CN109001283B - Self-constant-temperature electrochemical sheet type gas sensor and preparation method thereof - Google Patents
Self-constant-temperature electrochemical sheet type gas sensor and preparation method thereof Download PDFInfo
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- CN109001283B CN109001283B CN201811131005.2A CN201811131005A CN109001283B CN 109001283 B CN109001283 B CN 109001283B CN 201811131005 A CN201811131005 A CN 201811131005A CN 109001283 B CN109001283 B CN 109001283B
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Abstract
The invention relates to a self-constant temperature electrochemical sheet type gas sensor, which is characterized by comprising the following components: an electrochemical plate type gas sensor and a ceramic heating plate for providing and maintaining the electrochemical plate type gas sensor at a required working temperature. The self-constant temperature electrochemical chip gas sensor prepared by the invention can provide and maintain the working temperature required by the sensor by depending on a mobile power supply, and simultaneously, a complex temperature measurement and control system is avoided, so that the solid electrolyte type gas sensor can detect toxic and harmful gases under the environmental concentration in real time.
Description
Technical Field
The invention relates to a gas sensor, in particular to a self-constant temperature electrochemical sheet type gas sensor and a preparation method thereof.
Background
In recent years, with the unprecedented development of our country's economy, the problem of environmental pollution has become quite serious, haze weather frequently appears in various big cities, and atmospheric pollutants such as PM2.5, NOx and NH3、CO、SO2And the like, have brought great threats to the health of people. With the increasing concern of people on health problems, China has strict standards on the concentrations of various toxic and harmful gases, monitoring analysis and monitoring alarm on the gases have profound influence on human production and life, and a gas sensor plays an important role in the process, so that the development of a sensor which is convenient to carry and use and is used for detecting the toxic and harmful gases at the environmental concentration in real time is urgently needed.
The concentration of toxic and harmful gas in the environment is determined by sampling in the field and carrying out chemical quantification in a laboratory, and the method has the advantages of accurate result, low efficiency, high cost, most important long time consumption, incapability of real-time detection and portability, and the concentration of the toxic and harmful gas in the environment is changed from moment to moment, so that the reference value of the sampling test result is greatly reduced. Solid electrolyte electrochemical sensors are highly sensitive,The low cost, short response time and general attention and research, Germany and Japan successively introduced NO suitable for automobile exhaust detection2A sensor. The solid electrolyte type gas sensor prepared at present is mostly heated through a tube furnace to ensure the normal working temperature of the sensor, so that the sensor is not easy to carry and can not be used under the daily living conditions of families, office areas and the like, and the practical application of the solid electrolyte sensor is seriously hindered.
Disclosure of Invention
The invention aims to provide an electrochemical gas sensor capable of detecting toxic and harmful gases in the environment in real time.
In order to achieve the above object, the present invention provides a self-thermostatic electrochemical plate-type gas sensor, comprising: an electrochemical plate type gas sensor and a ceramic heating plate for providing and maintaining the electrochemical plate type gas sensor at a required working temperature.
Preferably, the electrochemical plate type gas sensor is bonded with the ceramic heating plate through a high-temperature resistant adhesive.
Preferably, the high-temperature resistant binder is a high-temperature resistant heat-conducting glue with a heat conductivity coefficient larger than 1.5[ W/(m.k) ].
Preferably, the ceramic heating plate is a PTC ceramic heating plate or an MCH ceramic heating plate.
Preferably, the ceramic heater chip has the same size as the solid electrolyte type gas sensor substrate.
Preferably, the electrochemical chip gas sensor comprises a solid electrolyte gas sensor substrate, and a sensor electrode is arranged on the solid electrolyte gas sensor substrate.
The invention also provides a preparation method of the self-constant temperature electrochemical sheet type gas sensor, which is characterized by comprising the following steps: printing platinum paste on one surface of a solid electrolyte gas sensor substrate by a screen printing mode to be respectively used as a working electrode and a reference electrode or the working electrode, the reference electrode and a counter electrode; sensitive electrode slurry is screen-printed on the surfaces of the working electrode or the working electrode and the counter electrode; and (3) bonding the ceramic heating sheet on the other surface of the solid electrolyte gas sensor substrate by using a high-temperature-resistant bonding agent, and connecting the ceramic heating sheet to a mobile power supply with the voltage of less than or equal to 24V to obtain the self-constant-temperature electrochemical sheet type gas sensor.
Preferably, the mobile power supply is a battery.
The PTC or MCH ceramic heating sheet is bonded on the solid electrolyte gas sensor substrate by adopting the high-temperature resistant adhesive, and the ceramic heating sheet is powered by a mobile power supply such as a battery, so that the ceramic heating sheet can automatically reach and be stabilized at the working temperature required by the gas sensor without being provided with a temperature detection and control device. PTC and MCH ceramic heating sheets on the market are adopted, the sources are simple and easy to obtain, and the PTC and MCH ceramic heating sheets can be used for various solid electrolyte gas sensor substrates such as NASICON, GDC, YSZ and the like. The manufactured sensor has the advantages of small volume, simple structure and process, low cost, no need of special equipment and harsh conditions, strong controllability and easy realization of large-scale production. Because the PTC or MCH ceramic heating sheet is adopted to provide the working temperature for the sensor, the sensor is extremely portable, the development of the gas sensor to a simpler direction is promoted, the application range of the sensor is expanded, and meanwhile, a foundation is laid for the integrated networking application of the sensor.
Compared with the prior art, the invention has the beneficial effects that:
the self-constant temperature electrochemical chip gas sensor prepared by the invention can provide and maintain the working temperature required by the sensor by depending on a mobile power supply, and simultaneously, a complex temperature measurement and control system is avoided, so that the solid electrolyte type gas sensor can detect toxic and harmful gases under the environmental concentration in real time.
Drawings
FIG. 1 is a schematic structural view of a sensor device obtained in example 1 of the present invention;
fig. 2 is an enlarged view of a portion a in fig. 1.
FIG. 3 is a schematic structural view of a sensor device obtained in example 3 of the present invention;
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
Example 1:
as shown in fig. 1 and 2, a self-isothermal electrochemical plate-type gas sensor includes: an electrochemical plate type gas sensor and a ceramic heating plate 1 for providing and maintaining the electrochemical plate type gas sensor at a required working temperature. The electrochemical chip gas sensor comprises a solid electrolyte gas sensor substrate 3, a counter electrode 4, a working electrode 5 and a reference electrode 6 are arranged on the solid electrolyte gas sensor substrate 3, and the counter electrode 4, the working electrode 5 and the reference electrode 6 are respectively connected with a platinum wire 7. NaNO is arranged on the counter electrode 42A layer of electrode material, a working electrode 5 coated with TiO2The catalytic oxidation layer and the surface of the reference electrode 6 are sealed by an inorganic adhesive layer 8. The solid electrolyte gas sensor substrate 3 of the electrochemical chip gas sensor is bonded with the ceramic heating chip 1 through the high-temperature resistant adhesive 2. The ceramic heating plate is a PTC ceramic heating plate. The heat conductivity coefficient of the high-temperature resistant adhesive is more than 1.5[ W/(m.k)]The high-temperature resistant heat-conducting glue. The ceramic heating plate has the same size as the solid electrolyte type gas sensor substrate.
The preparation method of the self-constant temperature electrochemical sheet type gas sensor comprises the following specific steps:
1) NASICON (Na) preparation by high-temperature solid-phase method1+xZr2SixP3-XO12X 2) powder material, and preparing a NASICON blank under 160MPa pressure by using cold isostatic pressing, and then sintering at high temperature in a muffle furnace to obtain the NASICON substrate. Collecting NASICON solidPolishing a bulk electrolyte substrate to the thickness of 1.4mm, printing platinum paste on one surface of the NASCION substrate by screen printing to form three platinum electrodes which are not communicated with each other and respectively used as a counter electrode, a working electrode and a reference electrode, drying for 0.5h at 80 ℃, fixing the platinum wire on the platinum electrode by using the platinum paste, drying for 0.5h at 80 ℃, placing the device in a muffle furnace for calcining for 2h at 750 ℃, and coating a layer of inorganic binder (Hui 8767C high-temperature resistant glue) on the surface of the reference electrode to completely isolate the reference electrode from air. Then, mixing the components in a mass ratio of 1: 0.8 title of TiO2Terpineol and evenly mixing the terpineol by using a pendulum vibration ball mill to obtain TiO2And (4) slurry. According to the mass ratio of 1: 5 weighing NaNO2Terpineol and evenly mixing the terpineol by using a pendulum vibration ball mill to obtain NaNO2An electrode material; screen printing a layer of TiO on the working electrode2Drying the slurry, and calcining the dried slurry in a muffle furnace at 500 ℃ for 2h to form TiO2Catalytic oxidation layer, screen printing a layer of NaNO on the counter electrode2Drying the electrode material to form NaNO2A layer of electrode material.
2) Adhering the PTC ceramic heating plate to the other surface of the sensor substrate obtained in the step 1) by using a high-temperature resistant adhesive (Kafter K-5204K heat-conducting silica gel), standing for 24h, connecting the ceramic heating plate with a battery (voltage is 12V) through a lead when the high-temperature resistant adhesive reaches the highest strength, heating the sensor substrate to 150 ℃, and adding 1000ppb NO to the sensor substrate with the concentration range of 100-2The response sensitivity of NO and the response sensitivity of NO can reach 1.358nA/ppb and 0.765nA/ppb, and the lower limit of detection is 50 ppb. To obtain portable NOxA gas sensor.
Example 2:
as shown in fig. 1 and 2, a self-isothermal electrochemical plate-type gas sensor includes: an electrochemical plate type gas sensor and a ceramic heating plate 1 for providing and maintaining the electrochemical plate type gas sensor at a required working temperature. The electrochemical chip gas sensor comprises a solid electrolyte gas sensor substrate 3, a counter electrode 4, a working electrode 5 and a reference electrode 6 are arranged on the solid electrolyte gas sensor substrate 3, and the counter electrode 4, the working electrode 5 and the reference electrode 6 are respectively connected with a platinum wire 7. NaNO is arranged on the counter electrode 42Electrode material layer, working electrodeThe electrode 5 is coated with TiO2The catalytic oxidation layer and the surface of the reference electrode 6 are sealed by an inorganic adhesive layer 8. The solid electrolyte gas sensor substrate 3 of the electrochemical chip gas sensor is bonded with the ceramic heating chip 1 through the high-temperature resistant adhesive 2. The ceramic heating plate is a PTC ceramic heating plate. The heat conductivity coefficient of the high-temperature resistant adhesive is more than 1.5[ W/(m.k)]The high-temperature resistant heat-conducting glue. The ceramic heating plate has the same size as the solid electrolyte type gas sensor substrate.
The preparation method of the self-constant temperature electrochemical sheet type gas sensor comprises the following specific steps:
1) NASICON (Na) preparation by high-temperature solid-phase method1+xZr2SixP3-XO12X 2) powder material, and preparing a NASICON blank under 160MPa pressure by using cold isostatic pressing, and then sintering at high temperature in a muffle furnace to obtain the NASICON substrate. Taking a NASICON solid electrolyte substrate, polishing to the thickness of 1.4mm, screen-printing platinum paste on one surface of the NASICON substrate to form three platinum electrodes which are not communicated with each other, respectively serving as a counter electrode, a working electrode and a reference electrode, drying for 0.5h at 80 ℃, fixing a platinum wire on the platinum electrode by using the platinum paste, drying for 0.5h at 80 ℃, placing the device in a muffle furnace for calcining for 2h at 750 ℃, and coating a layer of inorganic binder (Hui 8767C high-temperature resistant adhesive) on the surface of the reference electrode to completely isolate the reference electrode from air. Then, mixing the components in a mass ratio of 1: 0.9 title of TiO2Terpineol and evenly mixing the terpineol by using a pendulum vibration ball mill to obtain TiO2Slurry, which is prepared from the following components in percentage by mass 1: 5 weighing NaNO2Terpineol and evenly mixing the terpineol by using a pendulum vibration ball mill to obtain NaNO2An electrode material; screen printing a layer of TiO on the working electrode2Drying the slurry, and calcining the dried slurry in a muffle furnace at 500 ℃ for 2h to form TiO2Catalytic oxidation layer, screen printing a layer of NaNO on the counter electrode2Drying the electrode material to form NaNO2A layer of electrode material.
2) Adhering the PTC ceramic heating plate to the other surface of the sensor substrate obtained in the step 1) by using a high-temperature resistant adhesive (Kafter K-5204K heat-conducting silica gel), standing until the high-temperature resistant adhesive reaches the highest strength, and allowing the ceramic heating plate to pass throughThe wires are connected with the battery (the voltage is 12V), and the sensor substrate is heated to the temperature of 150 ℃ and has the concentration range of 100-1000ppb NO2The response sensitivity of NO and the response sensitivity of NO can reach 1.028nA/ppb and 0.568nA/ppb, and the lower detection limit is 80 ppb. To obtain portable NOxA gas sensor.
Example 3:
as shown in fig. 3, a self-isothermal electrochemical plate-type gas sensor includes: an electrochemical plate type gas sensor and a ceramic heating plate 1 for providing and maintaining the electrochemical plate type gas sensor at a required working temperature. The electrochemical chip gas sensor comprises a solid electrolyte gas sensor substrate 3, a working electrode 5 and a reference electrode 6 are arranged on the solid electrolyte gas sensor substrate 3, and the working electrode 5 and the reference electrode 6 are respectively connected with a platinum wire 7. WO is arranged on the working electrode 53A sensitive electrode paste layer 9. The solid electrolyte gas sensor substrate 3 of the electrochemical chip gas sensor is bonded with the ceramic heating chip 1 through the high-temperature resistant adhesive 2. The heat conductivity coefficient of the high-temperature resistant adhesive is more than 1.5[ W/(m.k)]The high-temperature resistant heat-conducting glue. The ceramic heating plate has the same size as the solid electrolyte type gas sensor substrate.
The preparation method of the self-constant temperature electrochemical sheet type gas sensor comprises the following specific steps:
1) preparing GDC intermediate solid product by coprecipitation method, and calcining at high temperature to obtain GDC powder material. Adding 50g of powder material into 15mL of mixed solution of absolute ethyl alcohol and triethanolamine with the volume ratio of 99.7%, ball-milling for 24h, preparing a GDC green material by a tape casting method, and carrying out high-temperature treatment at 1450 ℃ for 10h to carry out ceramic treatment to obtain the GDC substrate. Taking a GDC solid electrolyte substrate, forming two platinum electrodes which are not communicated with each other on one side of the substrate by screen printing of platinum paste, drying for 0.5h at 80 ℃, fixing a platinum wire on the platinum electrode by utilizing the platinum paste, drying for 0.5h at 80 ℃, and then placing the device in a muffle furnace to calcine for 2h at 1400 ℃ to obtain a sheet type sample printed with the Pt electrode. Preparation of mesoporous WO by template method35g of WO was taken3Mixing the powder with 1mL of terpineol and ball-milling for 12h to obtain WO3Sensitive electrode paste; using screen printing process to print WO3Sensitive electrodeAnd printing the slurry on one electrode to completely cover the Pt electrode, drying to obtain a working electrode, and using the other electrode as a reference electrode.
2) Bonding the MCH ceramic heating plate on the other side surface of the sensor substrate obtained in the step 1) by using a high-temperature-resistant bonding agent (Hui glue HR-8777), standing until the high-temperature-resistant bonding agent reaches the highest strength, connecting the MCH ceramic heating plate with a battery (the voltage is 12V) through a lead, and adding 5% of O in volume fraction2And 95% of N2As background gas, NH3The concentration range is detected under the condition of 30ppm to 250ppm, the gas flow rate is controlled to be 50mL/min, and the electrochemical signal reaches 113.76mV/decade under the condition of 400 ℃.
Claims (3)
1. A self-thermostatting electrochemical plate gas sensor, comprising: the device comprises an electrochemical sheet type gas sensor and a ceramic heating sheet for providing and maintaining the electrochemical sheet type gas sensor at a required working temperature; the preparation method of the self-constant temperature electrochemical sheet type gas sensor comprises the following steps:
preparation of NASICON, Na, by high temperature solid phase method1+xZr2SixP3-XO12Preparing a NASICON blank from a powder material, wherein x is 2, preparing the NASICON blank under 160MPa of pressure by using cold isostatic pressing, and then sintering the NASICON blank at a high temperature in a muffle furnace to obtain an NASICON substrate; taking a NASICON solid electrolyte substrate, polishing to the thickness of 1.4mm, screen-printing platinum paste on one surface of the NASICON substrate to form three platinum electrodes which are not communicated with each other and respectively used as a counter electrode, a working electrode and a reference electrode, drying for 0.5h at 80 ℃, fixing a platinum wire on the platinum electrode by using the platinum paste, drying for 0.5h at 80 ℃, placing the device in a muffle furnace for calcining for 2h at 750 ℃, and coating a layer of inorganic binder on the surface of the reference electrode to completely isolate the reference electrode from air; then adding TiO2Terpineol and evenly mixing the terpineol by using a pendulum vibration ball mill to obtain TiO2Slurry; according to the mass ratio of 1: 5 weighing NaNO2Terpineol and evenly mixing the terpineol by using a pendulum vibration ball mill to obtain NaNO2An electrode material; screen printing a layer of TiO on the working electrode2Drying the slurry and placing the dried slurry inCalcining in a muffle furnace at 500 ℃ for 2h to form TiO2Catalytic oxidation layer, screen printing a layer of NaNO on the counter electrode2Drying the electrode material to form NaNO2A layer of electrode material; bonding the PTC ceramic heating plate on the other surface of the obtained sensor substrate by using a high-temperature-resistant bonding agent, standing for 24 hours, and connecting the ceramic heating plate with a battery through a lead when the high-temperature-resistant bonding agent reaches the highest strength;
or preparing a GDC intermediate solid product by a coprecipitation method, and calcining at high temperature to obtain a GDC powder material; adding 50g of powder material into 15mL of mixed solution of absolute ethyl alcohol and triethanolamine with the volume ratio of 99.7%, ball-milling for 24h, preparing a GDC green material by using a tape casting method, and carrying out high-temperature treatment at 1450 ℃ for 10h to carry out ceramic treatment to obtain a GDC substrate; taking a GDC solid electrolyte substrate, forming two platinum electrodes which are not communicated with each other on one side of the substrate by screen printing of platinum paste, drying at 80 ℃ for 0.5h, fixing a platinum wire on the platinum electrode by utilizing the platinum paste, drying at 80 ℃ for 0.5h again, and then placing the device in a muffle furnace to calcine at 1400 ℃ for 2h to obtain a sheet type sample printed with the Pt electrode; preparation of mesoporous WO by template method35g of WO was taken3Mixing the powder with 1mL of terpineol and ball-milling for 12h to obtain WO3Sensitive electrode paste; using screen printing process to print WO3Printing sensitive electrode slurry on one electrode to completely cover the Pt electrode, drying to obtain a working electrode, and using the other electrode as a reference electrode; and bonding the MCH ceramic heating plate on the other side surface of the obtained sensor substrate by using a high-temperature-resistant bonding agent, standing, and connecting the MCH ceramic heating plate with a battery through a wire when the high-temperature-resistant bonding agent reaches the highest strength.
2. The self-isothermal electrochemical plate gas sensor according to claim 1, wherein said high temperature resistant adhesive is a high temperature resistant thermally conductive glue having a thermal conductivity greater than 1.5W/(m-k).
3. The self-thermostatted electrochemical plate gas sensor of claim 1, wherein the ceramic heater plate is the same size as the solid electrolyte type gas sensor substrate.
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