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Controllable method for preparing nano zinc oxide powder

A technology of nano-zinc oxide powder and zinc nitrate, applied in the direction of zinc oxide/zinc hydroxide, etc., can solve the problems of corrosion of reaction equipment, increased production difficulty, rare nano-powder, etc., and achieve good dispersion, uniform particle size and reliable Control and process flow are reasonable and practical

Inactive Publication Date: 2010-06-16
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The nano-zinc oxide of the invention has a low threshold and extremely high gain, and is suitable for short-wave optoelectronic devices, such as ultraviolet emitting devices, ultraviolet laser devices, etc., and plays a very important role in improving the optical recording density and the access speed of optical information , its defect is that there are deficiencies in the selection of raw materials and the process flow, such as the use of zinc chloride in the selection of raw materials, which produces acidic hydrogen chloride gas, which is very corrosive to the reaction equipment; with zinc sulfate as the precursor, due to the sulfate ion The decomposition temperature is as high as 861°C. Low-temperature heat treatment is difficult to remove sulfate ions, and high-temperature heat treatment can easily lead to particle growth, making it difficult to obtain nano-powders with smaller particle sizes; zinc acetate as a raw material makes carbonization in the annealed product more serious ; In addition, the use of ethanol for multiple washings increases the difficulty of production for large-scale processing, and requires the use of vacuum drying, so further improvement is required

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  • Controllable method for preparing nano zinc oxide powder
  • Controllable method for preparing nano zinc oxide powder
  • Controllable method for preparing nano zinc oxide powder

Examples

Experimental program
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Effect test

example 1

[0021] 1. Weigh 8.9247g of zinc nitrate and 6.304g of citric acid, dissolve them in 50mL of deionized water to form a solution of zinc nitrate and citric acid with a molar ratio of 1:1, then stir magnetically for 30 minutes until completely dissolved to form a transparent and colorless solution . Weigh 6g polyethylene glycol 2000, dissolve it in 50mL deionized water to form a 0.3mol / L zinc nitrate solution, stir it magnetically for 30 minutes to form a transparent solution, then add the polyethylene glycol solution to the citric acid solution, the pH The value is 1.

[0022] 2. The mixed solution of zinc nitrate, citric acid, and polyethylene glycol 2000 was transferred to a three-necked flask, stirred in a water bath at 85°C, condensed and refluxed for 4 hours through a condenser, and naturally cooled to room temperature for 4 hours.

[0023] 3. The transparent sol was transferred to a jacketed glass reactor and gelled at 85°C to obtain a colorless transparent gel.

[0024]...

example 2

[0027] 1. Weigh 8.9247g of zinc nitrate and 6.304g of citric acid, dissolve them in 50mL of deionized water to form a solution of zinc nitrate and citric acid, the molar ratio is 1:1.5, and then stir magnetically for 30 minutes until completely dissolved to form a transparent and colorless solution . Weigh 6 g of polyethylene glycol 2000, dissolve it in 50 mL of deionized water to form a 0.3 mol / L zinc nitrate solution, stir it magnetically for 30 minutes to form a transparent solution, and then add the polyethylene glycol solution to the citric acid solution.

[0028] 2. Adjust the pH value to 7 with ammonia water.

[0029] 3. The mixed solution of zinc nitrate, citric acid, and polyethylene glycol 2000 was transferred to a three-necked flask, stirred in an 85°C water bath, condensed and refluxed through a condenser for 4 hours, and naturally cooled to room temperature for 4 hours.

[0030] 4. The transparent sol was transferred to a jacketed glass reactor and gelled at 85°C...

example 3

[0034] 1. Weigh 8.9247g of zinc nitrate and 6.304g of citric acid, dissolve them in 50mL of deionized water to form a solution of zinc nitrate and citric acid, the molar ratio is 1:1.5, and then stir magnetically for 30 minutes until completely dissolved to form a transparent and colorless solution . Weigh 6g polyethylene glycol 2000, dissolve it in 50mL deionized water to form a 0.3mol / L zinc nitrate solution, stir it magnetically for 30 minutes to form a transparent solution, then add the polyethylene glycol solution to the citric acid solution, the pH The value is 1.

[0035] 2. The mixed solution of zinc nitrate, citric acid, and polyethylene glycol 2000 was transferred to a three-necked flask, stirred in a water bath at 85°C, condensed and refluxed for 4 hours through a condenser, and naturally cooled to room temperature for 4 hours.

[0036] 3. The transparent sol was transferred to a jacketed glass reactor and gelled at 85°C to obtain a colorless transparent gel.

[0...

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Abstract

The invention relates to a controllable method for preparing nano zinc oxide powder, which is characterized by adopting the salt of inorganic zinc nitrate and the chelating agent of citric acid which has the complexing function as the raw materials and the ethylene glycol, the polyethylene glycol, or the polyvinyl alcohol as the surfactant. The controllable method for preparing the nano zinc oxide powder specifically comprises the following steps: preparing solution from the zinc nitrate, the citric acid and the surfactant according to a certain molar ratio, reflowing the solution with water bath, aging, gelatinizing, drying and annealing to obtain the nano zinc oxide powder with single component and uniform distribution of the agglomeration-free particle of 20-100 nm. The nano zinc oxide powder has low cost, high quality and high yield, is prepared with simple equipment and can realize the industrial production easily.

Description

technical field [0001] The invention relates to a large-scale controllable preparation method of nano-zinc oxide powder. The nano-zinc oxide powder can be widely used in the fields of varistors, cathodoluminescent materials, transparent conductive materials, gas-sensitive sensors, dye-sensitized solar cells, and the like. Background technique [0002] Due to the diversity of structures and properties, nanomaterials are widely used in new material compounding, catalysis, pressure-sensitive sensors and optoelectronics, which has attracted great attention and interest. Nano-zinc oxide particles generally have a grain size below 100nm, and exhibit many special physical and chemical properties due to the unique size effect, quantum size effect, and surface effect of nanomaterials. Nano-zinc oxide materials are widely used in functional ceramics, daily chemicals, coatings and photoelectric functional devices, and can be used in gas sensors, phosphors, ultraviolet shielding materia...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01G9/02
Inventor 张宇龙杨晔赵俊华宋伟杰谭瑞琴崔平
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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