismuth oxide by chemical precipitation is currently commonly used in the industrial synthesis of bismuth oxide differential, but there are problems of low purity, large pollution, and difficult to control the shape; organic precursor pyrolysis method can synthesize zero-dimensional, one-dimensional, and Two-dimensional polycrystalline thin film, but the process is complicated. To synthesize high-performance products, a large one-time investment is required, the process is complicated, and the requirements for multiple operators are high (Materials Letters 61(2007): 709-714), and the purity are also severely restricted

Method used

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  • Method for solvent-thermally synthesizing nano bismuth oxide single-crystal chips
  • Method for solvent-thermally synthesizing nano bismuth oxide single-crystal chips
  • Method for solvent-thermally synthesizing nano bismuth oxide single-crystal chips

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Embodiment 1

[0018] Take 10ml of 1mol / l. HNO 3 Placed in a beaker, add 1mmol of Bi(NO 3 ) 3 ·5H 2 O, stir, dissolve, then add 2mmol SDBS and 3ml oleic acid, stir evenly, continue to stir and drop NaOH solution to PH≈13, continue to add absolute ethanol to 80% of the closed container of the autoclave, after fully stirring, put The resulting mixture was transferred to an autoclave lined with polytetrafluoroethylene, the autoclave was sealed, and kept at 120°C for 8 hours of reaction. After the reaction, the final product was filtered, then washed several times with deionized water and absolute ethanol to completely remove the surfactant, and dried at 60° C. for 2 hours to obtain 0.224 g of nano-bismuth oxide single chip with a yield of 96 %.

Embodiment 2

[0020] Take 10ml of 0.5mol / l. HNO 3 Placed in a beaker, add 2mmol of Bi(NO 3 ) 3 ·5H 2 O, stir, dissolve, then add 1mmol SDBS and 4ml oleic acid, stir evenly, continue to stir and dropwise add NaOH solution to PH≈13, continue to add absolute ethanol to 80% of the closed container of the autoclave, after fully stirring, put The resulting mixture was transferred to an autoclave lined with polytetrafluoroethylene, the autoclave was sealed, and kept at 120°C for 8 hours of reaction. After the reaction, the final product was filtered, then washed several times with deionized water and absolute ethanol to completely remove the surfactant, and dried at 50° C. for 3 hours to obtain 0.416 g of nano-bismuth oxide single chip with a yield of 91.3 %.

Embodiment 3

[0022] Take 10ml of 1mol / l. HNO 3 Place in a beaker, add 5mmol of Bi(NO 3 ) 3 ·5H 2 O, stir, dissolve, then add 3mmol SDBS and 2ml oleic acid, stir evenly, continue to stir and dropwise add NaOH solution to PH≈10, continue to add absolute ethanol to 90% of the closed container of the autoclave, after fully stirring, put The resulting mixture was transferred to an autoclave lined with polytetrafluoroethylene, the autoclave was sealed, and kept at 120°C for 12 hours of reaction. After the reaction was finished, the final product was filtered, then washed several times with deionized water and absolute ethanol to completely remove the surfactant, and dried at 60°C for 2 hours to obtain a 1.06g (scale) nano-bismuth oxide single chip. The rate is 91%.

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Abstract

The invention discloses a preparation method for nano bismuth oxide single-crystal chips. The method can controllably synthesize a large amount of high-purity monoclinic single-crystal chip-shaped nano bismuth oxide powder by adopting cheap, easily obtained materials and a solvent-thermal synthesization method assisted by the composite surfactant of oleic acid and sodium dodecyl benzene sulfonate. The specific steps are as follows: Bi(NO3)3.5H2O is firstly added into HNO3 solution, and is stirred until being dissolved; the surfactant is then added and uniformly stirred; in the process of continuing stirring, NaOH solution is dripped to regulate the pH value; absolute ethyl alcohol is then added and uniformly stirred; afterwards, the mixture is transferred into a closed container to carry out solvent-thermal reaction; and finally, the reaction product is washed by distilled water and absolute ethyl alcohol and dried, so that nano bismuth oxide single-crystal chips are obtained. The method for preparing nano bismuth oxide single-crystal chips has the advantages of short process flow, simple operation and excellent product properties.

Description

technical field [0001] The invention belongs to the technical field of inorganic material preparation, in particular to a method for solvothermally synthesizing a nano-bismuth oxide single wafer. Background technique [0002] As an important doping material, bismuth oxide is widely used in the fields of microelectronic ceramics, digital storage, optical devices, fine chemicals, pharmaceuticals, and high-temperature superconducting materials. Therefore, the synthesis of nano-bismuth oxide with high purity and uniform morphology is of great significance to improve the performance of bismuth oxide-based functional materials and broaden their applications. [0003] At present, the methods for preparing nano-bismuth oxide mainly include direct high-temperature synthesis of simple substances, chemical precipitation, and pyrolysis of organic precursors. In the direct high-temperature synthesis of simple substances, it is easy to form oxides on the metal surface, which inhibits the...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C30B29/16C30B7/00C30B29/64C01G29/00
Inventor 陈光房国丽王雄
Owner NANJING UNIV OF SCI & TECH
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