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Preparation method of gallium oxide hydroxide nano-crystals

A technology of gallium oxyhydroxide and nanocrystals, which is applied in the field of preparation of IIIA group oxyhydroxide nanomaterials, can solve the problems of GaOOH preparation work without efficient progress, harsh conditions, and low sample yield, achieving low cost and inhibited reaction The effect of speed and simple preparation method

Inactive Publication Date: 2013-03-20
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] In recent years, 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 GaCl 3 The hydrolysis method is used to synthesize GaOOH, and the pH value of the solution is adjusted in the process to inhibit hydrolysis and finally control the morphology and size of the GaOOH it grows (J.Cryst.Growth.280,99-1062005.; J.Cryst.Growth. 8(4),1282-1287(2008).), the steps are extremely cumbersome; and because GaCl 3 It is easily hydrolyzed in the air, so the preparation process needs to be completed in a very high vacuum environment, the conditions are very harsh, and the yield of the prepared samples is also very low; at the same time, it is known from the previous literature research that there is no one in the synthesis of GaOOH Exceptionally, water is chosen to provide the hydroxyl groups required for the reaction, which for GaCl 3 For this substance that reacts rapidly with water, it has caused more difficulties in controlling the shape and size of GaOOH
[0005] The report of GaOOH (gallium oxyhydroxide) nanocrystals and GaOOH (gallium oxyhydroxide) nanobrush crystals prepared by alcoholysis has not yet appeared.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Embodiment 1 The whole process of preparing the best GaOOH nano brush.

[0028] Using high-purity gallium chloride, benzene, and methanol as raw materials, first dissolve gallium chloride in benzene to prepare a benzene-saturated solution of gallium chloride. Use a pipette to measure 1.5ml of the benzene saturated solution of gallium chloride prepared in advance and put it into a clean beaker, dilute it to 12ml with benzene to obtain the dilution. Afterwards, the beaker was placed in an ultrasonic instrument for ultrasonic treatment, and methanol was dropped into the diluent with a syringe at the same time during the ultrasonic treatment. Stop ultrasound when 25ml of methanol is added (dropping time is about 2 hours), take out the beaker, pour the liquid in the beaker into a self-made (40ml) polytetrafluoroethylene reaction kettle, seal and heat at 160°C for 48h. After the reaction, when the temperature of the reaction kettle dropped to room temperature, the liquid in ...

Embodiment 2

[0030]Example 2 The whole process of preparing GaOOH nanocrystals.

[0031] Using high-purity gallium chloride, benzene, and methanol as raw materials, first dissolve gallium chloride in benzene to prepare a benzene-saturated solution of gallium chloride. Use a pipette to measure 1.5ml of the benzene saturated solution of gallium chloride prepared in advance and put it into a clean beaker, dilute it to 12ml with benzene to obtain the dilution. Afterwards, the beaker was placed in an ultrasonic instrument for ultrasonication, and methanol was dropped into the diluent dropwise with a syringe at the same time during the ultrasonication process. Stop ultrasound when 25ml of methanol is added (dropping time is about 2 hours), take out the beaker, pour the liquid in the beaker into a self-made (40ml) Teflon reaction kettle, seal and heat at 160°C for 12h. After the reaction, when the temperature of the reaction kettle dropped to room temperature, the liquid in the kettle was taken ...

Embodiment 3

[0033] Example 3 The whole process of preparing GaOOH nanocrystals.

[0034] Using high-purity gallium chloride, benzene, and methanol as raw materials, first dissolve gallium chloride in benzene to prepare a benzene-saturated solution of gallium chloride. Use a pipette to measure 1.5ml of the benzene saturated solution of gallium chloride prepared in advance and put it into a clean beaker, dilute it to 12ml with benzene to obtain the dilution. Afterwards, the beaker was placed in an ultrasonic instrument for ultrasonication, and methanol was dropped into the diluent dropwise with a syringe at the same time during the ultrasonication process. Stop ultrasound when 25ml of methanol is added (dropping time is about 1.5 hours), take out the beaker, pour the liquid in the beaker into a self-made (40ml) Teflon reaction kettle, seal and heat at 180°C for 12h. After the reaction, when the temperature of the reaction kettle dropped to room temperature, the liquid in the kettle was tak...

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Abstract

The invention provides a preparation method of gallium oxide hydroxide nano-crystals and belongs to the technical field of preparation of gallium oxide hydroxide nano-materials. According to the reaction kettle sealed heating alcoholysis method and the liquid-liquid interface reaction principle, through gradually dropwise adding methanol into a gallium oxide benzene solution disposed in an ultrasonic appliance and then enabling the mixed solution to be subjected to sealed low-temperature heating reaction, the prepared sample is white powders. The crystals in nano brush shape and which in smooth in surface, complete in shape and uniform in size are prepared under a preferable condition. According to the invention, the synthesis of gallium oxide hydroxide nano-crystals is carried out by using the alcoholysis reaction method for the first time, the disadvantage that the gallium oxide is very liable to absorb water and be decomposed by moisture is overcome, the operations are finished without adjusting pH (potential of hydrogen) and without using a vacuum condition, the reaction speed of the gallium oxide is significantly inhibited, so that the shape of the generated gallium oxide hydroxide is more easy to control. In addition, the product prepared by the method provided by the invention is high in yield and high in purity; and the preparation method is simple, excellent in repeatability and low in cost.

Description

technical field [0001] The invention belongs to the field of preparation of IIIA group oxyhydroxide nanomaterials, and particularly provides a novel, simple and efficient method for preparing gallium oxyhydroxide (GaOOH) nanocrystals. Background technique [0002] Due to its 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 received more and more attention and applications 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. [0003] In recent years, compound semiconductor materials of gallium metal in group IIIA have been widely used in the fields of electronics, optoelectronics and electrochemistry...

Claims

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Application Information

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IPC IPC(8): C01G15/00B82Y30/00
Inventor 张剑史立慧吴思崔啟良
Owner JILIN UNIV
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