CN109142227B - Sample cavity for spectrum experiment - Google Patents
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- CN109142227B CN109142227B CN201811084091.6A CN201811084091A CN109142227B CN 109142227 B CN109142227 B CN 109142227B CN 201811084091 A CN201811084091 A CN 201811084091A CN 109142227 B CN109142227 B CN 109142227B
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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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- G01N21/0332—Cuvette constructions with temperature control
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Abstract
The invention relates to the field of physical experiments, in particular to a sample cavity for a spectrum experiment, which comprises an air inlet pipe, an upper cover, a capillary pipe, a connecting pipe, an air outlet pipe, a sample pipe, a lower cover, a sample, a carbon fiber pipe, a heating lamp, a heat shielding cavity, a bolometer, a thermometer, a heat conduction base, a water cooling table and a displacement device.
Description
Technical Field
The invention relates to the field of physical experiments, in particular to a sample cavity for spectrum experiments, which has high reliability and simple sample preparation process.
Background
Spectroscopic experiments such as absorption spectra, excitation spectra, diffraction experiments, etc. are common experimental means for studying the properties of substances, and generally, light of different wavelengths is incident on a sample and reflected light is detected. Typically, the sample is placed in a particular sample chamber, and the structure of the sample chamber varies from sample to sample and from one experimental requirement to another. Defect one of the prior art: in some experiments requiring sample heating, some prior arts heat the sample by ceramic or metal element heating, microwave resonance and other methods, the temperature measuring device is usually located near the sample, and because the heat source is nearer to the sample, it is harder to measure the temperature of the sample due to the influence of the radiant heat of the heat source, while other prior arts, the sample is located in a heating cavity, the temperature measuring device can achieve heat balance with the surrounding environment, and can accurately measure the temperature of the sample, but the heating cavity is larger in size, and some experiments requiring higher space size around the sample cannot be performed; the defects of the prior art are as follows: in some spectrum experiments, the power of the incident light needs to be accurately measured, but is limited by factors such as the structure and the temperature of a sample cavity, and the measurement accuracy of the power of the incident light is not high.
Disclosure of Invention
In order to solve the problems, the device of the invention adopts a simple structure to control the temperature of the sample through air flow, can accurately measure the temperature of the sample and accurately measure the radiation power of incident light, and in addition, the whole device has small heating value and small influence on the surrounding experimental environment. The device is a sample cavity for spectrum experiments, and needs to be used together with a gas storage tank, a light source and a spectrometer when the spectrum experiments are carried out.
The technical scheme adopted by the invention is as follows:
the sample cavity for the spectrum experiment mainly comprises an air inlet pipe, an upper cover, a capillary tube, a connecting pipe, an air outlet pipe, a sample pipe, a lower cover, a sample, a carbon fiber pipe, a heating lamp, a heat shielding cavity, a bolometer control circuit, a thermometer, a heat conduction base, a water cooling table and a displacement device, xyz is a three-dimensional space coordinate system, the air inlet pipe is connected with an air storage tank, argon is stored in the air storage tank, and the flow rate of the argon can be regulated; the experimental facility comprises a vacuum cavity, a gas storage tank, a light source and a spectrometer, wherein the carbon fiber tube, a heating lamp, a heat shielding cavity, a bolometer, a thermometer, a heat conduction base, a water cooling table and a displacement device are all positioned in the vacuum cavity, a small hole is formed in the vacuum cavity, the water cooling table is fixed on the displacement device, the heat conduction base is fixed on the water cooling table, the upper cover and the lower cover are both provided with internal threads, a connecting tube is provided with external threads, the upper cover, the connecting tube and the lower cover are sequentially connected in a threaded manner, the side surface of the connecting tube is connected with a gas outlet pipe, the sample tube is funnel-shaped comprising an upper section and a lower section, the upper section is a funnel-shaped part, the lower section is a thin tube, the lower end of the thin tube is closed, the upper section is nested in the lower cover, the lower section penetrates the lower surface of the lower cover, the outer diameter of the lower section is 0.9 millimeter, the inner diameter of the lower section is 0.7 millimeter, when the connecting tube is connected with the lower cover, the upper section of the sample tube can be pressed and fixed, and the lower section of the sample tube can be inserted into the vacuum cavity through the small hole in the vacuum cavity; the capillary tube comprises a thick section and a thin section, wherein the thick section is positioned between the connecting tube and the upper cover, when the connecting tube is screwed by the upper cover, the thick section of the capillary tube can be pressed and fixed, the upper part of the thick section is connected with the air inlet tube, the thin section downwards passes through the connecting tube and is nested in the sample tube, the lower end of the thin section is opened, and the outer diameter of the thin section is 0.5 millimeter, and the inner diameter of the thin section is 0.3 millimeter; the carbon fiber tube is fixed on the heat conduction base in a vertical state, a heat shielding cavity is nested outside the carbon fiber tube, a pair of heating lamps respectively positioned at two sides of the carbon fiber tube are fixed in the heat shielding cavity, a sample is positioned at the inner bottom of the lower section of the sample tube, the lower section of the sample tube is inserted into and nested in the inner central position of the carbon fiber tube, the bolometer is positioned in the heat shielding cavity and can move, a thermometer is arranged near the inner central position of the carbon fiber tube, the inner diameter of the carbon fiber tube is 1.5 mm, the outer diameter of the carbon fiber tube is 2.5 mm, a pair of through holes in the horizontal direction are formed in the side face of the central position of the carbon fiber tube, light emitted by a light source can irradiate the sample through one of the through holes, and the light scattered on the sample can leave the carbon fiber tube through the other through hole and finally enter the spectrometer; the radiation thermometer mainly comprises an outer shielding cover, an inner shielding cover, a heat absorber, a heat sensor, a metal sheet, a heater and a heat insulation sheet, wherein the outer shielding cover and the inner shielding cover are cylindrical, the bottom surface of one side of each of the outer shielding cover and the inner shielding cover is provided with a small hole, the inner shielding cover is coaxially connected in the outer shielding cover, the heat absorber is cylindrical and is connected with the bottom surface of one side of the inner shielding cover through the heat insulation sheet, the heat sensor is positioned on the inner side wall of the heat absorber, the metal sheet and the heater are arranged in the heat absorber, the heater is fixed on one surface of the metal sheet, and light can sequentially enter the metal sheet through the small hole of the outer shielding cover, the small hole of the inner shielding cover and the heat sensor; the radiation heat meter control circuit mainly comprises a resistor I, a direct current power supply, a variable capacitor, a resistor II, a resistor III, a resistor IV, an alternating current power supply and a phase-locked amplifier, wherein the phase-locked amplifier is provided with an input end and an output end, the direct current power supply, the resistor I and a heater are connected in a circulating way and can form a current loop, the direct current power supply is provided with a signal end, the output current of the direct current power supply can be controlled according to the input signal, the resistance value of the resistor I is 1.0 kiloohm, the thermal inductor, the resistor II, the resistor III, the resistor IV, the phase-locked amplifier and the alternating current power supply are connected in a Wheatstone bridge mode, the output signals of the thermal inductor, the resistor II, the resistor III and the resistor IV are bridge arms of the Wheatstone bridge respectively, the output signals of the Wheatstone bridge enter the input end of the phase-locked amplifier, the output end of the phase-locked amplifier is connected with the signal end of the direct current power supply, the variable capacitor is connected with the resistor II in parallel, the variable capacitor is 300 to 600pF, the thermal inductor is a thermistor, the resistance value at 20 ℃ is 9.2 kiloohm, the resistance value of the thermal inductor and the resistance value of the resistor IV is 10.0 kiloohm range, and the resistance value of the thermal inductor and the variable value of the resistor is 0.0 kiloohm range.
Principle of operation of bolometer:
the control circuit of the bolometer provides electric energy for the heating lamp and keeps the temperature of the heat absorber constant; in the absence of illuminating radiation, the bolometer reaches thermal equilibrium; when the illumination radiation is incident on the heat absorber, the heat energy of the illumination radiation is absorbed by the heat absorber, so that a heat load is generated, and the temperature of the heat absorber rises; the control circuit of the bolometer keeps the temperature of the heat absorber constant by reducing the current output to the heating lamp; the reduction amount of the electric energy output by the control circuit of the bolometer is equal to the optical radiation heat energy absorbed by the heat absorber, and the optical radiation heat energy absorbed by the heat absorber is determined by calculating the reduction amount of the electric energy output by the control circuit of the bolometer.
Principle of operation of the control circuit of the bolometer:
the thermal inductor, the resistor II, the resistor III, the resistor IV, the phase-locked amplifier and the alternating current power supply are connected in a Wheatstone bridge mode, the thermal inductor, the resistor II, the resistor III and the resistor IV are bridge arms of the Wheatstone bridge respectively, an output signal of the Wheatstone bridge enters an input end of the phase-locked amplifier, and an output end of the phase-locked amplifier is connected with the direct current power supply; the alternating current power supply outputs an alternating current signal with the effective voltage of 0.1V, the frequency of the alternating current signal is 731Hz, the output signal of the Wheatstone bridge is processed by the phase-locked amplifier, the output signal of the phase-locked amplifier enters the signal end of the direct current power supply, under the condition that illumination radiation is incident to the heat absorber, the temperature of the heat absorber rises, the resistance of the heat sensor changes, the output signal of the Wheatstone bridge changes, the signal output by the phase-locked amplifier to the signal end of the direct current power supply changes, the output current of the direct current power supply is controlled, and the current output to the heating lamp is reduced, so that the temperature of the heat absorber is kept constant.
Measuring the voltage V across the resistor I and the heating lamp respectively R And V H Calculating the electric power V of the heating lamp H V R /R R Wherein R is R The radiation heat energy of the light incident on the bolometer is obtained by the variation of the electric power of the heating lamp as the resistance value of the resistor I.
The method for carrying out the spectrum experiment by using the sample cavity for the spectrum experiment comprises the following steps:
placing a sample at the inner bottom of the lower section of the sample tube, embedding the upper section of the sample tube in the lower cover, enabling the lower section to penetrate through the lower surface of the lower cover, screwing a thread between the connecting tube and the lower cover, fixing the upper section of the sample tube, enabling the capillary thin section to downwards penetrate through the connecting tube and be embedded in the sample tube, screwing a thread between the upper cover and the connecting tube, fixing the capillary thick section, inserting and embedding the lower section of the sample tube into the carbon fiber tube, and enabling the sample to be positioned at the inner center position of the carbon fiber tube;
secondly, adjusting the temperature of the heating lamp, the size and the position of a heating focus so that the heating focus is positioned near the center of the heat shielding cavity;
thirdly, adjusting the position of the light source to enable light emitted by the light source to irradiate the focal position of the heating lamp, moving the bolometer to the focal position of the heating lamp, enabling the light to sequentially pass through the small holes of the outer shielding cover, the small holes of the inner shielding cover and the heat sensor and enter the metal sheet, and measuring radiation heat energy of the light at the focal position of the heating lamp;
fourthly, moving the bolometer away from the focus position of the heating lamp, and adjusting the displacement device to enable the center of the carbon fiber tube to move to the focus position of the heating lamp, and enabling light emitted by the light source to be emitted onto the sample through the through hole on the side face of the carbon fiber tube;
regulating the flow rate of argon entering the air inlet pipe through the air storage tank, wherein the typical flow rate value is 5SCCM to 30SCCM, and the argon flow sequentially passes through the air inlet pipe, the thick section and the thin section of the capillary pipe, reaches the sample, sequentially passes through the lower section of the sample pipe, the upper section of the sample pipe and the connecting pipe, is discharged from the air outlet pipe, can transfer heat on the capillary pipe to the sample, and measures the temperature of the sample through the thermometer;
and sixthly, carrying out a spectrum experiment, wherein light emitted by the light source is emitted to the sample through one through hole on the side surface of the carbon fiber tube, light scattered by the sample is emitted out of the carbon fiber tube through the other through hole on the side surface of the carbon fiber tube, and finally enters the spectrometer, and the optical information collected by the spectrometer is analyzed to obtain the relevant physical properties of the sample.
The beneficial effects of the invention are as follows:
the sample tube adopted by the device has compact structure, simple sample preparation process, and high precision, and the temperature of the sample can be accurately measured by controlling the temperature of the sample through the combination of the radiant heat of the heating lamp and the air flow and the radiant power of the incident light can be measured by the special bolometer.
Drawings
The following is further described in connection with the figures of the present invention:
FIG. 1 is a schematic side view of the present invention;
FIG. 2 is an enlarged schematic view of a bolometer;
fig. 3 is a schematic diagram of a bolometer control circuit.
In the figure, 1, an air inlet pipe, 2, an upper cover, 3, a capillary pipe, 4, a connecting pipe, 5, an air outlet pipe, 6, a sample pipe, 7, a lower cover, 8, a sample, 9, a carbon fiber pipe, 10, a heating lamp, 11, a heat shielding cavity, 12, a bolometer, 12-1, an outer shielding cover, 12-2, an inner shielding cover, 12-3, a heat absorber, 12-4, a heat inductor, 12-5, a metal sheet, 12-6, a heater, 12-7, a heat insulating sheet, 12-8, a resistor I,12-9, a direct current power supply, 12-10, a variable capacitor, 12-11, a resistor II,12-12, a resistor III,12-13, a resistor IV,12-14, an alternating current power supply, 12-15, a lock-in amplifier, 13, a thermometer, 14, a heat conducting base, 15, a water cooling table and 16 displacement device.
Detailed Description
As shown in fig. 1, xyz is a schematic side view of the invention, and is a three-dimensional space coordinate system, which comprises an air inlet pipe (1), an upper cover (2), a capillary tube (3), a connecting pipe (4), an air outlet pipe (5), a sample pipe (6), a lower cover (7), a sample (8), a carbon fiber pipe (9), a heating lamp (10), a heat shielding cavity (11), a bolometer (12), a thermometer (13), a heat conducting base (14), a water cooling table (15) and a displacement device (16), wherein the upper cover (2) and the lower cover (7) are respectively provided with internal threads, the connecting pipe (4) is provided with external threads, the upper cover (2), the connecting pipe (4) and the lower cover (7) are sequentially connected in a threaded manner, the side surface of the connecting pipe (4) is connected with an air outlet pipe (5), the sample pipe (6) is in a funnel shape comprising an upper section and a lower section, the upper section is a funnel part, the lower section is a thin pipe, the lower end of the thin pipe is closed, the upper section is nested in the lower cover (7), the lower section penetrates the lower surface of the lower cover (7), the lower section is 0.9 mm, the inner diameter of the lower section is 0.7, the inner diameter of the thin section is 0.7 mm, when the connecting section is connected with the connecting pipe (4) and the lower section (7) can be tightly pressed by the vacuum pipe (6), and the upper section can be inserted into the vacuum cavity (6); the capillary tube (3) comprises a thick section and a thin section, the thick section is positioned between the connecting tube (4) and the upper cover (2), when the upper cover (2) is screwed on the connecting tube (4), the thick section of the capillary tube (3) can be compressed and fixed, the air inlet tube (1) is connected above the thick section, the thin section downwards passes through the connecting tube (4) and is nested in the sample tube (6), the lower end of the thin section is opened, and the outer diameter of the thin section is 0.5 millimeter, and the inner diameter of the thin section is 0.3 millimeter; the air inlet pipe (1) is connected with an air storage tank, argon is stored in the air storage tank, and the flow rate of the argon can be adjusted; the carbon fiber tube (9), the heating lamp (10), the heat shielding cavity (11), the bolometer (12), the thermometer (13), the heat conduction base (14), the water cooling table (15) and the displacement device (16) are all positioned in the vacuum cavity, a small hole is formed in the vacuum cavity, the water cooling table (15) is fixed on the displacement device (16), the heat conduction base (14) is fixed on the water cooling table (15), the carbon fiber tube (9) is vertically fixed on the heat conduction base (14), the heat shielding cavity (11) is nested outside the carbon fiber tube (9), a pair of heating lamps (10) respectively positioned at two sides of the carbon fiber tube (9) are fixed in the heat shielding cavity (11), the sample (8) is positioned at the bottom in the lower section of the sample tube (6), the lower section of the sample tube (6) is inserted and nested in the inner center position of the carbon fiber tube (9), the bolometer (12) is positioned in the heat shielding cavity (11) and can move, the thermometer (13) is arranged near the inner center position of the carbon fiber tube (9), the inner diameter of the carbon fiber tube (9) is 1.5 mm, the inner diameter of the carbon fiber tube (9) is 2.5 mm, the light can irradiate the through hole in the horizontal direction of one of the light source (8) on the side surface of the sample, light scattered on the sample (8) can leave the carbon fiber tube (9) through the other of said through holes and finally enter the spectrometer.
Referring to fig. 2, which is an enlarged schematic diagram of a bolometer, the bolometer (12) mainly comprises an outer shielding cover (12-1), an inner shielding cover (12-2), a heat absorber (12-3), a heat sensor (12-4), a metal sheet (12-5), a heater (12-6) and a heat insulation sheet (12-7), wherein the outer shielding cover (12-1) and the inner shielding cover (12-2) are cylindrical with small holes on one side bottom surface, the inner shielding cover (12-2) is coaxially connected in the outer shielding cover (12-1), the heat absorber (12-3) is cylindrical and is connected with one side bottom surface of the inner shielding cover (12-2) through the heat insulation sheet (12-7), the heat sensor (12-4) is located on the inner side wall of the heat absorber (12-3), the metal sheet (12-5) and the heater (12-6) are arranged in the heat absorber (12-3), the heater (12-6) is fixed on one surface of the metal sheet (12-5), and the light can sequentially pass through the outer shielding cover (12-1), the inner shielding cover (12-2) and the small holes (12-4) are inducted into the metal sheet (12-2).
As shown in fig. 3, the control circuit of the bolometer (12) mainly comprises a resistor I (12-8), a direct current power supply (12-9), a variable capacitor (12-10), a resistor II (12-11), a resistor III (12-12), a resistor IV (12-13), an alternating current power supply (12-14) and a phase-locked amplifier (12-15), wherein the phase-locked amplifier (12-15) is provided with an input end and an output end, the direct current power supply (12-9), the resistor I (12-8) and the heater (12-6) are circularly connected and can form a current loop, the direct current power supply (12-9) is provided with a signal end, the output current of the direct current power supply (12-9) can be controlled according to the input signal, the resistance value of the resistor I (12-8) is 1.0 kiloohm, the thermal sensor (12-4), the resistor II (12-11), the resistor III (12-12), the resistor IV (12-13), the phase-locked amplifier (12-15) and the alternating current power supply (12-14) are connected in a wheatstone mode, the thermal bridge (12-12) is connected in a wheatstone mode, and the wheatstone bridge (12-13) is respectively, the output signal of the Wheatstone bridge enters the input end of a phase-locked amplifier (12-15), the output end of the phase-locked amplifier (12-15) is connected with the signal end of a direct current power supply (12-9), a variable capacitor (12-10) is connected with a resistor II (12-11) in parallel, the variable capacitance range is 300pF to 600pF, a thermal sensor (12-4) is a thermistor, the resistance value at 20 ℃ is 9.2 kiloohms, the resistance values of a resistor II (12-11) and a resistor IV (12-13) are all 10.0 kiloohms, the resistance of a resistor III (12-12) is a variable resistor, and the resistance range is 8.0 kiloohms to 12.0 kiloohms.
Principle of operation of the bolometer (12):
the control circuit of the bolometer (12) provides power to the heater (12-6) and keeps the temperature of the heat absorber (12-3) constant; in the absence of illuminating radiation, the bolometer (12) reaches thermal equilibrium; in the case that the illumination radiation is incident on the heat absorber (12-3), the heat energy of the illumination radiation is absorbed by the heat absorber (12-3), thereby generating a heat load, and the temperature of the heat absorber (12-3) rises; the control circuit of the bolometer (12) keeps the temperature of the heat absorber (12-3) constant by reducing the current output to the heater (12-6); the reduction amount of the electric energy output by the control circuit of the bolometer (12) is equal to the optical radiation heat energy absorbed by the heat absorber (12-3), and the optical radiation heat energy absorbed by the heat absorber (12-3) is determined by calculating the reduction amount of the electric energy output by the control circuit of the bolometer (12).
Principle of operation of a control circuit of a bolometer (12):
the thermal inductor (12-4), the resistor II (12-11), the resistor III (12-12), the resistor IV (12-13), the lock-in amplifier (12-15) and the alternating current power supply (12-14) are connected in a Wheatstone bridge mode, the thermal inductor (12-4), the resistor II (12-11), the resistor III (12-12) and the resistor IV (12-13) are bridge arms of the Wheatstone bridge respectively, an output signal of the Wheatstone bridge enters an input end of the lock-in amplifier (12-15), and an output end of the lock-in amplifier (12-15) is connected with the direct current power supply (12-9); the alternating current power supply (12-14) outputs an alternating current signal with the effective voltage of 0.1V, the alternating current signal frequency is 731Hz, the output signal of the Wheatstone bridge is processed by the phase-locked amplifier (12-15), the output signal of the phase-locked amplifier (12-15) enters the signal end of the direct current power supply (12-9), under the condition that illumination radiation is incident to the heat absorber (12-3), the temperature of the heat absorber (12-3) rises, the resistance of the heat sensor (12-4) changes, the output signal of the Wheatstone bridge changes, the signal output by the phase-locked amplifier (12-15) to the signal end of the direct current power supply (12-9) changes, the output current of the direct current power supply (12-9) is controlled, and the current output to the heater (12-6) is reduced, so that the temperature of the heat absorber (12-3) is kept constant.
Measuring the voltage V across the resistor I (12-8) and the heater (12-6), respectively R And V H Calculating the electric power V of the heater (12-6) H V R /R R Wherein R is R The radiation heat energy of the light incident on the radiation thermometer (12) is obtained by the variation of the electric power of the heater (12-6) as the resistance value of the resistor I (12-8).
The sample cavity for the spectrum experiment mainly comprises an air inlet pipe (1), an upper cover (2), a capillary tube (3), a connecting pipe (4), an air outlet pipe (5), a sample pipe (6), a lower cover (7), a sample (8), a carbon fiber pipe (9), a heating lamp (10), a heat shielding cavity (11), a bolometer (12) control circuit, a thermometer (13), a heat conduction base (14), a water cooling table (15) and a displacement device (16), xyz is a three-dimensional space coordinate system, the air inlet pipe (1) is connected with an air storage tank, argon is stored in the air storage tank, and the flow rate of the argon can be regulated; the experimental facility is provided with a vacuum cavity, an air storage tank, a light source and a spectrometer, wherein a carbon fiber tube (9), a heating lamp (10), a heat shielding cavity (11), a bolometer (12), a thermometer (13), a heat conduction base (14), a water cooling table (15) and a displacement device (16) are all positioned in the vacuum cavity, the vacuum cavity is provided with small holes, the water cooling table (15) is fixed on the displacement device (16), the heat conduction base (14) is fixed on the water cooling table (15), an upper cover (2) and a lower cover (7) are all provided with internal threads, a connecting tube (4) is provided with external threads, the upper cover (2), the connecting tube (4) and the lower cover (7) are sequentially connected in a threaded manner, an air outlet tube (5) is connected to the side surface of the connecting tube (4), the sample tube (6) is funnel-shaped comprising an upper section and a lower section, the upper section is a funnel-shaped part, the lower section is a thin tube, the lower end of the thin tube is closed, the upper section is nested in the lower cover (7), the lower section penetrates the lower surface of the lower cover (7), the lower section is 0.9 mm, the inner diameter is 0.7 mm, and the lower section is connected with the connecting tube (4) through the lower cover (7), and the small section can be tightly pressed by the upper section of the vacuum tube (6) when the upper section and the sample tube (6) can be tightly pressed by the upper section; the capillary tube (3) comprises a thick section and a thin section, the thick section is positioned between the connecting tube (4) and the upper cover (2), when the upper cover (2) is screwed on the connecting tube (4), the thick section of the capillary tube (3) can be compressed and fixed, the air inlet tube (1) is connected above the thick section, the thin section downwards passes through the connecting tube (4) and is nested in the sample tube (6), the lower end of the thin section is opened, and the outer diameter of the thin section is 0.5 millimeter, and the inner diameter of the thin section is 0.3 millimeter; the carbon fiber tube (9) is vertically fixed on the heat conduction base (14), a heat shielding cavity (11) is nested outside the carbon fiber tube (9), a pair of heating lamps (10) respectively positioned at two sides of the carbon fiber tube (9) are fixed in the heat shielding cavity (11), a sample (8) is positioned at the inner bottom of the lower section of the sample tube (6), the lower section of the sample tube (6) is inserted into and nested in the inner center position of the carbon fiber tube (9), a radiation thermometer (12) is positioned in the heat shielding cavity (11) and can move, a thermometer (13) is arranged near the inner center position of the carbon fiber tube (9), the inner diameter of the carbon fiber tube (9) is 1.5 mm, the outer diameter of the carbon fiber tube (9) is 2.5 mm, a pair of through holes in the horizontal direction are formed in the side face of the center position of the carbon fiber tube (9), light emitted by a light source can irradiate the sample (8) through one through the through hole, and light scattered on the sample (8) can leave the carbon fiber tube (9) through the other through the through hole and finally enter the spectrometer; the radiation thermometer (12) mainly comprises an outer shielding cover (12-1), an inner shielding cover (12-2), a heat absorber (12-3), a heat sensor (12-4), a metal sheet (12-5), a heater (12-6) and a heat insulation sheet (12-7), wherein the outer shielding cover (12-1) and the inner shielding cover (12-2) are cylindrical, the bottom surfaces of one sides of the outer shielding cover and the inner shielding cover are provided with small holes, the inner shielding cover (12-2) is coaxially connected in the outer shielding cover (12-1), the heat absorber (12-3) is cylindrical and is connected with the bottom surface of one side of the inner shielding cover (12-2) through the heat insulation sheet (12-7), the heat sensor (12-4) is positioned on the inner side wall of the heat absorber (12-3), the heat absorber (12-3) is internally provided with the metal sheet (12-5) and the heater (12-6), and the heater (12-6) is fixed on one side of the metal sheet (12-5), and light can sequentially enter the small holes of the outer shielding cover (12-1), the inner shielding cover (12-2) and the heat sensor (12-4) through the small holes of the heat absorber (12-5) and the heat sensor (12-4) of the heat absorber; the control circuit of the bolometer (12) mainly comprises a resistor I (12-8), a direct current power supply (12-9), a variable capacitor (12-10), a resistor II (12-11), a resistor III (12-12), a resistor IV (12-13), an alternating current power supply (12-14) and a phase-locked amplifier (12-15), wherein the phase-locked amplifier (12-15) is provided with an input end and an output end, the direct current power supply (12-9), the resistor I (12-8) and the heater (12-6) are circularly connected and can form a current loop, the direct current power supply (12-9) is provided with a signal end, the output current of the direct current power supply (12-9) can be controlled according to the input signal, the resistance value of the resistor I (12-8) is 1.0 kiloohm, the heat sensor (12-4), the resistor II (12-11), the resistor III (12-12), the resistor IV (12-13), the phase-locked amplifier (12-15) and the alternating current power supply (12-14) are connected in a wheatstone bridge mode, the heat sensor (12-4), the resistor II (12-12) and the wheatstone bridge (12-13) are respectively connected in a wheatstone bridge mode, the wheatstone bridge (12-11) is provided with the output end of the resistor (12-12) and the output bridge (12-13) is a wheatstone bridge, and the wheatstone bridge (12) is provided, the output end of the lock-in amplifier (12-15) is connected with the signal end of the direct current power supply (12-9), the variable capacitor (12-10) is connected with the resistor II (12-11) in parallel, the variable capacitor range is 300pF to 600pF, the thermal sensor (12-4) is a thermistor, the resistance value at 20 ℃ is 9.2 kiloohms, the resistance values of the resistor II (12-11) and the resistor IV (12-13) are 10.0 kiloohms, the resistor III (12-12) is a variable resistor, and the resistance range is 8.0 kiloohms to 12.0 kiloohms.
The sample tube has a simple structure, the sample preparation process is time-saving, the sample is uniformly heated by the radiant heat of the heating lamp, the temperature of the sample can be accurately controlled by combining the air flow, and the radiation power of the incident light can be accurately measured by adopting the specially designed bolometer.
Claims (1)
1. The utility model provides a sample chamber for spectral experiment, mainly include intake pipe (1), upper cover (2), capillary (3), connecting pipe (4), outlet duct (5), sample tube (6), lower cover (7), sample (8), carbon fiber tube (9), heating lamp (10), heat shield chamber (11), bolometer (12) control circuit, thermometer (13), heat conduction base (14), water-cooling platform (15) and displacement device (16), intake pipe (1) connect the gas holder, store the argon gas in the gas holder, and can adjust the velocity of flow of argon gas; the experimental facility comprises a vacuum chamber, a gas storage tank, a light source and a spectrometer, wherein the carbon fiber tube (9), a heating lamp (10), a heat shielding chamber (11), a bolometer (12), a thermometer (13), a heat conduction base (14), a water cooling table (15) and a displacement device (16) are all positioned in the vacuum chamber, the vacuum chamber is provided with small holes, the water cooling table (15) is fixed on the displacement device (16), the heat conduction base (14) is fixed on the water cooling table (15),
the method is characterized in that: the upper cover (2) and the lower cover (7) are both provided with internal threads, the connecting pipe (4) is provided with external threads, the upper cover (2), the connecting pipe (4) and the lower cover (7) are sequentially connected in a threaded manner, the side surface of the connecting pipe (4) is connected with the air outlet pipe (5), the sample pipe (6) is funnel-shaped and comprises an upper section and a lower section, the upper section is a funnel part, the lower section is a thin pipe, the lower end of the thin pipe is closed, the upper section is nested in the lower cover (7), the lower section penetrates through the lower surface of the lower cover (7), the outer diameter of the lower section is 0.9 millimeter, the inner diameter is 0.7 millimeter, when the connecting pipe (4) is connected with the lower cover (7), the upper section of the sample pipe (6) can be compressed and fixed, and the lower section of the sample pipe (6) can be inserted into a vacuum cavity through a small hole on the vacuum cavity; the capillary tube (3) comprises a thick section and a thin section, the thick section is positioned between the connecting tube (4) and the upper cover (2), when the upper cover (2) is screwed on the connecting tube (4), the thick section of the capillary tube (3) can be compressed and fixed, the air inlet tube (1) is connected above the thick section, the thin section downwards passes through the connecting tube (4) and is nested in the sample tube (6), the lower end of the thin section is opened, and the outer diameter of the thin section is 0.5 millimeter, and the inner diameter of the thin section is 0.3 millimeter;
the carbon fiber tube (9) is vertically fixed on the heat conduction base (14), a heat shielding cavity (11) is nested outside the carbon fiber tube (9), a pair of heating lamps (10) respectively positioned at two sides of the carbon fiber tube (9) are fixed in the heat shielding cavity (11), a sample (8) is positioned at the inner bottom of the lower section of the sample tube (6), the lower section of the sample tube (6) is inserted into and nested in the inner center position of the carbon fiber tube (9), a radiation thermometer (12) is positioned in the heat shielding cavity (11) and can move, a thermometer (13) is arranged near the inner center position of the carbon fiber tube (9), the inner diameter of the carbon fiber tube (9) is 1.5 mm, the outer diameter of the carbon fiber tube (9) is 2.5 mm, a pair of through holes in the horizontal direction are formed in the side face of the center position of the carbon fiber tube (9), light emitted by a light source can irradiate the sample (8) through one through the through hole, and light scattered on the sample (8) can leave the carbon fiber tube (9) through the other through the through hole and finally enter the spectrometer;
the radiation thermometer (12) mainly comprises an outer shielding cover (12-1), an inner shielding cover (12-2), a heat absorber (12-3), a heat sensor (12-4), a metal sheet (12-5), a heater (12-6) and a heat insulation sheet (12-7), wherein the outer shielding cover (12-1) and the inner shielding cover (12-2) are cylindrical, the bottom surfaces of one sides of the outer shielding cover and the inner shielding cover are provided with small holes, the inner shielding cover (12-2) is coaxially connected in the outer shielding cover (12-1), the heat absorber (12-3) is cylindrical and is connected with the bottom surface of one side of the inner shielding cover (12-2) through the heat insulation sheet (12-7), the heat sensor (12-4) is positioned on the inner side wall of the heat absorber (12-3), the heat absorber (12-3) is internally provided with the metal sheet (12-5) and the heater (12-6), and the heater (12-6) is fixed on one side of the metal sheet (12-5), and light can sequentially enter the small holes of the outer shielding cover (12-1), the inner shielding cover (12-2) and the heat sensor (12-4) through the small holes of the heat absorber (12-5) and the heat sensor (12-4) of the heat absorber;
the control circuit of the bolometer (12) mainly comprises a resistor I (12-8), a direct current power supply (12-9), a variable capacitor (12-10), a resistor II (12-11), a resistor III (12-12), a resistor IV (12-13), an alternating current power supply (12-14) and a phase-locked amplifier (12-15), wherein the phase-locked amplifier (12-15) is provided with an input end and an output end, the direct current power supply (12-9), the resistor I (12-8) and the heater (12-6) are circularly connected and can form a current loop, the direct current power supply (12-9) is provided with a signal end, the output current of the direct current power supply (12-9) can be controlled according to the input signal, the resistance value of the resistor I (12-8) is 1.0 kiloohm, the heat sensor (12-4), the resistor II (12-11), the resistor III (12-12), the resistor IV (12-13), the phase-locked amplifier (12-15) and the alternating current power supply (12-14) are connected in a wheatstone bridge mode, the heat sensor (12-4), the resistor II (12-12) and the wheatstone bridge (12-13) are respectively connected in a wheatstone bridge mode, the wheatstone bridge (12-11) is provided with the output end of the resistor (12-12) and the output bridge (12-13) is a wheatstone bridge, and the wheatstone bridge (12) is provided, the output end of the lock-in amplifier (12-15) is connected with the signal end of the direct current power supply (12-9), the variable capacitor (12-10) is connected with the resistor II (12-11) in parallel, the variable capacitor range is 300pF to 600pF, the thermal sensor (12-4) is a thermistor, the resistance value at 20 ℃ is 9.2 kiloohms, the resistance values of the resistor II (12-11) and the resistor IV (12-13) are 10.0 kiloohms, the resistor III (12-12) is a variable resistor, and the resistance range is 8.0 kiloohms to 12.0 kiloohms.
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