CN104101526B - A kind of carborundum content standard substance and preparation method thereof - Google Patents
A kind of carborundum content standard substance and preparation method thereof Download PDFInfo
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- CN104101526B CN104101526B CN201410341379.2A CN201410341379A CN104101526B CN 104101526 B CN104101526 B CN 104101526B CN 201410341379 A CN201410341379 A CN 201410341379A CN 104101526 B CN104101526 B CN 104101526B
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Abstract
The invention belongs to analysis and testing technology field.With SiC for bulk composition, with tetraethyl orthosilicate, aluminium salt for supplies, adopt alkalescence to accelerate hydrolysis preparation and uniformly blend the Al of SiC2O3、SiO2Collosol and gel, temperature programming sintering obtains.The carborundum content standard substance that the present invention relates to, for SiC, Al2O3、SiO2The powder body of composition, fineness is not more than 100um；SiC mass content is between (45-80) %.Its preparation method, prepare including carborundum pretreatment, aqueous sol-gel, sinter and this standard substance of definite value process, granule particle diameter loose, little, composition designability is strong, uniformity, good stability, when analyzing SiC content suitable in carbon and sulfur analytical instrument, the occasion such as the foundation of the calibration of instrument and method, quick and precisely tests for carborundum content and lays the foundation.
Description
Technical field
The invention belongs to analysis and testing technology field, relate to material amount standard substance assessment technique, the assessment technique of special stunt SiC content.
Background technology
Clay SiC goods are with artificial SiC for raw material, make as bonding agent with clay, there is the excellent properties performances such as hardness height, intensity height, antioxidation, corrosion-resistant and high conduction of heat, be widely applied in the industry parts such as iron and steel, non-ferrous metal metallurgy, glass cement, petrochemical industry, military project and high-temperature technology field.In clay SiC goods, SiC content is generally (50～90) %, the performance of goods is had direct impact by SiC content, from the quality control of product and formula, SiC content is to need strict control, and the analysis that the feature of clay SiC indissoluble infusibility gives its SiC content brings the problem such as difficulty and test result poor reproducibility, SiC content analysis method fast and accurately of setting up is the clay SiC problem analyzing that test industry is to be solved.
High-frequency induction burning infrared method carbon determination quick and precisely, is current a kind of universally recognized method in the world.In in clay SiC, only SiC contains carbon, and the carbon content that high frequency carbon and sulfur analytical instrument is analyzed in clay SiC goods therefore can be adopted to obtain the content of SiC in goods.In the analysis of high-frequency induction burning infrared method carbon determination, it is necessary to adopt standard substance to set up working curve, it is contemplated that the impact of matrix, analyzing clay SiC needs the standard substance adopting composition similar to set up working curve to guarantee the reliability of result.
(Shandong is metallurgical for Wei Chunyu etc. " high frequency carbon sulfur method measures SiC in carborundum ", 2003,25 (2): 59-60) adopting homemade standard sample when calibrating carbon and sulfur analytical instrument, standard sample preparation is as follows: take the clay (SiO being substantially free of Caustic soda2Content about 50%, Al2O3It is about 40%), mix with SiC after 950 DEG C of calcination 1h, make the standard sample of SiC content 70%.
Du Jianmin etc. " high frequency infrared ray carbon sulphur analyser measures iron runner material Free Carbon and carborundum " (metallurgical analysis, 2001,21 (2): 60-61) form basically identical in order to ensure standard sample and sample, adopt clay to do matrix, add carborundum and carry out calibration instrument.
Zheng Xunyan etc. " high frequency-infrared carbon sulfur instrument measures the SiC in carborundum " (Chemical Engineer, 2006 (5): 36) the standard sample preparation of SiC content is described, its process is as follows: according to the analysis method of SiC in GB/T3045-2003, the SiC that content is more than 99.0% is carried out pretreatment, the SiC after process and the pure SiO dried2Be configured to SiC content respectively 90.00%, 80.00%, 70.00%, 60.00%, 50.00%, 40.00% sample, weigh accurately to 0.001g during preparation, fully mix.
Domestic Gansu Quarantine Bureau have developed GSB02-1344-2001-C-1 (SiC content 98.73%, unreceipted total carbon content), GSB02-1344-2001-C-2 (SiC content 88.76%, unreceipted total carbon content), its preparation method adopts silicon-carbon heat source response, and this method is the method that current commercial production is extensively used.Analyze SiC refractory material time and improper.
Existing document about high frequency carbon and sulfur analytical instrument analyze SiC content test standard substance, be experimenter pass through blend homemade, there is the problems such as nominal value inaccuracy, lack of homogeneity, poor reliability.Vitrified bond SiC content standard substance have not been reported.
Summary of the invention
It is an object of the invention to provide the standard substance of one group of SiC content, the preparation method simultaneously also providing for this standard substance.
The object of the present invention is achieved like this, with SiC for bulk composition, with tetraethyl orthosilicate, aluminium salt for supplies, adopts alkalescence to accelerate hydrolysis preparation and uniformly blends the Al of SiC2O3、SiO2Collosol and gel, temperature programming sintering obtains uniform, stable SiC content standard substance.
The carborundum content standard substance that the present invention relates to, for SiC, Al2O3、SiO2The powder body of composition, fineness is not more than 100um；SiC mass content is between (45-80) %.
The preparation method of the carborundum content standard substance that the present invention relates to, prepares including carborundum pretreatment, aqueous sol-gel, sinters and definite value process, concrete steps:
1) carborundum pretreatment: adopt soda acid washing method that the dust of silicon carbide, impurity are processed；
2) prepared by aqueous sol-gel: prepare the hydrosol by tetraethyl orthosilicate and aluminium salt, and silicon carbide powder adds mix homogeneously in the hydrosol and obtains gel, and desiccant gel obtains precursor A；Described aluminium salt is aluminum chloride or aluminum isopropylate.；
3) sintering: precursor A temperature programming is sintered, 5 DEG C/min-10 DEG C/min of heating rate；Respectively at 150 DEG C～170 DEG C, 290 DEG C～310 DEG C, 390 DEG C～410 DEG C, 690 DEG C～710 DEG C, 790 DEG C～810 DEG C, 840 DEG C～860 DEG C, insulation of each stage 30min～40min, cooling obtains fluffy powder body, and ground 100um sieves, and obtains SiC content standard substance material standed for B；
4) definite value: to SiC content standard substance material standed for B definite value, obtain the standard substance of expection SiC content.
The preparation method of the carborundum content standard substance that the present invention relates to, prepares including carborundum pretreatment, aqueous sol-gel, sinters and definite value process, and described sintering process carries out under noble gas is protected.
The preparation method of the carborundum content standard substance that the present invention relates to, the mol ratio of the positive esters of silicon acis of aqueous sol-gel preparation process and aluminium salt is between 0.85～1.11.
The preparation method of the carborundum content standard substance that the present invention relates to, prepares including carborundum pretreatment, aqueous sol-gel, sinters and definite value process, and silicon carbide powder particle diameter used is not more than 500nm.
The carborundum content standard substance that the present invention relates to, granule particle diameter loose, little, composition designability is strong, uniformity, good stability, when analyzing SiC content suitable in carbon and sulfur analytical instrument, the occasion such as the foundation of the calibration of instrument and method, quick and precisely tests for carborundum content and lays the foundation.
Detailed description of the invention
Technical scheme invention related to below in conjunction with specific embodiment is described further, but not as the restriction of the particular content that invention relates to technical scheme, can prepare, by component ratio adjustment, the standard substance that carborundum content is different.
Embodiment one
Carborundum content standard substance, pre-designed SiC content 80%, SiO2Content 10%, Al2O3Content 10%.
Carborundum pretreatment: the carborundum (Shanghai Chao Cheng nanosecond science and technology company limited) of particle diameter 40nm is in 600 DEG C of calcination 2h, with [H2O:H2O2(30%): NH4OH (27%)=5:2:1] heated wash 20min, then ultrasonic cleaning 30min at (70～80) DEG C, change water after standing clarification and rinse next time, repeat 5 times, filter；With [H2O:H2O2(30%): HCl (37%)=6:1:1] heated wash 20min, ultrasonic cleaning 30min, filters；With chloroazotic acid [HCl (37%): HNO3(67%)=3:1] boil 30min, then ultrasonic cleaning 30min, filters；With HF acid and HNO3The mixed liquor [HF (40%): HNO of acid3(67%)=1:1] middle immersion 30min, then with deionized water rinsing to neutral；It is subsequently placed in drying baker to dry in 90 DEG C of conditions；
Prepared by aqueous sol-gel: be dissolved in 80g isopropanol by 40g (0.196 mole) aluminum isopropylate., 34.7g (0.167 mole) tetraethyl orthosilicate, 1g polyvinyl butyral, the pretreated SiC powder of 80g, ultrasonic disperse 40min is added to solution；Adding 40g water, warming-in-water, to 70 DEG C, reaches 9 with the adjustment of analytical pure (AR) ammonia to system pH, insulated and stirred 2 hours；Regulate pH with ammonia and obtain gel to 12；Being placed in drying baker by gel, under 120 DEG C of conditions, dry 30min, obtains precursor A；
Sintering: adopt temperature programming that presoma is sintered; argon shield; 10 DEG C/min of programming rate, respectively at 150 DEG C (insulation 30min), 290 DEG C (insulation 40min), 410 DEG C (insulation 30min), 690 DEG C (insulation 40min), 800 DEG C (insulation 40min), 840 DEG C (insulation 35min)；It is down to room temperature with stove, with agate mortar to the ground 100um sieve of sinter, obtains standard substance material standed for B；
Definite value: with CS844 carbon and sulfur analytical instrument to standard substance material standed for definite value, material standed for sample 1g, iron powder 0.5g, tungsten stannum cosolvent 1.5g, oxygen-enriched combusting time 1min.Randomly selecting 16 bottles of standard sample, make 3 times for every bottle, its data are as follows:
Carry out F inspection, F=1.28 < F (0.05,15,32)=1.99, it was shown that this Certified Reference Material Homogeneity is good.
Randomization, carries out 10 average value measured 79.4%, and namely nominal value is 79.4%.
Embodiment two
SiC content standard substance, pre-designed SiC content 70%, SiO2Content 15%, Al2O315%.
Purification of silicon carbide and definite value process are with embodiment one.Carborundum is Shanghai Chao Cheng nanosecond science and technology company limited, particle diameter 200nm.
Material forms: tetraethyl orthosilicate 52g (0.25 mole), water 85g, polyvinyl butyral 1.2g, isopropanol 85g, SiC70g, aluminum isopropylate. 60g (0.29 mole)；
Sintering condition is: 5 DEG C/min of programming rate, respectively at 150 DEG C (insulation 40min), 310 DEG C (insulation 30min), 390 DEG C (insulation 30min), 710 DEG C (insulation 30min), 790 DEG C (insulation 30min), 860 DEG C (insulation 30min)；
Definite value: with CS844 carbon and sulfur analytical instrument to standard substance material standed for definite value, nominal value is 70.1%.F checks: sample 16 bottles, tests 3 times for every bottle, F=1.35 < F (0.05,15,32)=1.99, it was shown that this Certified Reference Material Homogeneity is good.
Embodiment three
SiC content standard substance, pre-designed SiC content 60%, SiO2Content 18%, Al2O322%.
Purification of silicon carbide and definite value process are with embodiment one.Carborundum is carborundum is Shanghai Chao Cheng nanosecond science and technology company limited, particle diameter 400nm.
Material forms: tetraethyl orthosilicate 62.4g (0.3 mole), water 90g, polyvinyl butyral 1.3g, isopropanol 90g, SiC60g, aluminum isopropylate. 88g (0.43 mole)；
Sintering condition: helium is protected; 10 DEG C/min of programming rate, respectively at 170 DEG C (insulation 40min), 310 DEG C (insulation 30min), 400 DEG C (insulation 30min), 700 DEG C (insulation 35min), 810 DEG C (insulation 30min), 840 DEG C (insulation 30min)；
Definite value: with CS844 carbon and sulfur analytical instrument to standard substance material standed for definite value, nominal value is 60.3%.F checks: sample 16 bottles, tests 3 times for every bottle, F=1.76 < F (0.05,15,32)=1.99, it was shown that this Certified Reference Material Homogeneity is good.
Embodiment four
Carborundum content standard substance, pre-designed SiC content 50%, SiO2Content 25%, Al2O3Content 25%.
Carborundum pretreatment definite value is with embodiment one；Carborundum is Weifang Kingdom Corp., particle diameter 200nm.
Prepared by aqueous sol-gel:
Al2O3Colloidal sol: by 118.4g (0.45mol) AlCl3·6H2O dissolves in 225mL water, stirs and add 5g (CH under room temperature2)6N4, stir the transparent Al of 20min2O3Colloidal sol；
SiO2Colloidal sol: 86.7g (0.417 mole) silester, 25mL ethanol, 200mL distilled water mix homogeneously, obtain SiO by analytical pure (AR) ammonia regulation system to 9,60 DEG C of mechanical agitation 200min of pH value2Colloidal sol；
By Al2O3Colloidal sol, SiO2Mix homogeneously, adds 50g (1.25 moles) SiC powder processed, and 70 DEG C of stirring 20min make mix homogeneously, and room temperature is placed 48h and obtained gel, and 120 DEG C of dry 30min obtain precursor A；
Sintering: adopt temperature programming that presoma is sintered; argon shield; 5 DEG C/min of programming rate; respectively at 160 DEG C (insulation 35min), 310 DEG C (insulation 35min), 410 DEG C (insulation 35min), 710 DEG C (insulation 30min), 800 DEG C (insulation 35min), 850 DEG C (insulation 30min); it is down to room temperature with stove; with agate mortar to the ground 100um sieve of sinter, obtain standard substance material standed for B；
Definite value: with CS844 carbon and sulfur analytical instrument to standard substance material standed for definite value, nominal value is 49.9%.F checks: sample 16 bottles, tests 3 times for every bottle, F=1.25 < F (0.05,15,32)=1.99, it was shown that this Certified Reference Material Homogeneity is good.
Embodiment five
Carborundum content standard substance, pre-designed SiC content 45%, SiO2Content 30%, Al2O3Content 25%.
Carborundum pretreatment definite value is with embodiment one；Carborundum is Weifang Kingdom Corp., particle diameter 500nm.
Al2O3Colloidal sol material amounts is: 118.4g (0.45mol) AlCl3·6H2O, distilled water 225mL, 5g (CH2)6N4；The Al that stirring 20min is transparent2O3Colloidal sol；
SiO2Colloidal sol material amounts is: tetraethyl orthosilicate 104g (0.5 mole), ethanol 30mL, distilled water 250mL；Carborundum is Weifang Kingdom Corp., particle diameter 500nm, and consumption is 45g.
Sintering condition: argon shield; 10 DEG C/min of programming rate, respectively at 170 DEG C (insulation 40min), 300 DEG C (insulation 30min), 410 DEG C (insulation 40min), 690 DEG C (insulation 30min), 810 DEG C (insulation 30min), 840 DEG C (insulation 40min).
Definite value: with CS844 carbon and sulfur analytical instrument to standard substance material standed for definite value, nominal value is 45.1%.F checks: sample 16 bottles, tests 3 times for every bottle, F=1.86 < F (0.05,15,32)=1.99, it was shown that this Certified Reference Material Homogeneity is good.
Claims (4)
1. a preparation method for carborundum content standard substance, prepares including carborundum pretreatment, aqueous sol-gel, sinters and definite value process, concrete steps:
1) carborundum pretreatment: adopt soda acid washing method that the dust of silicon carbide, impurity are processed；
2) prepared by aqueous sol-gel: prepare the hydrosol by tetraethyl orthosilicate and aluminium salt, and silicon carbide powder adds mix homogeneously in the hydrosol and obtains gel, and desiccant gel obtains precursor A；Described aluminium salt is aluminum chloride or aluminum isopropylate.；
3) sintering: precursor A temperature programming is sintered, 5 DEG C/min-10 DEG C/min of heating rate；Respectively at 150 DEG C～170 DEG C, 290 DEG C～310 DEG C, 390 DEG C～410 DEG C, 690 DEG C～710 DEG C, 790 DEG C～810 DEG C, 840 DEG C～860 DEG C, insulation of each stage 30min～40min, cooling obtains fluffy powder body, and ground 100um sieves, and obtains carborundum content standard substance material standed for B；
4) definite value: to SiC content standard substance material standed for B definite value, obtain the standard substance of expection SiC content；
Described carborundum content standard substance is SiC, Al2O3、SiO2The powder body of composition, fineness is not more than 100um；SiC mass content is between (45-80) %.
2. the preparation method of carborundum content standard substance according to claim 1, prepares including carborundum pretreatment, aqueous sol-gel, sinters and definite value process, and described sintering process carries out under noble gas is protected.
3. the preparation method of carborundum content standard substance according to claim 1, the mol ratio of the positive esters of silicon acis of aqueous sol-gel preparation process and aluminium salt is between 0.85～1.11.
4. the preparation method of carborundum content standard substance according to claim 1, prepares including carborundum pretreatment, aqueous sol-gel, sinters and definite value process, and silicon carbide powder particle diameter used is not more than 500nm.
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| CN106568735A (en) * | 2016-10-25 | 2017-04-19 | 福建紫金矿冶测试技术有限公司 | High-frequency infrared carbon and sulfur analyzer standard sample selection and working curve production method |
| CN107340166A (en) * | 2017-07-25 | 2017-11-10 | 山东非金属材料研究所 | Aluminium oxide ceramics ingredient standard substance and preparation method thereof |
| CN110160908A (en) * | 2019-05-13 | 2019-08-23 | 航天科工防御技术研究试验中心 | The mass fraction detection method of SiC reinforcement body in a kind of aluminum matrix composite |
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