CN111474227A - Potential gas sensor with titanium-doped strontium ferrite as sensitive electrode - Google Patents

Potential gas sensor with titanium-doped strontium ferrite as sensitive electrode Download PDF

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CN111474227A
CN111474227A CN202010484409.0A CN202010484409A CN111474227A CN 111474227 A CN111474227 A CN 111474227A CN 202010484409 A CN202010484409 A CN 202010484409A CN 111474227 A CN111474227 A CN 111474227A
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易建新
张作彬
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University of Science and Technology of China USTC
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Abstract

The invention discloses a potential gas sensor using titanium-doped strontium ferrite as a sensitive electrode, which is perovskite oxide SrFe1‑xTixO3‑A potentiometric hydrogen sensor as sensitive electrode material, which is characterized by positive response to hydrogen, Volatile Organic Compounds (VOC), carbon monoxide, ammonia gas but not limited to these gases, and is applied to SrFe with positive response0.5Ti0.5O3‑In combination with the conventional electrode material of negative polarity response, the response of the sensor to hydrogen is further enhanced. The sensitive electrode material SrFe in the invention1‑xTixO3‑The positive response to hydrogen gas is opposite to the conventional negative response including but not limited to L SCF, and the two sensitive electrode materials SrFe are taken as hydrogen gas as an example0.5Ti0.5O3‑Has better electrochemical catalytic activity to hydrogen with L SCF, and contains SrFe0.5Ti0.5O3‑Gas sensors with L SCF as dual sensing electrodes can be further providedThe response to hydrogen is increased.

Description

Potential gas sensor with titanium-doped strontium ferrite as sensitive electrode
Technical Field
The invention belongs to the field of gas sensors, and particularly relates to a potentiometric gas sensor taking titanium-doped strontium ferrite as a sensitive electrode.
Background
In actual production life, a large amount of toxic and harmful gases such as volatile organic compound gas (VOC), carbon monoxide, ammonia gas and the like can be generated, and great harm is caused to the health of human beings. Hydrogen is used as a new energy source and has the advantages of high efficiency, reproducibility, no pollution and the like, but because the hydrogen is colorless and tasteless and is not easy to detect after leakage, and the hydrogen is extremely easy to combust and explode due to extremely low ignition energy (0.019mJ) and wider explosion limit (4% -75.6%), the monitoring and the detection of toxic, harmful, flammable and explosive gases such as volatile organic compound gases (VOCs), carbon monoxide, ammonia gas, hydrogen and the like are very important in various places of production and life.
At present, a gas sensor is a convenient and economic gas monitoring and detecting means, but the gas sensor has the defects of low sensor response performance, high sensor manufacturing cost and the like. In addition, in the current research results, when the conventional potentiometric gas sensor and the sensitive electrode material are connected with a data acquisition instrument, the response to the gas is generally represented as a negative polarity response (H.Zhang, J.X.Yi, X.Jiang, Fast response, high sensitivity and selective mixed-potential H)2sensor based on(La,Sr)(Cr,Fe)O3-perovskite sensing electrode,ACSAppl.Mater.Interfaces 9(2017)17218-17225.doi:10.1021/acsami.7b01901.)。
Research shows that perovskite oxide with good electrochemical catalytic activity on gas can be used as a sensitive electrode material to realize detection on gas. Pt is often used as a reference electrode in a mixed potential gas sensor for research, but the manufacturing cost of the sensor is increased due to the high cost of noble metals. The search for suitable electrode materials to achieve improved response to hydrogen and lower cost is a problem to be solved. SrFe1-xTixO3-The perovskite oxide has good electrochemical catalytic performance on hydrogen in the solid oxide fuel, can be used as a sensitive electrode of a sensor for research, and can further reduce the manufacturing cost of the sensor by replacing noble metal platinum with the perovskite oxide with relatively low manufacturing cost.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and aims to provide a potential gas sensor taking titanium-doped strontium ferrite as a sensitive electrode. The sensitive electrode material adopted by the invention has better electrochemical catalytic activity on hydrogen, Volatile Organic Compounds (VOC), carbon monoxide, ammonia gas and the like, and the invention preferably has the best detection performance on the hydrogen; meanwhile, the response of the sensor to the detection gas can be further improved by adopting the sensitive electrode material, and in addition, the perovskite oxide is used for replacing the traditional Pt reference electrode, so that the manufacturing cost of the sensor can be obviously reduced. The following description will be given taking a potential type hydrogen sensor as an example.
One of the potential hydrogen sensors of the present invention is a potential hydrogen sensor constructed by using perovskite oxide as a sensitive electrode material, and a reference electrode including, but not limited to, platinum, or other metals or oxides including, but not limited to, GDC, SDC, YSZ, NASICON, or the like as a solid electrolyte.
The perovskite oxide is SrFe1-xTixO3-0 x 0.9, and preferably 0.5 x, wherein oxygen vacancies are present and some elements are present in non-normal valence states, thus having a non-stoichiometric oxygen ratio.
Wherein GDC is Ce0.8Gd0.2O1.9-Is 20 mol% Gd2O3CeO (B) of2。
The preparation method of the potential hydrogen sensor comprises the following steps:
mixing a sensitive electrode material and modified terpineol in a mass ratio of 1:1, and grinding for 2 hours (the particle size is controlled to be less than or equal to 10 mu m); respectively coating the uniformly ground mixed slurry and platinum slurry on the same electrolyte substrate by a screen printing method and keeping the two slurries not in contact with each other, wherein the area of the electrode comprises but is not limited to 3mm2Sintering and compacting at 800-1000 ℃ to respectively obtain a sensitive electrode and a platinum electrode; the sensitive electrode is connected with the platinum electrode through a platinum wire (the diameter is 0.05mm), and then the positive response potential type hydrogen sensor can be obtained.
The second one of the potential type hydrogen sensors of the present invention is a double-sensitive electrode potential type hydrogen sensor, which is made of SrFe0.5Ti0.5O3-Is a sensing electrode, including but not limited to L SCF, and can be other conventional oxide or metal gas-sensitive materialsThe other sensitive electrode is preferably L SCF, and includes but is not limited to GDC, SDC, YSZ and NASICON, and the GDC is preferably solid electrolyte.
Wherein L SCF is L a0.8Sr0.2Cr0.5Fe0.5O3-The element is lanthanum chromate doped with 20 mol% of Sr and 50 mol% of Fe.
The preparation method of the potential hydrogen sensor comprises the following steps:
the sensitive electrode material SrFe0.5Ti0.5O3-L SCF nano powder is mixed with modified terpineol in a mass ratio of 1:1 and ground for 2h (the particle size is controlled to be less than or equal to 10 mu m), two kinds of evenly ground slurry are respectively coated on the same electrolyte substrate by a screen printing method and are kept not to be contacted with each other, and the electrode area includes but is not limited to 3mm2And sintering and compacting at 1000 ℃; SrFe0.5Ti0.5O3-The sensitive electrode and the L SCF sensitive electrode are connected by a platinum wire (the diameter is 0.05mm), and the double-sensitive-electrode potential type hydrogen sensor can be obtained.
The above SrFe0.5Ti0.5O3-L SCF nanopowder and GDC electrolyte substrate can be synthesized by itself or obtained commercially.
Compared with the prior art, the invention has the beneficial effects that:
1. in the potential gas sensor of the present invention, SrFe1-xTixO3-Perovskite oxides exhibit a positive polarity response to a material including, but not limited to, hydrogen, Volatile Organic Compounds (VOCs), carbon monoxide, ammonia, etc., as opposed to the negative polarity response of conventional materials, and 50 mol% Ti doped strontium ferrite oxide SrFe0.5Ti0.5O3-The highest response value to hydrogen (response value of 29.1mV at 500 ℃ for 100ppm hydrogen);
2. in the potential gas sensor of the present invention, SrFe0.5Ti0.5O3-Including but not limited to L SCF, and may be conventional other oxides or metalsGas sensitive materials two materials exhibit positive and negative polarity responses, respectively, to include but not limited to hydrogen, Volatile Organic Compounds (VOCs), carbon monoxide, ammonia, and the like, and SrFe is tested0.5Ti0.5O3-And the voltage response value between the two sensitive electrodes of L SCF is the sum of the voltage response values of the two sensitive electrodes respectively serving as the sensitive electrodes, so that the response value of the sensor to gas can be further improved, and the application of the sensor is expanded.
3. L SCF or any other conventional oxide or metal gas-sensitive material replaces the noble metal platinum in the invention, and the manufacturing cost is far lower than that of the noble metal platinum, so that the manufacturing cost of the sensor can be greatly reduced.
Drawings
FIG. 1 shows SrFe in example 10.8Ti0.2O3-/GDC/Pt、SrFe0.6Ti0.4O3-/GDC/Pt、SrFe0.5Ti0.5O3-/GDC/Pt、SrFe0.3Ti0.7O3-(GDC/Pt) and SrFe0.1Ti0.9O3-Schematic diagram of/GDC/Pt sensor.
FIG. 2 shows SrFe in example 20.5Ti0.5O3-Schematic diagram of/GDC/L SCF sensor.
FIG. 3 shows SrFe in example 11-xTixO3-XRD patterns of powder and electrolyte GDC.
FIG. 4 shows SrFe in example 11-xTixO3-Dynamic response plot for hydrogen.
FIG. 5 shows SrFe in example 10.5Ti0.5O3-the/GDC/Pt sensor detects the dynamic response diagram of gases such as hydrogen, ethanol, ammonia gas, carbon monoxide and the like.
FIG. 6 shows SrFe in example 20.5Ti0.5O3-/GDC/Pt and SrFe0.5Ti0.5O3-The response of the two sensors, GDC/L SCF, plotted linearly with the 20-100ppm hydrogen concentration.
FIG. 7 shows SrFe in example 20.5Ti0.5O3-(ii) GDC/Pt, L SCF/GDC/Pt and SrFe0.5Ti0.5O3-Dynamic response diagram of three sensors of/GDC/L SCF to hydrogen gas with concentration of 100-500 ppm.
Detailed Description
The following two examples are detailed descriptions of the present invention, both taking hydrogen detection as an example, and the following examples are implemented on the premise of the technical scheme of the present invention, and give detailed implementation manners, specific operation procedures and simple descriptions of the obtained results, and the following examples are only used to help understanding the implementation methods and core ideas of the present invention, but the scope of the present invention is not limited to the following examples.
Example 1:
in this embodiment, the doping amount of Ti is 20, 40, 50, 70, 90 mol% of strontium ferrite oxide SrFe0.8Ti0.2O3-、SrFe0.6Ti0.4O3-、SrFe0.5Ti0.5O3-、SrFe0.3Ti0.7O3-And SrFe0.1Ti0.9O3-The electrode is a sensitive electrode material, Pt is a reference electrode, and GDC is a solid electrolyte, and the preparation method comprises the following steps:
sensitive electrode material SrFe0.8Ti0.2O3-、SrFe0.6Ti0.4O3-、SrFe0.5Ti0.5O3-、SrFe0.3Ti0.7O3-And SrFe0.1Ti0.9O3-Mixing with modified terpineol at a mass ratio of 1:1, and grinding for 2h (particle diameter below 10 μm); respectively coating the uniformly ground sensitive electrode material and platinum paste on an electrolyte substrate by a screen printing method, wherein the electrode area is 3mm2Sintering and compacting at 800-1000 ℃ to respectively obtain a sensitive electrode and a platinum electrode; the sensitive electrode is connected with the platinum electrode through a platinum wire with the diameter of 0.05mm, and the SrFe is finished0.8Ti0.2O3-/GDC/Pt、SrFe0.6Ti0.4O3-/GDC/Pt、SrFe0.5Ti0.5O3-/GDC/Pt、SrFe0.3Ti0.7O3-(GDC/Pt) and SrFe0.1Ti0.9O3-/GDC/Pt sensingThe structure of the device is shown in figure 1.
FIG. 3 shows a sensitive electrode material SrFe0.8Ti0.2O3-、SrFe0.6Ti0.4O3-、SrFe0.5Ti0.5O3-、SrFe0.3Ti0.7O3-、SrFe0.1Ti0.9O3-And the XRD pattern of the solid electrolyte GDC, the material has good phase forming and no impurity peak.
The mixed potential type hydrogen sensor prepared in the embodiment is placed in a tubular muffle furnace, so that the sensor works at the temperature of 400-500 ℃, and an Agilent voltage data collector is used for detecting response values of the sensor under different hydrogen concentrations, wherein a sensitive electrode material is connected with the anode of the Agilent voltage data collector, and a reference electrode Pt is connected with the cathode of the Agilent voltage data collector.
FIG. 4 shows a sensor SrFe0.8Ti0.2O3-/GDC/Pt、SrFe0.6Ti0.4O3-/GDC/Pt、SrFe0.5Ti0.5O3-/GDC/Pt、SrFe0.3Ti0.7O3-(GDC/Pt) and SrFe0.1Ti0.9O3-The dynamic response of/GDC/Pt to 100ppm hydrogen at 500 deg.C was tested and it can be seen that SrFe1-xTixO3-The material responds positively to hydrogen at each ratio, i.e. V1＝ESrFe0.8Ti0.2O3--EPt＞0，V2＝ESrFe0.6Ti0.4O3--EPt＞0，V3＝ESrFe0.5Ti0.5O3--EPt＞0，V4＝ESrFe0.3Ti0.7O3--EPt＞0，V5＝ESrFe0.1Ti0.9O3--EPt> 0, and the sensor SrFe0.5Ti0.5O3-The response of/GDC/Pt to hydrogen is best, and is opposite to the response polarity of the rest (such as L SCF/GDC/Pt shows negative response to hydrogen in figure 6) potential type hydrogen sensor, which is a new response polarity, and the application of the sensor can be further expanded.
FIG. 5 shows SrFe0.5Ti0.5O3-the/GDC/Pt sensor detects hydrogen, ethanol, ammonia gas,Dynamic response diagram of gases such as carbon monoxide. The detection temperature is 500 ℃, the gas concentration is 100ppm, and the result shows that the sensor has positive response to gases such as hydrogen, ethanol, ammonia gas, carbon monoxide and the like.
Example 2:
this example is SrFe0.5Ti0.5O3-The hydrogen sensor is a positive-polarity sensitive electrode, L SCF is a negative-polarity sensitive electrode, and GDC is a solid electrolyte, and the preparation method comprises the following steps:
sensitive electrode material SrFe0.5Ti0.5O3-L SCF and modified terpineol are mixed and ground for 2h (the particle diameter is below 10 mu m) respectively according to the mass ratio of 1:1, the uniformly ground sensitive electrode material and platinum slurry are respectively coated on the same electrolyte substrate by a screen printing method, and the electrode area is 3mm2And sintering and compacting at 1000 ℃; in SrFe0.5Ti0.5O3-L SCF sensitive electrode and platinum electrode are respectively connected with platinum wire with diameter of 0.05mm to complete SrFe0.5Ti0.5O3-The structure of the manufactured/GDC/L SCF sensor is shown in figure 2.
FIG. 6 shows SrFe in example 20.5Ti0.5O3-/GDC/Pt and SrFe0.5Ti0.5O3-A linear relationship graph of response values of the two sensors of/GDC/L SCF and the hydrogen concentration of 20-100ppm can be obtained according to fitting, and SrFe0.5Ti0.5O3-/GDC/Pt and SrFe0.5Ti0.5O3-The response values and the concentrations of the two sensors of/GDC/L SCF respectively satisfy the relations that Y is 0.191x +8.8 and Y is 0.537x +17.6, when the hydrogen concentration is 0.5ppm, the two sensors still have the response values of 8.9mV and 17.8mV, and the sensors still have higher response values under low-concentration hydrogen.
FIG. 7 shows SrFe0.5Ti0.5O3-(ii) GDC/Pt, L SCF/GDC/Pt and SrFe0.5Ti0.5O3-The dynamic response graphs of three sensors of/GDC/L SCF to different concentrations of hydrogen are shown in the figure, and the material SrFe0.5Ti0.5O3-A positive polarity response is exhibited to the hydrogen gas,l SCF showed a negative polarity response to hydrogen, based on this phenomenon, with SrFe0.5Ti0.5O3-SrFe with L SCF as double sensitive electrode0.5Ti0.5O3-the/GDC/L SCF sensor can convert SrFe0.5Ti0.5O3-The response values of/GDC/Pt, L SCF/GDC/Pt to hydrogen are superposed, so that the response value of the sensor to hydrogen, namely V, is further improved6＝(ESrFe0.5Ti0.5O3--EPt)-(ELSCF-EPt)＝ESrFe0.5Ti0.5O3--ELSCF＝V3+|VLSCF/GDC/PtThe value is greater than 0, so that the SrFe material can be obtained1- xTixO3-The positive polarity of the representations responds to this new phenomenon for further applications.
Are merely exemplary embodiments of the present invention and are not intended to limit the enumerated SrFe of the present invention1-xTixO3-Any modification, equivalent replacement, and improvement made within the spirit and principle of the present invention shall be included in the protection scope of the present invention.

Claims (5)

1. A potential gas sensor taking titanium-doped strontium ferrite as a sensitive electrode is characterized in that:
the potential gas sensor is formed by a sensitive electrode, a reference electrode and a solid electrolyte, wherein the sensitive electrode is perovskite oxide SrFe1-xTixO3-X is more than or equal to 0 and less than or equal to 0.9; the reference electrode includes, but is not limited to, platinum, other metals or metal oxides; the solid electrolyte includes, but is not limited to, GDC, SDC, YSZ, NASICON, or the like.
2. A potentiometric gas sensor according to claim 1, wherein:
the detection objects of the potential gas sensor include, but are not limited to, hydrogen, volatile organic compounds, carbon monoxide, and ammonia.
3. A potentiometric gas sensor, comprising:
the potential gas sensor is a double-sensitive electrode potential gas sensor and is a mixed potential gas sensor constructed by double-sensitive electrodes and solid electrolyte; one of the sensitive electrodes is perovskite oxide SrFe1-xTixO3-0 ≦ x ≦ 0.9, another sensing electrode including, but not limited to L SCF, or other metal oxide or metal gas sensitive material, and a solid electrolyte including, but not limited to GDC, SDC, YSZ, or NASICON.
4. A potentiometric gas sensor according to claim 3, wherein:
the perovskite oxide is SrFe0.5Ti0.5O3-。
5. A potentiometric gas sensor according to claim 3 or 4, wherein:
the detection object of the potential type gas sensor includes, but is not limited to, hydrogen gas, volatile organic compounds, carbon monoxide, or ammonia gas.
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CN114018987A (en) * 2021-09-14 2022-02-08 湖北大学 Solid electrolyte type hydrogen sensor and manufacturing method thereof

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* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113189170A (en) * 2021-04-15 2021-07-30 上海交通大学 Double-working-electrode mixed potential type ammonia gas sensor and preparation method thereof
CN114018987A (en) * 2021-09-14 2022-02-08 湖北大学 Solid electrolyte type hydrogen sensor and manufacturing method thereof
CN114018987B (en) * 2021-09-14 2024-01-09 湖北大学 Solid electrolyte type hydrogen sensor and manufacturing method thereof

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