CN113933357A - Application of polytetrafluoroethylene film in gas sensor, metal pipe cap for gas sensor and nitrogen dioxide sensor - Google Patents
Application of polytetrafluoroethylene film in gas sensor, metal pipe cap for gas sensor and nitrogen dioxide sensor Download PDFInfo
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- CN113933357A CN113933357A CN202111370954.8A CN202111370954A CN113933357A CN 113933357 A CN113933357 A CN 113933357A CN 202111370954 A CN202111370954 A CN 202111370954A CN 113933357 A CN113933357 A CN 113933357A
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Images
Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
Abstract
The invention provides an application of a polytetrafluoroethylene film in a gas sensor, a metal pipe cap for the gas sensor and a nitrogen dioxide sensor, and relates to the technical field of gas sensors. According to the invention, the polytetrafluoroethylene film is arranged on the traditional gas nitrogen sensor for the first time, and the metal net cover is used as the supporting part of the polytetrafluoroethylene film, so that the polytetrafluoroethylene film with poor plasticity can be well packaged on the surface of the metal pipe cap of the gas sensor, the gas sensor can prevent water vapor from contacting with the gas sensitive material layer, and the humidity resistance and stability of the gas sensor sensitive to humidity are obviously improved. The nitrogen dioxide sensor provided by the invention takes flower-shaped indium oxide as a gas sensitive material layer, and the nitrogen dioxide sensor covered with the polytetrafluoroethylene film has excellent humidity resistance and stability under the relative humidity of 20-90%, so that a new idea is provided for improving the humidity resistance of a semiconductor metal oxide sensor sensitive to humidity.
Description
Technical Field
The invention relates to the technical field of gas sensors, in particular to application of a polytetrafluoroethylene film in a gas sensor, a metal pipe cap for the gas sensor and a nitrogen dioxide sensor.
Background
Indium oxide is a semiconductor functional material, and is widely used as a material of a sensor element due to its advantages of large forbidden bandwidth, small resistivity, good conductivity, strong thermal stability, easy micro-morphology construction and the like, and is particularly used as a gas-sensitive material layer of a sensor and commonly used for detecting toxic and harmful gases in the environment. However, the existing nitrogen dioxide sensor using indium oxide semiconductor material as gas sensitive sensing material is particularly obviously affected by environmental humidity in the detection process, and has poor stability.
Disclosure of Invention
In view of the above, the present invention aims to provide an application of a polytetrafluoroethylene film in a gas sensor, a metal cap for a gas sensor, and a nitrogen dioxide sensor. The nitrogen dioxide sensor packaged with the polytetrafluoroethylene film provided by the invention has excellent humidity resistance and stability under the relative humidity of 20-90%.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides an application of a polytetrafluoroethylene membrane in a gas sensor.
Preferably, the gas sensor comprises a nitrogen dioxide sensor.
The invention provides a metal pipe cap for a gas sensor, which comprises a metal retainer ring 21, a metal mesh enclosure 22 and a polytetrafluoroethylene film 23 positioned on the outer wall of the metal mesh enclosure; the metal retainer ring 21 fixes the edge of the metal mesh enclosure 22.
Preferably, the thickness of the polytetrafluoroethylene membrane 23 is 20 to 60 μm.
The invention provides a nitrogen dioxide sensor, which comprises a metal pipe cap and a sensing base, wherein the metal pipe cap is a metal pipe cap 2 for the gas sensor in the technical scheme, and the sensing base 1 is used for fixing the edge of the metal pipe cap 2;
the sensing pedestal 1 comprises a sensing body 11, wherein the sensing body 11 comprises an insulating tube 112, a first annular noble metal electrode 1131 and a second annular noble metal electrode 1132 which are encircled on the outer surface of the insulating tube 112, a gas sensing material layer 111 which covers the insulating tube 112, the first annular noble metal electrode 1131 and the second annular noble metal electrode 1132, and an alloy heating coil 114 which penetrates through the inner cavity of the insulating tube 112;
the material of the gas-sensitive material layer 111 is flower-shaped indium oxide.
Preferably, the thickness of the gas sensitive material layer 111 is 0.3-1 mm.
Preferably, the first annular noble metal electrode 1131 and the second annular noble metal electrode 1132 are connected with a noble metal wire 14.
Preferably, the sensing base 1 further comprises a bakelite tube seat 12 electrically connected with the sensing main body 11 and six metal pins 13 penetrating through the bakelite tube seat 12;
two of the six metal pins 13 are electrically connected to two ends of the alloy heating coil 114, the other two metal pins are electrically connected to the first annular noble metal electrode 1131, and the remaining two metal pins are electrically connected to the second annular noble metal electrode 1132.
Preferably, the preparation method of flower-like indium oxide comprises the following steps:
mixing water-soluble indium salt, a precipitator, a surfactant and water, and carrying out hydrothermal reaction to obtain a precursor;
and calcining the precursor to obtain flower-shaped indium oxide.
Preferably, the surfactant is an organic acid salt surfactant;
the mol ratio of the water-soluble indium salt to the precipitating agent to the surfactant is 1: 6-10: 2-4;
the temperature of the hydrothermal reaction is 100-140 ℃, and the time is 8-12 h;
the calcining temperature is 300-500 ℃, and the time is 2-3 h.
The invention provides an application of a polytetrafluoroethylene membrane in a gas sensor. According to the invention, the polytetrafluoroethylene film is covered on the outer surface of the metal pipe cap of the traditional gas sensor, and the gas sensor has excellent humidity resistance and stability under the relative humidity of 20-90%. The polytetrafluoroethylene film is used for the component of the gas sensor for the first time, and a new idea is provided for improving the humidity resistance of the semiconductor metal oxide sensor sensitive to humidity.
The invention provides a metal pipe cap for a gas sensor, which comprises a metal retainer ring 21, a metal mesh enclosure 22 and a polytetrafluoroethylene film 23 positioned on the outer wall of the metal mesh enclosure; the metal retainer ring 21 fixes the edge of the metal mesh enclosure 22. According to the invention, the polytetrafluoroethylene film is arranged on the traditional gas nitrogen sensor, and the metal net cover is used as a supporting part of the polytetrafluoroethylene film, so that the polytetrafluoroethylene film with poor plasticity can be well packaged on the surface of the metal pipe cap of the gas sensor, the gas sensor can prevent water vapor from contacting with the gas sensitive material layer, and the humidity resistance and stability of the gas sensor sensitive to humidity are obviously improved.
The invention provides a nitrogen dioxide sensor, which comprises a metal pipe cap and a sensing base, wherein the metal pipe cap is a metal pipe cap 2 for the gas sensor in the technical scheme, and the sensing base 1 is used for fixing the edge of the metal pipe cap 2; the sensing base 1 comprises a sensing body 11, wherein the sensing body 11 comprises an insulating tube 112, a first annular noble metal electrode 1131 and a second annular noble metal electrode 1132 which are encircled on the outer surface of the insulating tube, a gas sensing material layer 111 which covers the insulating tube 112, the first annular noble metal electrode 1131 and the second annular noble metal electrode 1132, and an alloy heating coil 114 which penetrates through the inner cavity of the insulating tube 112; the material of the gas-sensitive material layer 111 is flower-shaped indium oxide. The poor stability of the nitrogen dioxide sensors disclosed in the prior art is mainly due to the preferential adsorption of water molecules on O due to the high humidity2-On the adsorption sites, the amount of adsorbed oxygen is reduced and adsorbed species are changed, so that excessive water molecules are adsorbed on the surface of the material to cause poisoning, and the resistance and the sensor response are obviously reduced. The invention takes flower-shaped indium oxide as a gas-sensitive material layer, and when the sensor material is exposed to NO2When is NO2Adsorption to the surface of a semiconductor material to form NO2-And electrons are abstracted from the conduction band, so that the resistance of the material can be increased, and the sensing performance of the nitrogen dioxide gas is realized. Moreover, the traditional nitrogen dioxide sensor is provided with the polytetrafluoroethylene membrane, and the metal mesh cover is used as the supporting part of the polytetrafluoroethylene membrane, so that the nitrogen dioxide sensor canCan encapsulate the metal pipe cap surface at gas sensor with the poor polytetrafluoroethylene membrane of plasticity well for nitrogen dioxide sensor can block water vapour and gas sensitive material layer contact, is showing the moisture resistance ability and the stability that have improved nitrogen dioxide sensor.
Drawings
Fig. 1 is a schematic view of a metal cap for a gas sensor, in which 21 is a metal collar, 22 is a metal mesh, and 23 is a teflon film;
FIG. 2 is a schematic structural view of a nitrogen dioxide sensor;
FIG. 3 is a schematic structural view of a nitrogen dioxide sensor;
in fig. 2 to 3, 1 is a sensing substrate, 11 is a sensing body, 111 is a gas sensitive material layer, 112 is an insulating tube, 1131 is a first annular noble metal electrode, 1132 is a second annular noble metal electrode, 114 is an alloy heating coil, 12 is a bakelite tube base, 13 is a metal pin, 131 is a first metal pin, 132 is a second metal pin, 133 is a third metal pin, 134 is a fourth metal pin, 135 is a fifth metal pin, 136 is a sixth metal pin, and 14 is a noble metal wire; 2, a metal pipe cap for the gas sensor, 21 a metal retainer ring, 22 a metal net cover and 23 a polytetrafluoroethylene film;
FIG. 4 is an SEM image of flower-like indium oxide prepared in example 1;
FIG. 5 is an SEM image of a polytetrafluoroethylene membrane;
FIG. 6 is a graph of the contact angle of a polytetrafluoroethylene membrane;
FIG. 7 shows the results of gas sensitivity performance tests of the nitrogen dioxide sensors prepared in example 1 and comparative example 1 at different temperatures for nitrogen dioxide gas;
FIG. 8 shows the results of the gas sensitivity performance test of the nitrogen dioxide sensors prepared in example 1 and comparative example 1 on nitrogen dioxide gas at different humidities;
FIG. 9 shows the results of gas sensitivity tests of the nitrogen dioxide sensors prepared in example 1 and comparative example 1 on nitrogen dioxide gas obtained at different concentrations;
figure 10 is a graph showing the results of a nitrogen dioxide gas stability test performed on the nitrogen dioxide sensor prepared in example 1;
fig. 11 shows the results of selective detection of different gases by the nitrogen dioxide sensors prepared in example 1 and comparative example 1.
Detailed Description
The invention provides an application of a polytetrafluoroethylene membrane in a gas sensor. In the present invention, the gas sensor preferably includes a nitrogen dioxide sensor.
The metal cap for a gas sensor will be described in detail with reference to fig. 1.
The invention provides a metal pipe cap for a gas sensor, which comprises a metal retainer ring 21, a metal mesh enclosure 22 and a polytetrafluoroethylene film 23 positioned on the outer wall of the metal mesh enclosure; the metal retainer ring 21 fixes the edge of the metal mesh enclosure 22. The material of the metal collar 21 is not particularly limited in the present invention, and a simple metal or a metal alloy known to those skilled in the art may be used, specifically, stainless steel, iron, or an aluminum alloy. The material of the metal mesh enclosure 22 is not particularly limited in the present invention, and may be a simple metal or a metal alloy, such as stainless steel, iron, or an aluminum alloy, which are well known to those skilled in the art. In the invention, the thickness of the polytetrafluoroethylene membrane 23 is preferably 20-60 μm, and more preferably 20-40 μm; the source of the polytetrafluoroethylene membrane is not particularly limited in the invention, and a commercially available polytetrafluoroethylene membrane well known to those skilled in the art can be used; in an embodiment of the present invention, the polytetrafluoroethylene membrane is preferably purchased from mebor biofilm technology, inc.
The nitrogen dioxide sensor will be described in detail with reference to fig. 2 to 3.
The invention provides a nitrogen dioxide sensor, which comprises a metal pipe cap and a sensing base, wherein the metal pipe cap is a metal pipe cap 2 for the gas sensor in the technical scheme; the sensing base 1 fixes the edge of the metal pipe cap 2;
the sensing pedestal 1 comprises a sensing body 11, wherein the sensing body 11 comprises an insulating tube 112, a first annular noble metal electrode 1131 and a second annular noble metal electrode 1132 which are encircled on the outer surface of the insulating tube 112, a gas sensing material layer 111 which covers the insulating tube 112, the first annular noble metal electrode 1131 and the second annular noble metal electrode 1132, and an alloy heating coil 114 which penetrates through the inner cavity of the insulating tube 112;
the material of the gas-sensitive material layer 111 is flower-shaped indium oxide.
In the present invention, the sensing body 11 includes an insulating tube 112. In the present invention, the material of the insulating tube 112 preferably includes ceramic, silicon oxide or glass; the inner diameter of the insulating tube is preferably 0.5-1.5 mm, and more preferably 0.8-1 mm; the outer diameter of the insulating tube is preferably 1-1.5 mm, and more preferably 1.2-1.4 mm; the length of the insulating tube is preferably 2.5-4.5 mm, and more preferably 3-4 mm.
In the present invention, the sensing body 11 includes a first annular noble metal electrode 1131 and a second annular noble metal electrode 1132 surrounding the outer surface of the insulating tube 112. In the present invention, the widths of the first annular noble metal electrode 1131 and the second annular noble metal electrode 1132 are independently preferably 0.4 to 0.7mm, and more preferably 0.4 to 0.6 mm; the distance between the first annular noble metal electrode 1131 and the second annular noble metal electrode 1132 is preferably 1.5-2 mm, and more preferably 1.7-1.9 mm; the material of the first annular noble metal electrode 1131 and the second annular noble metal electrode 1132 independently preferably includes gold, palladium or platinum, and more preferably gold.
In the present invention, the first annular noble metal electrode 1131 and the second annular noble metal electrode 1132 are preferably connected with a noble metal wire 14; the material of the noble metal wire 14 preferably includes platinum, palladium or gold; the length of the noble metal lead 14 is preferably 4-7 mm, and more preferably 4-6 mm.
In the present invention, the sensing body 11 includes the gas sensitive material layer 111 covering the insulating tube 112, the first annular noble metal electrode 1131, and the second annular noble metal electrode 1132. In the invention, the thickness of the gas sensitive material layer is preferably 0.3-1 mm, and more preferably 0.4-0.7 mm.
In the present invention, the method for preparing flower-like indium oxide preferably includes the steps of:
mixing water-soluble indium salt, a precipitator, a surfactant and water, and carrying out hydrothermal reaction to obtain a precursor;
and calcining the precursor to obtain flower-shaped indium oxide.
In the present invention, all the raw material components are commercially available products well known to those skilled in the art unless otherwise specified.
According to the invention, water-soluble indium salt, a precipitator, a surfactant and water are mixed for hydrothermal reaction to obtain a precursor.
In the present invention, the water-soluble indium salt preferably comprises indium chloride (InCl)3·4H2O) and/or indium nitrate (In (NO)3)3·4H2O). In the present invention, the precipitant preferably includes urea, hexamethylenetetramine (C)6H12N4) And butanediamine (C)4H12N2) One or more of them. In the present invention, the surfactant preferably comprises sodium lauryl sulfate and/or trisodium citrate. In the present invention, the molar ratio of the water-soluble indium salt, the precipitant, and the surfactant is preferably 1: 6-10: 2-4, more preferably 1: 8-10: 2.5 to 3.5, and more preferably 1: 10: 3. in the present invention, the ratio of the amount of the substance of the water-soluble indium salt to the volume of water is preferably 1 mmol: 40-60 mL, more preferably 1 mmol: 45-55 mL, more preferably 1 mmol: 50 mL. In the present invention, the mixing manner is preferably stirring mixing, and the stirring mixing speed is not particularly limited, and the raw materials can be uniformly mixed; the temperature of the mixing is preferably room temperature.
In the invention, the temperature of the hydrothermal reaction is preferably 100-140 ℃, more preferably 110-130 ℃, and further preferably 120 ℃; the time of the hydrothermal reaction is preferably 8-12 h, more preferably 9-11 h, and further preferably 10 h; the hydrothermal reaction is preferably carried out in a reaction kettle. In the invention, the reactions in the hydrothermal reaction process are shown as formulas (1) to (2), the effect of the precipitant is to adjust the acid-base balance of the solution, keep the solution neutral or weakly alkaline and remove H by reaction+The forward reaction of the formula (1) is facilitated:
In3++3H2O→In(OH)3+3H+formula (1)
In(OH)3→InOOH+H2O formula (2).
After the hydrothermal reaction, the present invention preferably further comprises a post-treatment, which comprises: and cooling the reaction liquid obtained by the hydrothermal reaction to room temperature, carrying out first solid-liquid separation, and carrying out water washing, alcohol washing, second solid-liquid separation and drying on the obtained solid product in sequence to obtain a precursor. The cooling method of the present invention is not particularly limited, and a cooling method known to those skilled in the art may be used, specifically, natural cooling. The method for the first solid-liquid separation and the second solid-liquid separation is not particularly limited, and a solid-liquid separation method known to those skilled in the art, such as centrifugal separation, may be adopted; the speed of the centrifugal separation is preferably 6000-9500 rpm, and more preferably 7000-8000 rpm; the time for centrifugal separation is preferably 5-15 min, and more preferably 10 min. In the present invention, the number of washing with water is preferably 2 to 4, and more preferably 3. In the present invention, the alcohol washing alcohol preferably includes ethanol or methanol; the number of times of alcohol washing is preferably 2 to 4 times, and more preferably 3 times. In the invention, the drying temperature is preferably 60-80 ℃, more preferably 70 ℃, and the drying time is preferably 6-12 h, more preferably 8-10 h.
After the precursor is obtained, the precursor is calcined to obtain the flower-shaped indium oxide.
In the invention, the calcining temperature is 300-500 ℃, more preferably 350-450 ℃, and further preferably 400 ℃; the heating rate from the room temperature to the calcining temperature is preferably 2-10 ℃/min, and more preferably 5 ℃/min; starting timing by raising the temperature to the calcining temperature, wherein the calcining time is preferably 2-3 h, more preferably 2.2-2.8 h, and further preferably 2.5 h; the atmosphere for the calcination is preferably air. In the present invention, the reaction occurring during the calcination is represented by the formula (3):
2InOOH→In2O3+H2o formula (3).
After the calcination, the invention preferably further comprises cooling the reaction product obtained by the calcination to room temperature to obtain flower-like indium oxide. The cooling method of the present invention is not particularly limited, and a cooling method known to those skilled in the art may be used, specifically, natural cooling.
In the present invention, the sensing body 11 includes an alloy heating coil 114 passing through the lumen of the insulating tube 112. In the present invention, the alloy heating coil preferably includes a nickel cadmium (NiCr) heating coil or an iron nickel aluminum (alg) heating coil; the number of turns of the alloy heating coil is preferably 40-50 turns, and more preferably 40-45 turns.
In the present invention, the sensing base 1 preferably further includes a bakelite tube seat 12 electrically connected to the sensing body 11 and six metal pins 13 penetrating through the bakelite tube seat 12; two of the six metal pins are electrically connected to two ends of the alloy heating coil 114, the other two metal pins are electrically connected to the first annular noble metal electrode 1131, and the remaining two metal pins are electrically connected to the second annular noble metal electrode 1132. In the present invention, the electrical connection is preferably made by a noble metal wire 14, which is preferably welded by electric welding; the material of the noble metal wire preferably comprises platinum, palladium or gold. In the embodiment of the present invention, the 6 metal pins 13 are numbered as a first metal pin 131, a second metal pin 132, a third metal pin 133, a fourth metal pin 134, a fifth metal pin 135 and a sixth metal pin 136; in the embodiment of the present invention, the first and second metal pins 131 and 132 are preferably electrically connected to both ends of the alloy heating coil 114; the third metal pin 133 and the fourth metal pin 134 are electrically connected to the first annular noble metal electrode 1131; the fifth and sixth metal pins 135 and 136 are preferably electrically connected to the second annular noble metal electrode 1132.
The invention provides a preparation method of the nitrogen dioxide sensor in the technical scheme, which preferably comprises the following steps:
mixing flower-shaped indium oxide with a diluent, coating the obtained slurry on the outer surface of an insulating tube, and then aging to obtain a sensing main body; a first annular noble metal electrode 1131 and a second annular noble metal electrode 1132 are encircled on the outer surface of the insulating tube 112, and an alloy heating coil 114 penetrates through the inner cavity of the insulating tube 112;
and sealing the sensing main body and the gas sensor in the technical scheme by using a metal pipe cap to obtain the nitrogen dioxide sensor.
The flower-shaped indium oxide and the diluent are mixed, and the obtained slurry is coated on the outer surface of the insulating tube and then aged to obtain the sensing main body. In the invention, the diluent preferably comprises alcohol and/or water, and the alcohol preferably comprises one or more of ethanol, methanol, propanol and isopropanol; the water is preferably distilled and/or deionized water. In the present invention, the mixing method is preferably grinding, and the grinding method is not particularly limited, and flower-like indium oxide may be uniformly dispersed in a diluent. In the invention, the solid content of the slurry is preferably 0.02 to 0.04 wt%, more preferably 0.0211 to 0.0338 wt%, and even more preferably 0.0253 to 0.03 wt%. The coating method of the present invention is not particularly limited, and a coating method known to those skilled in the art may be used. After the coating, the invention preferably further comprises drying the gas-sensitive material obtained by the coating, wherein the drying mode is preferably airing. In the invention, the aging temperature is preferably 100-300 ℃, more preferably 150-250 ℃, and further preferably 200 ℃; the aging time is preferably 12-36 h, more preferably 15-30 h, and further preferably 20-25 h; the ageing is preferably carried out in a muffle furnace; the aging under the above conditions can improve the stability and the service life of the nitrogen dioxide sensor.
After the sensing main body is obtained, the sensing main body and the gas sensor in the technical scheme are sealed by the metal pipe cap to obtain the nitrogen dioxide sensor. In the invention, the blocking is preferably performed by using a blocking agent, and the blocking agent preferably comprises one or more of silicone rubber, epoxy resin glue and polyurethane glue.
After the sealing, the invention preferably further comprises electrically connecting the sensing body with the sensing base to obtain the nitrogen dioxide sensor. In the present invention, the electrical connection is preferably made by welding two of the six metal pins to both ends of the alloy heating coil, the other two to the first annular noble metal electrode 1131, and the remaining two to the second annular noble metal electrode 1132, by electric welding.
According to the invention, a test board is preferably inserted into the nitrogen dioxide sensor and then the nitrogen dioxide gas sensitivity test is carried out, the test board is inserted into a circuit card slot of a resistance type sensor tester, a load resistance card is selected to be inserted into a corresponding circuit card slot, and then the gas sensitivity performance of the nitrogen dioxide sensor is tested; the resistance type sensor tester is preferably a WS-30A resistance type sensor tester designed and produced by Weisheng electronics Limited company in Henan Zheng of China.
In the present invention, the operation principle of the nitrogen dioxide sensor is preferably as follows: by means of NO2Detection of NO by the change in physical properties such as conductivity occurring when the surface of flower-like indium oxide is brought into contact with the surface2A gas. When the sensor device is heated to a steady state, NO2And the material surface adsorbs the ions, and electrons are obtained from a conduction band of the indium oxide to form negative ion adsorption. Since flower-like indium oxide is a typical n-type semiconductor material, when oxidizing gas NO2The adsorption of carriers to the n-type semiconductor decreases, thereby increasing the resistance. Defining the response value as Rg/Ra，RgIs the resistance of the sensor in nitrogen dioxide gas, RaIs the resistance of the sensor in air.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. 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.
Example 1
1mmol of indium chloride (InCl)3·4H2O), 10mmol of urea and 2mmol of Sodium Dodecyl Sulfate (SDS) are placed in 60mL of distilled water and mixed for 1h at room temperature, and then the mixture is turnedMoving the mixture into a 100mL reaction kettle, carrying out hydrothermal reaction for 10h at 120 ℃, cooling to room temperature, carrying out centrifugal separation, washing the obtained solid product with deionized water for 3 times, washing with absolute ethyl alcohol for 3 times, carrying out centrifugal separation for 10min at 9000rpm, and drying the solid product in a vacuum drying oven at 60 ℃ for 6h to obtain the precursor. And (3) placing the precursor in a tube furnace, heating to 400 ℃ at a heating rate of 5 ℃/min, then carrying out heat preservation and calcination for 2h in an air atmosphere, and naturally cooling to room temperature to obtain flower-shaped indium oxide.
Cutting a polytetrafluoroethylene film 23 (purchased from Membori biomembrane technology Co., Ltd., thickness of 20 μm), closely covering the polytetrafluoroethylene film on the outer wall of the metal mesh enclosure 22, and fixing the edge of the metal mesh enclosure 22 by using a metal retainer ring 21 to obtain a metal pipe cap 2 for the gas sensor;
uniformly grinding the flower-shaped indium oxide and 0.15mL of ethanol, coating the obtained slurry on the outer surface of a ceramic tube 111 (length is multiplied by the diameter, and the diameter is multiplied by 3mm and the thickness is multiplied by l mm), standing and airing, putting the obtained ceramic tube into a muffle furnace, and aging at 300 ℃ to obtain a sensing main body 11, wherein the thickness of the flower-shaped indium oxide layer is 0.5 mm; the outer surface of the insulating tube 11 is surrounded by a first annular gold electrode 1131 and a second annular gold electrode 1132, and a NiCr heating coil 114 penetrating through the inner cavity of the insulating tube 112; welding the first metal pin 131 and the second metal pin 132 to both ends of the NiCr heating coil 114 by a platinum wire, and welding the third metal pin 133 and the fourth metal pin 134 to the first annular gold electrode 1131 by a platinum wire; welding the fifth metal pin 135 and the sixth metal pin 136 to the annular gold electrode 1132 by a platinum wire; and (3) sealing the metal pipe cap 2 and the bakelite pipe seat 12 for the gas sensor by using a silicon rubber end-capping agent, and airing to obtain the nitrogen dioxide sensor (marked as a film).
Comparative example 1
A nitrogen dioxide sensor was prepared as in example 1, except that the metal mesh enclosure was not covered with a teflon film on the outer wall, to obtain a nitrogen dioxide sensor (noted as no film).
FIG. 4 is an SEM image of flower-like indium oxide prepared in example 1. As can be seen from FIG. 4, the indium oxide prepared by the present invention has a flower-like structure and a size of 5 to 7 μm.
Fig. 5 is an SEM image of the polytetrafluoroethylene membrane. As can be seen from fig. 5, the PTFE film surface exhibits regular lines and surface wrinkles.
Fig. 6 is a contact angle graph of a polytetrafluoroethylene membrane. As can be seen from fig. 6, the PTFE film has a contact angle with water of 144 °, and its surface has hydrophobicity.
Test example 1
A test board is respectively inserted into the nitrogen dioxide sensors prepared in the example 1 and the comparative example 1, the test board is inserted into a circuit card slot of a WS-30A type resistance sensor tester designed and produced by weisheng electronics limited company in hennan zheng of china, and a load resistance card is inserted into the corresponding circuit card slot to test the gas sensitivity of the nitrogen dioxide sensor. Defining the response value as Rg/Ra，RgIs the resistance of the sensor in nitrogen dioxide gas, RaThe resistance of the sensor in the air is obtained, wherein the initial voltage of the test instrument is adjusted to 4.3-4.7V by the load resistance card, and the test result is shown as 5-8.
Fig. 7 shows the gas-sensitive performance test results of the nitrogen dioxide sensors prepared in example 1 and comparative example 1 for nitrogen dioxide gas at different temperatures, wherein the test temperature range is 50-200 ℃, the relative humidity is 80%, and the nitrogen dioxide concentration is 1 ppm. As can be seen from fig. 7, the optimum operating temperatures of the nitrogen dioxide sensors prepared in example 1 and comparative example 1 are the same, and are both 75 ℃; the response of the nitrogen dioxide sensor prepared in example 1 to 1ppm nitrogen dioxide is about 6 times that of the nitrogen dioxide sensor prepared in comparative example 1 at a relative humidity of 80%.
Fig. 8 shows the results of the gas sensitivity test of the nitrogen dioxide sensors prepared in example 1 and comparative example 1 to nitrogen dioxide gas under different humidity conditions, wherein the test temperature is 75 ℃, the relative humidity is 20-90%, and the nitrogen dioxide concentration is 1 ppm. As can be seen from fig. 8, the response value of the nitrogen dioxide sensor prepared in example 1 is hardly affected by humidity as humidity increases, whereas the nitrogen dioxide sensor prepared in comparative example 1 is greatly affected by humidity within a range of 30 to 90% relative humidity.
Fig. 9 shows the results of the gas-sensitive performance test of the nitrogen dioxide sensors prepared in example 1 and comparative example 1 on nitrogen dioxide gas with different concentrations, wherein the test temperature is 75 ℃, the relative humidity is 80%, and the nitrogen dioxide concentration is 0.5-5 ppm. As can be seen from fig. 9, the response value of the nitrogen dioxide sensor prepared in example 1 increases with the increase of the gas concentration, while the response value of the nitrogen dioxide sensor prepared in comparative example 1 does not change much, which indicates that the sensitivity of the nitrogen dioxide sensor prepared in comparative example 1 is severely reduced by the influence of humidity, while the nitrogen dioxide sensor prepared in example 1 is not influenced by humidity and shows better sensitivity with the increase of the concentration.
Fig. 10 shows the results of the stability test of the nitrogen dioxide sensor prepared in example 1 on nitrogen dioxide gas, the test temperature being 75 deg.c, the relative humidity being 80%, and the nitrogen dioxide concentration being 1 ppm. As can be seen from fig. 10, the response value of the nitrogen dioxide sensor prepared by the invention to 1ppm of nitrogen dioxide is maintained at about 180 days, and is not obviously reduced; the nitrogen dioxide sensor prepared by the method has good stability.
Figure 11 is a graph of the results of the nitrogen dioxide sensors prepared in example 1 and comparative example 1 tested for 1ppm nitrogen dioxide, 50ppm ethylamine, 50ppm ammonia, 50ppm ethanol, 100ppm formaldehyde, 50ppm methanol, 500ppm acetone, and 50ppm isobutanol at 75 c relative humidity of 20%. As can be seen from FIG. 11, the sensor responded only to nitrogen dioxide gas, but not to 50ppm ethylamine, 50ppm ammonia, 50ppm ethanol, 100ppm formaldehyde, 500ppm acetone, and 50ppm isobutanol. The nitrogen dioxide sensor prepared by the invention can realize selective detection of nitrogen dioxide.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (10)
1. Use of a polytetrafluoroethylene membrane in a gas sensor.
2. Use according to claim 1, wherein the gas sensor comprises a nitrogen dioxide sensor.
3. A metal pipe cap for a gas sensor comprises a metal retainer ring (21), a metal mesh enclosure (22) and a polytetrafluoroethylene film (23) positioned on the outer wall of the metal mesh enclosure; the metal retainer ring (21) is used for fixing the edge of the metal mesh enclosure (22).
4. The metal cap for a gas sensor according to claim 3, wherein the polytetrafluoroethylene film (23) has a thickness of 20 to 60 μm.
5. A nitrogen dioxide sensor, comprising a metal pipe cap and a sensing base, wherein the metal pipe cap is the metal pipe cap (2) for the gas sensor of any one of claims 3 to 4, and the sensing base (1) is fixed on the edge of the metal pipe cap (2);
the sensing base (1) comprises a sensing main body (11), wherein the sensing main body (11) comprises an insulating tube (112), a first annular noble metal electrode (1131) and a second annular noble metal electrode (1132) which surround the outer surface of the insulating tube (112), a gas sensing material layer (111) which covers the insulating tube (112), the first annular noble metal electrode (1131) and the second annular noble metal electrode (1132), and an alloy heating coil (114) which penetrates through the inner cavity of the insulating tube (112);
the material of the gas-sensitive material layer (111) is flower-shaped indium oxide.
6. The nitrogen dioxide sensor according to claim 5, wherein the gas-sensitive material layer (111) has a thickness of 0.3 to 1 mm.
7. The nitrogen dioxide sensor of claim 5, wherein the first annular noble metal electrode (1131) and the second annular noble metal electrode (1132) are connected by a noble metal lead (14).
8. The nitrogen dioxide sensor according to claim 5, wherein the sensing base (1) further comprises a bakelite stem (12) electrically connected with the sensing body (11) and six metal pins (13) penetrating the bakelite stem (12);
two metal pins in the six metal pins (13) are electrically connected with two ends of the alloy heating coil (114), the other two metal pins are electrically connected with the first annular noble metal electrode (1131), and the rest two metal pins are electrically connected with the second annular noble metal electrode (1132).
9. The nitrogen dioxide sensor according to claim 5 or 6, wherein the preparation method of flower-like indium oxide comprises the following steps:
mixing water-soluble indium salt, a precipitator, a surfactant and water, and carrying out hydrothermal reaction to obtain a precursor;
and calcining the precursor to obtain flower-shaped indium oxide.
10. The nitrogen dioxide sensor of claim 9, wherein the surfactant is an organic acid salt surfactant;
the mol ratio of the water-soluble indium salt to the precipitating agent to the surfactant is 1: 6-10: 2-4;
the temperature of the hydrothermal reaction is 100-140 ℃, and the time is 8-12 h;
the calcining temperature is 300-500 ℃, and the time is 2-3 h.
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