CN106769982A - The assay method of carborundum content in a kind of composite material of silicon carbide - Google Patents

The assay method of carborundum content in a kind of composite material of silicon carbide Download PDF

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Publication number
CN106769982A
CN106769982A CN201611138862.6A CN201611138862A CN106769982A CN 106769982 A CN106769982 A CN 106769982A CN 201611138862 A CN201611138862 A CN 201611138862A CN 106769982 A CN106769982 A CN 106769982A
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China
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silicon carbide
composite
carbon
carborundum
sample
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CN201611138862.6A
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Chinese (zh)
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白海香
赵永红
张庆明
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中核北方核燃料元件有限公司
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Priority to CN201611138862.6A priority Critical patent/CN106769982A/en
Publication of CN106769982A publication Critical patent/CN106769982A/en

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    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infra-red light
    • G01N21/3563Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infra-red light for analysing solids; Preparation of samples therefor
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N21/00Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
    • G01N21/17Systems in which incident light is modified in accordance with the properties of the material investigated
    • G01N21/25Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
    • G01N21/31Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
    • G01N21/35Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infra-red light
    • G01N21/3563Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infra-red light for analysing solids; Preparation of samples therefor
    • G01N2021/3572Preparation of samples, e.g. salt matrices
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2201/00Features of devices classified in G01N21/00
    • G01N2201/12Circuits of general importance; Signal processing
    • G01N2201/123Conversion circuit
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01NINVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
    • G01N2201/00Features of devices classified in G01N21/00
    • G01N2201/12Circuits of general importance; Signal processing
    • G01N2201/125Digital circuitry

Abstract

The invention belongs to chemical detection method technical field, and in particular to using carbon content in infrared absorption determining composite material of silicon carbide, the specific method of carborundum content is then drawn by conversion.Comprise the following steps:(1) composite material of silicon carbide sample is placed in constant weight platinum crucible, is placed on Muffle furnace calcination except carbon;(2) copper is weighed, ceramic crucible bottom is uniformly layered on;(3) sample is weighed, is placed in ceramic crucible;(4) ceramic crucible is placed in Efco-Northrup furnace together with sample powder, makes sample melt-combustion;(5) carbon dioxide for producing that composite material of silicon carbide sample powder burnt with high purity oxygen gas is carried and enters carbon dioxide absorption pond;(6) comparator level is set, and the integration spectrogram to being formed is modified, peak area is calculated;(7) calculate, obtain the mass fraction of carbon in carborundum sample, the percentage composition of carborundum is converted into according to chemistry.The carbon content of carborundum can be accurately determined using the above method.

Description

The assay method of carborundum content in a kind of composite material of silicon carbide
Technical field
The invention belongs to chemical detection method technical field, and in particular to using infrared absorption determining silicon carbide compound Carbon content in material, then draws the specific method of carborundum content by conversion.
Background technology
The problems such as zircaloy corrosion present in current light-water reactor, suction hydrogen, core-shell are reacted and generation Ⅳ System fuel element to the particular/special requirement of material, make with carborundum (SiC) as involucrum or matrix material New-type fuel element Conceptual design and it is prepared into a new focus for nuclear fuel element field.Wherein the purity of carborundum, directly affects carbon The performance of SiClx involucrum, or even have influence on the safe operation of light-water reactor.
The current country defines the analysis method of carborundum content in conventional abrasive Wilicon carbide material, but method detection time Long, accuracy of detection is poor, restrictive condition is more, is not suitable for the high-purity silicon carbide material in nuclear fuel element field, therefore have must Set up corresponding detection method.
The content of the invention
The technical problem to be solved in the present invention be according to detection requirements of one's work, based on the existing instrument and equipment in laboratory, The detection method of carborundum content in infrared absorption determining composite material of silicon carbide is set up, scientific research, the need of production detection are met Ask.
In order to realize this purpose, the present invention is adopted the technical scheme that:
The assay method of carborundum content in a kind of composite material of silicon carbide, is carried out using high frequency infrared ray carbon sulphur analyser, Comprise the following steps:
(1) composite material of silicon carbide sample is placed in constant weight platinum crucible, is placed on Muffle furnace calcination except carbon, one section of constant weight Time, the free carbon in removal carborundum sample;
(2) electronic balance weighing 1.5~2.5g copper is used, carbon content is less than 0.001% in copper, and copper is uniformly layered on ceramic earthenware Crucible bottom;
(3) electronic balance weighing 0.01~0.05g composite material of silicon carbide sample powders are used, load weighted carborundum is answered Condensation material sample powder is placed in ceramic crucible;
(4) ceramic crucible is placed in Efco-Northrup furnace together with composite material of silicon carbide sample powder, opens high Frequency induction furnace makes sample melt-combustion;
(5) carbon dioxide for producing that composite material of silicon carbide sample powder burnt with high purity oxygen gas is carried and enters titanium dioxide Carbon absorption pond, is detected by carbon detector to the infrared light for absorbing, and optical signal is changed into electric signal by A/D change-over panels;
(6) it is 1~3% to set comparator level, and the integration spectrogram to being formed is modified, and calculates peak area;
(7) calculated according to langbobier law, obtained the mass fraction of carbon in carborundum sample, converted according to chemistry Into the percentage composition of carborundum.
Further, in a kind of composite material of silicon carbide as described above carborundum content assay method, step (1) In, it is 800 DEG C~850 DEG C that the calcination of Muffle furnace removes carbon temperature.
Further, in a kind of composite material of silicon carbide as described above carborundum content assay method, step (1) In, the constant weight time is 4h.
Further, in a kind of composite material of silicon carbide as described above carborundum content assay method, step (2) In, the size of ceramic crucible determines according to the requirement of high frequency infrared ray carbon sulphur analyser.
Further, in a kind of composite material of silicon carbide as described above carborundum content assay method, step (3) In, the granularity of composite material of silicon carbide sample powder is less than 0.2mm, dries no moisture.
Further, in a kind of composite material of silicon carbide as described above carborundum content assay method, step (4) In, it is 10~30% to set Efco-Northrup furnace analysis low-power, and analysis high power is 40~50%.
Further, in a kind of composite material of silicon carbide as described above carborundum content assay method, step (4) In, analysis time is 30~50s.
Further, in a kind of composite material of silicon carbide as described above carborundum content assay method, high frequency-infrared The model CS600 of carbon and sulfur analytical instrument.
Further, in a kind of composite material of silicon carbide as described above carborundum content assay method, high frequency-infrared The condition of work of carbon and sulfur analytical instrument is:Carrier gas flux 3.0L/min, analyzes low-power 70%, high power 90% is analyzed, during analysis Between 50s, comparison level 2%, power atmospheric pressure 40Psi, nebulizer gas pressure 35Psi, system pressure 12Psi.
The beneficial effect of technical solution of the present invention is:
The detection method of carborundum content in infrared absorption determining composite material of silicon carbide is successfully established, using invention The experiment condition enumerated in content can accurately determine the carbon content of carborundum, quote accurate detection data, effectively coordinate The carrying out of special production.
Specific embodiment
Technical solution of the present invention is described in detail with reference to specific embodiment.
The assay method of carborundum content in a kind of composite material of silicon carbide of the present invention, using high frequency infrared ray carbon sulphur analyser Carry out, comprise the following steps:
(1) carborundum sample because of preparation technology the reason for contain certain free carbon, in order in Accurate Determining sample be carbonized The content of silicon is, it is necessary to by the free carbon removal in sample, it is therefore necessary to carborundum sample is pre-processed so that in sample Free carbon is without interference with Carbon analysis in carborundum.The amorphous such as carbon black fines, activated carbon carbon simple substance can be anti-with oxygen at 400 DEG C Carbon dioxide should be generated, and carborundum then needs just make more than 2750 DEG C carbon conversion therein for carbon dioxide is escaped, because This can carry out the separation of free carbon according to two kinds of properties of carbonaceous material.
Composite material of silicon carbide sample is placed in constant weight platinum crucible, Muffle furnace calcination is placed on except carbon, during one section of constant weight Between, the free carbon in removal carborundum sample;
In the present embodiment, it is 800 DEG C~850 DEG C that the calcination of Muffle furnace removes carbon temperature, and the constant weight time is 4h;
(2) electronic balance weighing 1.5~2.5g copper is used, carbon content is less than 0.001% in copper, and copper is uniformly layered on ceramic earthenware Crucible bottom;The size of ceramic crucible determines according to the requirement of high frequency infrared ray carbon sulphur analyser;
(3) when sample weighting amount is too small, balance error is larger;And sample weighting amount it is excessive when, the content of carbon gradually increases in carborundum, Certain influence is likely to result in for the absorption efficiency of cell for infrared absorption.Therefore, it is carbonized with 0.01~0.05g of electronic balance weighing Silicon composite sample powder, the granularity of composite material of silicon carbide sample powder is less than 0.2mm, dries no moisture;To weigh Composite material of silicon carbide sample powder be placed in ceramic crucible;
(4) ceramic crucible is placed in Efco-Northrup furnace together with composite material of silicon carbide sample powder, sets high Frequency induction furnace analysis low-power is 10~30%, and analysis high power is 40~50%, and analysis time is 30~50s;Open high frequency Induction furnace makes sample melt-combustion;
(5) carbon dioxide for producing that composite material of silicon carbide sample powder burnt with high purity oxygen gas is carried and enters titanium dioxide Carbon absorption pond, is detected by carbon detector to the infrared light for absorbing, and optical signal is changed into electric signal by A/D change-over panels;
(6) it is 1~3% to set comparator level, and the integration spectrogram to being formed is modified, and calculates peak area;
(7) calculated according to langbobier law, obtained the mass fraction of carbon in carborundum sample, converted according to chemistry Into the percentage composition of carborundum.
When determining condition of work, analysis power is too low, and carbon emissions are incomplete;But analysis power is too high, produce dust excessive, Hinder CO2Transmission or absorb CO2.Comparator be horizontally disposed with it is too low, cause instrument produce foreign gas be integrated, determine knot It is really higher;And comparator is horizontally disposed with too high, cause sample gas to be unable to complete integral, cause measurement result relatively low, precision is inclined It is low.The minimum comparator level that selection instrument does not trail is used as experiment parameter.With the increase of comparator level, analysis time is in Reduction trend, carborundum content measurement result tapers off trend, is consistent with theory analysis situation.
The model CS600 of high frequency infrared ray carbon sulphur analyser, condition of work is:Carrier gas flux 3.0L/min, analyzes low work( Rate 70%, analysis high power 90%, analysis time 50s, comparison level 2%, power atmospheric pressure 40Psi, nebulizer gas pressure 35Psi, System pressure 12Psi.
In the present embodiment, precision test is carried out with the carborundum sample of different carborundum contents, it is parallel to weigh 6 examinations Sample, is analyzed by set test procedure, obtains the measurement result of carborundum content.Knowable to measurement result, silicon carbide sample The precision of middle carborundum content assay method is better than 10%.Carbon content is in 29% or so, conventional mark-on in carborundum sample Absorption method cannot meet requirement, and through research, experiment selection carries out mark-on and returns using high-purity calcium carbonate primary standard substance as standard substance Acceptance test.The rate of recovery meets requirement of experiment between 85%~120%.

Claims (10)

1. in a kind of composite material of silicon carbide carborundum content assay method, carried out using high frequency infrared ray carbon sulphur analyser, its It is characterised by, comprises the following steps:
(1) composite material of silicon carbide sample is placed in constant weight platinum crucible, is placed on Muffle furnace calcination except carbon, during one section of constant weight Between, the free carbon in removal carborundum sample;
(2) electronic balance weighing 1.5~2.5g copper is used, carbon content is less than 0.001% in copper, and copper is uniformly layered on ceramic crucible bottom Portion;
(3) electronic balance weighing 0.01~0.05g composite material of silicon carbide sample powders are used, by load weighted silicon carbide compound material Material sample powder is placed in ceramic crucible;
(4) ceramic crucible is placed in Efco-Northrup furnace together with composite material of silicon carbide sample powder, opens high frequency sense Answering stove makes sample melt-combustion;
(5) carbon dioxide for producing that composite material of silicon carbide sample powder burnt with high purity oxygen gas is carried and enters carbon dioxide suction Receives pond, is detected by carbon detector to the infrared light for absorbing, and optical signal is changed into electric signal by A/D change-over panels;
(6) it is 1~3% to set comparator level, and the integration spectrogram to being formed is modified, and calculates peak area;
(7) calculated according to langbobier law, obtained the mass fraction of carbon in carborundum sample, carbon is converted into according to chemistry The percentage composition of SiClx.
2. in a kind of composite material of silicon carbide as claimed in claim 1 carborundum content assay method, it is characterised in that:Step Suddenly in (1), it is 800 DEG C~850 DEG C that the calcination of Muffle furnace removes carbon temperature.
3. in a kind of composite material of silicon carbide as claimed in claim 1 carborundum content assay method, it is characterised in that:Step Suddenly in (1), the constant weight time is 4h.
4. in a kind of composite material of silicon carbide as claimed in claim 1 carborundum content assay method, it is characterised in that:Step Suddenly in (2), the size of ceramic crucible determines according to the requirement of high frequency infrared ray carbon sulphur analyser.
5. in a kind of composite material of silicon carbide as claimed in claim 1 carborundum content assay method, it is characterised in that:Step Suddenly in (3), the granularity of composite material of silicon carbide sample powder is less than 0.2mm, dries no moisture.
6. in a kind of composite material of silicon carbide as claimed in claim 1 carborundum content assay method, it is characterised in that:Step Suddenly in (4), it is 10~30% to set Efco-Northrup furnace analysis low-power, and analysis high power is 40~50%.
7. in a kind of composite material of silicon carbide as claimed in claim 1 carborundum content assay method, it is characterised in that:Step Suddenly in (4), analysis time is 30~50s.
8. in a kind of composite material of silicon carbide as claimed in claim 1 carborundum content assay method, it is characterised in that:It is high The model CS600 of frequency infrared carbon sulfur analyzer.
9. in a kind of composite material of silicon carbide as claimed in claim 1 carborundum content assay method, it is characterised in that:It is high The condition of work of frequency infrared carbon sulfur analyzer is:Carrier gas flux 3.0L/min, analyzes low-power 70%, analyzes high power 90%, Analysis time 50s, comparison level 2%, power atmospheric pressure 40Psi, nebulizer gas pressure 35Psi, system pressure 12Psi.
10. in a kind of composite material of silicon carbide as claimed in claim 1 carborundum content assay method, it is characterised in that: In step (1), it is 800 DEG C~850 DEG C that the calcination of Muffle furnace removes carbon temperature, and the constant weight time is 4h;
In step (2), the size of ceramic crucible determines according to the requirement of high frequency infrared ray carbon sulphur analyser;
In step (3), the granularity of composite material of silicon carbide sample powder is less than 0.2mm, dries no moisture;
In step (4), it is 10~30% to set Efco-Northrup furnace analysis low-power, and analysis high power is 40~50%, during analysis Between be 30~50s;
The model CS600 of high frequency infrared ray carbon sulphur analyser, condition of work is:Carrier gas flux 3.0L/min, analyzes low-power 70%, analysis high power 90%, analysis time 50s, comparison level 2%, power atmospheric pressure 40Psi, nebulizer gas pressure 35Psi are System pressure 12Psi.
CN201611138862.6A 2016-12-12 2016-12-12 The assay method of carborundum content in a kind of composite material of silicon carbide CN106769982A (en)

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Application publication date: 20170531