CN109283151B - Device and method for realizing dielectric barrier discharge in-situ pool of in-situ infrared analysis device - Google Patents
Device and method for realizing dielectric barrier discharge in-situ pool of in-situ infrared analysis device Download PDFInfo
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- CN109283151B CN109283151B CN201811056064.8A CN201811056064A CN109283151B CN 109283151 B CN109283151 B CN 109283151B CN 201811056064 A CN201811056064 A CN 201811056064A CN 109283151 B CN109283151 B CN 109283151B
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/01—Arrangements or apparatus for facilitating the optical investigation
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- Spectroscopy & Molecular Physics (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Chemical & Material Sciences (AREA)
- Analytical Chemistry (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
- Immunology (AREA)
- Pathology (AREA)
- Investigating Or Analysing Materials By Optical Means (AREA)
Abstract
The invention discloses a device and a method for realizing dielectric barrier discharge in an in-situ pool of an in-situ infrared analysis device, wherein the device comprises the following steps: a high voltage power supply; an infrared spectrometer; the in-situ cell comprises a base, a sample cell positioned on the base and a conical dome covering the sample cell, wherein the base is also provided with a gas inlet and a gas outlet, an incident window, an exit window and an observation window are arranged on the conical dome, and infrared light enters the sample cell through the incident window, is reflected and partially refracted and then is emitted from the exit window; the dielectric barrier discharge assembly comprises an insulating sleeve extending into the conical dome above the sample cell, an electrode I inserted into the insulating sleeve and an electrode II arranged at the bottom in the sample cell, wherein the electrode I and the electrode II are connected with a high-voltage power supply. The invention realizes plasma discharge and infrared spectrum analysis at the same time, does not influence the analysis result, solves the uncertain factors which possibly influence the sample in the previous sample transfer process, and leads the discharge process and the infrared spectrum analysis process to be rapid and simple.
Description
Technical Field
The invention relates to the field of analysis and detection, in particular to a device and a method for realizing dielectric barrier discharge in an in-situ pool of an in-situ infrared analysis device.
Background
Plasma is a fourth state of matter other than gases, liquids, and solids. As the energy level increases, the state of the substance can change from a solid to a liquid to a gas and finally to a plasma state. Gas discharge generationThe low-temperature plasma mainly takes the forms of glow discharge, corona discharge, microwave discharge and dielectric barrier discharge. Basic process of gas discharge: 1) the electrons cause gas breakdown; 2) starting to transmit current; 3) electrochemical reaction occurs in the electric field, gas molecules (O)2、H2O, etc.) absorb energy of electrons to form radicals (O, OH, etc.); 4) the free radicals having strong oxidative activity cause or participate in a series of chemical reactions in the electric field.
The plasma is applied to many fields, and mainly comprises sterilization, disinfection, pollutant degradation in 'three wastes', electrostatic dust removal and the like in the environmental field; the material field comprises modification of synthetic fiber, modification of graphene, modification of carbon nitride, preparation of nano catalyst and the like by utilizing plasma; can be used for processing fuel oil, reforming diesel oil and the like in the aspect of energy.
For example, chinese utility model patent with publication number CN 207125267U discloses a plasma air sterilizer for food, including fuselage, power key, plasma source and sterilizer, the bottom of fuselage is equipped with the locker, the below of sterilizer is equipped with the sterilizer lock, and the one end fixed mounting of sterilizer has the sterilizer door handle, one side of power key is equipped with temperature regulation button and display screen, and the opposite side of power key is equipped with the start key that disinfects, one side of start key that disinfects is equipped with the stop display lamp, the top of stop display lamp is equipped with the operation display lamp, and the below of stop display lamp is equipped with the fault display lamp, the one end of plasma source is equipped with heat preservation device.
However, the research on the intermediate substances of the active chemical substances and reactants generated by the discharge is not much, such as the plasma coupled catalyst removes pollutants such as PM, VOCs and the like, oxygen atoms and carbon are combined to form various carbon oxides or are adsorbed on the active sites of the catalyst, but the specific formation of what substances and what radicals are not clear, so that the plasma is used for removing carbon particulate matters, VOCs and NOXEtc. have been hampered.
Disclosure of Invention
The invention provides a device and a method for realizing dielectric barrier discharge in an in-situ cell of an in-situ infrared analysis device, which can realize real-time monitoring of a discharge intermediate product by a diffuse reflection Fourier transform infrared spectrometer.
A device for realizing dielectric barrier discharge in an in-situ pool of an in-situ infrared analysis device comprises:
a high voltage power supply;
an infrared spectrometer;
the in-situ cell comprises a base, a sample cell positioned in the base and a conical dome which covers the sample cell and is detachably and fixedly connected with the base, wherein the base is also provided with a gas inlet communicated to the upper part of the sample cell and a gas outlet communicated to the bottom of the sample cell, the conical dome is provided with three windows, two windows are provided with an infrared window sheet, the other window sheet is used as an observation window, one infrared window sheet is used as an incident window of infrared light from the infrared spectrometer, the other infrared window sheet is used as an exit window for reflecting and partially refracting the infrared light, the infrared light enters the sample cell through the incident window, and is emitted from the exit window after being reflected and partially refracted;
the dielectric barrier discharge assembly comprises an insulating sleeve extending into the conical dome above the sample cell and with a closed bottom end, an electrode I inserted into the insulating sleeve and an electrode II arranged at the bottom in the sample cell, wherein part or all of the edge of the electrode II is in contact with the wall of the sample cell, and the electrode I and the electrode II are connected with the high-voltage power supply.
The device mainly reforms the diffuse reflection infrared in-situ cell, namely, a dielectric barrier discharge space is arranged above the sample cell in the infrared in-situ cell to realize the infrared reflection-absorption spectrum analysis of the intermediate product on the surface of the sample under the 'in-situ' and 'original reaction conditions' during plasma discharge. Oxygen molecules, water, nitric oxide and other oxygen-containing substances contained in the gas generate active substances under the action of high-voltage discharge, the active substances are adsorbed on the surface of a sample to react, and reaction intermediate products generated on the surface can be analyzed and detected by a diffuse reflection infrared spectrometer. Can be used for monitoring the intermediate product of the plasma discharge carbon oxide particles,can also be used for removing Nitrogen Oxide (NO) by analyzing plasma with a catalystX) Or Volatile Organic Compounds (VOCs). The invention can be used for deeply knowing the change of the catalyst surface group in the discharge plasma in the plasma discharge reaction process, and is helpful for disclosing the reaction mechanism of the catalyst in the discharge plasma field for catalyzing and oxidizing carbon particles, volatile organic compounds, selectively catalyzing and reducing nitrogen oxides and other substances.
The voltage waveform output by the high-voltage power supply is in a pulse shape or an alternating current shape, the voltage peak value is between 100V and 150kV, and the frequency is between 1Hz and 10 kHz; the electrode I and the electrode II are made of iron, copper, silver, gold, platinum, aluminum, titanium, magnesium, manganese, lead, tin, stainless steel, copper alloy or aluminum alloy; the in-situ cell can bear any temperature between 0 ℃ and 910 ℃, and the infrared window comprises calcium fluoride, zinc selenide, potassium bromide, lead bromide, zinc sulfide, magnesium fluoride or quartz window.
Reaction gas enters through the gas inlet of the in-situ cell, spreads from the periphery of the sample cup to enter the upper part of the sample cup, namely a discharge space area, and then passes through the sample from top to bottom above the sample cup, the gas is discharged from the bottom of the sample cup, and the bottom of the sample cup is supported by an inert metal net, so that a powder sample is prevented from falling into the bottom of the in-situ cell; the electrode I and the electrode II apply an electric field to gas in a discharge space through voltage output by a high-voltage power supply, so that the gas generates an ionization phenomenon; active chemical substances generated in the electric field of the discharge space, such as generated oxygen atoms, are absorbed by the noble metal catalyst in the sample to form a metal with multiple valence states adsorbed by the oxygen atoms; the resulting oxygen atoms or ozone and carbon combine to form various forms of carbon oxides; the reactive intermediate species on the surface can be detected by diffuse reflection infrared reflectance-absorption spectroscopy.
Preferably, the three windows on the conical dome are symmetrically distributed on the horizontal projection plane of the conical dome with the center of the projection plane.
Preferably, the dielectric barrier discharge assembly further comprises an electrode i fixing sleeve fixedly connected with the observation window of the conical dome and located outside the conical dome, and the insulating sleeve is fixed in the electrode i fixing sleeve.
The insulating tube for dielectric barrier discharge is arranged on an observation window of the in-situ cell and is fixed by an insulating fixing sleeve, one part of the insulating tube is arranged outside the in-situ cell, the other part of the insulating tube is arranged inside the in-situ cell, the bottom of the insulating tube inside the in-situ cell is sealed, and a metal electrode (an electrode I) is inserted into the insulating tube; the high-voltage output end of the high-voltage power supply for discharging is connected with a metal electrode I inserted into the insulating tube, and the grounding electrode is connected with the stainless steel in-situ tank.
Preferably, the insulating sleeve is obliquely inserted into the conical dome at an included angle of 30-60 degrees with the horizontal plane.
Further preferably, the electrode I is inserted right above the center of the sample cell.
Further preferably, the distance between the bottom of the insulating sleeve and the top surface of the sample in the sample cell is 0.1-10 mm.
Preferably, the electrode I is inserted into the bottom of the insulating tube and the space between the electrode I and the inner surface of the insulating tube is filled with a conductive material (e.g., tin, zinc, aluminum).
The insulating tube is made of metal oxide and inorganic material; the oxide is aluminum oxide, titanium oxide, zinc oxide, iron oxide, zirconium oxide, chromium oxide, nickel oxide or magnesium oxide; the inorganic material is silicon oxide, quartz glass, or mica. The insulating tube has an outer diameter of 0.1 mm to 10 mm, an inner diameter of 0.1 mm to 10 mm, a length of 1 cm to 10 cm, and a shape of a tube such as a circle, an ellipse, a triangle, or a polygon.
Preferably, the bottom of the sample cell is sequentially provided with a metal mesh, an insulating gasket and the electrode II from bottom to top, and a sample to be detected is arranged above the electrode II.
A sample placing space, namely a sample cell, is arranged in the in-situ cell base, a metal electrode (electrode II) is arranged below the sample placing space, the electrode II is contacted with the stainless steel in-situ cell, and a sample to be subjected to infrared analysis is placed above the metal electrode; the high-temperature-resistant insulating plate is arranged below the electrode II, and the distance between the electrode I and the electrode II can be adjusted by changing the thickness of the high-temperature-resistant insulating plate; and the bottommost part is supported by an inert metal net, so that the powder sample is prevented from falling into the bottom of the in-situ tank.
The shape of the electrode II is oval, triangular or polygonal, the electrode II is a non-porous flat plate, a hollow net shape or a non-porous wrinkle shape, and the thickness of the electrode II is 0.1-5 mm.
Preferably, part or all of the edges of the electrode II are in contact with the sample wall.
Preferably, a heating device is arranged in the sample cell. Further preferably, the heating device employs a thermocouple.
The invention also provides a method for realizing dielectric barrier discharge and monitoring intermediate substances in an in-situ pool of the in-situ infrared analysis device by using the device, which comprises the following steps:
placing a sample to be detected in a sample tank, introducing reaction gas into the in-situ tank, wherein the reaction gas spreads from the periphery of the sample tank to a discharge space above the sample tank, then passing the sample from top to bottom above the sample tank, and the gas is discharged from the bottom of the sample tank;
simultaneously turning on a high-voltage power supply and the infrared spectrometer, and applying an electric field to the gas in the discharge space by the electrode I and the electrode II through the voltage output by the high-voltage power supply to ensure that the gas generates an ionization phenomenon and a reaction intermediate substance is generated in the electric field in the discharge space; the generated reaction intermediate substance is analyzed and detected by diffuse reflection infrared reflection-absorption spectrum.
Oxygen-containing substances such as oxygen molecules, water, nitric oxide and the like contained in the gas generate active substances such as active oxygen atoms, ozone, hydroxyl radicals, nitrogen dioxide and the like under the action of high-voltage discharge, and the active substances are adsorbed on the surface of a sample; the reaction intermediates generated at these surfaces can be detected by diffuse reflectance infrared reflectance-absorption spectroscopy.
The intermediate product on the surface of the sample under the action of the electric field between the electrode I and the electrode II is monitored in real time through the diffuse reflection infrared reflection-absorption spectrum, so that the change of a catalyst surface group in a discharge plasma in the plasma discharge reaction process is deepened, and the reaction mechanism of the catalyst in the discharge plasma field for catalyzing and oxidizing carbon particles, volatile organic compounds, selective catalytic reduction of nitrogen oxides and other substances is disclosed.
The invention can realize plasma discharge and infrared spectrum analysis. Meanwhile, the analysis result is not influenced at all, the uncertain factors which possibly influence the sample in the previous sample transfer process are solved, and the discharge process and the infrared spectrum analysis process are quick and simple. The set of device realizes integration of discharging and analyzing.
Drawings
FIG. 1 is a schematic front view of a plasma discharge in-situ infrared analysis apparatus according to the present invention;
FIG. 2 is a top view of a plasma discharge in-situ infrared analysis apparatus of the present invention;
FIG. 3 is a schematic view of the right side cross-sectional structure of FIG. 1;
FIG. 4 is a schematic view showing the internal structure of the sample cell of FIG. 3;
FIG. 5 is a graph of the infrared spectrum of graphite discharge infrared as a function of time.
FIG. 6 is Al2O3Catalyst surface discharge infrared spectrogram.
The reference numerals shown in FIGS. 1-4 are as follows:
1-electrode I2-insulating sleeve 3-conical dome
4-infrared window I5-electrode I fixing sleeve 6-infrared window II
7-base 8-gas inlet 9-gas outlet
10-wire I11-wire II 12-screw
13-fixed plate 14-sample cell 15-sample
16-electrode II 17-high temperature resistant insulating gasket 18-metal mesh
19-high voltage power supply 20-infrared spectrometer 21-in-situ cell
Detailed Description
As shown in fig. 1 to 4, a device for realizing dielectric barrier discharge in an in-situ cell of an in-situ infrared analysis device comprises a high-voltage power supply 19, an infrared spectrometer 20, an in-situ cell 21 and a dielectric barrier discharge component, wherein the infrared spectrometer adopts a fourier transform infrared spectrometer, the voltage waveform output by the high-voltage power supply is in a pulse shape or an alternating current shape, the voltage peak value is between 100V and 150kV, and the frequency is between 1Hz and 10 kHz.
The in-situ cell 21 comprises a base 7 and a conical dome 3, the base is made of stainless steel, an inward-concave sample cell 14 is arranged in the center of the top surface of the base, a gas inlet 8 and a gas outlet 9 are formed in the base, the gas inlet is communicated to the periphery of the sample cell, the gas outlet is communicated to the bottom of the sample cell, gas spreads to the upper portion of the sample cell from the periphery of the sample cell, then enters the sample cell downwards, and is discharged from the bottom of the sample cell after passing through a sample.
The conical dome 3 covers the sample cell, the conical dome 3 is fixedly connected with the base through the fixing plate 13 and the screw 12, 3 windows are symmetrically arranged on the conical dome 3 by taking the center of the dome as the center, one window is used as an observation window, the other two windows are used as an infrared light inlet and outlet window respectively, and an infrared window piece I4 and an infrared window piece II 6 are arranged at the two infrared light inlet and outlet windows respectively. Infrared light enters from the infrared window I to reach the surface of the sample, is reflected and partially refracted, then exits from the infrared window II, and is collected by the infrared spectrometer; gas enters the in-situ cell from the gas inlet 8, reaches the periphery of the sample cup, then spreads to the upper part of the sample, passes through the sample and the electrode II 16, and then is discharged from the gas outlet 9, and the sample placing space is provided with a heating device
Dielectric barrier discharge assembly includes electrode I1 and electrode II 16, set up I fixed cover 5 of electrode on the surface of the observation window of toper calotte, I fixed cover bottom of electrode is fixed with observation window department, the pipe box part outwards extends with the contained angle of 30 ~ 60 degrees with the horizontal plane, insulation support 2 runs through the pipe box part and stretches into in the toper calotte, the insulation support bottom is sealed and extends to directly over the sample cell, electrode I1 inserts in the insulation support, including filling conducting material between electrode I1 and the insulation support inner wall, I partly of electrode is located the toper calotte, partly is located outside the toper calotte.
The high-voltage output end of the high-voltage power supply is connected with the electrode I through a lead I10, and the grounding electrode is connected with the stainless steel in-situ tank through a lead II 11.
The working mode is as follows:
reaction gas enters through a gas inlet of the in-situ cell, spreads from the periphery of the sample cup to the upper part of the sample cup, namely a discharge space area, passes through the sample from top to bottom above the sample cup, the gas is discharged from the bottom of the sample cup, and the bottom of the sample cup is supported by an inert metal net, so that a powder sample is prevented from falling into the bottom of the in-situ cell; the electrode I and the electrode II apply an electric field to gas in a discharge space through voltage output by a high-voltage power supply, so that the gas generates an ionization phenomenon; active chemical substances generated in the electric field of the discharge space, such as generated oxygen atoms, are absorbed by the noble metal catalyst in the sample to form a metal with multiple valence states adsorbed by the oxygen atoms; the resulting oxygen atoms or ozone and carbon combine to form various forms of carbon oxides; the reactive intermediate species on the surface can be detected by diffuse reflection infrared reflectance-absorption spectroscopy.
The specific structure and the method of using the plasma discharge in-situ infrared analysis device of the present invention are specifically illustrated by the following two examples.
Example 1
In the example, the electrode I and the electrode II are made of stainless steel materials, the insulating tube is made of quartz glass materials, the electrode II is a square of a non-porous flat plate, and two high-temperature-resistant gaskets made of circular alumina materials with the thickness of 0.5mm are placed below the electrode II, so that the thickness of a sample is 2mm, and the distance between the electrode I and the electrode II is 2.5 mm.
The method comprises the following steps in practical use:
(1) the electrode I1 and the electrode II 16 are respectively connected with a high-voltage power supply through a lead I10 and a lead II 11, and the lead II 11 is simultaneously grounded.
(2) High voltage is output by a high-voltage power supply and is loaded on the electrode I1 and the electrode II 16, so that an electric field is formed in a discharge space above the sample between the electrode I1 and the electrode II 16, and electrons and ions are generated after gas in the discharge space is ionized. The electrons (i.e. electrons generated after ionization or electrons originally existing in the gas) gain energy under the action of the electric field, and then collide with molecules or atoms in the gas to decompose the molecules or atoms. Various chemical reactions are initiated by the adsorption of various chemical substances generated by decomposition on the surface of a sample
(3) Detecting and analyzing the infrared spectrum of the surface of the sample by using a diffuse reflection Fourier transform infrared spectrometer (the change of the infrared spectrum of the surface after the carbon particle plasma is discharged is shown as follows):
samples were 100: 10: 1, introducing 45mL of helium and 5mL of oxygen into the mixture, and controlling the temperature at 50 ℃; then, collecting a background spectrum, turning on a high-voltage pulse power supply, and adjusting the high-voltage peak value of the pulse to be 4kV and the pulse frequency to be 500 Hz; the sample spectra were collected at 30min, 60min, 90min, 120min, 150min, and 180min of discharge treatment, respectively, and the results are shown in fig. 5 below.
After discharge, active oxygen is generated and comprises ozone and active oxygen atoms, after the active oxygen is combined with C atoms on graphite, a carbon oxygen compound is formed, and then the carbon oxygen compound is decomposed to generate CO or CO2，1683cm-1And 1173cm-1C ═ O and C — O for lactones; 1649cm-1-COOH or quinone C ═ O; 1519cm-1Is an inorganic carbonate; 1040cm-1Is an ether C-O-C; 934cm-1Is C-O. From the peak area change, the amount of surface carbon-oxygen compounds (C-O) increased first to 90min saturation with the increase of discharge time, and did not increase any more. The change in surface groups after different spotting times can be seen from the spectra.
Example 2
Placing Al in an in-situ pool2O3Catalyst, introduction of CO2And discharging and regenerating the catalyst after adsorption. The purpose is to observe Al in the discharge plasma field2O3Change of catalyst surface, thereby deducing Al under the action of plasma2O3Catalyst and process for preparing sameThe reaction mechanism of regeneration.
When in specific use, the method comprises the following steps:
(1) mixing Al2O3Catalyst powder is filled in a sample cell, the surface of the sample is coated and leveled, and the gas temperature in the in-situ cell is controlled at 25 ℃ (thermostat control); the electrode I10 and the electrode II 16 are respectively connected with a high-voltage power supply through a metal stainless steel lead I21 and a metal stainless steel lead II 22, and the metal stainless steel lead II 22 is simultaneously grounded.
(2) Introducing helium gas with the total gas flow of 50mL/min for 10min into the in-situ cell, and collecting a background spectrum; the total flow of the introduced gas is 50mL/min, and the total flow of the introduced gas is 300ppm CO2Balancing helium, adsorbing for 10min, and collecting a sample spectrum with a background spectrum subtracted; gas with a total flow rate of 50mL/min, 14% O is introduced2，2％H2And balancing with helium, starting discharging for 5min, and collecting the sample spectrum with the background spectrum subtracted.
(3) The voltage waveform applied by the high-voltage power supply is positive and negative pulses and negative and positive pulses, and the absolute value of the voltage peak is 6 kV.
The IR spectrum is shown in FIG. 6 by comparing the change in IR spectra under different conditions. CO 22Adsorbed Al2O3Monodentate carbonate (1384 cm) appears on the surface-1) And bicarbonate (1432 cm)-1、1546cm-1And 1620cm-1) And CO in adsorbed state2(2335cm-1) After water and oxygen are introduced, monodentate carbonate and bicarbonate on the surface are obviously reduced, and after discharge, the monodentate carbonate disappears and the bicarbonate is greatly reduced. Therefore, the influence of the discharge on the surface regeneration reaction is deduced, and evidence is provided for mechanism inference.
The above description is only an embodiment of the present invention, but the technical features of the present invention are not limited thereto, and any person skilled in the relevant art can change or modify the present invention within the scope of the present invention.
Claims (6)
1. A device for realizing dielectric barrier discharge in an in-situ pool of an in-situ infrared analysis device is characterized by comprising:
a high voltage power supply;
an infrared spectrometer;
the in-situ cell comprises a base, a sample cell positioned in the base and a conical dome which covers the sample cell and is detachably and fixedly connected with the base, wherein the base is also provided with a gas inlet communicated to the upper part of the sample cell and a gas outlet communicated to the bottom of the sample cell, the conical dome is provided with three windows, two windows are provided with an infrared window sheet, the other window sheet is used as an observation window, one infrared window sheet is used as an incident window of infrared light from the infrared spectrometer, the other infrared window sheet is used as an exit window for reflecting and partially refracting the infrared light, the infrared light enters the sample cell through the incident window, and is emitted from the exit window after being reflected and partially refracted;
the dielectric barrier discharge assembly comprises an insulating sleeve which extends into the conical dome and is above the sample cell and the bottom end of which is closed, an electrode I inserted into the insulating sleeve and an electrode II arranged at the bottom in the sample cell, wherein part or all of the edge of the electrode II is in contact with the wall of the sample cell, and the electrode I and the electrode II are connected with the high-voltage power supply; the dielectric barrier discharge assembly also comprises an electrode I fixed sleeve fixedly connected with the observation window of the conical dome and positioned outside the conical dome, and the insulating sleeve is fixed in the electrode I fixed sleeve;
the bottom of the sample cell is sequentially provided with a metal mesh, an insulating gasket and the electrode II from bottom to top, and a sample to be detected is arranged above the electrode II.
2. The device of claim 1, wherein the insulating sleeve is inserted into the conical dome at an angle of 30-60 ° from the horizontal.
3. The apparatus of claim 2, wherein the electrode I is inserted above the sample cell.
4. The apparatus of claim 2, wherein the bottom of the insulating sleeve is spaced from the top surface of the sample in the sample cell by a distance of 0.1 mm to 10 mm.
5. The device of claim 1, wherein a heating device is disposed in the sample cell.
6. A method for performing dielectric barrier discharge and intermediate substance monitoring in an in-situ cell of an in-situ infrared analysis device using the device of claim 1, comprising the steps of:
placing a sample to be detected in a sample tank, introducing reaction gas into the in-situ tank, wherein the reaction gas spreads from the periphery of the sample tank to a discharge space above the sample tank, then passing the sample from top to bottom above the sample tank, and the gas is discharged from the bottom of the sample tank;
simultaneously turning on a high-voltage power supply and the infrared spectrometer, and applying an electric field to the gas in the discharge space by the electrode I and the electrode II through the voltage output by the high-voltage power supply to ensure that the gas generates an ionization phenomenon and a reaction intermediate substance is generated in the electric field in the discharge space; the generated reaction intermediate substance is analyzed and detected by diffuse reflection infrared reflection-absorption spectrum.
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| CN110514593A (en) * | 2019-08-26 | 2019-11-29 | 江苏大学 | A kind of Energetic Materials by In-Situ Diffuse Reflection device of generation and fortifying catalytic agent surface-discharge |
| CN111024732B (en) * | 2019-12-31 | 2022-08-16 | 安徽微宇仪器科技有限公司 | Dynamic in-situ gas phase reaction tank for soft X-ray spectroscopy experiment |
| CN114199774A (en) * | 2021-11-12 | 2022-03-18 | 江苏大学 | In-situ transmission infrared reaction tank under action of jet plasma and testing method |
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