CN111537585A - Based on YSZ and CoTiO3Mixed potential type NO of sensitive electrode2Sensor, preparation method and application thereof - Google Patents
Based on YSZ and CoTiO3Mixed potential type NO of sensitive electrode2Sensor, preparation method and application thereof Download PDFInfo
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- CN111537585A CN111537585A CN202010303885.8A CN202010303885A CN111537585A CN 111537585 A CN111537585 A CN 111537585A CN 202010303885 A CN202010303885 A CN 202010303885A CN 111537585 A CN111537585 A CN 111537585A
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Abstract
The invention discloses a mixed-potential high-temperature NO2 sensor based on YSZ and CoTiO3 sensitive electrodes, a preparation method and application thereof in automobile exhaust monitoring; the sensor consists of an Al2O3 ceramic plate with a Pt heating electrode, a YSZ substrate, a Pt reference electrode and a sensing electrode in sequence; the reference electrode and the sensitive electrode are separately and symmetrically prepared at two ends of the upper surface of the YSZ substrate, and the lower surface of the YSZ substrate is bonded with the Al2O3 ceramic plate with the Pt heating electrode; the material of the sensitive electrode is CoTiO 3. The YSZ-based mixed-potential high-temperature NO2 gas sensor with good sensing characteristics on NO2 is constructed by taking YSZ as an ion conducting layer and using a CoTiO3 composite oxide material with high electrochemical catalytic activity as a sensitive electrode.
Description
Technical Field
The invention relates to a sensor, in particular to NO2A sensor.
Background
In the last decade, with the continuous progress and implementation of automobile industry combustion furnaces in various countries around the world, great influence is generated on the emission of various harmful health and atmospheric pollution gases. Nitrogen dioxide (NO)2) Is one of the harmful pollutants generated in the combustion process of automobiles, not only directly causes ozone layer cavities and damages the health of human bodies, but also generates environmental disasters such as acid rain, photochemical smog, greenhouse effect and the like. Development of high-Performance, reliable NO2Sensor for monitoring and controlling NO2Is an urgent need. In addition, since the exhaust emission of the automobile engine is in a typical long-term high-temperature, high-humidity and multi-gas coexisting environment, the sensor needs to operate under the above-mentioned severe conditions, and not only is good sensitivity characteristics (sensitivity, selectivity and response/recovery characteristics) required for the sensor, but also good stability in the use environment is required. Very fortunately, mixed-potential gas sensors based on YSZ and metal oxide sensitive electrodes can meet the above requirements.
Stabilized zirconia-based mixed-potential NO2The sensitive mechanism of the sensor is as follows: NO in the atmosphere2Diffusion through the sensitive electrode layer to the three-phase reaction interface, NO occurring during the diffusion process due to the reaction (1)2Will gradually decrease and the porosity of the oxide sensitive electrode will determine the NO2The degree of reduction in concentration. Simultaneous generation of NO at the gas/sensing electrode/YSZ three-phase interface2When the reaction rates of the two are equal, the reaction reaches equilibrium, a mixed potential is formed on the sensitive electrode, and the potential difference between the mixed potential and the reference electrode is used as a detection signal of the sensor. The magnitude of the detection signal is determined by the rate of the electrochemical reactions (2) and (3), and the reaction rate depends on the electrochemical and chemical catalytic activity of the sensitive electrode material, and the microstructure of the electrode material (such as porosity, particle size, morphology and the like of the material).
The reaction formula is as follows:
NO2→ NO + 1/2 O2（1）
NO2+ 2e-→ NO + O2-（2）
O2-→ 1/2O2+ 2e-（3）
at present, most researchers at home and abroad are dedicated to the research of sensitive electrode materials in order to prepare sensors with higher sensitive characteristics. For example, the subject group is made of Cr2O3-WO3YSZ-based mixed potential NO as sensitive electrode material2Sensor pair 100ppm NO2The Mixed potential value of (1) was 52mV (Quan Diao, Chengguo Yin, Yingwei Liu, JianguoLi, Xun Gong, Xishuang Liang, Shiqi Yang, Hong Chen, Geyu Lu, Mixed-potential-type NO2sensor using stabilized zirconia and Cr2O3-WO3nanocomposites, sensors and activators B180 (2013) 90-95). This NO is2The sensors, while having acceptable sensitivity performance, continue to be developed for use with NO2Sensitive electrode materials with high electrochemical catalytic activity for gas detection are still very necessary.
Disclosure of Invention
The invention aims to provide a mixed-potential NO based on YSZ and CoTiO3 sensitive electrodes2The sensor, the preparation method and the application thereof also have lower detection lower limit, good selectivity, moisture resistance and stability.
The purpose of the invention is realized as follows: YSZ and CoTiO3 sensitive electrode-based mixed potential NO2Sensor, in turn made of Al with Pt heating electrode2O3The ceramic plate, the YSZ substrate, the Pt reference electrode and the sensitive electrode are combined; the reference electrode and the sensitive electrode are separately and symmetrically arranged at two ends of the upper surface of the YSZ substrate, the lower surface of the YSZ substrate and Al with a Pt heating electrode2O3The ceramic plates are bonded together; the method is characterized in that: the material of the sensitive electrode is CoTiO3Which is prepared by the following method,
separately calledTaking the molar ratio of 1: 2 Co (NO)3)2·6H2Dissolving O and CA in deionized water, dropwise adding a certain amount of ammonia water with the mass concentration of 25-28% into the solution under the condition of continuous stirring, adjusting the pH value of a reaction system to 8-10, slowly adding a certain amount of tetrabutyl titanate and ethylene glycol into the solution, and continuously stirring at 60-80 ℃ until gel is formed; drying the obtained gel for 12-24 hours at 80-90 ℃ under vacuum condition to obtain dry gel, and finally calcining the obtained dry gel for 2-4 hours at 800-1200 ℃ to obtain CoTiO3A sensitive electrode material; wherein Co (NO)3)2·6H2The molar ratio of the O to the tetrabutyl titanate is 1: 1.
YSZ and CoTiO3 sensitive electrode-based mixed potential NO2The preparation method of the sensor comprises the following steps:
(1) manufacturing a Pt reference electrode: manufacturing a Pt reference electrode with the thickness of 15-20 microns on one end of the upper surface of the YSZ substrate by using Pt slurry, folding a Pt wire, adhering the Pt wire to the middle position of the reference electrode to be used as an electrode lead, baking the YSZ substrate at 90-120 ℃ for 1-2 hours, calcining the YSZ substrate at 1000-1200 ℃ for 1-2 hours, removing terpineol in the platinum slurry, and cooling to room temperature;
(2) making CoTiO3A sensitive electrode: adding CoTiO3The sensitive electrode material is mixed into slurry with deionized water, and the mass concentration is 2-20%; preparing a sensitive electrode with the thickness of 20-30 microns on a platinum point, which is connected with a platinum wire, at the other end of the upper surface of the YSZ substrate which is symmetrical to the reference electrode, of the slurry;
(3) calcining the YSZ substrate with the reference electrode and the sensitive electrode at 800-1000 ℃ for 1-3 hours;
(4) using inorganic adhesive to make lower surface of YSZ substrate and Al with Pt heating electrode2O3The ceramic plates are bonded together;
(5) welding and packaging the bonded device to prepare the YSZ and CoTiO based material3Mixed potential type NO of sensitive electrode2A sensor.
As a further limitation of the present invention, the temperature increase rate during the calcination in the step (3) is 1 to 2 ℃/min.
YSZ and CoTiO3 sensitive electrode-based mixed potential NO2The application of the sensor is to be applied to automobile exhaust monitoring.
Compared with the prior art, the invention has the beneficial effects that:
(1) the sensor utilizes a typical solid electrolyte, namely stabilized zirconia (YSZ), has good thermal stability and chemical stability, and can detect NO2 in a harsh environment;
(2) the sol-gel method is adopted to prepare the high-performance composite oxide CoTiO3 as a sensor sensitive electrode, the preparation method is simple, and the mass industrial production is facilitated;
(3) by comparing the response values of the sensor to different gases, the YSZ-based mixed potential type device with CoTiO3 as a sensitive electrode shows the highest response to NO2 at high temperature, has higher response value, good sensitivity, selectivity, repeatability, moisture resistance and stability, and has potential application prospect in the aspect of automobile exhaust monitoring.
Drawings
FIG. 1 shows a mixed potential NO mode based on YSZ and CoTiO3 sensitive electrodes2The structure of the sensor is shown schematically;
wherein the names of each part are as follows: CoTiO3 sensitive electrode 1, YSZ substrate 2, Pt reference electrode 3, Pt wire 4, Pt dot 5, Al2O3 ceramic plate 6 with Pt heating electrode, and inorganic adhesive 7.
FIG. 2 is an XRD pattern of a sensitive electrode material prepared according to the present invention;
wherein the abscissa is angle and the ordinate is intensity.
FIG. 3 is an SEM image of the sensitive electrode material prepared by the invention at the calcination temperature of 800 ℃.
FIG. 4 is a response characteristic curve of a sensor constructed by using CoTiO3 calcined at 800 ℃ as a sensitive electrode material to NO2 with different concentrations;
wherein, the abscissa is NO2 concentration, the ordinate is response value size, and operating temperature is 650 degrees.
FIG. 5 is a graph of the sensitivity of the sensor of the present invention to NO2 using 800 ℃ calcined CoTiO3 as the sensing electrode material;
wherein the abscissa is NO2 concentration, the ordinate is potential difference, and the operating temperature is 650 ℃.
FIG. 6 is a graph showing the selectivity of a sensor of the present invention using 800 ℃ calcined CoTiO3 as the sensing electrode material;
wherein the abscissa is the potential difference value and the ordinate is the test gas.
Detailed Description
The present invention is further illustrated by the following specific examples.
Example 1:
a mixed potential type NO based on YSZ and CoTiO3 sensitive electrodes as shown in figure 12Sensor, in turn made of Al with Pt heating electrode2O3Ceramic plate 6, YSZ substrate 2, Pt reference electrode 3 and CoTiO3A sensitive electrode 1; pt reference electrode 3 and CoTiO3The sensitive electrodes 1 are separately and symmetrically arranged at two ends of the upper surface of the YSZ substrate 2, the lower surface of the YSZ substrate 2 and Al with Pt heating electrodes2O3The ceramic plates 6 are bonded together.
Preparation of CoTiO by sol-gel method3Material, CoTiO to be produced3Calcining at 800 ℃ to be used as a sensitive electrode material to manufacture a YSZ-based mixed potential sensor, and testing NO of the sensor2The specific process of the gas-sensitive property of (1) is as follows:
1. manufacturing a Pt reference electrode: a layer of Pt reference electrode with the size of 0.5mm multiplied by 2mm and the thickness of 15 mu m is manufactured at one end of the upper surface of a YSZ substrate with the length, the width and the thickness of 2 multiplied by 2mm and the thickness of 0.2mm by using Pt slurry, and meanwhile, a Pt wire is folded in half and then is adhered to the middle position of the reference electrode to lead out an electrode lead; then the YSZ substrate was baked at 100 ℃ for 1.5 hours, and then the YSZ substrate was calcined at 1000 ℃ for 1 hour to remove terpineol from the platinum slurry, and finally cooled to room temperature.
2. Making CoTiO3A sensitive electrode: firstly, preparing CoTiO by a sol-gel method3A material; 3mmol Co (NO) were weighed out separately3)2·6H2Dissolving O and 6mmol CA in 12mL deionized water, dropwise adding ammonia water with a certain mass concentration of 25% into the solution under the condition of continuous stirring, adjusting the pH value of a reaction system to 8, slowly adding 3mmol tetrabutyl titanate and 3mL ethylene glycol into the solution, and continuously stirring at 80 ℃ until gel is formed; drying the obtained gel for 12 hours at the temperature of 80 ℃ under vacuum condition to obtain dry gel, and finally calcining the obtained dry gel for 3 hours at the temperature of 800 ℃ to obtain CoTiO3A sensitive electrode material;
5mg of CoTiO was taken3The powder was slurried with 100mg of deionized water and the CoTiO3Coating a layer of sensitive electrode with the size of 0.5mm × 2mm and the thickness of 20 mu m on a platinum point of platinum wire connected with the other end of the upper surface of the YSZ substrate which is symmetrical to the reference electrode by the slurry, and folding a platinum wire in half and then adhering the platinum wire on the sensitive electrode to lead out an electrode lead;
and heating the prepared YSZ substrate with the reference electrode and the sensitive electrode to 800 ℃ at the heating rate of 2 ℃/min, keeping the temperature for 2 hours, and then cooling to room temperature.
3. Bonding a ceramic plate having a heating electrode; using an inorganic binder (Al)2O3And water glass Na2SiO3·9H2O, about 5: 1 preparation) the lower surface (the side not coated with the electrode) of the YSZ substrate was brought into contact with the same size of Al with Pt heater electrode2O3The ceramic plates (length and width 2 × 2mm, thickness 0.2 mm) were bonded.
4. And welding and packaging the device. Welding the device on the hexagonal tube seat, sleeving the protective cover on the hexagonal tube seat, and finishing the preparation of the mixed potential NO2A sensor.
As shown in FIG. 2, which is an XRD pattern of a CoTiO3 sensitive electrode material, by comparing with a standard spectrogram, the synthesized sensitive electrode material is consistent with a standard card JCPDS (File NO.72-1069), which indicates that the sensitive electrode material prepared by the invention is a CoTiO3 material.
As shown in fig. 3, which is an SEM image of a sensing electrode material of CoTiO3 calcined at 800 ℃, it can be seen that the surface of the sensing electrode material is composed of loose porous particles, and the porosity of the electrode is favorable for gas diffusion.
The sensor was connected to a Rigol Signal tester and placed in air at 500 ppb NO2、1 ppmNO2、2 ppm NO2、5 ppm NO2、10 ppm NO2、20 ppm NO2、50 ppm NO2、100 ppm NO2、200 ppm NO2The voltage signal test is performed in the atmosphere of (1). The testing method of the device adopts a traditional static testing method, and comprises the following specific processes:
1. connecting the sensor to a Rigol signal tester, placing the device in a test bottle filled with air with a volume of 1L to achieve stability, namely obtaining the electromotive force value (V) of the device in the airAir (a)）。
2. Rapidly transferring the sensor to the container with NO to be measured2In a test bottle of gas until the response signal is stabilized, i.e. the device is in NO2Electromotive force value (V) ofNO2）。
3. And transferring the device back to the empty gas cylinder until the device is stable, and finishing a response recovery process by the device. Device in NO2And the electromotive force difference in air (Δ V = V)NO2-VAir (a)) I.e. the device is aligned to this concentration NO2The response value of (2). The sensitivity of the sensor is determined by the slope of the linear relation between the response value of the sensor in a certain measured concentration range and the corresponding concentration logarithm.
The CoTiO respectively calcined at 800 ℃ are shown in Table 13YSZ-based mixed potential type sensor as sensitive electrode for different concentrations of NO2The difference between the electromotive force in the atmosphere and the electromotive force in air is dependent on NO2The value of the change in concentration. As can be seen from the table, the sensitivity (slope) of the device is 60 mV/decade. It can be seen that we have developed a novel 800 ℃ calcined CoTiO3Device pair formed by sensitive electrode material and NO2Shows good sensitivity, and obtains YSZ-based mixed potential NO with high sensitivity2A sensor.
TABLE 1 CoTiO calcined at 800 deg.C3Delta V with NO for devices that are sensitive electrodes2A change in concentration;
as shown in FIG. 4, the response characteristic curve of the sensor with CoTiO3 sintered at 800 ℃ as a sensitive electrode to different concentrations of NO2 shows that at the operating temperature of 650 ℃, the device is subjected to 100ppm of NO2The response value of (2) is 130mV, and the detection lower limit can reach 0.5 ppm.
As shown in fig. 5, is a CoTiO calcined at 800 deg.C3Sensor pair NO as sensitive electrode material2The sensitivity curve of (A) shows that the device is used for 0.5-200 ppm NO2Has a sensitivity of 60mV/decade, and can detect 500 ppb of NO at the lowest2The sensor exhibits good sensitivity and a low detection limit.
As shown in FIG. 6, is 800 ℃ calcined CoTiO3Selectivity of the sensor as a sensitive electrode material, it can be seen from the figure that the device is sensitive to 100ppm NO2The highest response value is shown, and the response values to other gases are lower, so that the device has good selectivity.
The present invention is not limited to the above-mentioned embodiments, and based on the technical solutions disclosed in the present invention, those skilled in the art can make some substitutions and modifications to some technical features without creative efforts according to the disclosed technical contents, and these substitutions and modifications are all within the protection scope of the present invention.
Claims (4)
1. YSZ and CoTiO3 sensitive electrode-based mixed potential NO2Sensor, in turn made of Al with Pt heating electrode2O3The ceramic plate, the YSZ substrate, the Pt reference electrode and the sensitive electrode are combined; the reference electrode and the sensitive electrode are separately and symmetrically arranged at two ends of the upper surface of the YSZ substrate, the lower surface of the YSZ substrate and Al with a Pt heating electrode2O3The ceramic plates are bonded together; the method is characterized in that: the material of the sensitive electrode is CoTiO3Which is prepared by the following method,
respectively weighing the components in a molar ratio of 1: 2 Co (NO)3)2·6H2Dissolving O and CA in deionized water, dropwise adding a certain amount of ammonia water with the mass concentration of 25-28% into the solution under the condition of continuous stirring, adjusting the pH value of a reaction system to 8-10, slowly adding a certain amount of tetrabutyl titanate and ethylene glycol into the solution, and continuously stirring at 60-80 ℃ until gel is formed; drying the obtained gel for 12-24 hours at 80-90 ℃ under vacuum condition to obtain dry gel, and finally calcining the obtained dry gel for 2-4 hours at 800-1200 ℃ to obtain CoTiO3A sensitive electrode material; wherein Co (NO)3)2·6H2The molar ratio of the O to the tetrabutyl titanate is 1: 1.
2. YSZ and CoTiO3 sensitive electrode-based mixed potential NO2The preparation method of the sensor is characterized by comprising the following steps of:
(1) manufacturing a Pt reference electrode: manufacturing a Pt reference electrode with the thickness of 15-20 microns on one end of the upper surface of the YSZ substrate by using Pt slurry, folding a Pt wire, adhering the Pt wire to the middle position of the reference electrode to be used as an electrode lead, baking the YSZ substrate at 90-120 ℃ for 1-2 hours, calcining the YSZ substrate at 1000-1200 ℃ for 1-2 hours, removing terpineol in the platinum slurry, and cooling to room temperature;
(2) making CoTiO3A sensitive electrode: adding CoTiO3The sensitive electrode material is mixed into slurry with deionized water, and the mass concentration is 2-20%; preparing a sensitive electrode with the thickness of 20-30 microns on a platinum point, which is connected with a platinum wire, at the other end of the upper surface of the YSZ substrate which is symmetrical to the reference electrode, of the slurry;
(3) calcining the YSZ substrate with the reference electrode and the sensitive electrode at 800-1000 ℃ for 1-3 hours;
(4) using inorganic adhesive to make lower surface of YSZ substrate and Al with Pt heating electrode2O3The ceramic plates are bonded together;
(5) welding and packaging the bonded device to prepare the YSZ and CoTiO based material3Mixed potential of sensitive electrodeForm NO2A sensor.
3. The YSZ and CoTiO3 sensitive electrode-based mixed-potential NO of claim 22The sensor preparation method is characterized by comprising the following steps: and (4) the temperature rise rate during the calcination in the step (3) is 1-2 ℃/min.
4. YSZ and CoTiO3 sensitive electrode-based mixed potential NO2The application of the sensor is characterized in that the sensor is applied to automobile exhaust monitoring.
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