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Analysis method for impurity elements in tin-oxide-containing nanopowder

A technology of impurity element and analysis method, applied in the field of impurity element analysis in tin oxide-containing nano-powder, can solve the problem that tin oxide-containing nano-powder is not easy to dissolve, and achieve the effect of good application effect, good precision and high accuracy

Inactive Publication Date: 2013-03-27
725TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] The technical problem to be solved by the present invention is to provide a method for analyzing impurity elements in nano-powder containing tin oxide. By selecting the type, dosage and method of reagents for dissolving nano-powder containing tin oxide, the difficulty of dissolving the nano-powder containing tin oxide can be solved. problems; through the reasonable selection of test conditions including acidity conditions and instrument parameter conditions, as well as interference and elimination experiments, the problems of easy hydrolysis of tin and antimony and interference in the test are solved; through the detection limit, precision and recovery of the method A large number of experiments such as testing to determine the accuracy of the built method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0061] 1) The parameters of the instrument are set as follows:

[0062] High frequency power: 1.2KW; cooling air flow: 15L / min; auxiliary air flow: 0.40L / min; atomizing air flow: 0.70L / min; sample flow: 1.2mL / min; stabilization time: 14s; sample lift Time: 20s; atomizer cleaning time: 5s; repeat measurement times: 1 time.

[0063] 2) Test method

[0064] Accurately weigh 0.1000g of the sample, use 1g of sodium hydroxide and 0.5g of sodium peroxide as a mixed solvent, keep it at 580°C for 20min, take it out and cool it to room temperature. After rinsing the outer wall with water, place it in a 250mL beaker with warm water for leaching, rinse the crucible and crucible lid and take it out. Add 20mL of hydrochloric acid to the beaker and heat to dissolve. After cooling, set the volume to a 250mL polytetrafluoroethylene volumetric flask.

[0065] Make a blank solution along with the sample.

[0066] Under selected conditions, measure the blank solution and the standard solutio...

Embodiment 2

[0068] 1) The parameters of the instrument are set as follows:

[0069] High-frequency power: 1.3KW; cooling air flow: 16L / min; auxiliary air flow: 0.60L / min; atomizing air flow: 0.60L / min; sample flow: 1.3mL / min; stabilization time: 20s; sample lifting Time: 12s; atomizer cleaning time: 8s; repeat measurement times: 3 times.

[0070] 2) Test method

[0071] Accurately weigh 1.0000g sample, use 5g sodium hydroxide and 5g sodium peroxide as a mixed flux, keep it at 610°C for 40min, take it out and cool it to room temperature. After rinsing the outer wall with water, place it in a 250mL beaker with warm water for leaching, rinse the crucible and crucible lid and take it out. Add 40mL hydrochloric acid to the beaker and heat to dissolve. After cooling, set the volume to a 250mL polytetrafluoroethylene volumetric flask.

[0072] Make a blank solution along with the sample.

[0073]Under selected conditions, measure the blank solution and the standard solution, establish a cal...

Embodiment 3

[0075] 1) The parameters of the instrument are set as follows:

[0076] High-frequency power: 1.5KW; cooling air flow: 18L / min; auxiliary air flow: 0.8L / min; atomizing air flow: 0.80L / min; sample flow: 1.5mL / min; stabilization time: 17s; sample lifting Time: 17s; atomizer cleaning time: 10s; repeat measurement times: 2 times.

[0077] 2) Test method

[0078] Accurately weigh 0.4000g of the sample, use 4g of sodium hydroxide and 3g of sodium peroxide as a mixed flux, keep it warm at 650°C for 35min, take it out and cool it to room temperature. After rinsing the outer wall with water, place it in a 250mL beaker with warm water for leaching, rinse the crucible and crucible lid and take it out. Add 30mL hydrochloric acid to the beaker and heat to dissolve. After cooling, set the volume to a 250mL polytetrafluoroethylene volumetric flask.

[0079] Make a blank solution along with the sample.

[0080] Under selected conditions, measure the blank solution and the standard soluti...

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Abstract

The invention provides an analysis method for impurity elements in tin-oxide-containing nanopowder, and aims to solve the problem that the tin-oxide-containing nanopowder is not easy to decompose by adopting an inductive coupling plasma atomic emission spectroscopy method and selecting the reagent type, dosage and method adopted for the dissolving sample of the tin-oxide-containing nanopowder; experiment interference is eliminated by selecting acid conditions and instrument parameters, thereby solving the difficulties that tin and antimony are easy to hydrolyze, interference elements are more and difficult to test and test background value is high and the like; with the method, the detection limit is below 0.003%, the relative standard deviation is within 10%, the method correlation coefficient is above 0.998, and the recovery rate is between 85% and 130%; and the analysis speed is high, the data is accurate, the errors meet conventional requirements, and the quality and the performance stability of the tin-oxide-containing nanopowder can be ensured.

Description

technical field [0001] The invention relates to a material analysis and testing technology, in particular to a method for analyzing impurity elements in tin oxide-containing nanopowder. Background technique [0002] With the rapid development of science and technology, nanomaterials have been widely used because of their special and excellent properties. Nano powder containing tin oxide includes nano powder containing tin oxide, nano powder containing indium oxide and tin oxide (ie ITO powder), nano powder containing tin oxide and antimony oxide, nano powder containing indium oxide, tin oxide and antimony oxide, etc. These tin oxide-containing nanopowders have excellent properties and are widely used. For example, ITO has excellent electrical conductivity and visible light transparency. As an important electronic material product in today's information industry, it is mainly used in liquid crystal displays, solar cells, solid electrochromic (EC) devices, electromagnetic shi...

Claims

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Application Information

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IPC IPC(8): G01N21/71
Inventor 杜米芳高灵清杜丽丽
Owner 725TH RES INST OF CHINA SHIPBUILDING INDAL CORP
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