CN110646474A - Based on WO3Wireless passive H2Gas sensor and preparation method thereof - Google Patents
Based on WO3Wireless passive H2Gas sensor and preparation method thereof Download PDFInfo
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- CN110646474A CN110646474A CN201911027841.0A CN201911027841A CN110646474A CN 110646474 A CN110646474 A CN 110646474A CN 201911027841 A CN201911027841 A CN 201911027841A CN 110646474 A CN110646474 A CN 110646474A
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- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
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Abstract
The invention discloses a method based on WO3Wireless passive H2A gas sensor and a method for manufacturing the same, the gas sensor comprising: the outer end of the inductance coil is connected with one end of the composite gas-sensitive resistor through silver paste filled in a through hole of the ceramic substrate, and the inner end of the inductance coil is connected with the other end of the composite gas-sensitive resistor to form an LR sensitive loop; the ceramic substrate is prepared by taking an alumina green ceramic tape as a material and adopting an HTCC process, the inductance coil is prepared by taking Ag as slurry and adopting a screen printing process, and the composite gas-sensitive resistor is prepared by adopting Pt-WO3The composite material is prepared by a magnetron sputtering process. The gas sensor provided by the invention can accurately realize the H value of the gas to be measured under the low-temperature condition by analyzing the Q value changed along with the resistance by using a wireless non-contact measuring method2The detection is carried out by adopting mature silk-screen printing and magnetron sputteringThe preparation process has the advantages of simple and convenient processing, low cost and the like.
Description
Technical Field
The invention relates to the technical field of gas sensors, in particular to a gas sensor based on WO3Wireless passive H2A gas sensor and a method for manufacturing the same.
Background
As a renewable energy source, hydrogen is widely applied to various important fields, however, hydrogen is extremely flammable, leakage is easy to occur in the using process, explosion is easy to occur, and unpredictable results are caused, so that real-time detection of hydrogen is very important. The traditional hydrogen sensor mostly adopts an active wired test structure, the front end of the sensor needs to be connected with a power supply, the rear end of the sensor needs to be connected with a complex circuit structure, the traditional hydrogen sensor has the defects of complex structure, difficulty in design and the like, and the working temperature of the traditional hydrogen sensor is generally higher. Therefore, it is highly desirable to invent a new wireless passive H2The gas sensor is used for detecting hydrogen in different temperature environments.
Disclosure of Invention
In order to solve the technical problem, the invention provides a method based on WO3Wireless passive H2The gas sensor and the preparation method thereof can realize the detection of hydrogen in different temperature environments (room temperature-400 ℃).
In order to achieve the purpose, the invention adopts the technical scheme that:
based on WO3Wireless passive H2A gas sensor, comprising: the outer end of the inductance coil is connected with one end of the composite gas-sensitive resistor through silver paste filled in a through hole of the ceramic substrate, and the inner end of the inductance coil is connected with the other end of the composite gas-sensitive resistor to form an LR sensitive loop; the inductance coil is prepared by taking Ag as slurry and adopting a screen printing process, and the composite gas-sensitive resistor is prepared by adopting Pt-WO3The composite material is prepared by a magnetron sputtering process, Pt is used as a doped film, and WO can be improved3Film pair H2While reducing the operating temperature of the sensor.
Further, the inductance coil is in a rectangular spiral shape, and the outer end of the inductance coil extends to the through hole.
Further, the ceramic substrate is sintered by adopting a mature HTCC process.
Furthermore, the composite gas sensitive resistor is formed by connecting 3 resistors in series, so that the sensitivity of the gas sensor can be improved.
Furthermore, the gas sensor adopts a wireless non-contact test principle, and realizes the H value of the gas to be tested by analyzing the Q value changed along with the resistance2Non-contact testing of (2).
Based on WO3Wireless passive H2The preparation method of the gas sensor comprises the following steps:
s1 preparation of alumina ceramic substrate
S11, cutting the alumina green porcelain strips into a group of 50 x 50mm in size by using a cutting machine 23 green ceramic chips in total;
s12, punching a through hole with the inner diameter of 2mm at the same position of the 3 layers of green ceramic chips, namely the joint of the outer end of the inductance coil and the gas-sensitive resistor by utilizing a laser drilling technology;
s13, laminating 3 layers of green ceramic chip laminations into a compact whole;
s14, putting the raw ceramic chip group which is laminated into a whole into a muffle furnace for high-temperature sintering, so that the raw ceramic becomes mature ceramic, the performance of the ceramic chip is achieved, and the preparation of the sensor substrate is completed;
s2 preparation of inductance coil
S21, fixing the printing screen on a screen printing table, and placing the ceramic substrate cleaned by alcohol wiping below the printing screen to be aligned with the patterns of the induction coils on the printing screen;
s22, uniformly coating a certain amount of metal silver paste on the screen printing plate, and repeatedly and slowly moving the rubber scraper to print the inductance pattern on the ceramic substrate;
s23, after printing, placing the ceramic wafer in a mesh belt dryer at 150 ℃ and drying for 10 min;
s24, repeating the steps S21-S23, printing an inductor on the other surface of the ceramic substrate, extending the outer end of the inductor to the through hole, and filling silver paste in the through hole to realize the connection between the outer end of the inductor and the gas sensitive resistor, so as to form an LR sensitive loop:
s25, placing the printed ceramic substrate on a burning board, placing the ceramic substrate in a muffle furnace, heating and sintering at a heating rate of 10 ℃/min to 850 ℃, and keeping the temperature for 45min to volatilize organic impurities in the slurry;
s3 preparation of composite gas-sensitive resistor
S31, covering the inductance coil by using an insulating adhesive tape to avoid damage of the inductance coil in a sputtering process, and meanwhile, adding a layer of dust-free paper between the adhesive tape and the inductance coil to prevent silver paste from falling off when the adhesive tape is torn;
s32, respectively placing the ceramic substrate and the sputtering target tungsten (with the purity of 99.95%) on a sample base and a target source installation position in a sputtering chamber, starting a power supply, firstly pumping the vacuum degree of the sputtering chamber to be below 30Pa by using a mechanical pump, and then pumping the sputtering chamber to be vacuum degree lower than 4 x 10 by using a molecular pump-4And Pa, closing the vacuumizing valve, opening the air inlet valve, opening a power supply of the mass flow meter, adjusting the flow rate of gas to ensure that argon and oxygen are slowly introduced into the sputtering chamber at the flow rates of 30sccm and 10sccm respectively, adjusting the molecular pump baffle valve to ensure that the working pressure in the sputtering chamber is kept unchanged when the working pressure in the sputtering chamber is 2Pa, starting the sputtering power supply, setting the sputtering power to be 300W, and starting sputtering. When the thickness of the tungsten oxide film reaches 400nm, the power supply is turned off, the power supply knob is adjusted to 0, the gas flow is adjusted to off, the gas guide valve is closed, the sputtering is stopped, and WO3Finishing the preparation of the film;
s33, taking Pt as a sputtering target (with the purity of 99.95 percent) and Ar as a sputtering gas, adopting a direct current sputtering process under the conditions that the pressure is 0.5Pa and the sputtering power is 8W, and in WO3And sputtering a Pt film with the thickness of 10nm on the surface of the film, thus finishing the preparation of the gas sensor.
The invention has the following beneficial effects:
in gas-sensitive materials WO3The surface is doped with sputtered Pt, so that the reaction rate can be accelerated, the working temperature can be reduced, the gas-sensitive response can be improved, and the sensitivity of the sensor can be improved;
the invention adopts the screen printing and magnetron sputtering process, and has the advantages of simple and convenient manufacture, low cost, convenient batch production and the like;
the invention adopts a wireless non-contact measurement principle, analyzes the Q value of the sensor changing along with the gas concentration through the electromagnetic coupling of the sensor inductance and the reading antenna, realizes the hydrogen detection in a low-temperature environment, avoids the use of an electric lead and is convenient for detection and realization.
Drawings
FIG. 1 shows an embodiment of the present invention based on WO3Wireless passive H2A process flow diagram for preparing the gas sensor.
FIG. 2 is a diagram of an embodiment of the present invention based on WO3Wireless passive H2The structure of the gas sensor is a three-dimensional structure.
FIG. 3 is a diagram of an embodiment of the present invention based on WO3Wireless passive H2A cross-sectional view of a gas sensor.
FIG. 4 is a diagram of an embodiment of the present invention based on WO3Wireless passive H2Working principle diagram of the gas sensor.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
As shown in fig. 2 to 3, an embodiment of the present invention provides a WO-based system3Wireless passive H2The gas sensor adopts a wireless non-contact test principle and realizes the H value of the gas to be tested by analyzing the Q value which changes along with the resistance2Comprises: the sensor comprises a high-temperature-resistant ceramic substrate 1, an inductance coil 2 and a composite gas-sensitive resistor 3, wherein the inductance coil 2 and the composite gas-sensitive resistor are printed on the ceramic substrate 1, the outer end of the inductance coil is connected with one end of the composite gas-sensitive resistor through silver paste filled in a through hole 4 of the ceramic substrate, and the inner end of the inductance coil is connected with the other end of the composite gas-sensitive resistor to form an LR sensitive loop; the thickness of the ceramic substrate is 1mm, the ceramic substrate is formed by laminating and sintering three green ceramic chips, the inner diameter of the through hole is 2mm, and the inductance coil is in the shape ofThe rectangular spiral shape, the outer end extending to the through hole, Ag as slurry, and prepared by silk screen printing process, the composite gas sensitive resistor is Pt-WO3The thickness of the composite gas-sensitive resistor is 410nm, wherein WO3The thickness is 400nm, the thickness of Pt sputtered on the Pt is 10nm, and the Pt is prepared by a magnetron sputtering process.
As shown in figure 1, the embodiment of the invention also provides the WO based on the same3Wireless passive H2The preparation method of the gas sensor comprises the following steps:
s1 preparation of alumina ceramic substrate
S11, cutting the alumina green porcelain strips into a group of 50 x 50mm in size by using a cutting machine 23 green ceramic chips in total;
s12, punching a through hole with the inner diameter of 2mm at the same position of the 3 layers of green ceramic chips, namely the joint of the outer end of the inductance coil and the gas-sensitive resistor by utilizing a laser drilling technology;
s13, forming the 3-layer green ceramic sheets into a compact whole through the processes of lamination and lamination (the pressure is 21MPa, and the temperature is 70 ℃);
s14, putting the raw ceramic chip group laminated into a whole into a muffle furnace for high-temperature sintering (the peak temperature is 1550 ℃, and the heat preservation time is 40min), so that the raw ceramic chip becomes mature ceramic, the performance of the ceramic chip is achieved, and the preparation of the sensor substrate is completed;
s2 preparation of inductance coil
S21, fixing the printing screen on a screen printing table, and placing the ceramic substrate cleaned by alcohol wiping below the printing screen to be aligned with the patterns of the induction coils on the printing screen;
s22, uniformly coating a certain amount of metal silver paste on the screen printing plate, and repeatedly and slowly moving the rubber scraper to print the inductance pattern on the ceramic substrate;
s23, after printing, placing the ceramic wafer in a mesh belt dryer at 150 ℃ and drying for 10 min;
s24, repeating the steps S21-S23, printing an inductor on the other surface of the ceramic substrate, extending the outer end of the inductor to a through hole, and filling silver paste in the through hole to realize the connection between the outer end of the inductor and the gas sensitive resistor so as to form an LR sensitive loop;
s25, placing the printed ceramic substrate into a muffle furnace, heating up and sintering to 850 ℃ at a heating rate of 10 ℃/min, and keeping the temperature for 45min to volatilize organic impurities in the slurry;
s3 preparation of composite gas-sensitive resistor
The main process of preparing the composite gas-sensitive resistor is to prepare the composite gas-sensitive resistor on the surface of the printed ceramic substrate by utilizing a magnetron sputtering process, and the specific preparation process comprises the following steps:
s31, covering the inductance coil by using an insulating adhesive tape to avoid damage of the inductance coil in a sputtering process, and meanwhile, adding a layer of dust-free paper between the adhesive tape and the inductance coil to prevent silver paste from falling off when the adhesive tape is torn;
s32, respectively placing the ceramic substrate and the sputtering target tungsten (with the purity of 99.95%) on a sample base and a target source installation position in a sputtering chamber, starting a power supply, firstly pumping the vacuum degree of the sputtering chamber to be below 30Pa by using a mechanical pump, and then pumping the sputtering chamber to be vacuum degree lower than 4 x 10 by using a molecular pump-4And Pa, closing the vacuumizing valve, opening the air inlet valve, opening a power supply of the mass flow meter, adjusting the flow rate of gas to ensure that argon and oxygen are slowly introduced into the sputtering chamber at the flow rates of 30sccm and 10sccm respectively, adjusting the molecular pump baffle valve to ensure that the working pressure in the sputtering chamber is kept unchanged when the working pressure in the sputtering chamber is 2Pa, starting the sputtering power supply, setting the sputtering power to be 300W, and starting sputtering. When the thickness of the tungsten oxide film reaches 400nm, the power supply is turned off, the power supply knob is adjusted to 0, the gas flow is adjusted to off, the gas guide valve is closed, the sputtering is stopped, and WO3Finishing the preparation of the film;
s33, taking Pt as a sputtering target (with the purity of 99.95 percent) and Ar as a sputtering gas, adopting a direct current sputtering process under the conditions that the pressure is 0.5Pa and the sputtering power is 8W, and in WO3And sputtering a Pt film with the thickness of 10nm on the surface of the film, thus finishing the preparation of the gas sensor.
FIG. 4 is a wireless passive H2Schematic diagram of working principle of gas sensor, when the sensor is arranged at H2Ambient, reducing gas H2With WO3Surface adsorbed oxygen anionThe ions are oxidized and reduced to generate H2O and release electrons to WO3Conduction band of WO3The Q value of the sensor is increased due to the fact that the conductivity of the antenna is increased and the resistance value of the antenna is reduced, the Q value is transmitted into an impedance analyzer through wireless non-contact coupling with a reading antenna end, the Q value is analyzed, and H can be achieved2Detection of (3).
The above embodiments describe in detail a wireless passive H provided by the present invention2The purpose of the sensor preparation process is to allow those skilled in the art to make various changes or modifications within the scope of the claims, without affecting the essence of the invention. This summary should not be construed to limit the present invention.
Claims (5)
1. Based on WO3Wireless passive H2A gas sensor, comprising: the outer end of the inductance coil is connected with one end of the composite gas-sensitive resistor through silver paste filled in a through hole of the ceramic substrate, and the inner end of the inductance coil is connected with the other end of the composite gas-sensitive resistor to form an LR sensitive loop; the inductance coil is prepared by taking Ag as slurry and adopting a screen printing process, and the composite gas-sensitive resistor is prepared by adopting Pt-WO3The composite material is prepared by a magnetron sputtering process.
2. A WO-based product as claimed in claim 13Wireless passive H2The gas sensor is characterized in that the inductance coil is in a rectangular spiral shape, and the outer end of the inductance coil extends to the through hole.
3. A WO-based product as claimed in claim 13Wireless passive H2The gas sensor is characterized in that the composite gas sensitive resistor is formed by connecting 3 resistors in series, and the purpose is to improve the sensitivity of the sensor.
4. A WO-based product as claimed in claim 13Wireless passive H2Gas sensor, characterized in thatThe gas sensor adopts a wireless non-contact test principle, and realizes the H value of the gas to be tested by analyzing the Q value changing along with the resistance2Non-contact testing of (2).
5. A WO-based product as claimed in claim 13Wireless passive H2The preparation method of the gas sensor is characterized by comprising the following steps of:
s1 preparation of alumina ceramic substrate
S11, cutting the alumina green porcelain strips into a group of 50 x 50mm in size by using a cutting machine23 green ceramic chips in total;
s12, punching a through hole with the inner diameter of 2mm at the same position of the 3 layers of green ceramic chips, namely the joint of the outer end of the inductance coil and the gas-sensitive resistor by utilizing a laser drilling technology;
s13, laminating 3 layers of green ceramic chip laminations into a compact whole;
s14, laminating the green ceramic chips into a wholeGroup ofPlacing the ceramic wafer into a muffle furnace for high-temperature sintering to enable the raw ceramic to become mature ceramic, so that the performance of the ceramic wafer is achieved, and the preparation of the sensor substrate is completed;
s2 preparation of inductance coil
S21, fixing the printing screen on a screen printing table, and placing the ceramic substrate cleaned by alcohol wiping below the printing screen to be aligned with the patterns of the induction coils on the printing screen;
s22, uniformly coating a certain amount of metal silver paste on the screen printing plate, and repeatedly and slowly moving the rubber scraper to print the inductance pattern on the ceramic substrate;
s23, after printing, placing the ceramic wafer in a mesh belt dryer at 150 ℃ and drying for 10 min;
s24, repeating the steps S21-S23, printing an inductor on the other surface of the ceramic substrate, extending the outer end of the inductor to the through hole, and filling silver paste in the through hole to realize the connection between the outer end of the inductor and the gas sensitive resistor to form an LR sensitive loop;
s25, placing the printed ceramic substrate into a muffle furnace, heating and sintering to 850 ℃ at a heating rate of 10 ℃/min, and keeping the temperature for 45min to volatilize organic impurities in the slurry;
s3 preparation of composite gas-sensitive resistor
S31, covering the inductance coil by using an insulating tape, and meanwhile, adding a layer of dust-free paper between the tape and the inductance coil to prevent silver paste from falling off when the tape is torn;
s32, respectively placing the shielded ceramic substrate and tungsten sputtering target on a sample base in a sputtering chamber and at a target source installation position, starting a power supply, firstly pumping the vacuum degree of the sputtering chamber to be below 30Pa by using a mechanical pump, and then pumping the sputtering chamber to be lower than 4 x 10 by using a molecular pump-4Pa, closing a vacuumizing valve, opening an air inlet valve, opening a power supply of a mass flow meter, adjusting the flow rate of gas to ensure that argon and oxygen are slowly introduced into the sputtering chamber at the flow rates of 30sccm and 10sccm respectively, adjusting a molecular pump baffle valve to ensure that the working pressure in the sputtering chamber is kept unchanged when the working pressure in the sputtering chamber is 2Pa, starting a sputtering power supply, setting the sputtering power to be 300W, and starting sputtering; when the thickness of the tungsten oxide film reaches 400nm, the sputtering power supply is closed, the power supply adjusting knob is adjusted to 0, the gas flow is adjusted to off, the gas guide valve is closed, the sputtering is stopped, and WO3Finishing the preparation of the film;
s33, taking Pt as a sputtering target material and Ar as a sputtering gas, adopting a direct current sputtering process under the conditions that the pressure is 0.5Pa and the sputtering power is 8W, and performing sputtering under the conditions of WO3And sputtering a Pt film with the thickness of 10nm on the surface of the film, thus finishing the preparation of the gas sensor.
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