CN102175665B - Experiment device for simulating atomic oxygen oxidation ground of super-high temperature heat-protection material - Google Patents
Experiment device for simulating atomic oxygen oxidation ground of super-high temperature heat-protection material Download PDFInfo
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Abstract
The invention relates to an experiment device for simulating atomic oxygen oxidation ground of a super-high temperature heat-protection material, and the device provided by the invention can be used for solving the problem that no device capable of simulating the high-temperature, low-pressure and atomic oxygen oxidation environments exists, and is suitable for simulating the atomic oxygen oxidation environment of the super-high temperature heat-protection material in different states. The experiment device provided by the invention comprises a quartz tube, an atomic oxygen generating device, an electromagnetic induction heating device and a pressure control device, wherein the output end of the atomic oxygen generating device is connected to the atomic oxygen input end of the quartz tube; the air output end of the quartz tube is connected with the air input end of the pressure control device; and the output end of the heating device is respectively connected with one input end of the induction heating coil which is sheathed on the external wall of the middle of the quartz tube. The experiment device provided by the invention meets the experiment requirements of the atomic oxygen oxidation of the heat-protection material of a hypersonic aircraft at the temperature of 1000-2000 DEG C and the pressure of 10-5000Pa and is suitable for the oxidation action research under the atomic oxygen environment of the high-temperature material.
Description
Technical field
The present invention relates to experiment device for simulating atomic oxygen oxidation ground of super-high temperature heat-protection material.
Background technology
Earth orbital flight device and other celestial body detecting devices, such as lunar orbiter, reenter and be about first, the second cosmic velocity, the reentry velocity of intercontinental missile bullet is about 7km/s, aircraft has very high initial kinetic energy when reentering, be subjected to simultaneously the terrestrial gravitation field action, also has high potential energy, along with the decline of height, these energy change into kinetic energy, and aircraft will have very high flying speed, in the high-speed flight process, aircraft surface contacts with air, causes sharply compression and temperature rises rapidly of gas volume, so that the hypersonic aircraft surface temperature is near 2000 ℃; In the aerocraft real flight course, since the high-speed flight characteristics determined gas on vehicle construction material surface owing to Fast Compression is dissociated into plasma environment, the activity of this plasma induced by atomic oxygen will be far above the air under the state of nature, so under the plasma environment elemental oxygen to the oxidation of material apparently higher than air, the antioxygenic property of hypersonic aircraft surfacing under true Service Environment is a critical problem always, and the various countries scholar has carried out a large amount of experimental studies to this, but the oxidation of practical study hypersonic aircraft surfacing is limited by the restriction of equipment, carries out oxidation experiment research and can't form atomic oxygen environment; What various countries' scholar's research oxidation was adopted usually all is the air of a standard atmospheric pressure, and aircraft is along with the variation of flying height, the air pressure of its flight experience obviously reduces, and does not simulate the experimental provision of superhigh temperature heat insulation material under the high temperature under the true Service Environment, low pressure, elemental oxygen well-oxygenated environment at present.
Summary of the invention
The present invention is in order to solve the problem of the experimental provision of also not simulating at present the high temperature of superhigh temperature heat insulation material under true Service Environment, low pressure, elemental oxygen oxidation, and then a kind of experiment device for simulating atomic oxygen oxidation ground of super-high temperature heat-protection material is provided.The purpose of this invention is to provide the atomic oxygen environment of a kind of basic reproduction conduction superhigh temperature thermally protective materials under hypersonic service condition, and can carry out easily the device that parameter regulates to study material atomic oxygen oxidation behavior under the different conditions.
Experiment device for simulating atomic oxygen oxidation ground of super-high temperature heat-protection material, it comprises quartz ampoule 1, elemental oxygen generating means 2, electromagnetic induction heater 3 and pressure control device 4, the output terminal of elemental oxygen generating means 2 is connected to the elemental oxygen input end of quartz ampoule 1, the air output terminal of quartz ampoule 1 is connected to the air input end of pressure control device 4, and the output terminal difference adapter sleeve of electromagnetic induction heater 3 is at an input end of the load coil 9 of quartz ampoule 1 middle part outer wall.
The present invention is directed to the experimental provision of transition metal boride based ultra-high temperature heat insulation material elemental oxygen oxidation susceptibility research under the hypersonic flight plasma ambient, the present invention also is applicable to have the elemental oxygen oxidation behavior research work of other high-temperature materials of excellent conductive performance.Satisfied temperature of the present invention between 1000～2000 ℃, the requirement of experiment of the elemental oxygen oxidation of the hypersonic aircraft heat insulation material of pressure between 10～5000Pa.
Description of drawings
Fig. 1 is the structural representation of apparatus of the present invention, Fig. 2 is the structural representation of elemental oxygen generating means of the present invention, Fig. 3 is the structural representation of pressure control device of the present invention, Fig. 4 is the structural representation of electromagnetic induction heater of the present invention, Fig. 5 is the schematic diagram of apparatus of the present invention, and Fig. 6 is that specimen size of the present invention is Φ 10 * 3mm
3The time experimentation temperature and pressure curve map (fine rule representation temperature curve, thick line representative pressure curve among the figure, the line style among Fig. 8, Figure 10, Figure 12, Figure 14 herewith), Fig. 7 is that specimen size of the present invention is Φ 10 * 3mm
3The time experiment induced by atomic oxygen utilizing emitted light spectrogram, Fig. 8 is that specimen size of the present invention is Φ 15 * 4mm
3The time experimentation temperature and pressure curve map, Fig. 9 is that specimen size of the present invention is Φ 15 * 4mm
3The time experiment induced by atomic oxygen utilizing emitted light spectrogram, Figure 10 is that specimen size of the present invention is Φ 20 * 3mm
3The time experimentation temperature and pressure curve map, Figure 11 is that specimen size of the present invention is Φ 20 * 3mm
3The time experiment induced by atomic oxygen utilizing emitted light spectrogram, Figure 12 specimen size of the present invention is Φ 25 * 4mm
3The time experimentation temperature and pressure curve map, Figure 13 is that specimen size of the present invention is Φ 25 * 4mm
3The time experiment induced by atomic oxygen utilizing emitted light spectrogram, Figure 14 is that specimen size of the present invention is Φ 30 * 3mm
3The time experimentation temperature and pressure curve map, Figure 15 is that specimen size of the present invention is Φ 30 * 3mm
3The time experiment induced by atomic oxygen utilizing emitted light spectrogram.
Embodiment
Embodiment one
In conjunction with Fig. 1, Fig. 5 present embodiment is described, it comprises quartz ampoule 1, elemental oxygen generating means 2, electromagnetic induction heater 3 and pressure control device 4 present embodiment, the elemental oxygen output terminal of elemental oxygen generating means 2 is connected to the elemental oxygen input end of quartz ampoule 1, the air output terminal of quartz ampoule 1 is connected to the air input end of pressure control device 4, and the output terminal difference adapter sleeve of electromagnetic induction heater 3 is at an input end of the load coil 9 of quartz ampoule 1 middle part outer wall.
This experimental provision is a kind of environment that can reproduce the high temperature of hypersonic aircraft in flight course, low pressure, elemental oxygen, experimental provision to the research of electric conductivity heat insulation material oxidation behavior, it is 1000～2000 ℃ that this experimental provision can adapt in temperature range, pressure is the experiment in 10～5000Pa scope, and this device can produce microwave power 0～1500W.
Embodiment two
In conjunction with Fig. 2, Fig. 5 illustrates present embodiment, the elemental oxygen generating means 2 of present embodiment comprises welding bottle 18, reduction valve 17, flowrate control valve 14, microwave generator 5, jet vectoring valve 15 and excitation cavity 16, the output terminal of welding bottle 18 is connected to the input end of reduction valve 17, the output terminal of reduction valve 17 is connected to the input end of flowrate control valve 14, the oxygen output terminal of flowrate control valve 14 is connected to the oxygen input end of microwave generator 5, the output terminal of microwave generator 5 is connected to the input end of jet vectoring valve 15, the output terminal of jet vectoring valve 15 is connected to the input end of excitation cavity 16, and the output terminal of excitation cavity 16 is connected to the elemental oxygen input end of quartz ampoule 1.Other composition is identical with embodiment one with annexation.
Embodiment three
In conjunction with Fig. 3, Fig. 5 present embodiment is described, the pressure control device 4 of present embodiment comprises vacuum pump 10, gas outlet 11, thermocouple vacuum gauge 12 and pressure-sensitive vacuum meter 13, the air output terminal of quartz ampoule 1 is connected to the air input end of vacuum pump 10, the air output terminal of vacuum pump 10 is connected to the air input end of gas outlet 11, and the internal pressure signal output part of quartz ampoule 1 is connected to the input end of thermocouple vacuum gauge 12 and pressure-sensitive vacuum meter 13.Other composition is identical with embodiment one with annexation.
Embodiment four
In conjunction with Fig. 4, Fig. 5 present embodiment is described, the electromagnetic induction heater 3 of present embodiment comprises two colorimetric infrared pyrometers 6 and induction heating power 7, adapter sleeve is at an input end of the load coil 9 of quartz ampoule 1 middle part outer wall respectively for the output terminal of induction heating power 7, and two colorimetric infrared pyrometers 6 are suspended on the top of quartz ampoule 1 and camera lens and quartz ampoule 1 dead in line of two colorimetric infrared pyrometers 6.Other composition is identical with embodiment one with annexation.
Embodiment five
In conjunction with Fig. 4, Fig. 5 present embodiment is described, not being both it and also comprising plus lens 21, optical fiber 20 and spectrometer 8 of present embodiment and embodiment four, the spectrum of quartz ampoule 1 induced by atomic oxygen focuses on the spectrum input end of optical fiber 20 through plus lens 21, the spectrum output terminal of optical fiber 20 is connected to the spectrum input end of spectrometer 8.Other composition is identical with embodiment one with annexation.
Embodiment six
In conjunction with Fig. 4, Fig. 5 present embodiment is described, not being both it and also comprising cooling device 19 of present embodiment and embodiment five, load coil 9 is that the hollow copper tubing coiling forms, the cooling water circulation in-out end of hollow copper tubing is communicated with by the two ends of high-pressure water pipe with cooling device 19 respectively, excitation cavity 16 is arranged in the cooling jacket, and the cooling water circulation in-out end of cooling jacket is communicated with the turnover water end (W.E.) of cooling device 19 by high-pressure water pipe respectively.Other composition is identical with embodiment one with annexation.
The object of the present invention is achieved like this: it comprises microwave generator 5, and microwave energy forms the elemental oxygen jet body through waveguide transmission system to the resonator cavity energized oxygen and enters quartz ampoule 1 reaction zone; Control pressurer system 4 links to each other with quartz ampoule 1 with microwave generator 5 respectively by corrugated tube, and by control pressurer system 4 control reacting gas flow velocity and quartz ampoule 1 reaction zone internal pressures; Experimental stand places in the quartz ampoule 1; Load coil 9 is enclosed within quartz ampoule 1 outer wall and parallel with stand, and load coil 9 links to each other with induction heating power 7 and control system; The excitation cavity of microwave generator 5, transmission system, reaction chamber, pressure vacuum pump 10, induction heating power 7 and load coil 9 link to each other with cooling device 19 by high-pressure water pipe; Two colorimetric infrared pyrometers 6 hang on the upper end of quartz ampoule 1, and link to each other with controller; Tested zirconium boride-carborundum ceramic matric composite test specimen polishes smooth, and surface smoothness is lower than 1 μ m, and clamping places the elemental oxygen flow field to stand; High temperature atomic oxygen flow field focuses on by long burnt plus lens 21, images in the end face of silica fibre 20, and signal carries out data communication by optical fiber 20 input spectrum instrument 8 and with computing machine.
Regulate pressure control device 4 and microwave generator 5 regulating and controlling reaction zone environmental pressures, elemental oxygen jet velocity, regulate induction heating current Control Assay heating rate and surface heating temperature, reproduce heat insulation material surface atom oxygen oxidation behavior in the hypersonic flight plasma ambient, spectrometer 8, pressure control device 4 and electromagnetic induction heater 3 all carry out exchanges data by data line and computing machine, realize Real-time Measuring quantitative response district environmental pressure, elemental oxygen intensity and specimen surface temperature data.
Elemental oxygen test platform fine position assembly is comprised of helical riser, horizontal translation platform (having connected the micrometer screw mandrel), on the horizontal translation platform aperture is set, by jackscrew one end of optical fiber 20 is fixed, the fine position assembly can be regulated height and the horizontal level of optical fiber 20, degree of regulation is 0.01mm, described imaging plus lens 21 and optical fiber 20 are installed on the guide rail by regulating support respectively, and plus lens 21 and optical fiber 20 can move freely at moving guide rail.
Specific embodiment one:
In conjunction with Fig. 6, Fig. 7 present embodiment is described, the experiment exemplar that present embodiment adopts the zirconium boride-carborundum ceramic matric composite to make is of a size of Φ 10 * 3mm
3, adopt diamond paste that the exemplar surface finish is lower than below the 1 μ m to smooth finish.Sample after the polishing is put on the experimental stand of airtight quartz ampoule 1 two colorimetric infrared pyrometers 6 registration coupon centers; Preset 1100 ℃ of sample microwave oxidizing temperatures, the pressure in the quartz ampoule 1 is controlled at 2000Pa, and microwave generator anode current value is controlled at 200mA.Experimental period is 17 minutes, and experimentation temperature and pressure control curve as shown in Figure 6; The elemental oxygen emission spectrum as shown in Figure 7; In the experimentation, the specimen surface temperature is 1100 ± 10 ℃ of fluctuations, from Fig. 6, can obviously find out the fluctuation of temperature, for the temperature stability of oxy-acetylene (200 ℃ of temperature fluctuations) or other high-temperature heaters (20～30 ℃ of temperature fluctuations), this experimental provision temperature reliability is high; Pressure is in 2000 ± 10Pa fluctuation, and collecting the elemental oxygen wavelength is 844.61nm, and relative intensity is 3668;
Specific embodiment two:
In conjunction with Fig. 8, Fig. 9 present embodiment is described, the experiment exemplar that present embodiment adopts the zirconium boride-carborundum ceramic matric composite to make is of a size of Φ 15 * 4mm
3, adopt diamond paste that the exemplar surface finish is lower than below the 1 μ m to smooth finish.Sample after the polishing is put on the experimental stand of airtight quartz ampoule 1 two colorimetric infrared pyrometers 6 registration coupon centers; Preset 1200 ℃ of sample microwave oxidizing temperatures, the pressure in the quartz ampoule 1 is controlled at 1000Pa, and microwave generator anode current value is controlled at 240mA.Experimental period is 15 minutes, and experimentation temperature and pressure control curve as shown in Figure 8; The elemental oxygen emission spectrum as shown in Figure 9; In the experimentation, the specimen surface temperature is 1200 ± 15 ℃ of fluctuations, from Fig. 8, can obviously find out the fluctuation of temperature, for the temperature stability of oxy-acetylene (200 ℃ of temperature fluctuations) or other high-temperature heaters (20～30 ℃ of temperature fluctuations), this experimental provision temperature reliability is high; Pressure is in 1000 ± 10Pa fluctuation, and collecting the elemental oxygen wavelength is 844.61nm, and relative intensity is 4649;
Specific embodiment three:
In conjunction with Figure 10, Figure 11 present embodiment is described, the experiment exemplar that present embodiment adopts the zirconium boride-carborundum ceramic matric composite to make is of a size of Φ 20 * 3mm
3, adopt diamond paste that the exemplar surface finish is lower than below the 1 μ m to smooth finish.Sample after the polishing is put on the experimental stand of airtight quartz ampoule 1 two colorimetric infrared pyrometers 6 registration coupon centers; Preset 1300 ℃ of sample microwave oxidizing temperatures, the pressure in the quartz ampoule 1 is controlled at 500Pa, and microwave generator anode current value is controlled at 270mA.Experimental period is 16 minutes, and experimentation temperature and pressure control curve as shown in figure 10; The elemental oxygen emission spectrum as shown in figure 11; In the experimentation, the specimen surface temperature is 1300 ± 15 ℃ of fluctuations, from Figure 10, can obviously find out the fluctuation of temperature, for the temperature stability of oxy-acetylene (200 ℃ of temperature fluctuations) or other high-temperature heaters (20～30 ℃ of temperature fluctuations), this experimental provision temperature reliability is high; Pressure is in 500 ± 10Pa fluctuation, and collecting the elemental oxygen wavelength is 844.61nm, and relative intensity is 5149;
Specific embodiment four:
In conjunction with Figure 12, Figure 13 present embodiment is described, the experiment exemplar that present embodiment adopts the zirconium boride-carborundum ceramic matric composite to make is of a size of Φ 25 * 4mm
3, adopt diamond paste that the exemplar surface finish is lower than below the 1 μ m to smooth finish.Sample after the polishing is put on the experimental stand of airtight quartz ampoule 1 two colorimetric infrared pyrometers 6 registration coupon centers; Preset 1400 ℃ of sample microwave oxidizing temperatures, the pressure in the quartz ampoule 1 is controlled at 100Pa, and microwave generator anode current value is controlled at 300mA.Experimental period is 13 minutes, and experimentation temperature and pressure control curve as shown in figure 12; The elemental oxygen emission spectrum as shown in figure 13; In the experimentation, the specimen surface temperature is 1400 ± 20 ℃ of fluctuations, from Figure 12, can obviously find out the fluctuation of temperature, for the temperature stability of oxy-acetylene (200 ℃ of temperature fluctuations) or other high-temperature heaters (20～30 ℃ of temperature fluctuations), this experimental provision temperature reliability is high; Pressure is in 100 ± 5Pa fluctuation, and collecting the elemental oxygen wavelength is 844.61nm, and relative intensity is 5362;
Specific embodiment five:
In conjunction with Figure 14, Figure 15 present embodiment is described, the experiment exemplar that present embodiment adopts the zirconium boride-carborundum ceramic matric composite to make is of a size of Φ 30 * 3mm
3, adopt diamond paste that the exemplar surface finish is lower than below the 1 μ m to smooth finish.Sample after the polishing is put on the experimental stand of airtight quartz ampoule 1 two colorimetric infrared pyrometers 6 registration coupon centers; Preset 1500 ℃ of sample microwave oxidizing temperatures, the pressure in the quartz ampoule 1 is controlled at 40Pa, and microwave generator anode current value is controlled at 350mA.Experimental period is 10 minutes, and experimentation temperature and pressure control curve as shown in figure 14; The elemental oxygen emission spectrum as shown in figure 15; In the experimentation, the specimen surface temperature is 1500 ± 25 ℃ of fluctuations, from Figure 14, can obviously find out the fluctuation of temperature, for the temperature stability of oxy-acetylene (200 ℃ of temperature fluctuations) or other high-temperature heaters (20～30 ℃ of temperature fluctuations), this experimental provision temperature reliability is high; Pressure is in 40 ± 5Pa fluctuation, and collecting the elemental oxygen wavelength is 844.61nm, and relative intensity is 6010.
Claims (1)
1. experiment device for simulating atomic oxygen oxidation ground of super-high temperature heat-protection material, it is characterized in that it comprises quartz ampoule (1), elemental oxygen generating means (2), electromagnetic induction heater (3), pressure control device (4), plus lens (21), optical fiber (20), spectrometer (8) and cooling device (19), the output terminal of elemental oxygen generating means (2) is connected to the elemental oxygen input end of quartz ampoule (1), the air output terminal of quartz ampoule (1) is connected to the air input end of pressure control device (4), and the output terminal adapter sleeve of electromagnetic induction heater (3) is at an input end of the load coil (9) of quartz ampoule (1) middle part outer wall;
Elemental oxygen generating means (2) comprises welding bottle (18), reduction valve (17), flowrate control valve (14), microwave generator (5), jet vectoring valve (15) and excitation cavity (16), the output terminal of welding bottle (18) is connected to the input end of reduction valve (17), the output terminal of reduction valve (17) is connected to the input end of flowrate control valve (14), the oxygen output terminal of flowrate control valve (14) is connected to the oxygen input end of microwave generator (5), the output terminal of microwave generator (5) is connected to the input end of jet vectoring valve (15), the output terminal of jet vectoring valve (15) is connected to the input end of excitation cavity (16), and the output terminal of excitation cavity (16) is connected to the elemental oxygen input end of quartz ampoule (1);
Pressure control device (4) comprises vacuum pump (10), gas outlet (11), thermocouple vacuum gauge (12) and pressure-sensitive vacuum meter (13), the air output terminal of quartz ampoule (1) is connected to the air input end of vacuum pump (10), the air output terminal of vacuum pump (10) is connected to the air input end of gas outlet (11), and the internal pressure signal output part of quartz ampoule (1) is connected to the input end of thermocouple vacuum gauge (12) and pressure-sensitive vacuum meter (13);
Electromagnetic induction heater (3) comprises two colorimetric infrared pyrometers (6) and induction heating power (7), the output terminal adapter sleeve of induction heating power (7) is at an input end of the load coil (9) of quartz ampoule (1) middle part outer wall, and two colorimetric infrared pyrometers (6) are suspended on the top of quartz ampoule (1) and camera lens and quartz ampoule (1) dead in line of two colorimetric infrared pyrometer (6);
The spectrum of quartz ampoule (1) induced by atomic oxygen focuses on the spectrum input end of optical fiber (20) through plus lens (21), the spectrum output terminal of optical fiber (20) is connected to the spectrum input end of spectrometer (8);
Load coil (9) is that the hollow copper tubing coiling forms, the cooling water circulation in-out end of hollow copper tubing is communicated with by the two ends of high-pressure water pipe with cooling device (19) respectively, excitation cavity (16) is arranged in the cooling jacket, and the cooling water circulation in-out end of cooling jacket is communicated with by the turnover water end (W.E.) of high-pressure water pipe with cooling device (19) respectively.
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| CN103234956A (en) * | 2013-04-28 | 2013-08-07 | 哈尔滨工业大学 | Testing device for catalytic coefficient of thermal shielding material and method for testing catalytic coefficient of thermal shielding material by utilizing device |
| CN104375161B (en) * | 2014-11-05 | 2017-02-15 | 北京卫星环境工程研究所 | atomic oxygen beam energy testing system |
| CN105188173B (en) * | 2015-08-05 | 2018-01-16 | 哈尔滨工业大学 | A kind of structure thermal environment simulation method and device based on sensing heating |
| CN108974398B (en) * | 2018-09-18 | 2020-08-11 | 上海空间电源研究所 | Multi-angle atomic oxygen test online monitoring device and monitoring method |
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