CN107966415A - The contactless online test method and device of SiC oxidation reactions - Google Patents
The contactless online test method and device of SiC oxidation reactions Download PDFInfo
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- CN107966415A CN107966415A CN201711156383.1A CN201711156383A CN107966415A CN 107966415 A CN107966415 A CN 107966415A CN 201711156383 A CN201711156383 A CN 201711156383A CN 107966415 A CN107966415 A CN 107966415A
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- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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- G—PHYSICS
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- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
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Abstract
The present invention relates to a kind of contactless online test method of SiC oxidation reactions, comprise the following steps：The spectral signal of the SiC sample near surface area of space gases in oxygen environment is dissociated by focused light passages real-time detection；Judge that the SiC samples near surface whether there is Si atoms by analyzing the spectral signal, be that then definite SiC samples near surface occurs actively to aoxidize, passive oxidation otherwise occurs.The invention further relates to a kind of contactless on-line measuring device of SiC oxidation reactions, can real-time online detection SiC material oxidation reaction state, relative to the test method of material analysis after conventional oxidation, the experimental amount of SiC oxidations and later stage material analysis is greatly reduced in the present invention, has saved cost.
Description
Technical field
The present invention relates to the contactless online test method in measuring for materials field, more particularly to SiC oxidation reactions
And device.
Background technology
Currently with ZrB2- SiC, C/SiC are hypersonic aircraft key hot arc position candidate's heat insulation material of representative,
The oxidation resistance in 1200-1500 DEG C of section relies primarily on silicon substrate component, and research silica-base material oxidation mechanism is lifting solar heat protection material
Expect the premise and key of oxidation resistance.With the raising of hypersonic aircraft speed, air-flow passes through shock wave compression or viscosity
Retardance slow down, cause a large amount of kinetic energy to be transformed into thermal energy, temperature of gas mixture raises and energy excitation occurs, dissociation, ionization, electricity
The a series of physical chemical reaction such as son excitation, occurs so-called " high-temperature gas effect ", at this time for aircraft termination, nose of wing
Deng key position heat insulation material face be high temperature, low pressure, dissociation oxygen medium.
SiC material has good antioxygenic property under normal pressure, molecule oxygen environment, this is because under the high temperature conditions
The SiO one layer very thin, fine and close, be firmly combined with of SiC material Surface Creation2Film, oxygen is in SiO2Diffusion coefficient in film is non-
It is often small, therefore the oxidation of SiC material is very slow, under these conditions, the slow oxidation of SiC is known as passive oxidation, chemical formula
For：SiC(s)+32O2(g)=SiO2(s)+CO(g)。
But when the environmental pressure of surrounding reduces, oxide isolation becomes dissociation oxygen from molecular oxygen, SiC material oxidation rate increases
Add, and be changed into from passive oxidation to active oxidation transformation, chemical formula：SiC(s)+O2(g)=SiO (g)+CO (g).At this time, aoxidize
Product is by SiO2Oxidation-resistant film becomes volatility SiO so that SiC material loses antioxidation.The transformation of this oxidation reaction,
Directly determine the use scope and application field of the heat insulation material of SiC bases.Therefore, for the active/passive oxidation reaction of SiC material
Research be always heat insulation material focus and emphasis.
At present, researcher is mainly judged by analyzing SiC oxidized materials Surface Phases and heterogeneous microstructure
It happens is that active oxidation reaction, or passive oxidation reaction under the experimental state.Such method only can determine that specific oxidation
The reactiveness of SiC material under environment (oxide isolation, temperature, pressure), it is impossible to which on-line checking, nothing are carried out to SiC oxidation reactions
Method obtains the reactiveness of SiC material under any oxidation environment.
The content of the invention
The technical problem to be solved in the present invention is solve the prior art to carry out real-time online to SiC oxidation reactions type
Detection, obtains the problem of main passive oxidations of SiC change this key parameters.
In order to solve the above technical problem, the present invention provides a kind of contactless on-line checking side of SiC oxidation reactions
Method, detection method of the present invention are：First according to the active/passive features of SiC, the chemistry side that can reflect response feature is chosen
The chemical equation of formula, wherein dependent response is：
SiC(s)+3/2O2(g)=SiO2(s)+CO(g)
The chemical equation of active reaction is：
SiC(s)+O2(g)=SiO (g)+CO (g)
Material surface produces a kind of SiO gas-phase products when can be seen that active reaction according to above-mentioned chemical reaction, passes through reality
When on-line water flushing SiO gases spectral signal can determine whether SiC occurs active reaction.SiO molecule band spectrum coverages compared with
Width, wide spectrum range signals are weaker, plus the influence of material surface hyperthermia radiation, it is difficult to detect effective molecule band spectrum.
Found by analysis, the characteristics of gaseous state SiO is unstable, Si and SiO are easily decomposed into after departing from specimen surface2, and the hair of Si atoms
Penetrate spectrum has stronger characteristic peak at 288nm.It is characteristic of the invention that it is by detecting high temperature sample near surface area of space
It is no there are Si atoms, that is, test whether the region atomic features spectral line occurs at 288nm, and then judge under atomic oxygen environment
The transition point of SiC master/dynamic oxidation.Further, it is also possible to the power of actively oxidation is judged by characteristic spectral line intensity.
The detection method of the present invention comprises the following steps：
S1, the spectrum by the SiC sample near surface area of space gases in focused light passages real-time detection dissociation oxygen environment
Signal；
S2, by analyzing the spectral signal judge that the SiC samples near surface whether there is Si atoms, is then definite institute
State SiC samples to occur actively to aoxidize, passive oxidation otherwise occurs.
Further, the method further includes：
S3, the reaction condition for changing test zone residing for SiC samples, under the conditions of execution step S1 and S2 record differential responses
The oxidation type of SiC samples, determines actively to be oxidizing to the transition point of passive oxidation.
Further, in the step S3：When detecting SiC samples generation passive oxidation, the test section is gradually reduced
Pressure in domain, until judging that SiC sample near surface area of space there are Si atoms, determines at this time according to the spectral signal of detection
For the transition point of main dynamic oxidation to passive oxidation.
Further, received in the step S1 using the real image at lens group convergence SiC sample near surfaces by optical fiber
In the real image input light spectrometer, and by inputting computer after photomultiplier；Wherein described lens group is included in SiC samples
Narrow band pass filter, focal length convex lens and the short focus convex lens that the side of residing test zone is set gradually, the narrow band pass filter,
The geometric center of the focal length convex lens and the short focus convex lens is in same horizontal line with the SiC samples near surface,
And level interval is set so that the real image of the SiC samples near surface converges at the optical fiber sensor head that described optical fiber one end is set
Place, the optical fiber other end are connected by fiber adapter with the input terminal of the spectrometer.
Further, the SiC samples are placed in the dissociation oxygen environment examination of thermally protective materials high-temperature low-pressure in the step S1
In experiment device oxygen environment is dissociated to provide.
Present invention also offers a kind of contactless on-line measuring device of SiC oxidation reactions, including at least spectra collection
Device and analytical equipment；
The spectra collection device is used for the near surface area of space for the SiC samples that real-time detection is in dissociation oxygen environment
The spectral signal of gas；
The analytical equipment is used to judge that the SiC samples near surface is former with the presence or absence of Si by analyzing the spectral signal
Son, is that then the definite SiC samples occur actively to aoxidize, passive oxidation otherwise occurs.
Further, the contactless on-line measuring device further includes：
Test device, including environmental chamber and the sample stage that is arranged in the environmental chamber, the sample stage are treated for placement
The SiC samples of survey, the environmental chamber is used to produce different dissociation oxygen environments, and adjusts the environment temperature residing for the sample stage
And/or pressure, the side of the environmental chamber are provided with observation window.
Further, the analytical equipment includes peakology unit, for by analyzing the peak in the spectral signal
Value information, judges that the type of oxidation reaction, and the response intensity of active oxidation reaction occur for the SiC samples.
Further, the analytical equipment includes transition point analytic unit, for by recording SiC under the conditions of differential responses
The oxidation type of sample, determines passive oxidation to the transition point of active oxidation.
Further, the analytical equipment includes experimental rig control unit, instructs control environmental chamber to change for sending
The reaction condition of test zone residing for SiC samples.
Further, the transition point analytic unit passes through experiment when detecting SiC samples near surface generation passive oxidation
Device control units gradually reduces the pressure in the test zone, until judging that SiC samples are near according to the spectral signal of detection
There are Si atoms on surface.
Further, the spectra collection device includes lens group, optical fiber, spectrometer and photomultiplier；The lens
Group is included in narrow band pass filter, focal length convex lens and the short focus convex lens that the side of test zone residing for SiC samples is set gradually,
At the geometric center of the narrow band pass filter, the focal length convex lens and the short focus convex lens and the SiC samples near surface
In in same horizontal line, and level interval is set so that the real image of the SiC samples near surface converges at described optical fiber one end and sets
At the optical fiber sensor head put；The optical fiber other end is connected by fiber adapter with the input terminal of the spectrometer, spectrometer
Output terminal by being connected to the analytical equipment after photomultiplier.
Implement the contactless online test method and device of the SiC oxidation reactions of the present invention, have the following advantages that：This hair
The spectral signal of the bright SiC sample near surface area of space gases dissociated using focused light passages real-time detection in oxygen environment, is realized
Under conditions of SiC samples are not contacted, real-time detection is carried out to SiC sample oxidation reactions state；Secondly, the present invention is based on spectrum
Diagnosis principle, and judge SiC samples near surface with the presence or absence of Si atoms by analyzing spectral signal and sentence
Disconnected oxidation type, it is possible to achieve the on-line checking of the active/passive oxidation reaction transformation of SiC samples, relative to tradition
The test method of oxidized material analysis, is greatly reduced the experimental amount of SiC oxidations and later stage material analysis, cost-effective.
Brief description of the drawings
Fig. 1 is the module diagram of the contactless on-line measuring device of SiC oxidation reactions in the embodiment of the present invention one；
Fig. 2 is the structure diagram of the contactless on-line measuring device of SiC oxidation reactions in the embodiment of the present invention one；
Fig. 3 is the module diagram of the contactless on-line measuring device of SiC oxidation reactions in the embodiment of the present invention two；
Fig. 4 is the structure diagram of the contactless on-line measuring device of SiC oxidation reactions in the embodiment of the present invention two；
Fig. 5 is the structure diagram of test device in the embodiment of the present invention two；
Fig. 6 is the module diagram of analytical equipment in the embodiment of the present invention three；
Fig. 7 is the module diagram of analytical equipment in the embodiment of the present invention four；
Fig. 8 is the module diagram of analytical equipment in the embodiment of the present invention five；
Fig. 9 is the step schematic diagram of the contactless online test method of SiC oxidation reactions in the embodiment of the present invention six；
Figure 10 is spectral signal figure under the dissociation oxygen environment of different pressures 1375 DEG C in the embodiment of the present invention six；
Figure 11 is the step schematic diagram of the contactless online test method of SiC oxidation reactions in the embodiment of the present invention seven；
Figure 12 is active reaction spectral signal figure under 50Pa dissociation oxygen environments 1400 DEG C in the embodiment of the present invention seven；
Figure 13 is active reaction spectral signal figure under 100Pa dissociation oxygen environments 1500 DEG C in the embodiment of the present invention seven；
Figure 14 is the active/passive reaction transformation point diagram under representative condition in the embodiment of the present invention seven.
In figure：1：Spectra collection device；11：Three-dimensional light path adjusts platform；12：Narrow band pass filter；13：Focal length convex lens；14：
Short focus convex lens；15：Optical fiber sensor head；16：Optical fiber；17：Fiber adapter；18：Spectrometer；19：Photomultiplier；
2：Analytical equipment；21：Peakology unit；22：Transition point analytic unit；23：Experimental rig control unit；
3：Test device；31：Radio-frequency power supply；32：Inlet flange, 33：High saturating quartz window, 34：Plate coil, 35：
With case, 36：Double color comparison temperature measurement instrument, 37：Observation window；38：Cooling water inlet pipe, 39：Sample stage, 311：Water cooled holder, 312：Take
Sample window, 313：Cooling water return pipe, 314：Refrigeration machine, 315：Optical table, 316：Second tunnel cooling cycle water pipe, 317：Heating
Laser, 318：Vacuum Z axis displacement platform, 319：3rd tunnel cooling cycle water pipe, 320：Laser transmission fiber；321：Environmental chamber,
322：Heating window, 323：Vacuum flange, 324：Laser adjustment camera lens, 325：Laser adjustment stent, 326：Vacuum solenoid,
327：Vacuum pump.
4：SiC samples.
Embodiment
To make the purpose, technical scheme and advantage of the embodiment of the present invention clearer, below in conjunction with the embodiment of the present invention
In attached drawing, the technical solution in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is
The part of the embodiment of the present invention, instead of all the embodiments.Based on the embodiments of the present invention, ordinary skill people
Member's all other embodiments obtained on the premise of creative work is not made, belong to the scope of protection of the invention.
Embodiment one
As depicted in figs. 1 and 2, the embodiment of the present invention one provides a kind of contactless on-line checking of SiC oxidation reactions
Device, including at least spectra collection device 1 and analytical equipment 2.Wherein, spectra collection device 1 is used for real-time detection in dissociation
The spectral signal of the near surface area of space gas of SiC samples 4 in oxygen environment, such as in the experimental enviroment of high-temperature low-pressure,
SiC samples 4 aoxidize.Preferably, near surface area of space herein refers in the range of 4 surface 0-100mm of distance SiC samples
Area of space.Analytical equipment is used to judge that 4 near surface of SiC samples whether there is Si atoms by analyzing spectral signal, is then
Determine that SiC samples 4 occur actively to aoxidize, passive oxidation otherwise occurs.Analytical equipment 2 in the present embodiment can use computer
Realize.
Preferably, as shown in Fig. 2, spectra collection device 1 includes：Spectra collection device 1 includes lens group, optical fiber 16, light
Spectrometer 18 and photomultiplier 19.It is further preferred that lens group is included in one of test zone residing for SiC samples 4 to be measured
Narrow band pass filter 12, focal length convex lens 13 and the short focus convex lens 14 that side is set gradually.Wherein, narrow band pass filter 12, focal length are convex
Lens 13 and short focus convex lens 14 are placed on three-dimensional light path adjustment platform 11, narrow band pass filter 12, focal length convex lens 13 and short focus
The geometric center of convex lens 14 is in same horizontal line with the near surface of SiC samples 4, and is adjusted platform 11 by three-dimensional light path and adjusted
The real image of test zone, the optical fiber sensor head of 16 one end of optical fiber is converged at based on image-forming principle by each optics in whole lens group
On 15, i.e., optical fiber sensor head 15 is arranged at real image convergence, and the other end of optical fiber 16 passes through fiber adapter 17 and spectrometer 18
Input terminal connection, the output terminal of spectrometer 18 after photomultiplier 19 by being connected to analytical equipment 2.
It should be noted that, although the specific example of spectra collection device 1 is given in the embodiment, but the present invention is not
This is only limitted to, and can be known using any this area basic technology personnel and can apply to the optics of detecting light spectrum signal
To build light path.
The curve of spectrum of selected characteristic reaction product, time domain and the spatial domain change of detectable material near surface reaction product are advised
Rule, judges the reactiveness of SiC material under the conditions of temperature, pressure consecutive variations, can also obtain the active/passive oxidation of SiC material
The environmental characteristic point (temperature, pressure) changed is reacted, obtains changing rule of the active reaction with temperature, pressure.
According to the characteristics of SiC oxidation reactions, the chemical equation of SiC dependent responses is：
SiC(s)+3/2O2(g)=SiO2(s)+CO(g)
The chemical equation of SiC active reactions is：
SiC(s)+O2(g)=SiO (g)+CO (g)
When SiC active reactions, material surface produces a kind of gas-phase product SiO, and SiO molecule band spectrum coverages are wider,
Wide spectrum range signals are weaker, plus the influence of material surface hyperthermia radiation, it is difficult to detect effective molecule band spectrum.Work as examination
Sample is under hot conditions, and the high temp, infrared radiation of material surface can cause spectrometer to be visited in the wavelength region of 500-1400nm
A piece of peak value is measured, this peak value can cover the atom peak-to-peak signal and SiO molecules peak letter of oxygen atom (844.6nm, 770.5nm etc.)
Number, thus can not by detecting the oxygen atom in this region, SiO molecules peak value judges that it is main passive whether SiC material occurs
Oxidation reaction.But gaseous state SiO have the characteristics that it is unstable, depart from material surface after be easily decomposed into Si and SiO2, and Si atoms
Emission spectrum has stronger characteristic spectral line at 288nm, avoids the wavelength region of the 500-1400nm of hyperthermia radiation influence,
Exactly overcome the influence of infra-red radiation.
The device of the contactless on-line checking for the SiC oxidation reactions that the present embodiment is provided is based on spectroscopic diagnostics principle,
The suitable detection spectral line of screening, overcomes the influence of high temp, infrared radiation, whether there is by detecting sample near surface area of space
Si atoms, that is, test whether the region atomic features spectral line occurs at 288nm, and then judges that the oxidation of 4 near surface of SiC samples is anti-
The type answered, the device of the contactless on-line checking for the SiC oxidation reactions that the present embodiment is provided can be in the condition of high temperature
Under, the active/passive oxidation reaction state of SiC material is detected in real time, and it is simple in structure, it is easy to operate, it can effectively reduce experiment work
Measure and save the cost of detection.Further, it is also possible to the power of actively oxidation is judged by characteristic spectral line intensity.
Embodiment two
As shown in Figure 3 and Figure 4, the present embodiment two and embodiment one are essentially identical, and something in common repeats no more, difference
It is：The contactless on-line measuring device for the SiC oxidation reactions that the present embodiment two provides further includes：
Test device 3, including environmental chamber 321 and the sample stage 39 being arranged in environmental chamber 321, sample stage 39 is for placing
SiC samples 4 to be measured, environmental chamber 321 is used to produce different dissociation oxygen environments, and adjusts the environment temperature residing for sample stage 39
And/or pressure, the side of environmental chamber 321 are provided with observation window 37.Spectra collection device 2 is arranged on the side of observation window 37, can
The spectral information in 4 near surface space of SiC samples is collected by observation window 37.
Preferably, as shown in figure 5, the test device 3 in the present embodiment employ a kind of thermally protective materials high-temperature low-pressure from
Solve oxygen environment experimental rig, including optical table 315, environmental chamber 321, radio-frequency power supply 31, matching box 35, refrigeration machine 314 and add
Thermal laser device 317.Environmental chamber 321 is placed on optical table 315, and radio-frequency power supply 31 is exported to the plate coil in matching box 35
34, discharge through plate coil 34 working gas for entering environmental chamber 321 by inlet flange 32, form dissociation oxygen environment, SiC examinations
Sample 4 is placed on sample stage 39, and sample stage 39 is placed in water cooled holder 311, and water cooled holder 311 is placed in vacuum Z axis displacement platform 318
Interior, vacuum Z axis displacement platform 318 is placed in environmental chamber 321, and 321 top of environmental chamber is provided with high quartz window 33 thoroughly, environmental chamber 321
Bottom is provided with heating window 322, and 321 side-lower of environmental chamber is provided with sampling window 312, and 321 side of environmental chamber is provided with observation window 37；Light
Learn in platform 315 and adjust camera lens 324 equipped with laser adjustment camera lens 324 and laser adjustment stent 325, laser and adjusted installed in laser
On stent 325, heating laser 317 is sequentially connected laser transmission fiber 320 and laser adjustment camera lens 324, laser adjustment camera lens
324 transmitting laser project the back wall of SiC samples 4 by heating window 322, observe SiC samples 4 by observation window 37 and heat feelings
Condition, and using the double color comparison temperature measurement instrument 36 hung on above 321 axis of environmental chamber SiC samples are monitored through high quartz window 33 thoroughly
The temperature variations on 4 surfaces；321 bottom of environmental chamber is equipped with aspirating hole, and the gas in environmental chamber 321 is arranged by vacuum extractor
Go out, first via cooling cycle water pipe includes cooling water inlet pipe 38 and cooling water return pipe 313, cooling water inlet pipe 38 successively with
Matching box 35, radio-frequency power supply 31 and environmental chamber 321 connect, and enter refrigeration machine 314,39 He of sample stage by cooling water return pipe 313
Water cooled holder 311 accesses refrigeration machine 314 by the second tunnel cooling cycle water pipe 316, and laser adjusts camera lens 324 and followed by the cooling of the 3rd tunnel
Ring water pipe 319 accesses refrigeration machine 314, and heating laser 317 is directly cooled down by refrigeration machine 314.
It is further preferred that vacuum extractor includes vacuum flange 323, vacuum valve, vacuum solenoid 326 and vacuum
Pump 327 is connected, by controlling vacuum valve with vacuum solenoid 326 with the vacuum in adjusting ambient cabin 321, using resistance
Rule, ionization gauge real time monitoring.Test device 3 can be controlled by computer, can also pass through manual control.
Test device 3 can simulate high-temperature hot protection material under hypersonic service condition used by the present embodiment
High temperature, low pressure, dissociation oxygen oxidation environment, by the decoupling of each parameter and separately adjustable, research thermally protective materials are in dissociation oxygen oxygen
Change the response under environment and evolutionary process.
The contactless on-line measuring device for the SiC oxidation reactions that the present embodiment two provides, which employs, can adjust test wrapper
The test device 3 in border, in use, the reaction condition of SiC samples 4, detection temperature and pressure can be changed in real time by test device 3
The active/passive oxidation reaction of SiC material under the conditions of power consecutive variations.The contactless on-line measuring device that the present embodiment two provides
Effective experimental data of the active/passive oxidation reaction of SiC material can be increased considerably, is the verification of the Theoretical Prediction of oxidation mechanism
The comparative experimental data completed is provided.
Embodiment three
As shown in fig. 6, the present embodiment three and embodiment one are essentially identical, something in common repeats no more, and difference is：
In the contactless on-line measuring device for the SiC oxidation reactions that the present embodiment three provides, analytical equipment 2 includes peakology unit
21, for by analyzing the peak information in spectral signal, judging that the type of oxidation reaction, and active oxygen occur for SiC samples 4
Change reaction response intensity, if detection less than, be passive oxidation, if spectral signal can be detected, be actively aoxidize, and
Signal is stronger, and reaction is more violent, and signal is weaker, and reaction is weaker.
Certainly in other embodiments, the present invention is added in the present embodiment before spectra collection device 1 that can also be to implement
The test device 3 that example two is introduced.
The contactless on-line measuring device of SiC oxidation reactions provided in this embodiment can be according to the active oxygen detected
Change reaction product spectral signal intensity, inverting active oxidizing reaction rate with oxide isolation, temperature and pressure quantitative change
Rule, actively aoxidizes process variable and provides data supporting further to probe into.
Example IV
As shown in fig. 7, the present embodiment four and embodiment three are essentially identical, something in common repeats no more, and difference is：
In the contactless on-line measuring device for the SiC oxidation reactions that the present embodiment three provides, analytical equipment 2 further includes transformation point analysis
Unit 22, for the oxidation type by recording SiC samples 4 under the conditions of differential responses, determines passive oxidation to active oxidation
Transition point.
Certainly in other embodiments, the present invention is added in the present embodiment before spectra collection device 1 that can also be to implement
The test device 3 that example two is introduced.
The contactless on-line measuring device for the SiC oxidation reactions that the present embodiment four provides can be analyzed and recorded different anti-
The oxidation type of the SiC samples 4 of condition is answered, and can be used in researching and analysing the transition point of the active/passive oxidation reactions of SiC.
Embodiment five
As shown in figure 8, the present embodiment five is essentially identical with example IV, something in common repeats no more, and difference is：
In the contactless on-line measuring device of SiC oxidation reactions provided in this embodiment, analytical equipment 2 further includes experimental rig control
Unit 23, for sending the reaction condition for instructing control environmental chamber 321 to change test zone residing for SiC samples 4.
In the present embodiment, experimental rig control unit 23 is entity, is integrated in a computer, in other embodiments
In, it can also be realized using manual control, such as manual control environment cabin 321 changes the anti-of test zone residing for SiC samples 4
Answer condition.
The contactless on-line measuring device of SiC oxidation reactions provided in this embodiment can detect SiC material master/quilt in real time
Dynamic oxidation reactiveness, relative to the test method of material analysis after conventional oxidation, is greatly reduced SiC oxidations and later stage material
The experimental amount of analysis, it is cost-effective；Adjustable SiC reaction conditions, and detect oxide isolation, temperature and pressure consecutive variations condition
The active/passive oxidation reaction of lower SiC material, relative to the test method of traditional selected characteristic point, can increase considerably effective reality
Data are tested, the comparative experimental data completed is provided for the verification of the Theoretical Prediction of oxidation mechanism；Can be according to the active oxygen detected
Change reaction product spectral signal intensity, inverting active oxidizing reaction rate with oxide isolation, temperature and pressure quantitative change
Rule, actively aoxidizes process variable and provides data supporting further to probe into.
Embodiment six
As shown in figure 9, the embodiment of the present invention six provides a kind of contactless online test method of SiC oxidation reactions, bag
Include following steps：
S1, the spectrum by the 4 near surface area of space gas of SiC samples in focused light passages real-time detection dissociation oxygen environment
Signal；
S2, by analyzing the spectral signal judge that 4 near surface of SiC samples whether there is Si atoms, is then definite
The SiC samples 4 occur actively to aoxidize, and passive oxidation otherwise occurs.
The curve of spectrum of selected characteristic reaction product, time domain and the spatial domain change of detectable material near surface reaction product are advised
Rule, judges the reactiveness of SiC material under the conditions of temperature, pressure consecutive variations, can also obtain the active/passive oxidation of SiC material
The environmental characteristic point (oxide isolation concentration, temperature, pressure) changed is reacted, obtains change of the active reaction with temperature, pressure
Law.
According to the characteristics of SiC oxidation reactions, the chemical equation of SiC dependent responses is：
SiC(s)+3/2O2(g)=SiO2(s)+CO(g)
The chemical equation of SiC active reactions is：
SiC(s)+O2(g)=SiO (g)+CO (g)
When SiC active reactions, material surface produces a kind of gas-phase product SiO, and SiO molecule band spectrum coverages are wider,
Wide spectrum range signals are weaker, plus the influence of material surface hyperthermia radiation, it is difficult to detect effective molecule band spectrum, but gas
State SiO have the characteristics that it is unstable, depart from material surface after be easily decomposed into Si and SiO2, and the emission spectrum of Si atoms exists
There is stronger characteristic spectral line at 288nm.
The principle of the contactless online test method of SiC oxidation reactions of the present invention is near by detecting sample
Space surface region whether there is Si atoms, that is, test whether the region atomic features spectral line occurs at 288nm, and then judge
The type of 4 near surface oxidation reaction of SiC samples.
When SiC active reactions, material surface produces a kind of gas-phase product SiO, gaseous state SiO have the characteristics that it is unstable,
Si and SiO are easily decomposed into after departing from material surface2, and the emission spectrum of Si atoms has stronger characteristic spectral line at 288nm.
Preferably, the SiC samples 4 are placed in thermally protective materials high-temperature low-pressure dissociation oxygen environment experimental rig in step S1
In with provide dissociate oxygen environment；Using the real image at 4 near surface of lens group convergence SiC samples, the reality is received by optical fiber 16
In picture input light spectrometer 18, and analyzed and processed by inputting computer after photomultiplier 19.
Specific in the present embodiment, lens group is included in the arrowband that the side of test zone residing for SiC samples 4 is set gradually
Optical filter 12, focal length convex lens 13 and short focus convex lens 14, the narrow band pass filter 12, the focal length convex lens 13 and described short
The geometric center of burnt convex lens 14 is in same horizontal line with 4 near surface of SiC samples, and level interval is set so that institute
The real image for stating 4 near surface of SiC samples is converged at the optical fiber sensor head 15 of 16 one end of optical fiber setting, and the other end of optical fiber 16 passes through
Fiber adapter 17 is connected with the input terminal of spectrometer 18.
In use, the real image of 4 near-surface region gas-phase product of SiC samples is entered after lens group focuses on by optical fiber 16
Spectrometer 18, through grating beam splitting, the grating angle by adjusting spectrometer 18 obtains the wave-length coverage of detection spectral line, after light splitting
Spectral signal is converged on the sensing head of photomultiplier 19, and response signal is transmitted to computer.If it can see at 288nm
Obvious atom peak, illustrates that SiC material happens is that active oxidation reaction, if cannot, illustrate to happens is that passive oxidation reacts.
Specifically, it is 1375 DEG C for reaction condition, 10Pa and 1375 DEG C, the SiC samples 4 of 100Pa are compared respectively,
Obtained spectral signal is as shown in Figure 10, it can be seen that reaction condition is 1375 DEG C, in the spectral signal of the SiC samples 4 of 10Pa
It can be seen that obvious atomic features spectral line, illustrates that under conditions of 10Pa, SiC material happens is that master at 1375 DEG C at 288nm
Dynamic oxidation is reacted；And reaction condition is 1375 DEG C, no atomic features at 288nm in the spectral signal of the SiC samples 4 of 100Pa
Spectral line, illustrates at 1375 DEG C, and under conditions of 100Pa, SiC material happens is that passive oxidation reacts.
A kind of contactless online test method of SiC oxidation reactions is present embodiments provided, SiC material can be detected in real time
Oxidation reaction state, relative to by oxidized material take out carry out analysis test method, can be greatly reduced SiC oxidation
It is cost-effective with the experimental amount of later stage material analysis.
Embodiment seven
As shown in figure 11, the embodiment of the present invention seven and embodiment six are essentially identical, and something in common repeats no more, difference
It is to further include：
S3, the reaction condition for changing test zone residing for SiC samples 4, perform step S1 and S2 record differential responses condition
The oxidation type of lower SiC samples 4, determines actively to be oxidizing to the transition point of passive oxidation.
Preferably, before step S1, the surfaces of SiC samples 4 is polished, is put into test zone, and to SiC samples 4 into
Row heating, is heated to oxidizing temperature；In step s3, when detecting 4 near surface of SiC samples generation passive oxidation, gradually reduce
Pressure in the test zone, makes the passive oxidation of 4 near surface of SiC samples towards active oxidation transformation, until according to detection
Spectral signal judge 4 near surface of SiC samples there are Si atoms, the oxidation reaction that SiC occurs is actively to aoxidize.At this time anti-
The transition point that condition is the main passive oxidations of SiC is answered, it is passive that test parameters when record produces spectral signal can obtain SiC master
The changing condition of oxidation.
Specifically, the SiC samples 4 of Φ 12mm × 3mm are used in the present embodiment, are placed in thermally protective materials high-temperature low-pressure dissociation
In oxygen environment experimental rig, SiC samples 4 are heated, are heated to oxidizing temperature (1400~1800 DEG C), and adjust sample stage
Ensure that SiC samples 4 are placed on the central axes of reaction chamber.Then adjusting three-dimensional light path adjustment platform 11 tests 4 near surface of SiC samples
Region and the geometric center of narrow band pass filter 12, focal length convex lens 13 and short focus convex lens 14 are in out on a horizontal line, three
Each eyeglass is moved horizontally on dimension light path adjustment platform 11, it is ensured that the picture of 4 near surface test zone of SiC samples converges at 16 one end of optical fiber
Optical fiber sensor head 15 on；After light path is adjusted, open thermally protective materials high-temperature low-pressure and dissociate oxygen environment experimental rig to target
Temperature and goal pressure, at this time SiC samples 4 oxidation reaction takes place, the spectral signal of material surface oxidation product converges at
In the optical fiber sensor head 15 of 16 one end of optical fiber, 16 other end of optical fiber is connected with 17 entrance of fiber adapter of spectrometer 18, gas phase
The spectral signal of product enters after spectrometer 18 through grating beam splitting with optical fiber 16, and spy is obtained by adjusting 18 grating angle of spectrometer
The wave-length coverage of spectral line is surveyed, the spectral signal after light splitting is converged on 19 detector sensing head of photomultiplier, and response signal passes
Computer is transported to, obtains spectral response signal.If no signal responds, illustrate the passive oxidation that SiC occurs at this time.
In the present embodiment, the specific goal response condition of six samples of A~F is as shown in the table：
The target temperature and target of thermally protective materials high-temperature low-pressure dissociation oxygen environment experimental rig are set according to above table
Pressure, the SiC samples 4 for numbering six Φ 12mm × 3mm for being A~F are tested and record corresponding spectral signal one by one.
It it is 1400 DEG C for reaction condition, the C sample of 50Pa, it is as shown in figure 12 to obtain spectral signal, at this time at 288nm
It can be seen that obvious atomic features spectral line, illustrates under 1400 DEG C, the dissociation oxygen environment of 50Pa, SiC material happens is that master
Dynamic oxidation is reacted.It it is 1500 DEG C for reaction condition, the E samples of 100Pa, obtained spectral signal is as shown in figure 13, equally may be used
It can be seen that obvious atomic features spectral line, illustrates under 1500 DEG C, the dissociation oxygen environment of 100Pa, SiC material at 288nm
It happens is that active oxidation reaction, and the intensity of the atomic features spectral line of E samples is more than C sample in Fig. 3, illustrates E samples actively
The degree of oxidation is apparently higher than C sample.
By the processing of A~F samples corresponding test result analysis, judge the corresponding spectral signal of sample at 288nm whether
There is obvious atomic features spectral line, it can be seen that 1375 DEG C, 20Pa (A samples), 1400 DEG C, 50Pa (C sample), 1500 DEG C,
100Pa (E samples) is main dynamic oxidation, 1375 DEG C, 50Pa (B samples), 1400 DEG C, 100Pa (D samples), 1500 DEG C, 150Pa (F
Sample) it is passive oxidation.According to its reaction condition, the curve that the main passive oxidation of SiC samples 4 changes is drawn, as shown in figure 14.
In Figure 14 transition curve be to the fitting result of active/passive oxidation transformation point, can be with if need to further be verified
Change reaction condition to be tested.The passive oxidation reaction condition close to oxidation transformation curve is selected to be tested, when response is believed
Computer number is transmitted to, and then obtains gas-phase product spectral signal, if no signal responds, illustrate the passive of SiC generations at this time
Oxidation, gradually reduces the pressure in experimental rig, makes passive oxidation towards active oxidation transformation, until spectral signal is captured,
The oxidation reaction that SiC occurs is active oxidation reaction, and pressure and temperature at this time is the transition point of the main passive oxidations of SiC.
Present embodiments provide a kind of contactless online test method of SiC oxidation reactions, can in real time detection temperature and
Under the conditions of pressure consecutive variations, the active/passive oxidation reaction of SiC material, the method tested relative to selected characteristic point, this
The method that embodiment is provided can increase considerably effective experimental data, the active/passive oxidation reaction transformation of detection SiC material
Point, the comparative experimental data completed is provided for the verification of the Theoretical Prediction of oxidation mechanism.Also, the present embodiment is by detecting
The spectral signal intensity of active oxidation reaction product, can inverting active oxidizing reaction rate with oxide isolation, temperature and pressure
Quantitative changing rule, actively aoxidize process variable further to probe into data supporting be provided.
Finally it should be noted that：The above embodiments are merely illustrative of the technical solutions of the present invention, rather than its limitations；Although
The present invention is described in detail with reference to the foregoing embodiments, it will be understood by those of ordinary skill in the art that：It still may be used
To modify to the technical solution described in foregoing embodiments, or equivalent substitution is carried out to which part technical characteristic；
And these modification or replace, do not make appropriate technical solution essence depart from various embodiments of the present invention technical solution spirit and
Scope.
Claims (10)
1. a kind of contactless online test method of SiC oxidation reactions, it is characterised in that comprise the following steps：
S1, the spectral signal by the SiC sample near surface area of space gases in focused light passages real-time detection dissociation oxygen environment；
S2, by analyzing the spectral signal judge that the SiC samples near surface whether there is Si atoms, is then definite described
SiC samples occur actively to aoxidize, and passive oxidation otherwise occurs.
2. the contactless online test method of SiC oxidation reactions according to claim 1, it is characterised in that the side
Method further includes：
S3, the reaction condition for changing test zone residing for SiC samples, perform SiC under the conditions of step S1 and S2 record differential responses
The oxidation type of sample, determines actively to be oxidizing to the transition point of passive oxidation.
3. the contactless online test method of SiC oxidation reactions according to claim 2, it is characterised in that the step
In rapid S3：When detecting SiC samples generation passive oxidation, the pressure in the test zone is gradually reduced, until according to detection
Spectral signal judge SiC sample near surface area of space there are Si atoms, determine at this time as main dynamic oxidation to passive oxidation
Transition point.
4. according to the contactless online test method of SiC oxidation reactions according to any one of claims 1 to 3, its feature
It is, using the real image at lens group convergence SiC sample near surfaces in the step S1, the real image is received by optical fiber and is inputted
In spectrometer, and by inputting computer after photomultiplier；Wherein described lens group is included in test zone residing for SiC samples
The side narrow band pass filter, focal length convex lens and the short focus convex lens that set gradually, the narrow band pass filter, the focal length convex lens
The geometric center of mirror and the short focus convex lens is in same horizontal line with the SiC samples near surface, and level interval is set
Put so that the real image of the SiC samples near surface is converged at the optical fiber sensor head that described optical fiber one end is set, the optical fiber is another
One end is connected by fiber adapter with the input terminal of the spectrometer.
5. according to the contactless online test method of SiC oxidation reactions according to any one of claims 1 to 3, its feature
It is, the SiC samples is placed in thermally protective materials high-temperature low-pressure dissociation oxygen environment experimental rig to carry in the step S1
For dissociating oxygen environment.
A kind of 6. contactless on-line measuring device of SiC oxidation reactions, it is characterised in that：Including at least spectra collection device and
Analytical equipment；
The spectra collection device is used for the near surface area of space gas for the SiC samples that real-time detection is in dissociation oxygen environment
Spectral signal；
The analytical equipment is used to judge that the SiC samples near surface whether there is Si atoms by analyzing the spectral signal,
It is that then the definite SiC samples occur actively to aoxidize, passive oxidation otherwise occurs.
7. the contactless on-line measuring device of SiC oxidation reactions according to claim 6, it is characterised in that：It is described non-
Contact on-line measuring device further includes：
Test device, including environmental chamber and the sample stage being arranged in the environmental chamber, the sample stage is used to place to be measured
SiC samples, the environmental chamber be used for produce different dissociation oxygen environments, and adjust the environment temperature residing for the sample stage and/
Or pressure, the side of the environmental chamber are provided with observation window；
The analytical equipment includes peakology unit, for by analyzing the peak information in the spectral signal, judging institute
State the type that oxidation reaction occurs for SiC samples, and the response intensity of active oxidation reaction.
8. the contactless on-line measuring device of SiC oxidation reactions according to claim 7, it is characterised in that：Described point
Analysis apparatus includes transition point analytic unit, and for the oxidation type by recording SiC samples under the conditions of differential responses, it is passive to determine
It is oxidizing to the transition point of actively oxidation.
9. the contactless on-line measuring device of SiC oxidation reactions according to claim 8, it is characterised in that：Described point
Analysis apparatus includes experimental rig control unit, instructs control environmental chamber to change the anti-of test zone residing for SiC samples for sending
Answer condition；
The transition point analytic unit passes through experimental rig control unit when detecting SiC samples near surface generation passive oxidation
The pressure in the test zone is gradually reduced, until judging that SiC samples near surface is former there are Si according to the spectral signal of detection
Son.
10. the contactless on-line measuring device of the SiC oxidation reactions according to any one of claim 6~9, its feature
It is：The spectra collection device includes lens group, optical fiber, spectrometer and photomultiplier；The lens group is included in SiC examinations
Narrow band pass filter, focal length convex lens and the short focus convex lens that the side of test zone residing for sample is set gradually, the narrow-band-filter
The geometric center of piece, the focal length convex lens and the short focus convex lens is in same horizontal line with the SiC samples near surface
On, and level interval is set so that the real image of the SiC samples near surface converges at the Fibre Optical Sensor that described optical fiber one end is set
At head；The optical fiber other end is connected by fiber adapter with the input terminal of the spectrometer, and the output terminal of spectrometer passes through
The analytical equipment is connected to after photomultiplier.
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