CN104198547B - NiO-sensitive-electrode-based YSZ-based HCs gas sensor and preparation method thereof - Google Patents
NiO-sensitive-electrode-based YSZ-based HCs gas sensor and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a NiO-sensitive electrode-based YSZ-based HCs gas sensor and a preparation method thereof. The YSZ solid oxygen ion conductor material is used as the solid electrolyte of the HCs sensor, the flower-shaped nano NiO is used as the sensitive electrode, no liquid phase component is generated, the safety is high, the sensitivity is high, the selectivity is good, the safety is good, the sensor is simple in structure, small in size and simple in preparation process. The HCs sensor of the invention can detect HCs concentration range of 0-500ppm without external working voltage when working.
Description
Technical Field
The invention relates to preparation of a YSZ-based HCs gas sensor based on a flower-like nano-morphology sensitive electrode for HCs concentration measurement.
All references to HCs herein are to hydrocarbons.
Background
With the rapid increase of automobile ownership in China, the atmospheric pollution in urban areas in China is developing from soot type pollution to automobile exhaust type pollution; automobile exhaust pollution becomes the first pollution source of air pollution in China, and under the condition that urban traffic is more and more congested, automobiles can generate more gases such as CO and NO which are harmful to human health under the idling state2HCs, etc., which also seriously affect the health of the occupants. Although there are restrictions of relevant environmental regulations and standards on the emission of automobile exhaust, the amount of pollutants emitted varies with the extension of the service life of the automobile and the change of the loading capacity, and it is necessary to track and monitor the pollutants in real time at any time.
There are many mature methods for detecting and analyzing hazardous gases such as toxic, harmful, flammable and explosive gases, such as spectroscopic method, infrared absorption spectroscopic method, gas chromatography, ion mobility spectrometry, mass spectrometry, and combination method of each individual technique; also, various gas sensors, such as thermal catalysis, thermal conductance, electrochemistry, solid electrolytes, gas sensitive diodes, gas sensitive field effect transistors, semiconductor polymers, semiconductor metal oxides, and other gas sensitive elements, can be used to detect various gases to be detected, wherein the semiconductor metal oxide gas sensor has been widely used due to its advantages of high sensitivity, capability of detecting various gases, fast response, small volume, low price, long life, and the like.
However, due to the cross-sensitivity of the metal oxide gas sensor to multiple gases, it is difficult to detect a component in a complex mixed gas such as automobile exhaust. At present, a plurality of metal oxide gas sensors with different sensitivity characteristics are generally adopted to simultaneously detect mixed gas of a certain specific component, and a neural network method is adopted to perform data processing so as to qualitatively or semi-quantitatively judge the type of the detected gas and the concentration of each component. However, the reliability of this method depends on the design and training of the neural network, and this training requires a standard sample set, and the composition of the exhaust gas of automobiles is hundreds of, and the composition is unknown and varies widely, and it is difficult to perform such training, and moreover, the characteristics of the metal oxide gas sensor strongly depend on the ambient temperature, humidity, and the like, so that the reliability of detection is poor.
At present, pollutants such as NOx, CO and HCs emitted by automobiles are seriously out of limits, wherein the generated HCs are a main source for generating photochemical smog. HCs sensors based on Yttrium Stabilized Zirconia (YSZ) as a solid electrolyte have attracted much attention because they can perform simple, fast and real-time monitoring of HCs content in automobile exhaust. However, the influence of the morphology of the sensitive electrode on the response performance of the YSZ-based Hydrocarbon (HCs) sensor is obvious.
Disclosure of Invention
In order to solve the problems, the invention discloses a YSZ-based HCs gas sensor based on a flower-like nano-morphology NiO sensitive electrode and a preparation method thereof.
The invention discloses a NiO-based YSZ-based HCs gas sensor based on a sensitive electrode, which comprises a solid electrolyte, a sensitive electrode and a reference electrode, wherein the sensitive electrode and the reference electrode are respectively printed on two sides of the solid electrolyte, the sensitive electrode is a porous nano electrode, the reference electrode is a porous Pt electrode, a Pt slurry layer is coated on the sensitive electrode, electrode leads are respectively led out from the sensitive electrode and the reference electrode, and the thickness of the sensitive electrode is 20-30 mu m. Preferably, the thickness of the sensing electrode is 28 μm, and the HCs gas is gradually activated into an ion-free state in an active channel (as shown in fig. 3) of the sensing electrode, so that sufficient reaction for detecting HCs components is ensured, and interference of gaseous impurity gas is reduced by preferable selectivity of the reaction, thereby improving accuracy and selectivity of the sensor.
Preferably, the thickness of the solid electrolyte is 0.5 to 0.7mm (excluding 0.6 mm). More preferably, the thickness of the solid electrolyte is 0.55mm, and at this time, the sensing electrode has a suitable oxygen ion migration length when the sensor works and the ion hole concentration of the YSZ material of the sensing electrode can control the passing capacity of oxygen ions in unit time through a suitable length, so that the sensor has good oxygen ion concentration control capacity, thereby ensuring that the electrochemical reaction of the sensor on gases such as HCs is normally performed, reducing the activity on other gases, and improving the selectivity of the sensor.
Preferably, the sensitive electrode is formed by printing NiO electrode paste by using a thick-film screen printing technology.
The invention discloses a preparation method of a NiO sensitive electrode YSZ-based HCs gas sensor based on claim 1, which comprises the following steps:
a, preparing a YSZ green ceramic chip with the thickness of 0.5-0.7mm (excluding 0.6 mm) by adopting a tape casting technology, removing glue in air at 350-400 ℃ for 20 hours, and then putting the YSZ green ceramic chip into a sintering furnace for sintering and forming;
b, preparing a flower-like nano NiO sensitive electrode material by adopting a hydrothermal synthesis method;
c, providing sensitive electrode slurry of porous nano NiO on one side of the YSZ solid electrolyte, wherein the preparation method of the sensitive electrode slurry comprises the steps of mixing NiO powder prepared by the step B and terpineol slurry (prepared from 70% of terpineol and 30% of ethyl cellulose) in an agate mortar, and uniformly grinding, wherein the thickness of the sensitive electrode is 20-30 mu m;
d, drying the sample obtained in the step C in a drying oven, spot-coating a Pt slurry layer on the upper surface of the sensitive electrode, and leading out an electrode lead;
e, a porous Pt reference electrode is arranged on the other side of the YSZ solid electrolyte, and an electrode lead is led out;
and F, drying the sample obtained in the step E, and then keeping the dried sample in a sintering furnace at the temperature of 900-1000 ℃ for 2-3 hours for sintering and forming.
Preferably, the solid electrolyte (1) is prepared by placing YSZ green ceramic chips prepared by a tape casting technology into a sintering furnace at 1200-1400 ℃ for 2h after removing glue at 350-400 ℃ for 20 h.
Preferably, the sensitive electrode in the step C is formed by printing flower-like nano-morphology NiO electrode paste by using a thick-film screen printing technology.
Preferably, the reference electrode in step E is formed by printing Pt paste by using thick film screen printing technology.
Preferably, step F is specifically to keep the sample obtained in step E at 900 ℃ for 2 hours for sintering and forming after drying in a sintering furnace, the sample is qualified for inspection, uniform in texture, good in adhesion with the surface of the solid electrolyte 1, and free of cracks and gaps, and is a finished product, at this time, the sintering temperature of the sensitive electrode and the reference electrode is proper, so that the problems that the electrode has too low sintering temperature, too low activity, weak association ability, too low strength and influence on the response time and detection quality of the sensor are avoided, and the phenomenon of material burnout and deactivation due to too high temperature is also avoided.
Compared with the prior art, the invention has the advantages that the gas sensor based on the YSZ base has very high response and sensitivity to HCs at high temperature and stronger anti-interference capability to other gases by adopting the flower-shaped nano-morphology sensitive electrode material, and the gas sensor has simple structure, small volume and simple preparation process. And the HCs sensor is based on a mixed potential type, the reference electrode and the sensitive electrode can be simultaneously exposed in the atmosphere to be measured, and a good result is obtained within the gas measurement range of 0-500 ppm.
Drawings
FIG. 1 is a diagram of the morphology of flower-like nanometer NiO of the sensitive electrode of the HCs sensor of the invention;
FIG. 2 is a schematic cross-sectional view of an HCs sensor according to the present invention;
FIG. 3 is a schematic diagram of the operation of the HCs sensor of the present invention;
FIG. 4 is a graph of the response of the HCs sensor of the present invention at different temperatures;
FIG. 5 is a schematic graph of the step response curve of the HCs sensor of the present invention;
FIG. 6 is a graph of the gas response dependence of the HCs sensor of the present invention;
list of reference numerals:
1. a solid electrolyte; 2. a sensitive electrode; 3. a reference electrode;
4. a Pt slurry layer; 5. an electrode lead; 6. three-phase interface.
Detailed Description
The present invention will be further illustrated with reference to the accompanying drawings and specific embodiments, which are to be understood as merely illustrative of the invention and not as limiting the scope of the invention. It should be noted that the terms "front," "back," "left," "right," "upper" and "lower" used in the following description refer to directions in the drawings, and the terms "inner" and "outer" refer to directions toward and away from, respectively, the geometric center of a particular component.
The invention discloses a NiO-based YSZ-based HCs gas sensor based on a sensitive electrode, which comprises a solid electrolyte 1, a sensitive electrode 2 and a reference electrode 3, wherein the sensitive electrode 2 and the reference electrode 3 are respectively printed on two sides of the solid electrolyte 1, the sensitive electrode 2 is a porous nano electrode, the reference electrode 3 is a porous Pt electrode, a Pt slurry layer 4 is coated on the sensitive electrode 2, electrode leads 5 are respectively led out from the sensitive electrode 2 and the reference electrode 3, and the thickness of the sensitive electrode 2 is 20-30 mu m. Preferably, the thickness of the sensing electrode 2 is 28 μm, and the HCs gas is gradually activated into an ion-free state in an active channel (as shown in fig. 3) of the sensing electrode, so that sufficient reaction for detecting HCs components is ensured, and interference of gaseous impurity gas is reduced by preferential selectivity of the reaction, thereby improving accuracy and selectivity of the sensor.
Preferably, the thickness of the solid electrolyte (1) is 0.5 to 0.7mm (excluding 0.6 mm). More preferably, the thickness of the solid electrolyte 1 is 0.55mm, and at this time, the sensing electrode has a suitable oxygen ion migration length when the sensor works and the ion hole concentration of the YSZ material of the sensing electrode can control the passing capacity of oxygen ions in unit time through a suitable length, so that the sensor has a good oxygen ion concentration control capacity, thereby ensuring that the electrochemical reaction of the sensor on gases such as HCs is normally performed, reducing the activity on other gases, and improving the selectivity of the sensor.
Preferably, the sensing electrode 3 is NiO electrode paste printed and formed by a thick-film screen printing technology.
The invention discloses a preparation method of a NiO sensitive electrode YSZ-based HCs gas sensor based on claim 1, which comprises the following steps:
a, preparing a YSZ green ceramic chip with the thickness of 0.5-0.7mm (excluding 0.6 mm) by adopting a tape casting technology, removing glue in air at 350-400 ℃ for 20 hours, and then putting the YSZ green ceramic chip into a sintering furnace for sintering and forming;
b, preparing a flower-like nano NiO sensitive electrode material by adopting a hydrothermal synthesis method;
c, providing sensitive electrode slurry of porous nano NiO on one side of the YSZ solid electrolyte, wherein the preparation method of the sensitive electrode slurry comprises the steps of mixing NiO powder prepared by the step B and terpineol slurry (prepared from 70% of terpineol and 30% of ethyl cellulose) in an agate mortar, and uniformly grinding, wherein the thickness of the sensitive electrode is 20-30 mu m;
d, drying the sample obtained in the step C in a drying oven, spot-coating a Pt slurry layer on the upper surface of the sensitive electrode, and leading out an electrode lead;
e, a porous Pt reference electrode is arranged on the other side of the YSZ solid electrolyte, and an electrode lead is led out;
f, drying the sample obtained in the step E, and then keeping the sample at 900-1000 ℃ in a sintering furnace for 2-3 hours for sintering and forming;
preferably, the solid electrolyte (1) is prepared by placing YSZ green ceramic chips prepared by a tape casting technology into a sintering furnace at 1200-1400 ℃ for 2h after removing glue at 350-400 ℃ for 20 h.
Preferably, the sensitive electrode 2 in the step C is formed by printing the flower-like nano-morphology NiO electrode paste by using a thick-film screen printing technology.
Preferably, the reference electrode 3 in step E is formed by printing Pt paste by using thick film screen printing technology.
Preferably, step F is specifically to keep the sample obtained in step E at 900 ℃ for 2 hours for sintering and forming after drying in a sintering furnace, the sample is qualified for inspection, uniform in texture, good in adhesion with the surface of the solid electrolyte 1, and free of cracks and gaps, and is a finished product, at this time, the sintering temperature of the sensitive electrode and the reference electrode is proper, so that the problems that the electrode has too low sintering temperature, too low activity, weak association ability, too low strength and influence on the response time and detection quality of the sensor are avoided, and the phenomenon of material burnout and deactivation due to too high temperature is also avoided.
Table 1: parameter setting tables of examples 1 to 6
Note: the particle size of NiO nano material as the material of the sensing electrode in examples 1-6 was selected to be 60-100nm, the NiO nano material content was adjusted to be 20-25% (wt) by terpineol slurry, and the thickness of the sensing electrode described in examples 1-6 above was formed after multiple printing by the silk screen printing technique.
Examples 7-11 differ from examples 1-5 only in that the NiO nanomaterial of the sensing electrode material was selected to have a particle size of 80-120nm, adjusted to a NiO nanomaterial content of 25-30% (wt) with terpineol slurry, and printed multiple times using screen printing techniques to form the thickness of the sensing electrode, solid electrolyte, as described in examples 1-5 aboveThe strip temperature corresponds to examples 1 to 5 The glue discharging temperature in the process is respectively changed into: 358 deg.C, 350 deg.C, 380 deg.C, 370 deg.C, 400 deg.C. Namely, the glue discharging temperature in the embodiment 7 is 358 ℃; in example 8, the glue discharging temperature is 350 ℃; in example 9, the rubber discharging temperature is 380 ℃; example 10 temperature of gel dischargeThe temperature is 370 ℃; in example 11, the binder removal temperature was 400 deg.C (the explanations in other parts of this paragraph are similar to the ones marked in this paragraph, and the explanations apply to this sentence, with the exception of other explanations).
Examples 12-16 differ from examples 1-5 only in that the particle size of the NiO nanomaterial as the sensing electrode material was selected to be 130-150nm, the NiO nanomaterial content was adjusted to be 25-30% (wt) by terpineol slurry, and after multiple printing by the screen printing technique, the thickness of the sensing electrode as described in examples 1-5 above was formed, and the dielectric thickness of the solid electrolyte was changed to correspond to the dielectric thickness of the solid electrolyte in examples 1-5, respectively: 0.55, 0.61, 0.5, 0.7, 0.65.
Examples 17-21 differ from examples 1-5 only in that the particle size of NiO nanomaterial as the sensing electrode material was selected to be 140-160nm, the NiO nanomaterial content was adjusted to 30-35% (wt) by terpineol slurry, and after multiple printing by the screen printing technique, the thickness of the sensing electrode described in examples 1-5 above was formed, and the sintering temperature of the solid electrolyte was changed to correspond to the sintering temperature of the solid electrolyte in examples 1-5: 1200 deg.C, 1240 deg.C, 1400 deg.C, 1320 deg.C, 1280 deg.C.
Examples 22-26 differ from examples 1-5 only in that the particle size of NiO nanomaterial as the sensing electrode material is selected to be 150-170nm, the NiO nanomaterial content is adjusted to be 30-35% (wt) by terpineol slurry, the sensing electrode thickness as described in examples 1-5 above is formed after multiple printing by the silk screen printing technique, and the drying temperature of the sensing electrode is changed corresponding to the drying temperature of the sensing electrode in examples 1-5: 160 deg.C, 200 deg.C, 140 deg.C, 100 deg.C, 120 deg.C.
Examples 27-31 differ from examples 1-5 only in that the particle size of the NiO nanomaterial as the sensing electrode material was selected to be 160-180nm, the NiO nanomaterial content was adjusted to be 30-35% (wt) by terpineol slurry, and after multiple prints by the screen printing technique, the thickness of the sensing electrode was changed corresponding to the thickness of the sensing electrode in examples 1-5: 24. 20, 30, 26, 22.
Examples 32-36 differ from examples 1-5 only in the NiO nanomaterial particles of the material of the sensing electrodeThe diameter is 150-170nm, the NiO nano material content is 30-35% (wt) through terpineol slurry, and the thickness of the sensitive electrode and the electrode are formed through multiple printing by the silk screen printing technology in the above-mentioned embodiments 1-5Is/are as followsThe sintering temperatures corresponding to the sintering temperatures of the electrodes in examples 1 to 5 were changed to: 900 deg.C, 940 deg.C, 1000 deg.C, 980 deg.C, 920 deg.C.
Examples 37-41 differ from examples 1-5 only in that the NiO nanomaterial used as the sensing electrode material has a particle size of 160-180nm, and is adjusted to have a NiO nanomaterial content of 30-35% (wt) by terpineol slurry, and after multiple printing by the screen printing technique, the thickness of the sensing electrode described in examples 1-5 above is formed, and the baking time of the electrode is changed corresponding to the sintering of the electrode in examples 1-5: 2.9, 2.5, 2, 2.3, 2.7.
In view of the fact that the embodiments of the present invention are numerous, the experimental data of each embodiment is huge, and the embodiments are not suitable for being listed and described one by one, but the contents of the verification required by each embodiment are close to the final conclusion obtained, so the contents of the verification of each embodiment are not described one by one here, and only the embodiment 6 is taken as a representative to describe the excellent points of the present invention.
For example, in the HCs sensor manufactured by using the method of the present invention in example 6, the thickness of the solid electrolyte (YSZ powder of which YSZ substrate is sieved by 500 mesh, prepared into slurry with YSZ content of 20-25% (wt%) by mixing with the slurry, and tape-casting on the surface of a nano polytetrafluoroethylene mold) is 0.55mm, the patterned nano-morphology NiO (shown in fig. 1) is used as the sensitive electrode material, the particle size of the NiO nano-material is selected to be 60-100nm, and the NiO nano-material is prepared by terpineol slurry and then is printed to form the sensitive electrode, and the thickness of the sensitive electrode is 28 μm. The structure of the sensor of the invention is schematically shown in fig. 2, and the working principle is shown in fig. 3:
as shown in fig. 3, a three-phase interface 6 is formed between the flower-like nano-morphology NiO sensitive electrode and the solid electrolyte YSZ, a part of the gas to be detected undergoes a gas-phase reaction before the gas enters the three-phase interface 6 of the sensor, and the following electrochemical reactions occur after the gas to be detected enters the three-phase interface 6 of the sensitive electrode and the YSZ:
and (3) anode reaction:
and (3) cathode reaction:
and (3) total reaction: 2C3H6+9O2—6CO2+6H2O
When C is present3H6Anodic current and O2When the cathode currents are equal, a mixed potential can be obtained, and therefore the response value of the sensor to the gas can be obtained, and the response value of the sensor and the logarithm of the concentration of the gas to be measured have a linear relation, so that the concentration of the gas to be measured can be obtained from the response value of the sensor.
FIG. 4 shows the sensor at different temperatures for 100 ppm C3H6The response value of (2). It can be seen that: the output voltage of the sensor is different at different temperatures and has the best response value at 600 ℃.
FIG. 5 shows an HCs sensor with a sensing electrode obtained by sintering a nickel oxide nano-sensing electrode material with 900 deg.C for 2h at 600 deg.C, 5 vol.% O2C at various concentrations3H6(0-500 ppm) step response plot of the sensor under gas. It can be clearly seen that: the sensor shows good repeatability and stability.
FIG. 6 is a graph of gas dependence for an HCs sensor showing a good linear relationship between the sensor response and the logarithm of the gas concentration. Sintering nickel oxide nano sensitive electrode material with 900 ℃ for 2h to obtain HCs sensor of the sensitive electrode, wherein O is 5 vol.% at 600 DEG C2Lower, C3H6As can be seen from the response graph of the sensor obtained after the logarithm of the concentration is taken when the gas concentration is changed from 0-500ppm, the HCs sensor prepared by the method has excellent linearity, all points are basically on the same straight line, namely the response value of the sensor and the logarithm value of the gas concentration have obvious linear relation, and the Nernst equation is satisfied
The technical means disclosed by the scheme of the invention are not limited to the technical means disclosed by the technical means, and the technical scheme also comprises the technical scheme formed by any combination of the technical characteristics. While the foregoing is directed to embodiments of the present invention, it will be appreciated by those skilled in the art that various changes may be made in the embodiments without departing from the principles of the invention, and that such changes and modifications are intended to be included within the scope of the invention.
Claims (5)
1. A NiO-based sensitive electrode YSZ-based HCs gas sensor comprises a solid electrolyte (1), a sensitive electrode (2) and a reference electrode (3), and is characterized in that:
a sensitive electrode (2) and a reference electrode (3) are respectively printed on two sides of the solid electrolyte (1), and the thickness of the solid electrolyte (1) is 0.5-0.7mm and 0.6mm is excluded;
the sensitive electrode (2) is a porous nano electrode, a Pt slurry layer (4) is coated on the sensitive electrode (2), the thickness of the sensitive electrode (2) is 20-30 mu m, the sensitive electrode is made of a NiO sensitive electrode material with flower-shaped nano morphology, and the particle size range of the NiO sensitive electrode material is 60-120nm and 130-180 nm;
the reference electrode (3) is a porous Pt electrode, and electrode leads (5) are led out from the sensitive electrode (2) and the reference electrode (3);
the sensitive electrode (2) is formed by printing NiO slurry by adopting a thick film screen printing technology.
2. The preparation method of the NiO sensitive electrode YSZ-based HCs gas sensor based on claim 1, characterized by comprising the following steps:
a, preparing a YSZ green ceramic chip with the thickness of 0.5-0.7mm and 0.6mm by adopting a tape casting technology, discharging glue in air at 350-400 ℃ for 20 hours, and then putting the ceramic chip into a sintering furnace for sintering and forming;
b, preparing a flower-like nano NiO sensitive electrode material by adopting a hydrothermal synthesis method;
c, providing sensitive electrode slurry of porous nano NiO on one side of the YSZ solid electrolyte, wherein the preparation method of the sensitive electrode slurry comprises the steps of mixing the NiO powder prepared by the step B and terpineol slurry in an agate mortar, uniformly grinding, and enabling the thickness of the sensitive electrode to be 20-30 mu m, wherein the terpineol slurry is prepared from 70% of terpineol and 30% of ethyl cellulose;
d, drying the sample obtained in the step C in a drying oven, spot-coating a Pt slurry layer on the upper surface of the sensitive electrode, and leading out an electrode lead;
e, a porous Pt reference electrode is arranged on the other side of the YSZ solid electrolyte, and an electrode lead is led out; and F, drying the sample obtained in the step E, and then keeping the sample in a sintering furnace at 900-1000 ℃ for 2-3 hours for sintering and forming.
3. The preparation method of the NiO-based sensitive electrode YSZ-based HCs gas sensor according to claim 2, wherein the solid electrolyte (1) is prepared by placing YSZ green ceramic chips prepared by tape casting technology into a sintering furnace at 1200-1400 ℃ for 2h after removing glue at 350-400 ℃ for 20 h.
4. The preparation method of the YSZ-based HCs gas sensor based on the NiO sensitive electrode is characterized in that the sensitive electrode (2) in the step C is formed by printing flower-like nano-morphology NiO electrode material by using a thick film screen printing technology.
5. The method for preparing the NiO-based sensitive electrode YSZ-based HCs gas sensor according to claim 2, wherein the reference electrode (3) in the step E is formed by printing Pt paste by using a thick-film screen printing technology.
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| CN104865304A (en) * | 2015-04-09 | 2015-08-26 | 宁波大学 | YSZ base HCs gas sensor based on Mn2O3 reference electrode |
| CN105334256A (en) * | 2015-10-29 | 2016-02-17 | 宁波大学 | Potentiometric CO sensor based on Ni-doped PdO sensitive electrode and preparation method of potentiometric CO sensor |
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