CN107884446B - Ethanol gas sensor based on multi-element metal oxide sensitive material - Google Patents
Ethanol gas sensor based on multi-element metal oxide sensitive material Download PDFInfo
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Abstract
The invention relates to an ethanol gas sensor based on a multi-element metal oxide sensitive material, which is an indirectly heated structure and comprises: the device consists of an alumina ceramic tube, a sensitive material and a nichrome heating coil, wherein the outer surface of the alumina ceramic tube is provided with 2 parallel and separated annular gold electrodes, the sensitive material is coated on the surface of the ceramic tube, and the nichrome heating coil penetrates through the ceramic tube; the sensitive material is formed by mixing a sensitive material A and a sensitive material B, wherein the sensitive material A is ZnO nanofiber, and the sensitive material B is a ternary metal oxide CuZnSnO4And (3) a nanorod structure.
Description
Technical Field
The invention relates to the technical field of ethanol gas sensors, in particular to an ethanol gas sensor based on a multi-metal oxide sensitive material.
Background
Human beings have already stepped into a highly information-oriented society into the 21 st century. Sensor technology, as a leading-edge technology of modern technology, is one of three major pillars in the modern information industry. The variety of sensors is wide, and sensitive materials are the core of sensor manufacturing, and in recent years, with the continuous development of semiconductor materials, nano materials gradually exert advantages in the field of sensors. The types and the amount of gases used in the production process and gases generated in the production process are increased, wherein many gases are inflammable and explosive or toxic, and for the sake of safety, the gases have to be monitored in aspects of use, transportation, storage and the like, so that the gas sensor has wide application fields and wide application prospects.
ZnO and SnO2The material is the sensitive material of the gas sensor which is developed at the earliest time, and has excellent performance, however, the single metal oxide material has the defects of poor selectivity, high working temperature and the like. Researches show that the construction of the multi-metal oxide material is an effective way for improving the gas-sensitive characteristic of the sensor.
Disclosure of Invention
Based on the technical problems mentioned above, the present invention aims to provide an ethanol gas sensor based on a multi-metal oxide sensitive material, so as to solve the problems mentioned above.
The embodiment of the invention provides an ethanol gas sensor based on a multi-metal oxide sensitive material, which is characterized in thatThe gas sensor is indirectly hot type structure, includes: the device consists of an alumina ceramic tube, a sensitive material and a nichrome heating coil, wherein the outer surface of the alumina ceramic tube is provided with 2 parallel and separated annular gold electrodes, the sensitive material is coated on the surface of the ceramic tube, and the nichrome heating coil penetrates through the ceramic tube; the sensitive material is formed by mixing a sensitive material A and a sensitive material B, wherein the sensitive material A is ZnO nanofiber, and the sensitive material B is a ternary metal oxide CuZnSnO4And (3) a nanorod structure.
The technical scheme provided by the embodiment of the invention can have the following beneficial effects:
in the ethanol gas sensor, ZnO nano-fiber and CuZnSnO are mixed4The nano-rod is mixed to be used as a sensitive material, wherein the ZnO nano-fiber has a large specific surface area, the fiber has a microporous structure and can provide a good gas diffusion path, and in addition, CuZnSnO4The nano-rod is doped to increase the surface and interface states of the material, and simultaneously, the components cooperatively play a role different from that of a single material, so that the nano-rod has the comprehensive performance generated by the cooperative action of the components on the basis of keeping the independence of the materials, and the performance of the sensor is greatly improved.
Additional aspects and advantages of the invention will be set forth in part in the description which follows and, in part, will be obvious from the description, or may be learned by practice of the invention. It is to be understood that both the foregoing general description and the following detailed description are exemplary and explanatory only and are not restrictive of the invention, as claimed.
Drawings
The invention is further illustrated by means of the attached drawings, but the embodiments in the drawings do not constitute any limitation to the invention, and for a person skilled in the art, other drawings can be obtained on the basis of the following drawings without inventive effort.
Fig. 1 is a schematic structural diagram of a gas sensor according to an embodiment of the present invention.
Detailed Description
Reference will now be made in detail to the exemplary embodiments, examples of which are illustrated in the accompanying drawings. When the following description refers to the accompanying drawings, like numbers in different drawings represent the same or similar elements unless otherwise indicated. The embodiments described in the following exemplary embodiments do not represent all embodiments consistent with the present invention. Rather, they are merely examples of apparatus and methods consistent with certain aspects of the invention, as detailed in the appended claims.
The embodiment of the invention relates to an ethanol gas sensor based on a multi-element metal oxide sensitive material, as shown in figure 1, the gas sensor is of an indirectly heated type structure and comprises: the device consists of an alumina ceramic tube 12 with 2 parallel and discrete annular gold electrodes 11 on the outer surface, a sensitive material 13 coated on the surface of the ceramic tube 12 and a nichrome heating coil 14 penetrating through the ceramic tube 12, wherein each gold electrode 11 is connected with two platinum wire pins.
The sensitive material 13 is formed by mixing a sensitive material A and a sensitive material B, wherein the sensitive material A is ZnO nanofiber, and the sensitive material B is a ternary metal oxide CuZnSnO4A nanorod structure;
specifically, the ZnO nanofiber is prepared from polyvinyl alcohol and zinc nitrate by an electrostatic spinning method; the CuZnSnO4The nano-rod is formed by SnCl4·5H2O、Zn(NO3)2·6H2O、Cu(NO3)2·3H2Prepared by an O hydrothermal method.
In the sensitive material, the sensitive material A is ZnO nanofiber, and the sensitive material B is CuZnSnO4The technical proposal of the invention is to mix ZnO nano-fiber with CuZnSnO4The nano-rod is mixed to be used as a sensitive material, wherein the ZnO nano-fiber has a large specific surface area, the fiber has a microporous structure and can provide a good gas diffusion path, and in addition, CuZnSnO4The nano-rod is doped to increase the surface and interface states of the material, and simultaneously, the components cooperatively play a role different from that of a single material, so that the nano-rod has the comprehensive performance generated by the cooperative action of the components on the basis of keeping the independence of the materials, and the performance of the sensor is greatly improved.
Preferably, in the sensitive material, the mass ratio of the sensitive material A to the sensitive material B is 5: 1.
The mass ratio of the sensitive material A, B in the sensitive materials is controlled to be 5:1, so that the detection sensitivity of the ethanol gas sensor to ethanol is greatly improved, and unexpected technical effects are achieved.
In the sensitive material, the sensitive material A is ZnO nanofiber, the ZnO nanofiber is prepared by an electrostatic spinning method, and the average diameter of the ZnO nanofiber is 230 nm.
ZnO is an n-type wide bandgap semiconductor material with a wurtzite structure, has unique performances in the aspects of optics, electrics, catalysis and the like, and has practical application in the fields of sensors, solar cells, lithium batteries, catalysis and the like. Particularly in the context of gas sensors. At present, the research on ZnO-based gas sensors mainly adopts the ways of nanostructure control, doping, compounding and the like to improve the performance; meanwhile, electrostatic spinning is a simple and convenient method for preparing nano materials, but the technical scheme of preparing zinc oxide nano fibers as sensitive materials by adopting the electrostatic spinning method in the current technical scheme of the zinc oxide gas sensor is few; in the technical scheme of the invention, ZnO nano-fiber prepared by an electrostatic spinning method and CuZnSnO are mixed4The nano-rod is mixed to be used as a sensitive material of the sensor, and the ZnO nano-fiber has large specific surface area and a microporous structure, so that CuZnSnO can be ensured4The nano-rod is fully fused into the ZnO nano-fiber, so that the obtained sensor has the advantages of high sensitivity and quick response.
When the average diameter of the ZnO nano-fiber is 230nm, the detection sensitivity of the ethanol gas sensor to ethanol is greatly improved, and unexpected technical effects are achieved.
In the above sensitive material, the sensitive material B is CuZnSnO4And the nanorod has the diameter of 40nm and the length of 120 nm.
As described above, ZnO is one of the most developed metal oxide gas-sensitive materials, but in practical use, the material has problems of poor selectivity, high operating temperature, and the like. The doping is the main method for improving the sensitivity performance of the material, and the inventionCuZnSnO4The nanorod combines Zn, Sn and Cu elements to construct a ternary metal oxide composite material which has good physical and chemical stability, and the Zn, Sn and Cu elements are combined to show good selectivity to gas.
The preparation process of the sensitive material A comprises the following steps:
step 1, firstly, respectively taking 4.6g and 50g of polyvinyl alcohol and distilled water, mixing to obtain a mixed solution, violently stirring at 80 ℃, uniformly mixing, then adding zinc nitrate into the mixed solution, and continuously stirring for 4 hours to obtain a mixed solution A;
step 2, filling the mixed solution A into a spinneret tube, using a copper wire as a positive electrode and an aluminum foil as a negative electrode of a receiving plate, carrying out electrostatic spinning with the applied voltage of 16kV and the distance between a spinneret and the receiving plate of 19.5cm to obtain composite fibers, and drying the composite fibers in a vacuum drying oven for later use;
and 3, sintering the dried composite fiber in a high-temperature resistance furnace in the air atmosphere, calcining for 5 hours at 800 ℃ to remove the high-molecular polyvinyl alcohol, and naturally cooling to obtain the ZnO nanofiber.
The preparation process of the sensitive material B comprises the following steps:
step 1, taking Cu (NO)3)2·3H2O、Zn(NO3)2·6H2O、SnCl4·5H2O is 10mmol, the O is mixed and dissolved in deionized water to form a mixed solution, and the mixed solution is magnetically stirred for 2 hours;
step 2, adding 0.2M NaOH solution into the mixed solution, adjusting the pH value to 12 to obtain a mixed solution B, then transferring the mixed solution B into an autoclave, and reacting for 14 hours at 200 ℃;
step 3, after the reaction is finished, taking the mixed solution B out of the reaction kettle, and naturally cooling at room temperature; then centrifuging and washing the reaction product, drying at 80 deg.C for 20h, and finally drying the powder in O2Annealing for 2h under the condition of 516 ℃ in the atmosphere to obtain a final product, namely CuZnSnO4And (4) nanorods.
Further, the ZnO nanofiber and CuZnSnO thus obtained were used4And uniformly mixing the nanorods according to the mass ratio of 5:1, adding ethanol, preparing into paste slurry, coating the paste slurry on a ceramic tube, and drying for 5 hours at 96 ℃ after the slurry is solidified to obtain a sensitive material 13, thereby obtaining the gas sensor.
Comparative example 1
An ethanol gas sensor based on a multi-element metal oxide sensitive material, wherein the gas sensor is of an indirectly heated structure and comprises: the device consists of an alumina ceramic tube 12 with 2 parallel and discrete annular gold electrodes 11 on the outer surface, a sensitive material 13 coated on the surface of the ceramic tube 12 and a nichrome heating coil 14 penetrating through the ceramic tube 12, wherein each gold electrode 11 is connected with two platinum wire pins.
The sensitive material 13 is formed by mixing a sensitive material A and a sensitive material B, wherein the sensitive material A is ZnO nanofiber, and the sensitive material B is a ternary metal oxide CuZnSnO4A nanorod structure; in the sensitive material, the mass ratio of the sensitive material A to the sensitive material B is 5: 1.
Specifically, the ZnO nanofiber is prepared from polyvinyl alcohol and zinc nitrate by an electrostatic spinning method, and the average diameter of the ZnO nanofiber is 230 nm.
The preparation process of the sensitive material A comprises the following steps:
step 1, firstly, respectively taking 4.6g and 50g of polyvinyl alcohol and distilled water, mixing to obtain a mixed solution, violently stirring at 80 ℃, uniformly mixing, then adding zinc nitrate into the mixed solution, and continuously stirring for 4 hours to obtain a mixed solution A;
step 2, filling the mixed solution A into a spinneret tube, using a copper wire as a positive electrode and an aluminum foil as a negative electrode of a receiving plate, carrying out electrostatic spinning with the applied voltage of 16kV and the distance between a spinneret and the receiving plate of 19.5cm to obtain composite fibers, and drying the composite fibers in a vacuum drying oven for later use;
and 3, sintering the dried composite fiber in a high-temperature resistance furnace in the air atmosphere, calcining for 5 hours at 800 ℃ to remove the high-molecular polyvinyl alcohol, and naturally cooling to obtain the ZnO nanofiber.
The CuZnSnO4The nano-rod is formed by SnCl4·5H2O、Zn(NO3)2·6H2O、Cu(NO3)2·3H2The nanorod prepared by the O hydrothermal method has the diameter of 40nm and the length of 120 nm.
The preparation process of the sensitive material B comprises the following steps:
step 1, taking Cu (NO)3)2·3H2O、Zn(NO3)2·6H2O、SnCl4·5H2O is 10mmol, the O is mixed and dissolved in deionized water to form a mixed solution, and the mixed solution is magnetically stirred for 2 hours;
step 2, adding 0.2M NaOH solution into the mixed solution, adjusting the pH value to 12 to obtain a mixed solution B, then transferring the mixed solution B into an autoclave, and reacting for 14 hours at 200 ℃;
step 3, after the reaction is finished, taking the mixed solution B out of the reaction kettle, and naturally cooling at room temperature; then centrifuging and washing the reaction product, drying at 80 deg.C for 20h, and finally drying the powder in O2Annealing for 2h under the condition of 516 ℃ in the atmosphere to obtain a final product, namely CuZnSnO4And (4) nanorods.
Further, the ZnO nanofiber and CuZnSnO thus obtained were used4And uniformly mixing the nanorods according to the mass ratio of 5:1, adding ethanol, preparing into paste slurry, coating the paste slurry on a ceramic tube, and drying for 5 hours at 96 ℃ after the slurry is solidified to obtain a sensitive material 13, thereby obtaining the gas sensor.
The working temperature of the metal oxide semiconductor sensitive material is an important parameter for measuring the performance of the sensor, and the testing temperature when the responsiveness of the gas sensor to the testing gas reaches the maximum is defined as the optimal working temperature.
For this purpose, the sensors obtained above were subjected to a test of sensitivity to 100ppm of ethanol at 200 ℃, 230 ℃, 260 ℃, 290 ℃ and 320 ℃ respectively, and the results are shown in the following table:
| operating temperature | 200℃ | 230℃ | 260℃ | 290℃ | 320℃ |
| Sensitivity of the probe | 6 | 17 | 31 | 43 | 19 |
It is seen that the sensitivity of the sensor of the present invention increases with increasing temperature, reaching a maximum at 290 ℃ and then begins to decrease with further increases in temperature.
In order to test the selectivity of the sensor of the present invention to ethanol gas, the sensor was placed in 100ppm of ethanol, methanol, acetone, and toluene at 290 ℃ to test the sensitivity, and the results are as follows:
| type of gas | Ethanol | Methanol | Acetone (II) | Toluene |
| Sensitivity of the probe | 42 | 35 | 16 | 19 |
It can be seen that, at the same temperature, the sensor has the highest sensitivity to ethanol and good selectivity to ethanol in the ethanol, methanol, acetone and toluene.
Comparative example 2
An ethanol gas sensor based on a multi-element metal oxide sensitive material, wherein the gas sensor is of an indirectly heated structure and comprises: the device consists of an alumina ceramic tube 12 with 2 parallel and discrete annular gold electrodes 11 on the outer surface, a sensitive material 13 coated on the surface of the ceramic tube 12 and a nichrome heating coil 14 penetrating through the ceramic tube 12, wherein each gold electrode 11 is connected with two platinum wire pins.
The sensitive material 13 is formed by mixing a sensitive material A and a sensitive material B, wherein the sensitive material A is ZnO nanofiber, and the sensitive material B is a ternary metal oxide CuZnSnO4A nanorod structure; in the sensitive material, the mass ratio of the sensitive material A to the sensitive material B is 3: 1.
Specifically, the ZnO nanofiber is prepared from polyvinyl alcohol and zinc nitrate by an electrostatic spinning method, and the average diameter of the ZnO nanofiber is 130 nm.
The preparation process of the sensitive material A comprises the following steps:
step 1, firstly, respectively taking 4.6g and 50g of polyvinyl alcohol and distilled water, mixing to obtain a mixed solution, violently stirring at 80 ℃, uniformly mixing, then adding zinc nitrate into the mixed solution, and continuously stirring for 4 hours to obtain a mixed solution A;
step 2, filling the mixed solution A into a spinneret tube, using a copper wire as a positive electrode and an aluminum foil as a negative electrode of a receiving plate, carrying out electrostatic spinning with the applied voltage of 14kV and the distance between the spinneret and the receiving plate of 18.4cm to obtain composite fibers, and drying the composite fibers in a vacuum drying oven for later use;
and 3, sintering the dried composite fiber in a high-temperature resistance furnace in the air atmosphere, calcining for 5 hours at 800 ℃ to remove the high-molecular polyvinyl alcohol, and naturally cooling to obtain the ZnO nanofiber.
The CuZnSnO4The nano-rod is formed by SnCl4·5H2O、Zn(NO3)2·6H2O、Cu(NO3)2·3H2The nanorod prepared by the O hydrothermal method has the diameter of 40nm and the length of 120 nm.
The preparation process of the sensitive material B comprises the following steps:
step 1, taking Cu (NO)3)2·3H2O、Zn(NO3)2·6H2O、SnCl4·5H2O is 10mmol, the O is mixed and dissolved in deionized water to form a mixed solution, and the mixed solution is magnetically stirred for 2 hours;
step 2, adding 0.2M NaOH solution into the mixed solution, adjusting the pH value to 12 to obtain a mixed solution B, then transferring the mixed solution B into an autoclave, and reacting for 14 hours at 200 ℃;
step 3, after the reaction is finished, taking the mixed solution B out of the reaction kettle, and naturally cooling at room temperature; then centrifuging and washing the reaction product, drying at 80 deg.C for 20h, and finally drying the powder in O2Annealing for 2h under the condition of 516 ℃ in the atmosphere to obtain a final product, namely CuZnSnO4And (4) nanorods.
Further, the ZnO nanofiber and CuZnSnO thus obtained were used4The nano rods are uniformly mixed according to the mass ratio of 3:1, and then the B is addedAnd (3) preparing alcohol into pasty slurry, coating the pasty slurry on a ceramic tube, and drying for 5 hours at 96 ℃ after the slurry is solidified to obtain the sensitive material 13 and further obtain the gas sensor.
The working temperature of the metal oxide semiconductor sensitive material is an important parameter for measuring the performance of the sensor, and the testing temperature when the responsiveness of the gas sensor to the testing gas reaches the maximum is defined as the optimal working temperature.
For this purpose, the sensors obtained above were subjected to a test of sensitivity to 100ppm of ethanol at 200 ℃, 230 ℃, 260 ℃, 290 ℃ and 320 ℃ respectively, and the results are shown in the following table:
| operating temperature | 200℃ | 230℃ | 260℃ | 290℃ | 320℃ |
| Sensitivity of the probe | 4 | 14 | 27 | 39 | 15 |
It is seen that the sensitivity of the sensor of the present invention increases with increasing temperature, reaching a maximum at 290 ℃ and then begins to decrease with further increases in temperature.
In order to test the selectivity of the sensor of the present invention to ethanol gas, the sensor was placed in 100ppm of ethanol, methanol, acetone, and toluene at 290 ℃ to test the sensitivity, and the results are as follows:
| type of gas | Ethanol | Methanol | Acetone (II) | Toluene |
| Sensitivity of the probe | 27 | 21 | 13 | 12 |
It can be seen that the sensor has the highest sensitivity to ethanol but not the good selectivity to ethanol in the above ethanol, methanol, acetone, toluene at the same temperature.
By comparing the comparative example 1 with the comparative example 2, it can be seen that, in the sensitive material of the sensor, the mass ratio of the sensitive material A, B and the average diameter of the ZnO nanofibers have a great influence on the sensitivity of the sensor relative to the ethanol gas; when the mass ratio of the sensitive material A, B is controlled to be 5:1, and the average diameter of the ZnO nanofiber is 230nm, the ZnO nanofiber has good sensitivity and selectivity on ethanol.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, but rather as the subject matter of the invention is to be construed in all aspects and as broadly as possible, and all changes, equivalents and modifications that fall within the true spirit and scope of the invention are therefore intended to be embraced therein.
Claims (7)
1. An ethanol gas sensor based on a multi-element metal oxide sensitive material, wherein the gas sensor is of an indirectly heated structure and comprises: the device consists of an alumina ceramic tube, a sensitive material and a nichrome heating coil, wherein the outer surface of the alumina ceramic tube is provided with 2 parallel and separated annular gold electrodes, the sensitive material is coated on the surface of the ceramic tube, and the nichrome heating coil penetrates through the ceramic tube; the method is characterized in that the sensitive material is formed by mixing a sensitive material A and a sensitive material B, wherein the sensitive material A is ZnO nanofiber, and the sensitive material B is ternary metal oxide CuZnSnO4A nanorod structure; in the sensitive material, the mass ratio of the sensitive material A to the sensitive material B is 5: 1.
2. The ethanol gas sensor according to claim 1, wherein the ZnO nanofiber is prepared by electrospinning polyvinyl alcohol and zinc nitrate.
3. The ethanol gas sensor according to claim 2, wherein the ZnO nanofibers have an average diameter of 230 nm.
4. The ethanol gas sensor according to claim 3, wherein the sensitive material A is prepared by the following steps: step 1, firstly, respectively taking 4.6g and 50g of polyvinyl alcohol and distilled water, mixing to obtain a mixed solution, violently stirring at 80 ℃, uniformly mixing, then adding zinc nitrate into the mixed solution, and continuously stirring for 4 hours to obtain a mixed solution A; step 2, filling the mixed solution A into a spinneret tube, using a copper wire as a positive electrode and an aluminum foil as a negative electrode of a receiving plate, carrying out electrostatic spinning with the applied voltage of 16kV and the distance between a spinneret and the receiving plate of 19.5cm to obtain composite fibers, and drying the composite fibers in a vacuum drying oven for later use; and 3, sintering the dried composite fiber in a high-temperature resistance furnace in the air atmosphere, calcining for 5 hours at 800 ℃ to remove the high-molecular polyvinyl alcohol, and naturally cooling to obtain the ZnO nanofiber.
5. The ethanol gas sensor according to claim 1, wherein the CuZnSnO4The nano-rod is formed by SnCl4·5H2O、Zn(NO3)2·6H2O、Cu(NO3)2·3H2Prepared by an O hydrothermal method.
6. The ethanol gas sensor according to claim 5, wherein the CuZnSnO4The diameter of the nanorod is 40-60 nm, and the length of the nanorod is 120 nm.
7. The ethanol gas sensor according to claim 6, wherein the sensitive material B is prepared by the following steps: step 1, taking Cu (NO)3)2·3H2O、Zn(NO3)2·6H2O、SnCl4·5H2O is 10mmol, the O is mixed and dissolved in deionized water to form a mixed solution, and the mixed solution is magnetically stirred for 2 hours; step 2, adding 0.2M NaOH solution into the mixed solution, adjusting the pH value to 12 to obtain a mixed solution B, then transferring the mixed solution B into an autoclave, and reacting for 14 hours at 200 ℃; step 3, after the reaction is finished, taking the mixed solution B out of the reaction kettle, and naturally cooling at room temperature; then centrifuging and washing the reaction product, drying at 80 deg.C for 20h, and finally drying the powder in O2Annealing for 2h under the condition of 516 ℃ in the atmosphere to obtain a final product, namely CuZnSnO4And (4) nanorods.
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