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Method for measuring content of free boron oxide in boron nitride

A boron nitride and boron oxide technology, applied in the chemical field, can solve the problems of high detection cost, complex maintenance and repair requirements, and high equipment cost, and achieve the effects of simple operation steps, low detection cost and accurate data.

Inactive Publication Date: 2016-03-02
FUNIK ULTRAHARD MATERIAL
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Among them, boron oxide is the main impurity in boron nitride. During the artificial synthesis of boron nitride, boron oxide will react with the catalyst for synthesis under high temperature and pressure, thereby reducing the synthesis efficiency.
[0003] At present, the methods for detecting the purity of boron nitride and the content of free boron oxide in boron nitride mainly include X-ray diffraction characterization, scanning electron microscope characterization, laser particle size analysis, and specific surface area measurement. The detection process is complicated and the detection cost is high. For example, Scanning electron microscope characterization requires steps such as making standard observation sheets for the material to be tested in advance, and the cost of equipment is high, and maintenance requirements are complicated

Method used

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  • Method for measuring content of free boron oxide in boron nitride

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Embodiment 1

[0023] This embodiment provides a method for detecting the content of free boron oxide in boron nitride, which specifically includes the following steps:

[0024] Step 1, first use a drying oven to bake 5g of hexagonal boron nitride to constant weight; then weigh 1.0478g of the baked hexagonal boron nitride and place it in 5mL of dilute hydrochloric acid solution with a mass percentage of 20% Carry out acid leaching for 20 minutes to obtain acid leaching turbid solution; then place the acid leaching turbid solution on an electric furnace and heat and boil for 50 minutes, after cooling, filter and wash to obtain acid leaching filtrate, wherein the purpose of heating and boiling is to remove the Volatile components such as carbon dioxide in the acid leaching turbid solution.

[0025] Step 2, add 2mL indicator in the described acid leach filtrate of 180mL, wherein said indicator is by volume ratio be that the mass percent of 1:3:1 is 5% bromocresol green solution, methyl red solu...

Embodiment 2

[0030] This embodiment provides a method for detecting the content of free boron oxide in boron nitride. The specific steps are roughly the same as those in Example 1, except that:

[0031] The present embodiment is to measure the content of free boron oxide in the cubic boron nitride of 1.0396g;

[0032] Adopting 5mL mass percent in the described step 1 is that the dilute sulfuric acid solution of 30% carries out acid leaching to 1.0396g described cubic boron nitride;

[0033] In the said step 2, the dilute sulfuric acid solution with a mass percentage of 30% and the potassium hydroxide standard solution with a concentration of 2mol / L are used successively to neutralize and titrate the acid leaching filtrate, and then heated and boiled in an electric furnace for 20 minutes to obtain a boric acid mixture ;

[0034] In the step 3, the complex mixed solution of the potassium hydroxide standard solution with a concentration of 2mol / L is used to neutralize to present grayish blue...

Embodiment 3

[0038] This embodiment provides a method for detecting the content of free boron oxide in boron nitride. The specific steps are roughly the same as those in Example 1, except that:

[0039] In this embodiment, the content of free boron oxide in the boron nitride mixture composed of 1.0284g hexagonal boron nitride and cubic boron nitride is determined;

[0040] In the first step, 5 mL of dilute sulfuric acid solution with a volume ratio of 1:1 and a mass fraction of 30% is used for acid leaching the boron nitride mixture;

[0041] The content of free boron oxide in the hexagonal boron nitride detected in this embodiment is determined to be 0.15% by experiment.

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Abstract

The invention provides a method for measuring the content of free boron oxide in boron nitride. The method specifically comprises the following steps: boron nitride is subjected to acid pickling in an acid solution, filtering and acid-base neutralization titration, a neutral mixed solution is prepared and subjected to complexometric titration and acid-base neutralization titration by adopting an alcohol complexing agent and a strong base standard solution respectively, the volume difference of the consumed strong base standard solution is obtained through a blank test, and an established unary linear quantitative detection model for free boron oxide in boron nitride is used for calculation, so that the content of free boron oxide in boron nitride is obtained. The method has simple steps and high detection result accuracy.

Description

technical field [0001] The invention relates to a detection method in the field of chemistry, in particular to a method for detecting the content of free boron oxide in boron nitride. Background technique [0002] Boron nitride is widely used in solid lubrication, casting molding, composite ceramics, electrical insulation, ultra-high thermal conductivity, instrument coating and aerospace because of its good lubricity, electrical insulation, thermal conductivity and chemical corrosion resistance. The purity of boron nitride often affects the quality of processed products and the quality of products after silicon nitride crystal transformation. Among them, boron oxide is the main impurity in boron nitride. During the artificial synthesis of boron nitride, boron oxide will react with the catalyst for synthesis under high temperature and pressure, thereby reducing the synthesis efficiency. [0003] At present, the methods for detecting the purity of boron nitride and the conten...

Claims

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Application Information

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IPC IPC(8): G01N31/16G01N21/79
CPCG01N31/16G01N21/79
Inventor 李瑞歌
Owner FUNIK ULTRAHARD MATERIAL
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