CN109799234A - The measuring method of silicon carbide and contents of free si in a kind of reaction sintering silicon carbide ceramic - Google Patents
The measuring method of silicon carbide and contents of free si in a kind of reaction sintering silicon carbide ceramic Download PDFInfo
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- CN109799234A CN109799234A CN201910129922.5A CN201910129922A CN109799234A CN 109799234 A CN109799234 A CN 109799234A CN 201910129922 A CN201910129922 A CN 201910129922A CN 109799234 A CN109799234 A CN 109799234A
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Abstract
The present invention provides the measuring method of silicon carbide and contents of free si in a kind of reaction sintering silicon carbide ceramic, measures the area percentage of the SiC in certain area and the area percentage of free Si；The bulk density that reaction-sintering SIC ceramics are measured according to Archimedes principle, is calculated from the formula the mass percentage content of reaction-sintering SIC ceramics SiC and the mass percentage content of free Si.The measuring method is simple and efficient, strong operability, has good application effect.
Description
Technical field
The invention belongs to reaction sintering silicon carbide ceramic fields, and in particular to silicon carbide in reaction sintering silicon carbide ceramic
(SiC) or the measuring method of free silica (Si) content.
Background technique
The research that reaction sintering prepares SiC starts from the 1950s, by Carborandum company, the U.S.
The researchs such as P.Popper success.The basic process of reaction-sintering SIC is as follows: being made after SiC powder and C are mixed by certain ratio
Si is melted at a temperature of 1450-1750 DEG C or generates high temperature Si steam, liquid or gaseous state Si and seeped by capillarity by green body
Enter porous body, reacted with the C in green body and generate SiC, and is combined together to form with SiC particulate original in green body high-densit
SiC product.SiC and original SiC due to during the preparation process, reacting generation are combined together acquisition densification product, so
The SiC of kind technique preparation is also known as reaction bonded or self-bonding SiC.The source Si can using high-purity Si directly heat into liquid Si or
Si steam is generated, SiO can also be passed through2The high temperature pyrolysis such as reduction or (poly-) silane obtain.
In reaction-sintering SIC inevitably contain more free Si, dissociate Si content depend on seep Si mode and
Other technological parameters.Liquid phase method seeps Si and requires the green body porosity relatively high, often the free Si of remnants 10%~20%.Gas
Phase method seep Si can by green body the porosity and pore size control in smaller range, the density of green body can be as high as possible,
Therefore remnants Si content can generally guarantee that it is even lower 8% can be reduced to when minimum 10% or so.Lower free Si
Content is conducive to obtain preferable mechanical behavior under high temperature and preferable chemical stability.Reaction-sintering SIC often contains 8%~
20% free Si, should not be too high using temperature.The fusing point of Si be 1410 DEG C, when using temperature be higher than 1350 DEG C, material property
Sharply decline, under 1400 DEG C of temperatures above, then intensity is completely lost due to the fusing of Si.Therefore, reaction-sintering SIC is most
Operation at high temperature is generally limited to 1350 DEG C.Simultaneously as the presence of free Si, reaction-sintering SIC also should not in Strong oxdiative or
Compared with being used under the conditions of deep-etching.Therefore the measurement of reaction-sintering SIC ceramics SiC or free Si content is for understanding reaction-sintered
The performance of SiC ceramic evaluates its use environment and determines that it is played an important role in price.
But measurement reaction-sintering SIC ceramics SiC or the free accurate method of Si content are mainly chemistry point at present
Analysis method, but this method is more complicated, measurement cost price is expensive, and minute is longer, is not easy to accurately obtain rapidly
The data of SiC or free Si content in reaction-sintering SIC ceramics, therefore, it is difficult to obtain the popularization of reaction-sintering SIC Ceramics Enterprises
And application.
Summary of the invention
In order to solve the above technical problems, the present invention provides the measurement of a kind of reaction-sintering SIC ceramics SiC and free Si content
Method, which is characterized in that
Measure the area percentage A of the SiC in certain areaSiCThe area percentage A of % and free SiSi%；
The bulk density ρ of reaction-sintering SIC ceramics is measured according to Archimedes principle,
The mass percentage content α of reaction-sintering SIC ceramics SiC is calculated according to the following formulaSiCThe quality hundred of % and free Si
Divide than content αSi%:
Wherein, ρsiFor the bulk density of Si, ρsicFor the bulk density of SiC.
The measuring method is simple and efficient, strong operability, has good application effect.
Preferably, reaction-sintering SIC ceramics mainly include SiC and free Si two-phase.
Preferably, reaction-sintering SIC ceramics relative density >=99%.
Preferably, the ceramics sample for measuring reaction-sintering SIC ceramics sample bulk density according to Archimedes principle is many
In 3, bulk density is averaged.Its result is representative and generality.
Preferably, it polishes above-mentioned reaction-sintering SIC ceramics sample surface rubbing and through diamond polishing liquid, rough surface
Degree≤4nm.
It is in mirror effect after polishing as a result, convenient for observing the microstructure of sample.
Preferably, by the reaction-sintering SIC ceramics sample after above-mentioned polishing by optical microscopy or scanning electron microscope into
Row is taken pictures.
Preferably, according to statistical software to reaction-sintering SIC ceramic take a picture middle SiC and free Si two phase material area
Percentage is counted.
Detailed description of the invention
Fig. 1 is sintered sic ceramics sample optical photograph in embodiment 1；
Fig. 2 is statistical distribution result of the statistical software to Si in No. 1 sample；
Fig. 3 is sintered sic ceramics sample optical photograph in embodiment 2；
Fig. 4 is statistical distribution result of the statistical software to Si in No. 2 samples；
Fig. 5 is sintered sic ceramics sample stereoscan photograph in embodiment 3；
Fig. 6 is statistical distribution result of the statistical software to SiC in No. 3 samples.
Specific embodiment
The present invention is further illustrated below in conjunction with attached drawing and following embodiments, it should be appreciated that attached drawing and following embodiments
It is merely to illustrate the present invention, is not intended to limit the present invention.
The present invention is based on above-mentioned chemical analysis method complexity and the longer deficiency of minute, provide a kind of reaction-sintered
The measuring method of silicon carbide ceramics silicon carbide or contents of free si, this method is with strong applicability, can easy quickly measurement reaction
The content of sintered sic ceramics SiC or free Si.Reaction-sintering SIC ceramics mainly by two phase composition of SiC and free Si, burn by reaction
Tie SiC ceramic volume relative density >=99%.The measuring method is simple and efficient, strong operability, has application effect well
Fruit.
Specifically, taking reaction-sintering SIC ceramics sample in a preferred implementation form of the invention, utilizing Archimedes
Principle measures its bulk density.Preferably, it is polished ceramics sample surface rubbing and through diamond polishing liquid, surface by grinding machine
Roughness≤4nm.It is in mirror effect after polishing, convenient for observing the microstructure of sample.
Can be by optical microscopy or scanning electron microscopic observation ceramics sample burnishing surface 3 or more different location, and clap and take
Photo.Its result is representative and generality.
Si, SiC respectively area percentage that dissociates in reaction-sintering SIC ceramics sample are counted, SiC or trip are finally calculated
From Si content.
Specific method (infers three-dimensional structure from the two-dimensional structure observed, then theory according to volume rendering method principle
The method being summed up is known as volume rendering method, and this method is based on statistics):
In formula, ASi% is Si occupied area percentage, ASiC% is SiC occupied area percentage；ASiFor area shared by Si,
ASiCFor SiC occupied area, A is the area of reaction-sintering SIC ceramics sample；Vsi is volume shared by Si, and Vsic is shared by SiC
Volume, V be reaction-sintering SIC ceramics sample volume, msiFor the quality of Si, msicFor the quality of SiC, m is to answer sintered sic
The quality of ceramics sample；αSi% is the mass percentage that Si accounts for entire reaction-sintering SIC ceramics sample, αSiC% accounts for whole for SiC
The mass percentage of a reaction-sintering SIC ceramics sample.
Wherein it is assumed that the sintering of reaction-sintering SIC ceramics sample is completely fine and close, only containing free Si and SiC two-phase, wherein
Stomata is mutually zero.The bulk density ρ of Sisi=2.33g/cm3, SiC bulk density ρsic=3.21g/cm3.Therefore available:
The inventive method can be for example, by the face of Si or SiC in the software statistics reaction-sintering SIC ceramics of VG StudioMax etc.
Then product percentage calculates the mass content of Si or SiC in reaction-sintering SIC ceramics by formula.The method is simple and quick, can grasp
The property made is very strong, has extraordinary application effect.
Embodiment 1
Fig. 1 is sintered sic ceramics sample optical photograph in embodiment 1；Fig. 2 is statistical of the statistical software to Si in No. 1 sample
Cloth result.
Reaction-sintering SIC ceramics sample 3 are taken, measuring its average bulk density is 2.85g/cm3, sample is polished, and
Diamond polishing liquid polishing is carried out by polissoir, surface of polished roughness is 3nm, passes through optical microscope inspection difference
Position is simultaneously taken pictures, and the area percentage that Si is counted by statistical software is 35.08% (Fig. 1-2), can be calculated Si by formula
Mass percentage content is αSi%=35.08% × 2.33/2.85=28.68%.
Embodiment 2
Fig. 3 is sintered sic ceramics sample optical photograph in embodiment 2；Fig. 4 is statistical of the statistical software to Si in No. 2 samples
Cloth result.
Reaction-sintering SIC ceramics sample 3 are taken, measuring its average bulk density is 3.00g/cm3, sample is polished, and
Diamond polishing liquid polishing is carried out by polissoir, surface of polished roughness is 2nm, observes different positions by optical microphotograph
It sets and takes pictures, the area percentage that Si is counted by dedicated statistical software is 20.87% (Fig. 2-3), be can be calculated by formula
Si mass percentage content is αSi%=20.87% × 2.33/3.00=16.21%.
Embodiment 3
Fig. 5 is sintered sic ceramics sample stereoscan photograph in embodiment 3；Fig. 6 is system of the statistical software to SiC in No. 3 samples
Count distribution results.
Reaction-sintering SIC ceramics sample 3 are taken, measuring its average bulk density is 3.01g/cm3, sample is polished, and
Diamond polishing liquid polishing is carried out by polissoir, surface of polished roughness is 2nm, passes through scanning electron microscope observation difference position
It sets and takes pictures, the area percentage that SiC is counted by dedicated statistical software is 82.72% (Fig. 5-6), be can be calculated by formula
SiC mass percentage content is αSi%=82.72% × 3.21/3.01=88.22%.
Under the objective for not departing from essential characteristic of the invention, the present invention can be presented as diversified forms, therefore in the present invention
Implementation form be to be illustrative rather than definitive thereof, limited since the scope of the present invention is defined by the claims rather than by specification,
And all changes fallen in the full scope of equivalents of the range that claim defines or the range that it is defined be understood to include
In detail in the claims.
Claims (7)
1. the measuring method of SiC and free Si content in a kind of reaction-sintering SIC ceramics, which is characterized in that
Measure the area percentage A of the SiC in certain areaSiCThe area percentage A of % and free SiSi%；
The bulk density ρ of reaction-sintering SIC ceramics is measured according to Archimedes principle,
The matter of the mass percentage content α SiC% and free Si of SiC in reaction-sintering SIC ceramics are calculated according to the following formula
Measure degree α Si%:
Wherein, ρsiFor the bulk density of Si, ρsicFor the bulk density of SiC.
2. the method according to claim 1, wherein
Reaction-sintering SIC ceramics mainly include SiC and free Si two-phase.
3. method according to claim 1 or 2, which is characterized in that
Reaction-sintering SIC ceramics relative density >=99%.
4. the method according to claim 1, which is characterized in that
3 are no less than according to the ceramics sample that Archimedes principle measures reaction-sintering SIC ceramics sample bulk density, volume is close
Degree is averaged.
5. method as claimed in any of claims 1 to 4, which is characterized in that
It polishes above-mentioned reaction-sintering SIC ceramics sample surface rubbing and through diamond polishing liquid, surface roughness≤4nm.
6. method as claimed in any of claims 1 to 5, which is characterized in that
Reaction-sintering SIC ceramics sample after above-mentioned polishing is taken pictures by optical microscopy or scanning electron microscope.
7. method according to claim 6, which is characterized in that
According to statistical software ceramic to reaction-sintering SIC take a picture middle SiC and the progress of free Si two phase material area percentage
Statistics.
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