SiC (silicon carbide) content standard substance and preparation method thereof

A standard material, silicon carbide technology, applied in the field of analysis and testing, can solve the problems of poor uniformity, poor reliability, inaccurate nominal value, etc., and achieve the effect of strong component designability and good stability

Active Publication Date: 2014-10-15
NO 53 RES INST OF CHINA NORTH IND GRP
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0008] The existing literature on the high-frequency carbon and sulfur analyzer to analyze the standard product for SiC content test is self-made by the experimenter through mixing, and there are problems such as inaccurate nominal value, poor uniformity, and poor reliability.
Clay sintered SiC content standard substance has not been reported

Method used

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  • SiC (silicon carbide) content standard substance and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Silicon carbide content standard material, pre-designed SiC content 80%, SiO 2 Content 10%, Al 2 o 3 Content 10%.

[0024] Silicon carbide pretreatment: silicon carbide with a particle size of 40nm (Shanghai Chaocheng Nano Technology Co., Ltd.) was burned at 600°C for 2h, and [H 2 O:H 2 o 2 (30%): NH 4 OH (27%)=5:2:1] heated and cleaned at (70~80)°C for 20 minutes, then ultrasonically cleaned for 30 minutes, stood for clarification, changed the water for the next rinse, repeated 5 times, and filtered; 2 O:H 2 o 2 (30%): HCl (37%)=6:1:1] heating and cleaning for 20min, ultrasonic cleaning for 30min, filtering; use aqua regia [HCl (37%):HNO 3 (67%)=3:1] Boil for 30min, then ultrasonically clean for 30min, filter; use HF acid and HNO 3 Acid mixture [HF(40%):HNO 3 (67%)=1:1] soaked in 30min, then rinsed with deionized water to neutral; then placed in a drying oven at 90 ° C to dry;

[0025] Preparation of hydrosol gel: Dissolve 40g (0.196 mol) aluminum isopropoxi...

Embodiment 2

[0031] SiC content standard material, pre-designed SiC content 70%, SiO 2 Content 15%, Al 2 o 3 15%.

[0032] The process of silicon carbide purification and value determination is the same as in Example 1. Silicon carbide is Shanghai Chaocheng Nano Technology Co., Ltd., with a particle size of 200nm.

[0033] Material composition: Tetraethyl silicate 52g (0.25 mole), water 85g, polyvinyl butyral 1.2g, isopropanol 85g, SiC70g, aluminum isopropoxide 60g (0.29 mole);

[0034] The sintering conditions are: heating rate 5°C / min, respectively at 150°C (40min heat preservation), 310°C (30min heat preservation), 390°C (30min heat preservation), 710°C (30min heat preservation), 790°C (30min heat preservation), and 860°C (keep warm for 30 minutes);

[0035] Determination of value: use CS844 carbon-sulfur analyzer to determine the value of the standard substance candidate, and the nominal value is 70.1%. F test: 16 bottles were sampled, and each bottle was tested 3 times, F=1.35

Embodiment 3

[0037] SiC content standard material, pre-designed SiC content 60%, SiO 2 Content 18%, Al 2 o 3 twenty two%.

[0038] The process of silicon carbide purification and value determination is the same as in Example 1. Silicon carbide is silicon carbide from Shanghai Chaocheng Nano Technology Co., Ltd., with a particle size of 400nm.

[0039] Material composition: 62.4g (0.3 mole) of tetraethyl orthosilicate, 90g water, 1.3g polyvinyl butyral, 90g isopropanol, 60g SiC, 88g (0.43 mole) aluminum isopropoxide;

[0040] Sintering conditions: Helium protection, heating rate 10°C / min, respectively at 170°C (40min heat preservation), 310°C (30min heat preservation), 400°C (30min heat preservation), 700°C (35min heat preservation), 810°C (30min heat preservation) , 840°C (30 minutes of heat preservation);

[0041] Determination of value: use CS844 carbon-sulfur analyzer to determine the value of the standard substance candidate, and the nominal value is 60.3%. F test: 16 bottles were ...

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Abstract

The invention belongs to the technical field of analytical tests. SiC is used as a main body component, tetraethyl orthosilicate and an aluminium salt are used as auxiliary materials, Al2O3 and SiO2 sol-gel with the SiC mixed evenly is prepared through alkaline accelerating hydrolysis, and an SiC content standard substance is obtained through programmed temperature rising and sintering. The SiC content standard substance is powder formed by the SiC, Al2O3 and SiO2, and the fineness is not higher than 100 mu m; the SiC mass content is in a range of 45%-80%. A preparation method of the standard substance comprises processes of SiC pretreatment, aqueous sol-gel preparation, sintering and value fixation; the standard substance is loose in particle, small in particle size, high in component designability, good in uniformity and stability and applicable to places for instrument calibration, method establishment and the like when a carbon and sulfur analyzer is used for analyzing the SiC content, and a foundation is laid for rapid and accurate tests of the SiC content.

Description

technical field [0001] The invention belongs to the technical field of analysis and testing, and relates to the evaluation technology of material quality standard materials, especially the evaluation technology of SiC content. Background technique [0002] Clay SiC products are made of artificial SiC and clay as a binder. They have excellent properties such as high hardness, high strength, oxidation resistance, corrosion resistance and high heat conduction. They are used in steel, non-ferrous metal smelting, glass cement, petroleum It has been widely used in chemical industry, military industry and other industrial parts and high temperature technology fields. The SiC content in clay SiC products is generally (50-90)%. The SiC content has a direct impact on the performance of the product. From the perspective of product quality control and formulation, the SiC content needs to be strictly controlled, and clay SiC is insoluble and infusible. The characteristics of clay bring...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): G01N1/28G01N21/35
Inventor 柳洪超吴立军鲁毅郭国建尤瑜生刘霞傅兴天
Owner NO 53 RES INST OF CHINA NORTH IND GRP
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