Preparation method of hydroxyl gallium oxide nanometer crystal

A gallium oxyhydroxide, nanocrystal technology, applied in chemical instruments and methods, nanotechnology, nanotechnology, etc., can solve the problems of limiting the synthesis size and morphology of GaOOH crystals, the lack of efficient progress of GaOOH, and harsh conditions. , to achieve the effect of low cost, simple process and good repeatability

Inactive Publication Date: 2012-11-21
JILIN UNIV
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  • Abstract
  • Description
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  • Application Information

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Problems solved by technology

[0004] At present, due to the limitations of experimental conditions and technical means, the preparation of GaOOH has not progressed efficiently, and most of the work has focused on adjusting the pH value in the hydrothermal synthesis to inhibit hydrolysis and ultimately control the morphology and size of the grown GaOOH ( J Cryst Growth, 2005, 280: 99-106.; J Cryst Growth, 2008, 8 (4): 1282-1287.), the steps are extremely loaded down with trivial details; It is completed in a high vacuum environment, the conditions are very harsh, and the yield of the prepared samples is also very low. These reasons greatly limit the research on the size and morphology of GaOOH crystal synthesis.
[0005] The preparation of gallium oxyhydroxide (GaOOH) nanocrystals by liquid-liquid interfacial reaction has not yet been reported

Method used

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  • Preparation method of hydroxyl gallium oxide nanometer crystal
  • Preparation method of hydroxyl gallium oxide nanometer crystal
  • Preparation method of hydroxyl gallium oxide nanometer crystal

Examples

Experimental program
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Effect test

Embodiment 1

[0032] Example 1 The best overall process for preparing GaOOH nano-hexagonal prisms.

[0033] Using high-purity gallium chloride, benzene, CTAB and deionized aqueous solution as raw materials, first dissolve gallium chloride in benzene to prepare a benzene saturated solution of gallium chloride; dissolve 0.0546g CTAB in 30ml of deionized water to prepare 5mmol / L CTAB aqueous solution. Use a pipette to measure 1.5ml of the benzene saturated solution of gallium chloride prepared in advance into a clean beaker, and dilute it to 15ml with benzene. Afterwards, the beaker was placed in an ultrasonic instrument for ultrasonic treatment, and the prepared 5 mmol / L CTAB aqueous solution was dripped dropwise with a syringe during the ultrasonic treatment. When the upper layer of benzene solution is brown and the lower layer of aqueous solution is colorless and transparent and does not change any more, take out the beaker, pour the liquid in the beaker into a self-made polytetrafluoroeth...

Embodiment 2

[0036] Example 2 The whole process of preparing GaOOH nanocrystals.

[0037] Using high-purity gallium chloride, benzene, CTAB and deionized aqueous solution as raw materials, first dissolve gallium chloride in benzene to prepare a benzene saturated solution of gallium chloride; dissolve 0.1092g CTAB in 30ml of deionized water to prepare 10mmol / L CTAB aqueous solution. Use a pipette to measure 1.5ml of the benzene saturated solution of gallium chloride prepared in advance into a clean beaker, and dilute it to 16.5ml with benzene. Afterwards, the beaker was placed in an ultrasonic instrument for ultrasonication, and the prepared 10 mmol / L CTAB aqueous solution was dripped dropwise with a syringe during the ultrasonication process. When the benzene solution in the upper layer is brown and the aqueous solution in the lower layer is colorless and transparent and does not change any more, take out the beaker, pour the liquid in the beaker into a self-made polytetrafluoro reactor a...

Embodiment 3

[0039] Example 3 The whole process of preparing GaOOH nanocrystals.

[0040] Using high-purity gallium chloride, benzene, CTAB and deionized aqueous solution as raw materials, first dissolve gallium chloride in benzene to prepare a benzene saturated solution of gallium chloride; dissolve 1.092g CTAB in 30ml of deionized water to prepare 100mmol / L CTAB aqueous solution. Use a pipette to measure 1.5ml of the benzene saturated solution of gallium chloride prepared in advance into a clean beaker, and dilute it to 15ml with benzene. Afterwards, the beaker was placed in an ultrasonic instrument for ultrasonication, and the prepared 100 mmol / L CTAB aqueous solution was dripped dropwise with a syringe during the ultrasonication process. When the benzene solution in the upper layer is brown and the aqueous solution in the lower layer is colorless and transparent and does not change any more, take out the beaker, pour the liquid in the beaker into a self-made polytetrafluoro reactor an...

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Abstract

The invention relates to a preparation method of hydroxyl gallium oxide nanometer crystal, and belongs to the technical field of preparation of a nanometer material of oxyhydroxide. The preparation method comprises the following steps of: dripping a deionized water solution of CTAB (cetyltrimethyl ammonium bromide) into a benzene solution of gallium chloride under an ultrasonic environment by the adoption of a principle of a liquid-liquid interface reaction, putting the mixed solution into a reaction kettle to carrying out heating reaction, and obtaining a sample of white powders. The hydroxyl gallium oxide is the raw material for compounding gallium nitride and gallium oxide, and the microcosmic morphological feature of the hydroxyl gallium oxide has very important influence on the performances of the prepared gallium nitride and gallium oxide. The hydroxyl gallium oxide nanometer crystal, prepared by the method provided by the invention, is prism-shaped, and has the characteristics of smooth surface, complete shape, uniform size, etc. The preparation method, provided by the invention, conquers the shortcomings that gallium chloride is very easy to absorb water and cause deliquescence, and abandons the complicated step that the pH value must be regulated in the past and does not need the vacuum environment; and has the advantages of simplicity in operation, high yield, little energy consumption, high repeatability and the like.

Description

technical field [0001] The invention belongs to the technical field of preparing IIIA group oxyhydroxide nanomaterials, in particular to a simple and efficient method for preparing gallium oxyhydroxide nanocrystals. Background technique [0002] Due to their unique properties such as small size effect, surface effect, quantum size effect, and macroscopic quantum tunneling effect, nanomaterials have characteristics that ordinary materials do not have in terms of light, electricity, magnetism, and sensitivity. Therefore, nanomaterials have been widely used in recent years. For example, it has been widely used in optical materials, electronic materials, magnetic materials, sintering of high-density materials, catalysis, sensing, and ceramic toughening. In recent years, compound semiconductor materials of gallium metal in group IIIA have been widely used in the fields of electronics, optoelectronics and electrochemistry. Gallium oxide (Ga 2 o 3 ) has a bandgap E at room temp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G15/00B82Y30/00
Inventor 张剑史立慧吴思
Owner JILIN UNIV
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