CN115950940A - SO with strontium titanate as sensitive electrode 2 Sensor and preparation method and application thereof - Google Patents
SO with strontium titanate as sensitive electrode 2 Sensor and preparation method and application thereof Download PDFInfo
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Abstract
The invention discloses SO with strontium titanate as a sensitive electrode 2 A sensor and a preparation method and application thereof relate to the technical field of sulfur oxide detection. Sulfur dioxide sensor pair SO obtained by the preparation method of the invention 2 Has high sensitivity, SO 2 The lower detection limit of the sensor can reach 0.3ppm, and the sensor has strong gas immunity to other gases; in addition, the sensor has simple structure, low cost and convenient integration.
Description
Technical Field
The invention relates to the technical field of sulfur oxide detection, in particular to SO with strontium titanate as a sensitive electrode 2 A sensor and a preparation method and application thereof.
Background
With SO 2 The emission standard is more and more strict, and the desulfurization treatment of the waste gas becomes an urgent requirement for realizing the collaborative development of environmental protection and resource utilization in China. To prevent over-standard SO 2 The emission to the atmosphere causes pollution, and a desulfurization system must be provided with SO 2 Concentration detection equipment for SO in waste gas 2 The concentration is accurately monitored. Therefore, the development can be made inThe SO is continuously monitored in situ on line in the high-temperature severe waste gas environment 2 High performance SO of concentration 2 Gas sensor in industrial safety, SO 2 The monitoring and control and other fields have very important significance.
Conventional SO 2 The concentration detection equipment comprises a gas chromatograph, an ion chromatograph, a mass spectrometer and the like, and the devices have the disadvantages of large volume, high price, long analysis period and limited field application. In recent years, solid electrolyte gas sensors have been the subject of research because of their excellent thermal stability and portability, and can be used for SO in harsh environments (high temperature, high humidity, coexistence of multiple gases) 2 And (4) online monitoring of concentration.
The Chinese patent publication No. CN101091111A discloses an ultra-sensitive metal oxide gas sensor and a manufacturing method thereof, and discloses a method for preparing TiO 2 Fe-doped SrTiO 3 The sensor is added into a metal oxide semiconductor to control the gas reaction speed of the metal oxide semiconductor and change the dynamic range of the sensor, but the sensor mainly detects nitrogen oxide, and the semiconductor type sensor has certain technical problems in directly applying the sensor to the detection of the sulfur oxide and has larger detection limit value.
Human body to SO 2 Has a low tolerance limit, and is repeatedly exposed to low levels of SO 2 In the middle, permanent damage to the lungs and even asphyxiation can result. The occupational contact regulation limits for sulfur dioxide are: the short-time contact allowable concentration in the air of a workplace is not more than 10 mg/m 3 (about 3.5 ppm). Therefore, development was able to detect lower concentrations of SO 2 The gas sensor is a current research hotspot and has important significance.
Disclosure of Invention
In order to solve the technical problem, the invention provides SO taking strontium titanate as a sensitive electrode 2 Sensor, preparation method and application thereof, using SrTiO 3 The high-temperature-resistant sensor is prepared by taking YSZ as a sensitive electrode and solid electrolyte, the detection limit range is expanded, and ultralow-concentration SO can be detected 2 A gas.
In order to realize the technical purpose, the invention adopts the following scheme:
SO with strontium titanate as sensitive electrode 2 The preparation method of the sensor comprises the following steps:
s1, preparing a compact YSZ solid electrolyte: mixing YSZ electrolyte powder with PVB (polyvinyl butyral), performing wet ball milling, drying and pressing into a sheet after milling, and performing densification sintering to obtain a dense YSZ solid electrolyte substrate;
s2, preparing a YSZ solid electrolyte with a porous layer/compact layer double-layer structure: adding graphite powder into YSZ electrolyte powder as a pore-forming agent, carrying out wet grinding and uniformly mixing, uniformly mixing the uniformly mixed powder with an organic carrier, coating the mixture on one side of a YSZ solid electrolyte substrate, and calcining to obtain a YSZ solid electrolyte with a porous layer/compact layer double-layer structure;
s3, preparing a sensitive electrode SrTiO 3 ：
S3-1, dissolving tetrabutyl titanate in an organic solvent to form a solution A, dissolving citric acid and strontium nitrate in water to form a solution B, and adding the solution A into the solution B to obtain a solution C;
s3-2, adding EDTA and ammonia water into the solution C, keeping the pH of the solution =7 to 8, and finally adding NH 4 NO 3 Obtaining a solution D;
s3-3, heating and stirring the solution D in a water bath until milky sol is formed, and then drying and calcining to obtain the sensitive electrode material SrTiO 3 ；
S4, preparing a sensitive electrode material SrTiO 3 Uniformly distributed in a porous layer of YSZ solid electrolyte with a porous layer/dense layer double-layer structure, and calcined to obtain SrTiO 3 A solid electrolyte which is a sensitive electrode;
s5, binding and fixing Pt wires with SrTiO 3 And calcining two sides of the solid electrolyte which is a sensitive electrode to prepare the sulfur dioxide sensor.
The sulfur dioxide sensor obtained by the method is used for SO 2 And (6) detecting.
Compared with the prior art, the invention has the beneficial effects that: sulfur dioxide sensor pair SO obtained by the preparation method of the invention 2 Has high sensitivity to other gasesThe body has a very strong gas immunity, SO 2 The lower detection limit of (2) can reach 0.3 ppm; in addition, the sensor has simple structure, low cost and convenient integration.
The preferred scheme of the invention is as follows:
the PVB consumption in S1 is 1wt% of the YSZ electrolyte powder in S1, the densification sintering temperature is 1600 ℃, and the sintering time is 6h.
The organic carrier in S2 consists of 94wt% of terpineol and 6wt% of ethyl cellulose, and the mass ratio of the powder after grinding and uniform mixing to the organic carrier is 3.
The using amount of the graphite powder in the S2 is 30wt% of the YSZ electrolyte powder in the S2, the calcining temperature is 1450 ℃, and the calcining time is 3 hours.
N (amount of total metal species) in S3: n (citric acid): n (EDTA): n (NH) 4 NO 3 )=1:1.2:1:2。
And in the S3-3, the water bath heating temperature of the solution D is 80 ℃, the drying temperature is 120 ℃, the calcining temperature is 900 ℃ and the calcining time is 3 hours.
S4, preparing a sensitive electrode material SrTiO 3 Mixing with an organic carrier, continuously stirring for 24 hours, uniformly mixing, coating the uniformly mixed product on a porous layer of YSZ solid electrolyte with a porous layer/compact layer double-layer structure by using a screen printer, and calcining for 3 hours at 900 to 1050 ℃.
The calcination temperature in S5 is 800 ℃, and the calcination time is 1h.
Drawings
FIG. 1 shows SO with strontium titanate as a sensitive electrode according to an embodiment of the present invention 2 The structure of the sensor is schematic;
FIG. 2 shows a sensitive electrode material SrTiO provided in example 2 of the present invention 3 XRD pattern of (a);
FIG. 3 is a surface SEM image and a cross-sectional SEM image of a sensor proposed in example 2 of the present invention, wherein a is the surface SEM image and b is the cross-sectional SEM image;
FIG. 4 is a response recovery curve of the sensor provided in example 2 of the present invention at 350-500 ℃;
FIG. 5 shows the sensor response and SO values provided in embodiment 2 of the present invention 2 The relationship between the concentration logarithms;
fig. 6 shows the anti-interference performance of the sensor provided in embodiment 2 of the present invention with respect to other gases;
the labels in the figure are: 1. sensitive electrode material SrTiO 3 (ii) a 2. A porous YSZ layer; 3. a dense YSZ solid electrolyte substrate; 4. a Pt reference electrode; 5. and (3) Pt wires.
Detailed Description
The present invention will be described in detail with reference to the following embodiments in order to fully understand the objects, features and effects of the invention, but the present invention is not limited thereto.
As shown in figure 1, the invention provides SO with strontium titanate as a sensitive electrode 2 The sensor comprises a compact YSZ solid electrolyte substrate 3, a porous YSZ layer 2 and a sensitive electrode material SrTiO uniformly distributed on the porous YSZ layer 3 1 and Pt reference electrode 4.
YSZ electrolyte powder was purchased from Suzhou Youzi zirconium nanomaterial Co., ltd, where Y is 2 O 3 The content of (B) is 8 mol%.
Example 1
SO with strontium titanate as sensitive electrode 2 The preparation method of the sensor comprises the following steps:
s1, preparing a compact YSZ solid electrolyte: mixing 30 g of YSZ electrolyte powder with 0.3 g of adhesive PVB, carrying out wet ball milling, naturally drying after grinding, and pressing into a wafer with the diameter of 13 mm by using a cold isostatic press under 300 MPa. And finally, performing densification sintering at 1600 ℃ for 6 hours to obtain a dense YSZ solid electrolyte substrate 3.
S2, preparing a YSZ solid electrolyte with a porous layer/compact layer double-layer structure: weighing 10 g of YSZ electrolyte powder, adding 3 g of graphite powder pore-forming agent, grinding by a wet method, uniformly mixing, and naturally drying. Mixing the air-dried powder with an organic carrier (94% wt terpineol +6% wt ethylcellulose) in a mass ratio of 3:7, uniformly mixing, coating one side of the YSZ solid electrolyte substrate with the screen printing technology, calcining for 3 hours at 1450 ℃ to obtain a porous YSZ layer 2 with a certain thickness, and integrally forming the YSZ solid electrolyte with a porous layer/compact layer double-layer structure.
S3, preparing a sensitive electrode material SrTiO 3 ：
S3-1, dissolving 5 mmol of tetra-n-butyl titanate in 15 ml of ethylene glycol to form a solution A, dissolving 12 mmol of citric acid and 5 mmol of strontium nitrate in 5ml of water to form a solution B, and adding the solution A into the solution B to obtain a solution C;
s3-2, adding 10 mmol of EDTA and ammonia water into the solution C, keeping the pH of the solution = 7-8, and finally adding 20 mmol of NH 4 NO 3 To obtain a solution D.
S3-3, heating the solution D in a water bath to 80 ℃, stirring until a milky sol is formed, drying in a 120 ℃ oven, and calcining at 900 ℃ for 3 hours to obtain the sensitive electrode material SrTiO 3 1。
S4, preparing a sensitive electrode material SrTiO 3 Mixing with an organic carrier (94 wt% terpineol +6wt% ethylcellulose) (mass ratio 3. Then coating the slurry of the sensitive material on the porous layer of the solid electrolyte by a screen printer, and finally calcining for 3h at 900 ℃ to obtain the SrTiO 3 A solid electrolyte which is a sensitive electrode.
S5, fixing the fine Pt filaments 5 on SrTiO through the bonding effect of Pt slurry 3 And calcining the two sides of the solid electrolyte which is the sensitive electrode at 800 ℃ for 1h to prepare the sulfur dioxide sensor. The Pt slurry used was the procurement chemical.
Example 2
The preparation method was the same as in example 1 except that the final calcination temperature of S4 was adjusted to 950 ℃.
Example 3
The preparation method was the same as in example 1 except that the final calcination temperature of S4 was adjusted to 1050 ℃.
Comparative example
The preparation method was the same as in example 1 except that the final calcination temperature of S4 was adjusted to 850 ℃.
The sensor test system consists of a tubular resistance furnace, a sealed high-temperature-resistant quartz tube and a gas distribution system. The tube-type resistance furnace is used for controlling the test temperature, the sensor is arranged in the sealed high-temperature-resistant quartz tube, and the quartz tube is arranged in the heat preservation area of the tube-type furnace. The sealed quartz tube consists ofThe gas inlet is connected with a gas distribution system, and the gas outlet is connected with a sodium hydroxide absorption bottle. The gas distribution system consists of a mass flow meter and a mass flow display instrument, and SO is used for measuring the mass flow of the gas 2 Standard gas (156 ppm SO) 2 ，N 2 Beijing south China gas Limited) and background gas (air) are connected with a mass flow meter, and 0.3 to 2.5 ppm of SO is configured by adjusting the flow of each gas through a mass flow display instrument 2 . The total flow rate of the gas was fixed at 200 cm 3 And/min. The sensor was connected to an electrochemical workstation (CHI 660E) using two platinum wires for performance testing.
Test sensor Pair 2.5 ppm SO at 400 deg.C 2 The sensor response value of example 1 was 74.3 mV, the sensor response value of example 2 was 80.6 mV, the sensor response value of example 3 was 55.5 mV, and the sensor response value of comparative example was 34.4 mV.
For the sensitive electrode material SrTiO prepared in example 2 3 The powder was characterized as follows:
the prepared sensitive material powder was subjected to phase analysis using Rigaku pharmacological D/max-2500PC type X-ray diffractometer (XRD) with the X-ray source Cu K α (λ =0.154056 nm), and the results are shown in FIG. 2. The microscopic morphology and elemental composition of the sensor surface and cross-section obtained in example 2 were characterized by scanning electron microscopy (SEM, JSM-IT100, JEOL), and the results are shown in FIG. 3.
As can be seen from FIG. 2, srTiO 3 The diffraction peaks of the electrode material are in one-to-one correspondence with the standard card (JCPDS 01-089-493), and no other obvious impurity diffraction peaks are detected, which indicates that the prepared sensitive electrode material SrTiO is 3 Is a pure phase.
As can be seen from FIG. 3, srTiO 3 Is small particles with the diameter of 200 to 500 nm, still presents a fluffy porous structure after being calcined, and is beneficial to SO 2 Mass transfer diffusion of the gas. The porous layer of YSZ is about 10 μm thick and is intimately bonded to YSZ. The sensitive electrode particles enter the inside of the YSZ porous layer and maintain relatively uniform porosity.
By usingSrTiO prepared in example 2 was tested by the test method described in the sensor test systems section above 3 The sulfur dioxide sensor is a sensitive electrode.
As shown in FIG. 4, the sensor can effectively detect 0.3 to 2.5 ppm of SO within the temperature range of 350 to 500 DEG C 2 The sensor showed the highest response at 350 deg.C, but the baseline shifted slightly. The base line of the sensor is stable at 400-500 ℃, and the response value at 400 ℃ is obviously higher than 450 ℃ and 500 ℃.
As can be seen from FIG. 5, the response values of the sensor versus SO at the three test temperatures 2 The logarithm of the concentration shows a good linear relationship. The sensitivities at 350 deg.C, 400 deg.C, 450 deg.C and 500 deg.C are 81.2, 84.3, 74.7 and 46.3 mV/decade, respectively. It can be seen that the sensitivity of the sensor is highest at 400 ℃.
As shown in FIG. 6, the sensor pair of example 3 had 2.5 ppm SO alone at a test temperature of 400 deg.C 2 Has a response value of 80.6 mV in SO 2 Respectively mixing with CO of different concentrations 2 （1000 ppm）、H 2 （15 ppm）、CH 4 （15 ppm）、NO（15 ppm）、NO 2 （15 ppm）、H 2 S (15 ppm) and NH 3 After (15 ppm), the change rate of the sensor response value is within 10 percent. It can be seen that SrTiO 3 The sulfur dioxide sensor which is a sensitive electrode has better anti-interference performance.
Finally, it is noted that: the above-mentioned list is only the preferred embodiment of the present invention, and naturally those skilled in the art can make modifications and variations to the present invention, which should be considered as the protection scope of the present invention provided they are within the scope of the claims of the present invention and their equivalents.
Claims (10)
1. SO with strontium titanate as sensitive electrode 2 The preparation method of the sensor is characterized by comprising the following steps:
s1, preparing a compact YSZ solid electrolyte: mixing YSZ electrolyte powder with PVB, performing wet ball milling, drying, pressing into sheets, performing densification sintering, and thus obtaining a compact YSZ solid electrolyte substrate;
s2, preparing a YSZ solid electrolyte with a porous layer/compact layer double-layer structure: adding pore-forming agent graphite powder into YSZ electrolyte powder, carrying out wet grinding and uniformly mixing, uniformly mixing the uniformly mixed powder with an organic carrier, coating the mixture on one side of a YSZ solid electrolyte substrate, and calcining to obtain a YSZ solid electrolyte with a porous layer/compact layer double-layer structure;
s3, preparing a sensitive electrode material SrTiO 3 ：
S3-1, dissolving tetrabutyl titanate in an organic solvent to form a solution A, dissolving citric acid and strontium nitrate in water to form a solution B, and adding the solution A into the solution B to obtain a solution C;
s3-2, adding EDTA and ammonia water into the solution C, keeping the pH of the solution =7 to 8, and finally adding NH 4 NO 3 Obtaining a solution D;
s3-3, heating and stirring the solution D in a water bath until milky sol is formed, and then drying and calcining to obtain the sensitive electrode material SrTiO 3 ；
S4, preparing a sensitive electrode material SrTiO 3 Uniformly distributed in a porous layer of YSZ solid electrolyte with a porous layer/compact layer double-layer structure, and calcined to obtain SrTiO 3 A solid electrolyte which is a sensitive electrode;
s5, binding and fixing Pt wires on SrTiO 3 And calcining two sides of the solid electrolyte which is a sensitive electrode to prepare the sulfur dioxide sensor.
2. SO with strontium titanate as sensitive electrode according to claim 1 2 The preparation method of the sensor is characterized in that the PVB in S1 accounts for 1wt% of YSZ electrolyte powder in S1, the densification sintering temperature is 1600 ℃, and the sintering time is 6h.
3. SO with strontium titanate as sensitive electrode according to claim 1 2 The preparation method of the sensor is characterized in that the organic carrier in S2 consists of 94wt% of terpineol and 6wt% of ethyl cellulose, and the mass ratio of the ground and uniformly mixed powder to the organic carrier is 3:7。
4. SO with strontium titanate as sensitive electrode according to claim 1 2 The preparation method of the sensor is characterized in that the using amount of graphite powder in S2 is 30wt% of YSZ electrolyte powder in S2, the calcining temperature is 1450 ℃, and the calcining time is 3 hours.
5. SO with strontium titanate as sensitive electrode according to claim 1 2 A method for producing a sensor, characterized in that n (amount of total metal substance) in S3: n (citric acid): n (EDTA): n (NH) 4 NO 3 )=1:1.2:1:2。
6. SO with strontium titanate as sensitive electrode according to claim 1 2 The preparation method of the sensor is characterized in that the water bath heating temperature of the solution D in the S3-3 is 80 ℃, the drying temperature is 120 ℃, the calcining temperature is 900 ℃, and the calcining time is 3 hours.
7. SO with strontium titanate as sensitive electrode according to claim 1 2 The preparation method of the sensor is characterized in that S4 is used for preparing a sensitive electrode material SrTiO 3 Mixing with an organic carrier, continuously stirring for 24 h, uniformly mixing, coating the uniformly mixed product on a porous layer of YSZ solid electrolyte with a porous layer/compact layer double-layer structure by using a screen printer, and calcining for 3h at 900-1050 ℃.
8. SO with strontium titanate as sensitive electrode according to claim 1 2 The preparation method of the sensor is characterized in that the calcining temperature in S5 is 800 ℃, and the calcining time is 1h.
9. SO with strontium titanate as sensitive electrode according to any of claims 1-8 2 SO obtained by preparation method of sensor and taking strontium titanate as sensitive electrode 2 A sensor.
10. The method of claim 9 using strontium titanate as sensitive electrodePolar SO 2 The application of the sensor in sulfur dioxide detection.
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