CN109030556B - Device and method for measuring normal emissivity of opaque solid material based on heating of solar simulator - Google Patents
Device and method for measuring normal emissivity of opaque solid material based on heating of solar simulator Download PDFInfo
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Abstract
A solar simulator heating-based opaque solid material normal emissivity measuring device and a measuring method relate to a normal emissivity measuring device and a measuring method. The method aims to solve the problem that the method for measuring the high-temperature normal emissivity of the opaque solid material is poor in accuracy. According to the invention, the sample is directly heated through the solar simulator, so that the interference of multiple reflections caused by an optical window in a conventional high-temperature measurement light path on a measurement signal is avoided, and the thermal infrared imager ensures the temperature of the sample to be measured to be uniform; the background spectrum of the emission spectrum is measured before the emission spectrum is measured, the background spectrum is subtracted from the emission spectrum in calculation, the interference of background signals is removed, and the measurement deviation possibly existing between measurement light paths is eliminated through the measurement of the calibration coefficient. The glass screen can reduce the stray radiation of the light source. The method can accurately calculate the high-temperature normal emissivity of the opaque solid material. The method is suitable for measuring the high-temperature normal emissivity of the opaque solid material.
Description
Technical Field
The invention relates to a normal emissivity measuring device and a normal emissivity measuring method.
Background
With the development of the aerospace field, the high temperature application of metal materials and heat-proof and insulating materials is receiving more and more attention. Because radiation heat transfer is dominant under the high-temperature condition, the research on the emission characteristic of the opaque solid material at the high temperature has great significance in the fields of thermal radiation transmission, material performance optimization and the like, and the research on the measurement method of the high-temperature normal emissivity of the opaque solid material is urgently developed.
However, in the currently developed research, an optical window needs to be equipped in a closed high-temperature furnace body heating mode, and multiple reflections of a measurement signal exist in a light path system consisting of the window and a sample, so that the measurement signal is inconsistent with the actual situation; in the existing research, the temperature distribution condition of the surface of the sample to be measured is not specifically considered, and the background signal in the measured radiation intensity signal is not removed, so that the measurement result is deviated from the actual result. Therefore, the accuracy of the extraction of the normal emissivity spectrum of the sample in the existing research is poor.
Disclosure of Invention
The invention provides a device and a method for measuring the normal emissivity of an opaque solid material based on heating of a solar simulator, aiming at solving the problem of poor accuracy of the conventional method for measuring the high-temperature normal emissivity of the opaque solid material.
The invention relates to a solar simulator heating-based opaque solid material normal emissivity measuring device, which comprises a solar simulator, a glass screen, a high-temperature sample support, a thermocouple, a slide rail, a thermal infrared imager, a parabolic reflector, a Fourier infrared spectrometer, a black body furnace, a reflector base, a sample emergent surface shielding device and a thermal imager base;
the sample emergent surface shielding device consists of a front baffle, a rear baffle and a double-track slideway; the front baffle is plate-shaped, the middle part of the front baffle is a cavity, and the side part of the front baffle is provided with a cooling water inlet pipe and a cooling water outlet pipe which are communicated with the cavity; the rear baffle is plate-shaped, the middle part of the rear baffle is a cavity, and the side part of the rear baffle is provided with a cooling water inlet pipe and a cooling water outlet pipe which are communicated with the cavity; the front baffle and the rear baffle are respectively arranged between the two parallel double-rail slideways, the front baffle is arranged in one of the double-rail slideways, and the rear baffle is arranged in the other of the double-rail slideways; a first circular through hole vertical to the front baffle plate surface is formed in the center of the front baffle plate, and a second circular through hole vertical to the rear baffle plate surface is formed in the center of the rear baffle plate;
the solar simulator, the glass screen, the high-temperature sample support and the sample emergent surface shielding device are sequentially arranged on one side of the sliding rail, and the solar simulator is arranged far away from the sliding rail; a front baffle plate in the sample emergent surface shielding device is arranged towards the high-temperature sample support; the black body furnace is arranged on the other side of the slide rail, and the thermal imager base and the reflector base are arranged on the slide rail in parallel; the Fourier infrared spectrometer is arranged at one end of the slide rail, which is provided with the reflector base; a light passing round hole is formed in the center of the glass screen, and a light beam outlet of the solar simulator faces the light passing round hole of the glass screen; the paraboloid reflector is arranged on the reflector base, the upper surface of the reflector base is vertically and fixedly connected with a reflector rotating shaft, and a support of the paraboloid reflector is sleeved on the reflector rotating shaft; a light beam inlet of the Fourier infrared spectrometer is arranged towards the parabolic reflector; the thermal infrared imager is arranged on the thermal imager base; the high-temperature sample support is annular, a sample to be detected is arranged in the high-temperature sample support, and a thermocouple is arranged on the surface of the sample to be detected on one side of the thermal infrared imager; the diameter of the first circular through hole is 50-60 mm;
the glass screen is plate-shaped hollow quartz glass, and a cooling water inlet pipe and a cooling water outlet pipe are arranged on the side edge of the glass screen;
the high-temperature sample support is made of metal, and a heat insulation material is arranged between the annular inner surface of the high-temperature sample support and the sample; the high-temperature sample support is used for fixing a wafer-shaped sample, and the thickness of the sample is 0.1-1 mm; the high-temperature sample support is made of metal, the high-temperature sample support and the sample are separated through a heat insulation material, the heat conductivity of the heat insulation material is low, and the radial heat loss of the sample is reduced; meanwhile, the annular high-temperature sample support has the advantage of enabling the thermal stress and the mechanical stress on the circumference of the sample to be uniformly distributed; the force is evenly distributed, so that the deformation of the sample in the heating process can be prevented, the surface of the sample is a plane when the measurement is carried out, and the influence on the measurement direction can be avoided.
The thermocouple is connected with the computer through a USB data acquisition system; the USB data acquisition system is an OM-DAQ-USB-2400 series USB data acquisition system of American OMEGA company; daqpro software for displaying temperature is installed in the computer;
the bottom of the reflector base is provided with a first sliding chute which is sleeved on the sliding rail; the bottom of the thermal imager base is provided with a second sliding groove, and the second sliding groove is sleeved on the sliding rail.
The method for measuring the normal emissivity by using the device for measuring the normal emissivity of the opaque solid material heated by the solar simulator comprises the following steps:
first, obtain the background spectrum S related to sample emission spectrum measurement optical pathλ,extra；
Moving the reflector base to enable the light of the parabolic reflector, the sample to be detected and the glass screen to pass through the circular hole and the first circular through hole to be on the same straight line, and enabling the light of the glass screen to pass through the center of the circular hole and the center of the first circular through hole to be on the same straight line; the parabolic reflector is rotated to enable radiation light of a sample to be measured at normal temperature to be reflected and enter a light beam inlet of the Fourier infrared spectrometer, and the Fourier infrared spectrometer is used for obtaining a background spectrum S related to an optical path for measuring emission spectrum of the sampleλ,extra；
Secondly, obtaining the equilibrium temperature TsamEmission spectrum S of lower sample to be measuredλ,sam；
Starting a solar simulator, adjusting a high-temperature sample support to enable light emitted by the started solar simulator to be focused on an incident surface of a sample to be measured and form a light spot with the radius of 50-60 mm, and starting to heat the sample to be measured;
moving the thermal imager base to enable the thermal infrared imager to be aligned to the emission surface of the sample to be detected and obtain a temperature distribution image of the emission surface of the sample to be detected; taking a circular area with the temperature deviation within 5% from the central temperature of the image in the temperature distribution image of the emitting surface of the sample to be detected as a temperature uniform area, selecting a rear baffle plate provided with a second circular through hole with the same size as the temperature uniform area, and moving the rear baffle plate until the center of the second circular through hole and the center of the first circular through hole are on the same straight line;
a thermocouple is placed in the emission surface of the sample to be detected and close to the edge position in the temperature uniform area to monitor the temperature of the emission surface of the sample to be detected, and when the temperature fluctuation of the thermocouple is less than 5k, the equilibrium temperature T is reachedsam；
Removing the thermal imager, and moving the light mirror base to enable light of the parabolic reflector, the sample to be detected and the glass screen to pass through the circular holes to be on the same straight line; rotating the parabolic reflector to reflect the radiation light of the sample to be measured into the light beam inlet of the Fourier infrared spectrometer, and acquiring the equilibrium temperature T by using the Fourier infrared spectrometersamEmission spectrum S of lower sample to be measuredλ,sam；
Third, obtain and blackbody spectral measurement optical pathDiameter-dependent background spectrum Sλ,extra,b；
Adjusting the black body furnace to ensure that the distance from the radiation light outlet surface of the black body furnace to the rotary paraboloid reflector is equal to the distance from the emission surface of the sample to be measured to the rotary paraboloid reflector; the radiation light of the black body furnace is reflected to enter a light beam inlet of a Fourier infrared spectrometer by rotating a parabolic reflector, and a background spectrum S related to the optical path of the black body spectrum measurement is obtained by the Fourier infrared spectrometerλ,extra,b；
Fourthly, acquiring the temperature as TbEmission radiation spectrum S of lower blackbody furnaceλ,b(Tb)；
Opening the blackbody furnace and setting the temperature to TbObtaining the temperature T by means of a spectrometerbBlack body radiation spectrum S of lower black body furnaceλ,b(Tb) (ii) a When equilibrium temperature TsamNot more than the upper limit temperature of the blackbody furnace, Tb＝TsamWhen the equilibrium temperature T issamWhen the upper limit temperature of the black body furnace is higher than TbThe upper limit temperature of the black body furnace;
fifthly, acquiring a system calibration coefficient Cλ；
At a temperature TbMoving the black body furnace to the position of the sample to be measured, enabling the radiation light outlet face of the black body furnace to coincide with the emission face of the sample to be measured, rotating the parabolic reflector to enable the radiation light of the black body furnace to be reflected and enter the light beam inlet of the Fourier infrared spectrometer, acquiring the black body radiation spectrum by using the Fourier infrared spectrometer, and enabling the black body radiation spectrum and the temperature obtained in the step four to be TbBlack body radiation spectrum S of lower black body furnaceλ,b(Tb) Making a ratio, and obtaining the ratio which is the system calibration coefficient Cλ；
Sixthly, calculating the emission radiation intensity I of the sample to be measuredλ,sam；
seventhly, calculating the emissivity epsilon (T) of the sample to be measuredsam)；
The Planck function is used for describing the change of the spectral radiation force of a black body along with the wavelength, and the Planck function expression is as follows:
in the formula Iλ,bIs spectral radiant power, and has the unit of W/m3(ii) a λ is wavelength, in m; c. C1Is the first radiant flux of 3.7419 × 10-16W·m2；c2A second radiant flux of 1.4388 × 10-2m·K。
The principle and the beneficial effects of the invention are as follows:
1. the method is suitable for measuring the high-temperature normal emissivity of the opaque solid material, has a simple principle, and can accurately measure the normal emissivity of the opaque solid sample at high temperature. According to the invention, firstly, the uniform heating area of the sample to be measured is determined according to the temperature observation result of the thermal infrared imager, and the uniform temperature of the sample to be measured in the researched area is ensured; secondly, in the measuring process, the distance from the radiant light outlet surface of the black body furnace to the parabolic reflector is adjusted by the black body furnace, so that the distance from the radiant light outlet surface of the black body furnace to the parabolic reflector is equal to the distance from the transmitting surface of the sample to be measured to the parabolic reflector, and the transmission light paths of the black body furnace and the sample to be measured can be completely the same; before measuring the emission spectrum, measuring the background spectrum, and subtracting the background spectrum from the emission spectrum in actual calculation to remove the interference of background signals so as to ensure the reliability of the calculation result; in addition, through the measurement of the calibration coefficient, the measurement deviation possibly existing between the two measurement light paths is eliminated. The glass screen can shield stray radiation of a light source; therefore, the method can accurately calculate the high-temperature normal emissivity of the opaque and opaque solid material of the sample; the invention can adjust the heating temperature of the sample to be measured by adjusting the output power of the solar simulator, thereby adjusting the measurement temperature, wherein the measurement temperature reaches 1800K.
2. The sample emergent face shielding device comprises a front baffle and a rear baffle, when a temperature uniform area on a sample to be measured is determined, the rear baffle provided with a second round through hole with the same size as the temperature uniform area is selected, and the rear baffle is arranged between the parabolic reflector and the sample to be measured, so that the temperature uniformity of the sample in a measurement area can be ensured, and the radiation interference of a peripheral area on the side of a sample slideway on a measurement signal can be eliminated;
3. the invention is an open type measuring device, optical windows are not arranged on two sides of a sample to be measured, the sample is directly heated through the solar simulator, the interference of multiple reflections caused by the optical windows to measuring signals is avoided, and the measuring precision is high.
Drawings
FIG. 1 is a schematic diagram of the apparatus of the present invention;
fig. 2 is a schematic structural view of the glass screen 2;
FIG. 3 is a cross-sectional view of FIG. 2;
FIG. 4 is a schematic view of an emission surface of a sample 4 to be measured; in the figure, a is an emission surface of a sample 4 to be measured, b is a thermocouple 5, and c is a spectrometer monitoring area;
FIG. 5 is a schematic structural diagram of the sample exit surface shielding device 21;
FIG. 6 is a cross-sectional view of the dual rail slide 18 in the sample exit face shielding apparatus 21;
FIG. 7 is a calibration coefficient curve obtained in step five of example 1; as can be seen from fig. 7, the system calibration factor obtained in step five of example 1 is approximately 1;
FIG. 8 is a normal emissivity curve of a 6h-SiC sample obtained in example 1; as can be seen from FIG. 8, under the temperature condition of 800K, the emission spectrum of the sample is in the wave band range of 3-10 μm, and the normal emissivity is gradually increased along with the increase of the wavelength; within a wave band of 10-12.5 microns, the normal emissivity shows a sharp reduction trend along with the wavelength and reaches a minimum value at a position of 12.5 microns, and then the normal emissivity gradually increases along with the increase of the wavelength.
The specific implementation mode is as follows:
the technical scheme of the invention is not limited to the specific embodiments listed below, and any reasonable combination of the specific embodiments is included.
The first embodiment is as follows: this embodiment is based on opaque solid material normal emissivity measuring device of solar simulator heating
The device comprises a solar simulator 1, a glass screen 2, a high-temperature sample support 3, a thermocouple 5, a slide rail 7, a thermal infrared imager 8, a parabolic reflector 9, a Fourier infrared spectrometer 10, a black body furnace 11, a reflector base 12, a sample emergent surface shielding device 21 and a thermal imager base 13;
the sample emergent surface shielding device 21 is composed of a front baffle plate 17, a rear baffle plate 16 and a double-track slideway 18; the front baffle 17 is plate-shaped, the middle part of the front baffle 17 is a cavity, and the side part of the front baffle 17 is provided with a cooling water inlet pipe and a cooling water outlet pipe which are communicated with the cavity; the rear baffle 16 is plate-shaped, the middle part of the rear baffle 16 is a cavity, and the side part of the rear baffle 16 is provided with a cooling water inlet pipe and a cooling water outlet pipe which are communicated with the cavity; the front baffle 17 and the rear baffle 16 are respectively arranged between two parallel double-rail slideways 18, the front baffle 17 is arranged in one of the double-rail slideways 18, and the rear baffle 16 is arranged in the other slideway of the double-rail slideways 18;
a first circular through hole 20 vertical to the plate surface of the front baffle 17 is formed in the center of the front baffle 17, and a second circular through hole 19 vertical to the plate surface of the rear baffle 16 is formed in the center of the rear baffle 16;
the solar simulator 1, the glass screen 2, the high-temperature sample support 3 and the sample emergent surface shielding device 21 are sequentially arranged on one side of the sliding rail 7, and the solar simulator 1 is arranged far away from the sliding rail 7; the front baffle 17 in the sample emergent surface shielding device 21 is arranged towards the high-temperature sample support 3; the black body furnace 11 is arranged on the other side of the slide rail 7, and the thermal imager base 13 and the reflector base 12 are arranged on the slide rail 7 in parallel; the Fourier infrared spectrometer 10 is arranged at one end of the slide rail 7, which is provided with a reflector base 12; a light passing circular hole is formed in the center of the glass screen 2, and a light beam outlet of the solar simulator 1 faces the light passing circular hole of the glass screen 2; the parabolic reflector 9 is arranged on the reflector base 12, the upper surface of the reflector base 12 is vertically and fixedly connected with a reflector rotating shaft 15, and a support of the parabolic reflector 9 is sleeved on the reflector rotating shaft 15; the light beam inlet of the Fourier infrared spectrometer 10 is arranged towards the parabolic reflector 9; the thermal infrared imager 8 is arranged on the thermal imager base 13; the high-temperature sample support 3 is annular, a sample 4 to be measured is arranged in the high-temperature sample support 3, and a thermocouple 5 is arranged on the surface of the sample 4 to be measured on one side of the thermal infrared imager 8;
the diameter of the first circular through hole 20 is 50-60 mm.
The principle and the beneficial effects of the implementation mode are as follows:
1. the method is suitable for measuring the high-temperature normal emissivity of the opaque solid material, is simple in principle, and can accurately measure the normal emissivity of the opaque solid sample at high temperature. According to the invention, firstly, the uniform heating area of the sample 4 to be measured is determined according to the temperature observation result of the thermal infrared imager 8, and the uniform temperature of the sample 4 to be measured in the researched area is ensured; secondly, in the measuring process, the distance from the radiation light outlet surface of the black body furnace 11 to the parabolic reflector 9 is equal to the distance from the emission surface of the sample 4 to be measured to the parabolic reflector 9 by adjusting the black body furnace 11, so that the transmission light paths of the black body furnace 11 and the sample 4 to be measured can be completely the same; before measuring the emission spectrum, measuring the background spectrum, and subtracting the background spectrum from the emission spectrum in actual calculation to remove the interference of background signals so as to ensure the reliability of the calculation result; in addition, through the measurement of the calibration coefficient, the measurement deviation possibly existing between the two measurement light paths is eliminated. The glass screen 2 provided by the embodiment can shield stray radiation of a light source; therefore, the embodiment can accurately calculate the high-temperature normal emissivity of the opaque and opaque solid material of the sample; the heating temperature of the sample 4 to be measured can be adjusted by adjusting the output power of the solar simulator 1, so that the measurement temperature can be adjusted to 1800K.
2. In the embodiment, the sample emergent face shielding device 21 is composed of a front baffle 17 and a rear baffle 16, after the temperature uniform area on the sample 4 to be measured is determined, the rear baffle 16 provided with a second round through hole 19 with the same size as the temperature uniform area is selected, and the rear baffle 16 is arranged between the parabolic reflector 9 and the sample 4 to be measured, so that the temperature uniformity of the sample in the measurement area can be ensured, and the radiation interference of the peripheral area on the side of the sample slideway on the measurement signal can be eliminated;
3. the embodiment is an open type measuring device, optical windows are not arranged on two sides of a sample to be measured 4, the sample is directly heated through a solar simulator, interference of multiple reflections caused by the optical windows on measuring signals is avoided, and the measuring precision is high.
The second embodiment is as follows: the first difference between the present embodiment and the specific embodiment is: the glass screen 2 is a plate-shaped hollow quartz glass, and a cooling water inlet pipe and a cooling water outlet pipe are arranged on the side edge of the glass screen 2. Other steps and parameters are the same as in the first embodiment.
The third concrete implementation mode: the present embodiment differs from the first or second embodiment in that: and a heat insulating material is arranged between the annular inner surface of the high-temperature sample support 3 and the sample. Other steps and parameters are the same as in the first or second embodiment.
The fourth concrete implementation mode: the difference between this embodiment mode and one of the first to third embodiment modes is: the high-temperature sample support 3 is made of metal. Other steps and parameters are the same as in one of the first to third embodiments. The high-temperature sample support 3 is used for fixing a wafer-shaped sample, and the thickness of the sample is 0.1-1 mm; the high-temperature sample support 3 is made of metal, the high-temperature sample support 3 is separated from a sample through a heat insulation material, the heat conductivity of the heat insulation material is low, and the radial heat loss of the sample is reduced; meanwhile, the annular high-temperature sample support 3 has the advantage of enabling the thermal stress and the mechanical stress on the circumference of the sample to be uniformly distributed; the force is evenly distributed, so that the deformation of the sample in the heating process can be prevented, the surface of the sample is a plane when the measurement is carried out, and the influence on the measurement direction can be avoided.
The fifth concrete implementation mode: the difference between this embodiment and one of the first to fourth embodiments is: and the thermocouple 5 is connected with a computer through a USB data acquisition system. Other steps and parameters are the same as in one of the first to fourth embodiments.
The sixth specific implementation mode: the difference between this embodiment and one of the first to fifth embodiments is: the bottom of the reflector base 12 is provided with a first sliding chute which is sleeved on the sliding rail 7; the bottom of the thermal imager base 13 is provided with a second sliding groove which is sleeved on the sliding rail 7. Other steps and parameters are the same as in one of the first to fifth embodiments.
The seventh embodiment: the method for measuring the normal emissivity of the opaque solid material based on the solar simulator heating by using the device for measuring the normal emissivity is characterized by comprising the following steps of: the method comprises the following steps:
first, obtain the background spectrum S related to sample emission spectrum measurement optical pathλ,extra；
Moving the reflector base 12 to enable the parabolic reflector 9, the sample 4 to be detected and the glass screen 2 to pass through the circular hole and the first circular through hole 20 to be on the same straight line, and enabling the glass screen 2 to pass through the center of the circular hole and the center of the first circular through hole 20 to be on the same straight line; the parabolic reflector 9 is rotated to reflect the radiation light of the sample 4 to be measured at normal temperature to enter the light beam inlet of the Fourier infrared spectrometer 10, and the Fourier infrared spectrometer 10 is utilized to obtain the background spectrum S related to the sample emission spectrum measurement optical pathλ,extra；
Secondly, obtaining the equilibrium temperature TsamEmission spectrum S of lower sample 4 to be measuredλ,sam；
Starting the solar simulator 1, adjusting the high-temperature sample support 3 to enable light emitted by the started solar simulator 1 to be focused on an incident surface of a sample 4 to be measured and form a light spot with the radius of 50-60 mm, and starting to heat the sample 4 to be measured;
moving the thermal imager base 13 to enable the thermal infrared imager 8 to be aligned to the emission surface of the sample 4 to be detected and obtain a temperature distribution image of the emission surface of the sample 4 to be detected; taking a circular area with the temperature deviation within 5% from the central temperature of the image in the temperature distribution image of the emitting surface of the sample 4 to be detected as a temperature uniform area, selecting a rear baffle 16 provided with a second circular through hole 19 with the same size as the temperature uniform area, and moving the rear baffle 16 until the center of the second circular through hole 19 and the center of the first circular through hole 20 are on the same straight line;
the thermocouple 5 is placed in the temperature uniform area in the emission surface of the sample 4 to be detected to be close to the edge position to monitor the temperature of the emission surface of the sample 4 to be detected, and when the temperature fluctuation of the thermocouple 5 is less than 5k, the equilibrium temperature T is reachedsam；
The thermal imager 8 is removed, and the light mirror base 12 is moved until the light of the parabolic reflector 9, the sample 4 to be detected and the glass screen 2 passes through the circular holes and is on the same straight line; the parabolic reflector 9 is rotated to enable the radiation light of the sample 4 to be measured to be reflected and enter the light beam inlet of the Fourier infrared spectrometer 10, and the Fourier infrared spectrometer 10 is utilized to obtain the equilibrium temperature TsamEmission spectrum S of lower sample 4 to be measuredλ,sam；
Thirdly, acquiring a background spectrum S related to the blackbody spectrum measurement optical pathλ,extra,b；
Adjusting the black body furnace 11 to ensure that the distance from the radiant light outlet surface of the black body furnace 11 to the rotary paraboloid reflecting mirror 9 is equal to the distance from the emission surface of the sample 4 to be measured to the rotary paraboloid reflecting mirror 9; the parabolic reflector 9 is rotated to enable radiation light of the black body furnace 11 to be reflected and enter a light beam inlet of the Fourier infrared spectrometer 10, and the Fourier infrared spectrometer 10 is used for obtaining a background spectrum S related to the optical path of the black body spectrum measurementλ,extra,b；
Fourthly, acquiring the temperature as TbEmission radiation spectrum S of lower blackbody furnace 11λ,b(Tb)；
The blackbody furnace 11 is turned on and the temperature is set to TbThe temperature T is acquired by the spectrometer 10bBlackbody radiation spectrum S of lower blackbody furnace 11λ,b(Tb) (ii) a When equilibrium temperature TsamNot more than the upper limit temperature of the blackbody furnace 11, Tb＝TsamWhen the equilibrium temperature T issamGreater than the upper limit temperature of the blackbody furnace 11, TbThe upper limit temperature of the blackbody furnace 11;
fifthly, acquiring a system calibration coefficient Cλ；
At a temperature TbThen, the blackbody furnace 11 is moved to the position of the sample 4 to be measured, and the black color is changedThe radiant light outlet surface of the body furnace 11 coincides with the emission surface of the sample 4 to be measured, the parabolic reflector 9 is rotated to enable the radiant light of the body furnace 11 to be reflected and enter the light beam inlet of the Fourier infrared spectrometer 10, the Fourier infrared spectrometer 10 is used for obtaining the black body radiation spectrum, and the temperature obtained in the fourth step are TbBlackbody radiation spectrum S of lower blackbody furnace 11λ,b(Tb) Making a ratio, and obtaining the ratio which is the system calibration coefficient Cλ；
Sixthly, calculating the emission radiation intensity I of the sample 4 to be measuredλ,sam；
seventhly, calculating the emissivity epsilon (T) of the sample 4 to be measuredsam)；
The principle and the beneficial effects of the implementation mode are as follows:
1. the method is suitable for measuring the high-temperature normal emissivity of the opaque solid material, is simple in principle, and can accurately measure the normal emissivity of the opaque solid sample at high temperature. According to the invention, firstly, the uniform heating area of the sample 4 to be measured is determined according to the temperature observation result of the thermal infrared imager 8, and the uniform temperature of the sample 4 to be measured in the researched area is ensured; secondly, in the measuring process, the distance from the radiation light outlet surface of the black body furnace 11 to the parabolic reflector 9 is equal to the distance from the emission surface of the sample 4 to be measured to the parabolic reflector 9 by adjusting the black body furnace 11, so that the transmission light paths of the black body furnace 11 and the sample 4 to be measured can be completely the same; before measuring the emission spectrum, measuring the background spectrum, and subtracting the background spectrum from the emission spectrum in actual calculation to remove the interference of background signals so as to ensure the reliability of the calculation result; in addition, through the measurement of the calibration coefficient, the measurement deviation possibly existing between the two measurement light paths is eliminated. The glass screen 2 provided by the embodiment can shield stray radiation of a light source; therefore, the embodiment can accurately calculate the high-temperature normal emissivity of the opaque and opaque solid material of the sample;
2. in the embodiment, the sample emergent face shielding device 21 is composed of a front baffle 17 and a rear baffle 16, after the temperature uniform area on the sample 4 to be measured is determined, the rear baffle 16 provided with a second round through hole 19 with the same size as the temperature uniform area is selected, and the rear baffle 16 is arranged between the parabolic reflector 9 and the sample 4 to be measured, so that the temperature uniformity of the sample in the measurement area can be ensured, and the radiation interference of the peripheral area on the side of the sample slideway on the measurement signal can be eliminated;
3. the embodiment is an open type measuring device, optical windows are not arranged on two sides of a sample to be measured 4, the sample is directly heated through a solar simulator, interference of multiple reflections caused by the optical windows on measuring signals is avoided, and the measuring precision is high.
The specific implementation mode is eight: the seventh embodiment is different from the seventh embodiment in that: the Planck function is used for describing the change of the spectral radiation force of the black body along with the wavelength, and the Planck function expression is as follows:
The following examples were used to demonstrate the beneficial effects of the present invention:
example 1:
the device for measuring the normal emissivity of the opaque solid material based on the heating of the solar simulator comprises the solar simulator 1, a glass screen 2, a high-temperature sample support 3, a thermocouple 5, a slide rail 7, a thermal infrared imager 8, a parabolic reflector 9, a Fourier infrared spectrometer 10, a black body furnace 11, a reflector base 12, a sample emergent face shielding device 21 and a thermal imager base 13;
the sample emergent surface shielding device 21 is composed of a front baffle plate 17, a rear baffle plate 16 and a double-track slideway 18; the front baffle 17 is plate-shaped, the middle part of the front baffle 17 is a cavity, and the side part of the front baffle 17 is provided with a cooling water inlet pipe and a cooling water outlet pipe which are communicated with the cavity; the rear baffle 16 is plate-shaped, the middle part of the rear baffle 16 is a cavity, and the side part of the rear baffle 16 is provided with a cooling water inlet pipe and a cooling water outlet pipe which are communicated with the cavity; the front baffle 17 and the rear baffle 16 are respectively arranged between two parallel double-rail slideways 18, the front baffle 17 is arranged in one of the double-rail slideways 18, and the rear baffle 16 is arranged in the other slideway of the double-rail slideways 18;
a first circular through hole 20 vertical to the plate surface of the front baffle 17 is formed in the center of the front baffle 17, and a second circular through hole 19 vertical to the plate surface of the rear baffle 16 is formed in the center of the rear baffle 16;
the solar simulator 1, the glass screen 2, the high-temperature sample support 3 and the sample emergent surface shielding device 21 are sequentially arranged on one side of the sliding rail 7, and the solar simulator 1 is arranged far away from the sliding rail 7; the front baffle 17 in the sample emergent surface shielding device 21 is arranged towards the high-temperature sample support 3; the black body furnace 11 is arranged on the other side of the slide rail 7, and the thermal imager base 13 and the reflector base 12 are arranged on the slide rail 7 in parallel; the Fourier infrared spectrometer 10 is arranged at one end of the slide rail 7, which is provided with a reflector base 12; a light passing circular hole is formed in the center of the glass screen 2, and a light beam outlet of the solar simulator 1 faces the light passing circular hole of the glass screen 2; the parabolic reflector 9 is arranged on the reflector base 12, the upper surface of the reflector base 12 is vertically and fixedly connected with a reflector rotating shaft 15, and a support of the parabolic reflector 9 is sleeved on the reflector rotating shaft 15; the light beam inlet of the Fourier infrared spectrometer 10 is arranged towards the parabolic reflector 9; the thermal infrared imager 8 is arranged on the thermal imager base 13; the high-temperature sample support 3 is annular, a sample 4 to be measured is arranged in the high-temperature sample support 3, and a thermocouple 5 is arranged on the surface of the sample 4 to be measured on one side of the thermal infrared imager 8;
the diameter of the first circular through hole 20 is 60 mm;
the glass screen 2 is plate-shaped hollow quartz glass, and a cooling water inlet pipe and a cooling water outlet pipe are arranged on the side edge of the glass screen 2;
the high-temperature sample support 3 is made of metal, and a mullite heat-insulating material is arranged between the annular inner surface of the high-temperature sample support 3 and the sample; in the embodiment, the high-temperature sample support 3 is used for fixing a wafer-shaped 6h-SiC sample, and the thickness of the sample is 33 mm; the high-temperature sample support 3 is made of metal, the high-temperature sample support 3 is separated from a sample through a heat insulation material, the heat conductivity of the heat insulation material is low, and the radial heat loss of the sample is reduced; meanwhile, the annular high-temperature sample support 3 has the advantage of enabling the thermal stress and the mechanical stress on the circumference of the sample to be uniformly distributed; the force is evenly distributed, so that the deformation of the sample in the heating process can be prevented, the surface of the sample is a plane when the measurement is carried out, and the influence on the measurement direction can be avoided.
The thermocouple 5 is connected with a computer through a USB data acquisition system; the USB data acquisition system is an OM-DAQ-USB-2400 series USB data acquisition system of American OMEGA company; daqpro software for displaying temperature is installed in the computer;
the bottom of the reflector base 12 is provided with a first sliding chute which is sleeved on the sliding rail 7; the bottom of the thermal imager base 13 is provided with a second sliding groove which is sleeved on the sliding rail 7.
The method for measuring the normal emissivity by using the device for measuring the normal emissivity of the opaque solid material heated by the solar simulator comprises the following steps:
first, obtain the background spectrum S related to sample emission spectrum measurement optical pathλ,extra；
Moving the reflector base 12 to enable the parabolic reflector 9, the sample 4 to be detected and the glass screen 2 to pass through the circular hole and the first circular through hole 20 to be on the same straight line, and enabling the glass screen 2 to pass through the center of the circular hole and the center of the first circular through hole 20 to be on the same straight line; rotating the parabolic reflector 9 to make the sample to be measured at normal temperature4 into the beam entrance of the fourier infrared spectrometer 10, and obtaining a background spectrum S associated with the sample emission spectroscopy measurement optical path using the fourier infrared spectrometer 10λ,extra；
Secondly, obtaining the equilibrium temperature TsamEmission spectrum S of lower sample 4 to be measuredλ,sam；
Starting the solar simulator 1, adjusting the high-temperature sample support 3 to enable light emitted by the started solar simulator 1 to be focused on an incident surface of the sample 4 to be measured and form a light spot with the radius of 60mm, and starting to heat the sample 4 to be measured;
moving the thermal imager base 13 to enable the thermal infrared imager 8 to be aligned to the emission surface of the sample 4 to be detected and obtain a temperature distribution image of the emission surface of the sample 4 to be detected; taking a circular area with the temperature deviation within 5% from the central temperature of the image in the temperature distribution image of the emitting surface of the sample 4 to be detected as a temperature uniform area, selecting a rear baffle 16 provided with a second circular through hole 19 with the same size as the temperature uniform area, and moving the rear baffle 16 until the center of the second circular through hole 19 and the center of the first circular through hole 20 are on the same straight line;
the thermocouple 5 is placed in the temperature uniform area in the emission surface of the sample 4 to be detected to be close to the edge position to monitor the temperature of the emission surface of the sample 4 to be detected, and when the temperature fluctuation of the thermocouple 5 is less than 5k, the equilibrium temperature T is reachedsam(ii) a In this example Tsam＝800K；
The thermal imager 8 is removed, and the light mirror base 12 is moved until the light of the parabolic reflector 9, the sample 4 to be detected and the glass screen 2 passes through the circular holes and is on the same straight line; the parabolic reflector 9 is rotated to enable the radiation light of the sample 4 to be measured to be reflected and enter the light beam inlet of the Fourier infrared spectrometer 10, and the Fourier infrared spectrometer 10 is utilized to obtain the equilibrium temperature TsamEmission spectrum S of lower sample 4 to be measuredλ,sam；
Thirdly, acquiring a background spectrum S related to the blackbody spectrum measurement optical pathλ,extra,b；
The distance between the radiation light outlet surface of the black body furnace 11 and the paraboloidal rotary reflector 9 and the distance between the emission surface of the sample 4 to be measured and the paraboloidal rotary reflector 9 are adjusted by adjusting the black body furnace 11The separation is equal; the parabolic reflector 9 is rotated to enable radiation light of the black body furnace 11 to be reflected and enter a light beam inlet of the Fourier infrared spectrometer 10, and the Fourier infrared spectrometer 10 is used for obtaining a background spectrum S related to the optical path of the black body spectrum measurementλ,extra,b；
Fourthly, acquiring the temperature as TbEmission radiation spectrum S of lower blackbody furnace 11λ,b(Tb)；
The blackbody furnace 11 is turned on and the temperature is set to TbThe temperature T is acquired by the spectrometer 10bBlackbody radiation spectrum S of lower blackbody furnace 11λ,b(Tb) (ii) a When equilibrium temperature TsamNot more than the upper limit temperature of the blackbody furnace 11, Tb＝TsamWhen the equilibrium temperature T issamGreater than the upper limit temperature of the blackbody furnace 11, TbThe upper limit temperature of the blackbody furnace 11; in this example Tb＝Tsam＝800K；
Fifthly, acquiring a system calibration coefficient Cλ；
At a temperature TbMoving the black body furnace 11 to the position of the sample 4 to be measured, enabling the radiation light outlet surface of the black body furnace 11 to coincide with the emission surface of the sample 4 to be measured, rotating the parabolic reflector 9 to enable the radiation light of the black body furnace 11 to be reflected and enter the light beam inlet of the Fourier infrared spectrometer 10, obtaining the black body radiation spectrum by the Fourier infrared spectrometer 10, and enabling the temperature of the black body radiation spectrum and the temperature obtained in the step four to be TbBlackbody radiation spectrum S of lower blackbody furnace 11λ,b(Tb) Making a ratio, and obtaining the ratio which is the system calibration coefficient Cλ；
Sixthly, calculating the emission radiation intensity I of the sample 4 to be measuredλ,sam；
seventhly, calculating the emissivity epsilon (T) of the sample 4 to be measuredsam)；
The Planck function in the sixth step and the seventh step is used for describing the change of the spectral radiation force of the black body along with the wavelength, and the Planck function expression is as follows:
FIG. 4 is a schematic view of an emission surface of a sample 4 to be measured in example 1; in the figure, a is an emission surface of a sample 4 to be measured, b is a thermocouple 5, and c is a spectrometer monitoring area;
FIG. 7 is a calibration coefficient curve obtained in step five of example 1; as can be seen from fig. 7, the system calibration factor obtained in step five of example 1 is approximately 1;
FIG. 8 is a normal emissivity curve of a 6h-SiC sample obtained in example 1; as can be seen from FIG. 8, under the temperature condition of 800K, the emission spectrum of the sample is in the wave band range of 3-10 μm, and the normal emissivity is gradually increased along with the increase of the wavelength; within a wave band of 10-12.5 microns, the normal emissivity shows a sharp reduction trend along with the wavelength and reaches a minimum value at a position of 12.5 microns, and then the normal emissivity gradually increases along with the increase of the wavelength.
Claims (8)
1. The utility model provides an opaque solid material normal direction emissivity measurement device based on solar simulator heating which characterized in that: the device comprises a solar simulator (1), a glass screen (2), a high-temperature sample support (3), a thermocouple (5), a slide rail (7), a thermal infrared imager (8), a parabolic reflector (9), a Fourier infrared spectrometer (10), a black body furnace (11), a reflector base (12), a sample emergent face shielding device (21) and a thermal imager base (13);
the sample emergent surface shielding device (21) is composed of a front baffle plate (17), a rear baffle plate (16) and a double-track slideway (18); the front baffle (17) is plate-shaped, the middle part of the front baffle (17) is a cavity, and the side part of the front baffle (17) is provided with a cooling water inlet pipe and a cooling water outlet pipe which are communicated with the cavity; the rear baffle (16) is plate-shaped, the middle part of the rear baffle (16) is a cavity, and the side part of the rear baffle (16) is provided with a cooling water inlet pipe and a cooling water outlet pipe which are communicated with the cavity; the front baffle (17) and the rear baffle (16) are respectively arranged between the two parallel double-rail slideways (18), the front baffle (17) is arranged in one of the slideways of the double-rail slideways (18), and the rear baffle (16) is arranged in the other slideway of the double-rail slideways (18);
a first circular through hole (20) vertical to the plate surface of the front baffle (17) is formed in the center of the front baffle (17), and a second circular through hole (19) vertical to the plate surface of the rear baffle (16) is formed in the center of the rear baffle (16);
the solar simulator (1), the glass screen (2), the high-temperature sample support (3) and the sample emergent surface shielding device (21) are sequentially arranged on one side of the sliding rail (7), and the solar simulator (1) is arranged far away from the sliding rail (7); a front baffle plate (17) in the sample emergent surface shielding device (21) is arranged towards the high-temperature sample support (3); the black body furnace (11) is arranged on the other side of the slide rail (7), and the thermal imager base (13) and the reflector base (12) are arranged on the slide rail (7) in parallel; the Fourier infrared spectrometer (10) is arranged at one end of the slide rail (7) provided with the reflector base (12); a light passing round hole is formed in the center of the glass screen (2), and a light beam outlet of the solar simulator (1) faces the light passing round hole of the glass screen (2); the parabolic reflector (9) is arranged on the reflector base (12), the upper surface of the reflector base (12) is vertically and fixedly connected with a reflector rotating shaft (15), and a support of the parabolic reflector (9) is sleeved on the reflector rotating shaft (15); the light beam inlet of the Fourier infrared spectrometer (10) is arranged towards the parabolic reflector (9); the thermal infrared imager (8) is arranged on the thermal imager base (13); the high-temperature sample support (3) is annular, a wafer-shaped sample to be detected (4) is arranged in the high-temperature sample support (3), and a thermocouple (5) is arranged on the surface of the sample to be detected (4) on one side of the thermal infrared imager (8);
the diameter of the first circular through hole (20) is 50-60 mm;
the glass screen (2) is plate-shaped hollow quartz glass, and a cooling water inlet pipe and a cooling water outlet pipe are arranged on the side edge of the glass screen (2).
2. The solar simulator heating based opaque solid material normal emissivity measurement device of claim 1, wherein: and a heat insulating material is arranged between the annular inner surface of the high-temperature sample support (3) and the sample.
3. The solar simulator heating based opaque solid material normal emissivity measurement device of claim 2, wherein: the high-temperature sample support (3) is made of metal.
4. The solar simulator heating based opaque solid material normal emissivity measurement device of claim 1 or 3, wherein: the thermocouple (5) is connected with the computer through a USB data acquisition system.
5. The solar simulator heating based opaque solid material normal emissivity measurement device of claim 4, wherein: a first sliding groove is formed in the bottom of the reflector base (12), and the sliding rail (7) is sleeved with the first sliding groove; the bottom of the thermal imager base (13) is provided with a second sliding groove, and the second sliding groove is sleeved on the sliding rail (7).
6. The method for measuring the normal emissivity of the opaque solid material based on solar simulator heating according to claim 1, wherein the method comprises the following steps: the method comprises the following steps:
first, obtain the background spectrum S related to sample emission spectrum measurement optical pathλ,extra；
The light from the reflector base (12) to the paraboloidal reflector (9), the sample to be measured (4) and the glass screen (2) is transmitted through the round hole and the first round through hole (20) on the same straight line, and the glass screen is made to pass through(2) The center of the light passing through the round hole is on the same straight line with the center of the first round through hole (20); the parabolic reflector (9) is rotated to enable the radiation light of the sample (4) to be measured at normal temperature to be reflected and enter the light beam inlet of the Fourier infrared spectrometer (10), and the Fourier infrared spectrometer (10) is utilized to obtain the background spectrum S related to the sample emission spectrum measurement optical pathλ,extra；
Secondly, obtaining the equilibrium temperature TsamEmission spectrum S of lower sample (4) to be measuredλ,sam；
Starting a solar simulator (1), adjusting a high-temperature sample support (3) to enable light emitted by the started solar simulator (1) to be focused on an incident surface of a sample to be measured (4) and form a light spot with the radius of 50-60 mm, and starting to heat the sample to be measured (4);
moving the thermal imager base (13) to enable the thermal infrared imager (8) to be aligned to the emission surface of the sample (4) to be detected and obtain a temperature distribution image of the emission surface of the sample (4) to be detected; taking a circular area with the temperature deviation within 5% from the central temperature of the image in the temperature distribution image of the emitting surface of the sample (4) to be detected as a temperature uniform area, selecting a rear baffle (16) provided with a second circular through hole (19) with the same size as the temperature uniform area, and moving the rear baffle (16) until the center of the second circular through hole (19) and the center of the first circular through hole (20) are on the same straight line;
the thermocouple (5) is placed in the emission surface of the sample (4) to be detected, the temperature of the emission surface of the sample (4) to be detected is monitored by being close to the edge position in the temperature uniform area, and when the temperature fluctuation of the thermocouple (5) is less than 5k, the equilibrium temperature T is reachedsam；
The thermal imager (8) is removed, and the light mirror base (12) is moved to the parabolic reflector (9), the sample to be detected (4) and the glass screen (2) to enable the light to pass through the circular holes and be on the same straight line; the parabolic reflector (9) is rotated to enable the radiation light of the sample (4) to be measured to be reflected and enter the light beam inlet of the Fourier infrared spectrometer (10), and the balance temperature T is obtained by the Fourier infrared spectrometer (10)samEmission spectrum S of lower sample (4) to be measuredλ,sam；
Thirdly, acquiring a background spectrum S related to the blackbody spectrum measurement optical pathλ,extra,b；
Adjustment ofThe distance from the radiant light outlet surface of the black body furnace (11) to the rotary paraboloid reflector (9) is equal to the distance from the emission surface of the sample to be measured (4) to the rotary paraboloid reflector (9) by the black body furnace (11); the parabolic reflector (9) is rotated to enable radiation light of the black body furnace (11) to be reflected and enter a light beam inlet of the Fourier infrared spectrometer (10), and the Fourier infrared spectrometer (10) is utilized to obtain a background spectrum S related to the optical path of the black body spectrum measurementλ,extra,b；
Fourthly, acquiring the temperature as TbEmission radiation spectrum S of lower blackbody furnace (11)λ,b(Tb)；
The blackbody furnace (11) is opened and the temperature is set to be TbThe temperature T is acquired by the spectrometer (10)bBlackbody radiation spectrum S of lower blackbody furnace (11)λ,b(Tb) (ii) a When equilibrium temperature TsamWhen the temperature is not more than the upper limit temperature of the blackbody furnace (11), Tb＝TsamWhen the equilibrium temperature T issamWhen the temperature is higher than the upper limit temperature of the black body furnace (11), TbThe upper limit temperature of the black body furnace (11);
fifthly, acquiring a system calibration coefficient Cλ；
At a temperature TbMoving the black body furnace (11) to the position of the sample (4) to be detected, enabling the radiation light outlet surface of the black body furnace (11) to coincide with the emission surface of the sample (4) to be detected, rotating the parabolic reflector (9) to enable the radiation light of the black body furnace (11) to be reflected and enter the light beam inlet of the Fourier infrared spectrometer (10), acquiring the black body radiation spectrum by using the Fourier infrared spectrometer (10), and enabling the temperature of the black body radiation spectrum and the temperature obtained in the step four to be TbBlackbody radiation spectrum S of lower blackbody furnace (11)λ,b(Tb) Making a ratio, and obtaining the ratio which is the system calibration coefficient Cλ；
Sixthly, calculating the emission radiation intensity I of the sample (4) to be measuredλ,sam；
seventhly, calculating the emissivity epsilon (T) of the sample (4) to be measuredsam)；
7. The method for emissivity measurement by a solar simulator heating based opaque solid material normal emissivity measurement device of claim 6, wherein: sixthly, the Planck function is used for describing the change of the spectral radiation force of the black body along with the wavelength, and the Planck function expression is as follows:
8. The method for emissivity measurement by a solar simulator heating based opaque solid material normal emissivity measurement device of claim 6, wherein: seventhly, the Planck function is used for describing the change of the spectral radiation force of the black body along with the wavelength, and the Planck function expression is as follows:
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