CN113866095A - In-situ spectral analysis pool for gas-sensitive sensing exploration and application - Google Patents
In-situ spectral analysis pool for gas-sensitive sensing exploration and application Download PDFInfo
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Abstract
本发明公开了一种用于气敏传感探究的原位光谱分析池及应用，适用于红外光谱仪、显微拉曼光谱仪等设备的原位光谱分析，腔体顶部设有光学视窗，腔体顶盖与底部原位池主体间设有密封圈；密闭原位光谱分析池内部包括容载了温控元件和温度测量元件的样品控温台，该样品控温台可进行高度的调节；样品控温台其上即为样品测试区，周围设置有多位电学探针，用于测量待测样品的电学特性；密闭的原位光谱分析池设置有多个气体出入口，用于抽真空处理、将多种气体经过配气仪按特定比例混合后引入气体及排出气体。本发明将待测样品置于原位池中，由导气管进入原位池腔体的气体掠过样品表面，可原位采集气固反应过程中的光谱信息，并测量气敏传感器的电学特性。
The invention discloses an in-situ spectral analysis cell for gas-sensing sensing exploration and its application, which are suitable for in-situ spectral analysis of infrared spectrometers, micro Raman spectrometers and other equipment. The top of the cavity is provided with an optical window, and the cavity is A sealing ring is arranged between the top cover and the main body of the in-situ cell at the bottom; the inside of the closed in-situ spectral analysis cell includes a sample temperature control table containing temperature control elements and temperature measurement elements, and the sample temperature control table can be adjusted in height; The temperature control platform is the sample testing area, and there are multiple electrical probes around it to measure the electrical characteristics of the sample to be tested; the closed in-situ spectral analysis cell is provided with multiple gas inlets and outlets for vacuum treatment, A variety of gases are mixed in a specific ratio through a gas distribution instrument, and then the gas is introduced and exhausted. In the invention, the sample to be tested is placed in the in-situ cell, and the gas entering the in-situ cell cavity through the air duct swept across the surface of the sample, and the spectral information in the gas-solid reaction process can be collected in-situ, and the electrical characteristics of the gas sensor can be measured. .
Description
Technical Field
The invention belongs to the technical field of in-situ spectral analysis, and particularly relates to an in-situ spectral analysis pool for gas-sensitive sensing exploration and application thereof.
Background
The gas sensor is a converter which converts the volume fraction of a certain gas into a corresponding electric signal, can be used for identifying the gas type and detecting the gas concentration, can be used for the real-time detection of inflammable, explosive and toxic gases, and has wide application in the fields of environmental monitoring, medical diagnosis, national defense and military and the like. In order to effectively prevent the safety problem caused by gas leakage, people put forward higher requirements on the detection precision, selectivity and operation reliability of the gas sensor, and the gas-sensitive property of the gas sensor under the atmosphere with different temperatures, different humidities and different concentrations is required to be tested, so that new challenges are provided for the construction of a gas-sensitive test and a gas-sensitive material research and development system.
In the gas sensitive test, the conventional research method is to provide the sum of various microscopic information of a test system under the same condition, and it is difficult to accurately identify each reactant, intermediate product and the like of a complex system. With the development of the spectroscopic technology, the in-situ spectroscopic technology has become one of the effective means for studying various complex systems. In-situ spectroscopy technologies such as diffuse reflection Fourier transform infrared spectroscopy (DRIFTS), Micro-Raman spectroscopy (Micro-Raman), ultraviolet-visible diffuse reflection spectroscopy (UV-Vis DRS) and the like acquire some valuable surface reaction information by tracking and characterizing the on-site reaction adsorption state on a sample to be detected, and further analyze the reaction mechanism, and the in-situ characterization technology is increasingly paid attention. The spectrum of a sample is subjected to in-situ analysis, the gas-sensitive action mechanism of each component in a system and the interaction mechanism among the components can be explored, the generation of a reactant and the change of the reactant along with temperature, pressure, time and the like can be dynamically monitored, the adsorption, desorption and catalytic reaction of molecules in gas or liquid on the surface of a solid material can be studied in situ, and the in-situ analysis has an unique effect on the change rule of the performance of a gas-sensitive material of a test gas sensor along with the temperature, the pressure, the time, the gas type and the concentration.
However, due to the limitations of optical path layout and spatial layout, the conventional in-situ spectrum cell cannot introduce a probe for electrical test, and cannot simultaneously perform electrical characteristic test and in-situ spectrum analysis in the gas-sensitive performance test of the gas sensor, so that the electrical characteristic analysis and the material surface change analysis of the gas-sensitive material are forced to be performed separately, environmental parameters and electrical parameters cannot be obtained simultaneously, and the performance test work of the gas-sensitive sensor is greatly disturbed due to the influence of external factors (such as temperature, pressure, gas concentration and the like) on repeated experiments. Therefore, it is important to improve and develop the original test device, and to research and design a gas sensor performance test device with high reliability and more test functions.
Disclosure of Invention
The invention aims to provide an in-situ spectrum analysis pool for gas-sensitive sensing exploration and application aiming at the defect that the prior art cannot simultaneously obtain electrical parameters and perform spectrum analysis and has large influence on gas sensing mechanism analysis.
The purpose of the invention is realized by the following technical scheme: the utility model provides an in situ spectral analysis pond for gas sensitive sensing is probed, and in situ spectral analysis pond main part is the cylinder cavity, and exciting light passes the optical window that cell body upper portion set up and shines on the sample that awaits measuring, is equipped with the sealing washer between cavity top cap and the bottom in situ pond main part.
The in-situ pond cavity is internally provided with a sample temperature control table for containing and carrying a temperature control packaging assembly, which comprises a temperature control element and a temperature measurement element, and is used for directly heating or refrigerating the sample to be tested and collecting temperature, thereby adjusting the temperature of sample testing.
And a plurality of electrical probes are respectively arranged on the periphery of the sample test area, and the sample is placed in the sample test area for testing and is used for measuring the electrical characteristics of the sample to be tested.
The in-situ spectral analysis cell main body is provided with a plurality of gas inlets and outlets for vacuumizing treatment, introducing gas and leading out gas.
Further, the exciting light used for detection can be selected from infrared light and Raman light; the optical window for infrared test is made of zinc selenide or potassium bromide crystal material, preferably zinc selenide crystal with better water resistance. The optical window used for raman testing was selected from a quartz window.
Furthermore, the surface of the optical window is provided with a metal film or a metal oxide film or a catalyst film, and the thickness of the film is 0.001-100 μm; the thickness of the optical window is 0.5-5mm, the inner side of the window sheet is provided with a fluororubber sealing ring, and the outer side is provided with a polytetrafluoroethylene pressure ring.
Furthermore, the sample temperature control table can be lifted and adjusted in height so as to adjust the light path to focus on the sample to be measured.
Furthermore, the lead of the electrical probe, the temperature control element and the lead of the temperature measurement element are all led out from the electric wire temperature control guide port at the bottom of the sample temperature control table.
Furthermore, the gas inlet and outlet of the in-situ spectral analysis cell are provided with flow guide structures in conical distribution.
An in-situ infrared spectrum gas-sensitive testing device comprises the in-situ spectrum analysis cell, an infrared spectrometer and a diffuse reflection accessory. And placing the sample to be detected in an in-situ spectral analysis cell, and placing a diffuse reflection accessory provided with the in-situ infrared spectral analysis cell in an infrared spectrometer. The gas entering the cavity of the in-situ spectral analysis cell sweeps the surface of the sample, the infrared spectrum in the gas-solid reaction process is acquired in situ, and the electrical characteristics of the gas-sensitive sensor are detected by an electrical probe.
Further, the system also comprises a gas mass flow controller integrated gas distribution instrument, a gas chromatograph-mass spectrometer, a digital source meter and the like. And a gas mass flow controller integrated gas distribution instrument is arranged on a gas inlet pipeline of the in-situ spectral analysis cell, so that the content and the proportion of introduced gas components are accurately controlled. The gas outlet pipeline of the in-situ spectral analysis cell is connected with a gas chromatograph-mass spectrometer and outputs data of gas type and concentration; the digital source meter outputs the test data of the gas sensor to be tested.
An in-situ micro-Raman spectrum gas-sensitive testing device comprises the in-situ spectral analysis cell, an optical sliding table and a micro-Raman spectrometer. And placing the sample to be detected in an in-situ spectral analysis cell, fixing the in-situ spectral analysis cell on an optical sliding table, and placing the in-situ spectral analysis cell below a microscope of the micro-Raman spectrometer. Gas entering the cavity of the in-situ spectral analysis pool sweeps the surface of the sample, the Raman spectrum in the gas-solid reaction process is acquired in situ, and the electrical characteristics of the gas sensor are detected through an electrical probe.
Further, the system also comprises a gas mass flow controller integrated gas distribution instrument, a gas chromatograph-mass spectrometer, a digital source meter and the like. And a gas mass flow controller integrated gas distribution instrument is arranged on a gas inlet pipeline of the in-situ spectral analysis cell, so that the content and the proportion of introduced gas components are accurately controlled. The gas outlet pipeline of the in-situ spectral analysis cell is connected with a gas chromatograph-mass spectrometer and outputs data of gas type and concentration; the digital source meter outputs the test data of the gas sensor to be tested.
Compared with the prior art, the invention has the following beneficial effects:
(1) the invention can provide accurate electrical detection, flexible probe connection, accurate temperature regulation and convenient atmosphere control through integrated electrical, probe, micro-cavity and dynamic and static gas distribution design;
(2) four-position electrical probes are arranged in the in-situ spectral analysis pool to support two-wire or four-wire testing, and the connection mode and the number of the sensors can be customized according to requirements;
(3) the in-situ spectral analysis pool adopts a platform temperature control mode, and a heating electrode is not required to be additionally manufactured;
(4) the temperature control hot table contained in the in-situ spectral analysis cell can be used together with an infrared spectrometer and a micro-Raman spectrometer for spectral or microscopic in-situ analysis during electrical test;
(5) the micro cavity structure of the in-situ spectral analysis cell is also suitable for being connected with a gas-liquid gas distribution system with controllable humidity, can be used for on-line detection of gas sensitivity, humidity sensitivity and other properties while realizing the rapid replacement and balance of the atmosphere concentration and humidity of the cavity, and can also be connected with a vacuum pump and a barometer for performance test under vacuum or different air pressures;
(6) the in-situ spectral analysis cell supports matching with an LED light source or an external light path to carry out related researches such as photosensitivity, photoelectricity, photosensitive gas sensitivity and the like;
(7) the in-situ spectral analysis cell has wide application range and is suitable for photoelectric testing of millimeter-grade materials or devices (such as sensors, detectors and transistors) and in-situ comprehensive characteristic analysis of infrared spectrums, Raman spectrums, microscopes and the like.
Drawings
FIG. 1 is a schematic cross-sectional view of the internal structure of an in-situ spectroscopic cell of the present invention;
FIG. 2 is a schematic top view of an in situ spectroscopic cell of the present invention;
in the figure: 1 optical window, 2 cavity top covers, 3 sample temperature control platforms, 4 gas inlets, 5 vacuum diversion ports, 6 gas outlets, 7 temperature control packaging components, 8 lifting devices, 9 wire temperature control diversion ports, 10 in-situ pool main bodies, 11 sealing rings, 12 electrical probes and 13 sample test areas.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
As shown in fig. 1 and fig. 2, the in-situ spectrum analysis cell for gas sensor exploration is used for gas sensor performance testing.
The in-situ cell main body 10 is a cylindrical cavity, exciting light passes through an optical window 1 arranged on the upper part of the in-situ cell main body 10 to irradiate on a sample to be measured, and a sealing ring 11 is arranged between the cavity top cover 2 and the in-situ cell main body 10.
The in-situ cell main body 10 is internally provided with a sample temperature control table 3 for accommodating a temperature control packaging assembly 7, the temperature control packaging assembly 7 further comprises a temperature control element (resistance wire) and a temperature measuring element (thermocouple) for adjusting the temperature of sample testing, and the temperature control element is used for directly heating or refrigerating a sample to be tested; the temperature measuring element is used for collecting the temperature of a sample to be measured. The in-situ spectral analysis pool adopts a platform temperature control mode, does not need to additionally manufacture a heating electrode, and simplifies an experimental device.
The periphery of the sample testing area 13 is provided with a plurality of electrical probes 12, the leads of the electrical probes 12 are led out from the lower part of the in-situ cell sample temperature control table 3, and a sample is placed in the sample testing area 13 for testing the electrical characteristics of the gas sensor material, so that the electrical signals of the sample can be obtained in real time while spectral analysis is carried out. The existence of a plurality of pairs of electrodes can realize the test of the gas sensor array, and the test efficiency of the tested gas sensor is greatly improved. The lead of the electrical probe 12, the temperature control element and the lead of the temperature measuring element are all led out from the wire temperature control lead port 9 at the bottom of the sample temperature control platform 3.
The height of the sample thermal control table 3 can be adjusted by the lifting device 8. The upper part of the lifting device 8 is connected with the sample temperature control table 3, the lower part of the lifting device is connected with the bottom of the cavity of the in-situ cell main body 10, and the height of the sample temperature control table 3 is adjusted by adjusting bolts inside the lifting device, so that a light path is focused on a sample to be measured.
The front part of the in-situ tank main body 10 is provided with three gas inlets and outlets, namely a gas inlet 4, a vacuum diversion port 5 and a gas outlet 6. The gas inlet 4 is used for introducing gas, the vacuum diversion port 5 is used for vacuumizing the cavity of the in-situ cell main body 10, and the gas outlet 6 is used for leading out gas. The gas inlet 4 and the gas outlet 6 of the in-situ spectral analysis pool are both provided with a flow guide structure in conical distribution, so that smooth gas flow is ensured, uniform gas laminar flow and stable temperature field distribution can be formed, the generation of vortex and other phenomena is avoided, gas after reaction in the in-situ spectral analysis pool can be discharged as soon as possible, and the influence of the change of gas concentration in the reaction adsorption process on the test process is avoided.
The excitation light used for detection can be selected from infrared light and Raman light. The optical window 1 for infrared test is made of barium fluoride, magnesium fluoride, thallium bromide, rutile, germanium, silicon, zinc selenide or potassium bromide crystal material; the zinc selenide crystal with better water resistance is preferred, and has the advantages of low absorption rate of visible spectrum red end spectrum, no moisture absorption and stability in experimental environment. The surface of the optical window 1 is provided with a metal or metal oxide film or a catalyst film, and the thickness of the film is 0.001-100 μm. The optical window 1 for raman testing was selected from a quartz window. The thickness of the window sheet of the optical window 1 is 0.5-5 mm. The inner side of the optical window 1 is provided with a fluororubber sealing ring 11, and the outer side of the optical window is provided with a polytetrafluoroethylene pressure ring, so that the sealing performance is excellent.
The invention relates to an in-situ infrared spectrum gas-sensitive testing device, which is used for testing the working performance of a gas-sensitive sensor by combining an in-situ infrared spectrum method and mainly comprises a closed in-situ spectrum analysis pool (serving as an in-situ infrared spectrum analysis pool), a diffuse reflection accessory, a gas mass flow controller integrated gas distribution instrument, an infrared spectrometer, an online gas chromatograph-mass spectrometer GC-MS (gas chromatography-mass spectrometer), a high-precision digital source meter (comprising an electrical signal acquisition system), a computer and the like.
And placing the sample to be detected in an in-situ infrared spectrum analysis cell, and placing a diffuse reflection accessory provided with the in-situ infrared spectrum analysis cell in an infrared spectrometer. Gas entering the cavity of the in-situ cell main body 10 from the gas inlet 4 sweeps the surface of a sample, so that the infrared spectrum in the gas-solid reaction process can be acquired in situ, and the electrical characteristics of the gas sensor are detected by the electrical probe 12. Specifically, the method comprises the following steps:
the in-situ infrared spectrum analysis pool is made of stainless steel, aluminum, copper or polytetrafluoroethylene materials and has good mechanical property and corrosion resistance. The in-situ infrared spectrum analysis cell is a closed cavity formed by matching fastening elements, and can realize in-situ test of the gas sensor in a high-pressure environment. The bottom of the in-situ infrared spectrum analysis pool is provided with a mounting hole for being fixedly arranged in the diffuse reflection accessory.
And a gas distribution instrument integrated with a gas mass flow controller is arranged on a gas pipeline between a gas inlet 4 of the in-situ cell main body 10 and a gas bottle, so that the content and the proportion of introduced gas components are accurately controlled. The gas outlet 6 is connected with a tail gas device. The reaction gas entering the cavity of the in-situ cell body 10 sweeps across the surface of the sample.
The gas mass flow controller integrated gas distribution instrument is an important controller for accurately preparing the concentration of gas to be detected, the selection of the measuring range is determined according to the concentration range of the gas to be detected, the gas distribution within different concentration ranges of one gas can be realized, and the gas distribution can be carried out on different gases to be detected in a mixed manner.
The gas outlet 6 is connected with an online gas chromatograph-mass spectrometer and outputs the data of the type and the concentration of the gas.
The electrical probe 12 is connected with a high-precision digital source meter (including an electrical signal acquisition system) through a lead, and the digital source meter outputs test data of the gas sensor to be tested.
The invention discloses an in-situ micro-Raman spectrum gas-sensitive testing device which is used for testing the working performance of a gas-sensitive sensor by combining an in-situ micro-Raman spectrum method and mainly comprises a closed in-situ spectrum analysis pool (serving as the in-situ micro-Raman spectrum analysis pool), an optical sliding table, a gas mass flow controller integrated gas distribution instrument, a micro-Raman spectrometer, an online gas chromatograph-mass spectrometer (GC-MS), a high-precision digital source meter (comprising an electrical signal acquisition system), a computer and the like. And placing the sample to be detected in an in-situ micro-Raman spectrum analysis pool, fixing the in-situ micro-Raman spectrum analysis pool on an optical sliding table, and placing the in-situ micro-Raman spectrum analysis pool below a microscope of a micro-Raman spectrometer. Gas entering the cavity of the in-situ cell main body 10 from the gas inlet 4 sweeps the surface of a sample, so that the Raman spectrum in the gas-solid reaction process can be acquired in situ, and the electrical characteristics of the gas sensor are detected by the electrical probe 12.
The two gas-sensitive test devices mainly simulate a dynamic gas environment in an actual environment, and a gas source is switched and selected according to the type of the gas-sensitive sensor, such as sensitive materials which are easy to oxidize or need inert gas protection, and inert gas is generally selected and used as background gas. The background gas is supplied by a gas cylinder or a gas generator, and is quantitatively and stably output through a gas distribution instrument integrated with a gas mass flow controller. The gas circuit of the dynamic gas-sensitive testing device is built by a 316-material steel pipe, and the components of the gas circuit mainly comprise a check valve, a gas mass flow controller integrated gas distribution instrument and a 316-material stainless steel clamping sleeve. The stainless steel clamping sleeve made of 316 is a joint for connecting various gas circuits, and is acid-resistant, alkali-resistant, corrosion-resistant, and not easy to deform and leak.
The invention relates to a performance test method of a gas-sensitive sensor, which comprises the following steps:
step one, sample introduction. Tabletting a sample to be tested, wherein the thickness of the sample is 0.5-2mm, placing the pressed sample in a sample testing area 13 above a sample temperature control table 3, contacting an electrical probe 12 with the sample to be tested, fixing a cavity top cover 2 by using a screw, and fixing an in-situ spectral analysis cell on the specific position of a spectrometer.
And step two, connecting the experimental devices. After the in-situ cell main body 10 is sealed with the cavity top cover 2 through the sealing ring 11, the gas inlet 4 is connected with a gas mass flow controller integrated gas distribution instrument through a guide pipe, and the content ratio of each component of the introduced gas is accurately controlled; the gas outlet 6 conduit is connected with an online gas chromatograph-mass spectrometer (GC-MS), and the gas type and concentration are monitored in real time by the online GC-MS; the electric probe 12 is led out from the lower part of the in-situ cell sample temperature control table 3 through a lead, is connected to a high-precision digital source meter (an electric signal acquisition system), and outputs resistance test data of the tested gas-sensitive material; the temperature control element lead, the temperature measuring element lead and the electrical probe 12 lead are led out from the lower electric wire temperature control lead port 9 of the temperature control packaging assembly 7 together and are connected with a temperature controller (external instrument) for real-time temperature monitoring.
And step three, purging the atmosphere in the pool. And (3) sweeping the inside of the pool body by using background gas through the gas inlet 4, vacuumizing the atmosphere inside the pool body through the vacuum flow guide port 5 to replace the atmosphere, and closing the gas inlet valve 4 after sweeping.
Step four, setting reaction conditions. The type, flow and concentration of the gas are set according to the reaction requirement, and the temperature condition is set.
And step five, adjusting the sample stage lifting device 8 to enable the exciting light incident light path to enter the sample testing area 13 through the optical window 1. When the in-situ infrared spectrum gas-sensitive testing device is adopted, exciting light enters the sample testing area 13, is subjected to diffuse reflection, and is emitted out through the optical window 1 again.
And step six, signal acquisition. Collecting a sample spectrogram under the reaction condition set in the step four; the resistance change and the gas concentration change of the gas-sensitive material are detected in real time, and the type or concentration of the gas or the operation temperature can be changed to carry out a plurality of experiments.
And seventhly, analyzing results. And analyzing and processing the acquired spectrogram by combining the change of the gas concentration given by an online gas chromatograph-mass spectrometer (GC-MS), and analyzing the change of the resistance of the gas-sensitive material along with the type, the concentration and the time of the gas.
Example one
Take the gas sensing performance of graphene materials as an example.
Pressing graphene into a sheet by a tablet press, wherein the thickness of the sheet is 1mm, the diameter of the sheet is 6mm, placing the pressed graphene sheet sample at the center of a sample temperature control table 3, and contacting the sample by an electric probe 12. Four probes are selected and distributed around the sample temperature control table 3 at equal intervals, and the distance between the two probes in opposite positions is 4 mm. After the sample loading is finished, the cavity top cover 2 is fixed by screws, so that good air tightness in the cavity of the in-situ cell is ensured, and the in-situ cell is fixed in the diffuse reflection accessory and placed inside the infrared spectrometer. The gas inlet pipeline of the in-situ cell is connected with a gas steel cylinder through a gas mass flow controller integrated gas distribution instrument, and the gas outlet pipeline of the in-situ cell is connected with an online GC-MS (gas chromatography-mass spectrometer) for detecting the real-time gas outlet concentration. And a digital source meter, a temperature controller and a computer system are connected.
Opening a gas inlet and outlet, introducing high-purity nitrogen into the cavity of the in-situ tank, purging the atmosphere in the tank, detecting that the nitrogen gas reaches a certain purity and does not change any more through Online GC-MS, setting the temperature to 150 ℃, introducing 100ppm of acetylene gas, and setting the gas flow to 30sccm until the concentration of the acetylene gas in the cavity is kept constant. The concentration and the flow of acetylene gas are determined by adjusting a control panel of the gas mass flow controller integrated gas distribution instrument, acetylene and nitrogen gas are introduced into the gas mass flow controller integrated gas distribution instrument, the concentration of the acetylene gas is set to be 100ppm on the control panel of the gas mass flow controller integrated gas distribution instrument, and the flow of mixed gas is set to be 30 sccm. In the process of introducing acetylene gas until the gas concentration is constant, monitoring the gas concentration by means of online GC-MS, adsorbing or reacting the gas by passing through a sample, continuously acquiring the real-time infrared spectrum of the sample to be detected in situ in the whole experimental process, synchronously monitoring the resistance performance of the graphene sample by using a digital source meter, obtaining the gas-sensitive response mechanism of the graphene material to the acetylene gas with specific concentration from zero to 100ppm in the process of stabilizing the acetylene gas concentration with the time change of the resistance of the graphene sample.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (10)
1. An in-situ spectroscopic cell for gas-sensitive sensing exploration, comprising:
the in-situ spectral analysis tank main body is a cylindrical cavity, exciting light penetrates through an optical window arranged on the upper part of the tank body to irradiate on a sample to be measured, and a sealing ring is arranged between a top cover of the cavity and the bottom in-situ tank main body.
The in-situ pond cavity is internally provided with a sample temperature control table for containing and carrying a temperature control packaging assembly, which comprises a temperature control element and a temperature measurement element, and is used for directly heating or refrigerating the sample to be tested and collecting temperature, thereby adjusting the temperature of sample testing.
And a plurality of electrical probes are respectively arranged on the periphery of the sample test area, and the sample is placed in the sample test area for testing and is used for measuring the electrical characteristics of the sample to be tested.
The in-situ spectral analysis cell main body is provided with a plurality of gas inlets and outlets for vacuumizing treatment, introducing gas and leading out gas.
2. The in situ spectroscopy cell of claim 1, wherein: the exciting light used for detection can be infrared light or Raman light; the optical window for infrared test is made of zinc selenide or potassium bromide crystal material, preferably zinc selenide crystal with better water resistance. The optical window used for raman testing was selected from a quartz window.
3. The in situ spectroscopy cell of claim 1, wherein: the surface of the optical window is provided with a metal film or a metal oxide film or a catalyst film, and the thickness of the film is 0.001-100 mu m; the thickness of the optical window is 0.5-5mm, the inner side of the window sheet is provided with a fluororubber sealing ring, and the outer side is provided with a polytetrafluoroethylene pressure ring.
4. The in situ spectroscopy cell of claim 1, wherein: the sample temperature control table can be lifted and adjusted in height so as to adjust the light path to focus on the sample to be measured.
5. The in situ spectroscopy cell of claim 1, wherein: the lead of the electric probe, the temperature control element and the lead of the temperature measuring element are all led out from the electric wire temperature control lead port at the bottom of the sample temperature control platform.
6. The in situ spectroscopy cell of claim 1, wherein: and the gas inlet and outlet of the in-situ spectral analysis cell are provided with flow guide structures in conical distribution.
7. An in-situ infrared spectrum gas-sensitive testing device is characterized in that: comprising the in-situ spectral analysis cell of claim 1, an infrared spectrometer, and a diffuse reflection accessory. And placing the sample to be detected in an in-situ spectral analysis cell, and placing a diffuse reflection accessory provided with the in-situ infrared spectral analysis cell in an infrared spectrometer. The gas entering the cavity of the in-situ spectral analysis cell sweeps the surface of the sample, the infrared spectrum in the gas-solid reaction process is acquired in situ, and the electrical characteristics of the gas-sensitive sensor are detected by an electrical probe.
8. The in situ infrared spectroscopy gas sensitive test apparatus of claim 7, wherein: the gas mass flow controller integrated gas distribution instrument, the gas chromatograph-mass spectrometer, the digital source meter and the like are also included. And a gas mass flow controller integrated gas distribution instrument is arranged on a gas inlet pipeline of the in-situ spectral analysis cell, so that the content and the proportion of introduced gas components are accurately controlled. The gas outlet pipeline of the in-situ spectral analysis cell is connected with a gas chromatograph-mass spectrometer and outputs data of gas type and concentration; the digital source meter outputs the test data of the gas sensor to be tested.
9. An in-situ micro-Raman spectrum gas-sensitive testing device is characterized in that: comprising the in situ spectroscopic cell of claim 1, an optical slide, a micro-raman spectrometer. And placing the sample to be detected in an in-situ spectral analysis cell, fixing the in-situ spectral analysis cell on an optical sliding table, and placing the in-situ spectral analysis cell below a microscope of the micro-Raman spectrometer. Gas entering the cavity of the in-situ spectral analysis pool sweeps the surface of the sample, the Raman spectrum in the gas-solid reaction process is acquired in situ, and the electrical characteristics of the gas sensor are detected through an electrical probe.
10. The in situ micro-raman spectroscopy gas sensitive test device of claim 9, wherein: the gas mass flow controller integrated gas distribution instrument, the gas chromatograph-mass spectrometer, the digital source meter and the like are also included. And a gas mass flow controller integrated gas distribution instrument is arranged on a gas inlet pipeline of the in-situ spectral analysis cell, so that the content and the proportion of introduced gas components are accurately controlled. The gas outlet pipeline of the in-situ spectral analysis cell is connected with a gas chromatograph-mass spectrometer and outputs data of gas type and concentration; the digital source meter outputs the test data of the gas sensor to be tested.
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| CN114414044A (en) * | 2022-01-20 | 2022-04-29 | 河北建筑工程学院 | Device for testing gas-sensitive characteristic or photosensitive characteristic of material and using method thereof |
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