CN114137038A - Preparation method of porous indium oxide-based ethanol gas sensor and ethanol gas sensor - Google Patents
Preparation method of porous indium oxide-based ethanol gas sensor and ethanol gas sensor Download PDFInfo
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- CN114137038A CN114137038A CN202111281228.9A CN202111281228A CN114137038A CN 114137038 A CN114137038 A CN 114137038A CN 202111281228 A CN202111281228 A CN 202111281228A CN 114137038 A CN114137038 A CN 114137038A
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- indium oxide
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
- G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
- G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
- G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
- G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
- G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
Abstract
The invention provides a preparation method of a porous indium oxide-based ethanol gas sensor and the ethanol gas sensor, comprising the following steps: step S1: preparing a gold nanoparticle-loaded porous indium oxide nano composite ethanol sensitive material; step S2: preparing a gas sensor element with an indirectly heated ceramic tube structure, wherein the ceramic tube structure is provided with a gold electrode; step S3: and coating the porous indium oxide nano composite ethanol sensitive material on a gold electrode with a ceramic tube structure, thereby forming the gold nanoparticle-loaded porous indium oxide-based ethanol gas sensor. According to the invention, the catalytic action of noble metal is utilized, the porous morphology of the surface of the prepared pure indium oxide nano material is combined, the sensitivity of the pure indium oxide nano material to ethanol gas is improved, and meanwhile, the selectivity of the pure indium oxide nano material to ethanol gas is enhanced by the loading of gold nanoparticles.
Description
Technical Field
The invention relates to the field of preparation technology and application of a metal oxide semiconductor thin film material with special functions, in particular to a preparation method of an ethanol gas sensor taking a gold-loaded indium oxide composite semiconductor material as a gas sensitive material and an indirectly heated ceramic tube as a sensing device and the ethanol gas sensor.
Background
Ethanol is a flammable and explosive gas and has been widely used in various applications, particularly in biomedical, laboratory, etc. The long-term contact with the ethanol gas can cause the problems of skin irritation, traffic safety, central nervous system inhibition and the like. Therefore, in order to enable real-time monitoring, the development of an efficient and low-cost ethanol gas sensor is a research hotspot.
At present, many researches on indium oxide-based gas sensors are dedicated to improving the appearance and structure of indium oxide materials, so as to achieve the purpose of improving the sensing performance of indium oxide-based gas sensors. However, original In2O3The defects of poor selectivity, insufficient sensitivity and the like of the nano material limit In2O3Application to gas-based sensors. In addition to structural optimization, lattice doping, construction of heterojunctions, and surface loading are considered to be effective methods for improving the selectivity and sensitivity of metal oxide semiconductors.
Disclosure of Invention
The method aims to solve the problems of low sensitivity, long response time and recovery time and high power consumption of the gas sensor prepared by the traditional pure indium oxide nano semiconductor material. The invention provides a preparation method of a high-sensitivity gold nanoparticle-loaded porous indium oxide-based ethanol gas sensor. The method comprises the following steps of selecting proper process steps, and preparing the gas-sensitive material from the gold-loaded mesoporous indium oxide nanocomposite prepared by a hydrothermal method to prepare the indirectly heated ceramic tube gas-sensitive sensor element.
The preparation method of the porous indium oxide-based ethanol gas sensor provided by the invention comprises the following steps:
step S1: preparing a gold nanoparticle-loaded porous indium oxide nano composite ethanol sensitive material;
step S2: preparing a gas sensor element with an indirectly heated ceramic tube structure, wherein the ceramic tube structure is provided with a gold electrode;
step S3: and coating the porous indium oxide nano composite ethanol sensitive material on a gold electrode with a ceramic tube structure, thereby forming the gold nanoparticle-loaded porous indium oxide-based ethanol gas sensor.
Preferably, the preparation of the porous indium oxide composite ethanol sensitive material comprises the following steps:
In2O3preparing porous nano microspheres;
in accordance with2O3And preparing the gold-loaded indium oxide nano composite structure by using the porous nano microspheres.
Preferably, the In2O3The preparation of the porous nano-microsphere comprises the following steps:
adding InCl3·4H2Dissolving O in deionized water, stirring to form a mixed solution, and dropwise adding ammonia water and hydrochloric acid to adjust the pH value of the mixed solution in the stirring process;
loading the mixed solution into an autoclave, reacting under a hydrothermal condition, naturally cooling the autoclave to room temperature, collecting the prepared precipitate by centrifugation, and washing with deionized water and absolute ethyl alcohol for several times to remove unreacted InCl3·4H2O；
Drying the obtained precipitate to obtain white in (OH)3A precursor;
finally, in (OH)3And calcining the precursor in a tubular furnace in the air atmosphere to obtain the indium oxide nano material.
Preferably, In2O3The preparation of the indium oxide nano composite ethanol sensitive material loaded with gold by the porous nano microspheres comprises the following steps:
in is mixed with2O3Dispersing the powder, the chloroauric acid solution and polyvinylpyrrolidone into deionized water by ultrasonic, and slowly dripping the sodium citrate solution into the solution under continuous stirring to reduce the chloroauric acid into gold nanoparticles;
then continuously heating and stirring, collecting precipitate by centrifugation, washing with deionized water and ethanol, and drying;
and calcining the obtained sample in air to obtain the gold nanoparticle-loaded porous indium oxide ethanol sensitive material.
Preferably, the In2O3InCl in preparation of porous nano-microsphere3·4H2The concentration of O is 1 mmol/L; the pH of the mixed solution was adjusted to 11 by ammonia and hydrochloric acid.
Preferably, the chloroauric acid solution in the preparation of the indium oxide nano composite ethanol sensitive material is 0.01 mol/L.
Preferably, Au accounts for In mass fraction of 0.5 wt% In the preparation of the gold-loaded indium oxide nanocomposite ethanol sensitive material2O3The substrate is loaded.
Preferably, the step S3 includes the steps of:
mixing the synthesized porous indium oxide nano composite ethanol sensitive material and terpineol in a mortar to form homogeneous paste, and then coating the homogeneous paste on the surface of a ceramic tube structure to form a film;
after the film is dried at room temperature, inserting a Ni-Cr alloy coil as a heater into a ceramic tube and aging at 300 ℃ for at least 24 hours;
and finally, fixing the ceramic tube and the hexagonal base by welding to finish the preparation of the ethanol gas sensor based on the indirectly heated ceramic tube.
Preferably, the film coated on the surface of the ceramic tube structure has a thickness of 50-70 μm, a core length of 7 mm and an outer diameter of 1.5 mm; a pair of gold electrodes is attached to two ends of the surface of the ceramic tube, and each electrode is provided with a platinum wire.
According to the ethanol gas sensor provided by the invention, the preparation method of the porous indium oxide-based ethanol gas sensor is adopted for preparation.
Compared with the prior art, the invention has the following beneficial effects:
according to the invention, the catalytic action of noble metal is utilized, the porous morphology of the surface of the prepared pure indium oxide nano material is combined, the sensitivity of the pure indium oxide nano material to ethanol gas is improved, and meanwhile, the selectivity of the pure indium oxide nano material to ethanol gas is enhanced by the loading of gold nanoparticles.
Drawings
Other features, objects and advantages of the invention will become more apparent upon reading of the detailed description of non-limiting embodiments with reference to the following drawings:
FIG. 1 is a flow chart illustrating the steps of a method for fabricating a porous indium oxide-based ethanol gas sensor according to an embodiment of the present invention;
FIG. 2 is an X-ray diffraction pattern of pure indium oxide and gold-loaded porous indium oxide nanomaterials from an example of the invention;
FIG. 3 is a scanning electron micrograph of a gold-loaded porous indium oxide nanomaterial in an embodiment of the present invention;
FIG. 4 is a transmission electron micrograph of a gold-loaded porous indium oxide nanomaterial in an embodiment of the present invention;
FIG. 5 is a graph of the specific surface area and pore size of gold-loaded porous indium oxide nanomaterials in an embodiment of the invention;
FIG. 6 is a comparison of sensitivity curves of pure indium oxide material and gold-loaded porous indium oxide nanomaterial under different concentrations of ethanol in the examples of the present invention.
Detailed Description
The present invention will be described in detail with reference to specific examples. The following examples will assist those skilled in the art in further understanding the invention, but are not intended to limit the invention in any way. It should be noted that variations and modifications can be made by persons skilled in the art without departing from the spirit of the invention. All falling within the scope of the present invention.
The method is an effective method for effectively improving the selectivity and the sensitivity of the metal oxide semiconductor by loading the noble metal on the surface of the sensitive material, and in the sensing process, the loaded noble metal plays a role in catalysis, so that the chemical reaction between the gas-sensitive sensing material and the gas to be detected is enhanced.
In based on noble loading2O3Sensor and pure In2O3Compared with the sensor, the sensor has the advantages of low power consumption, high response and short response and recovery time. Noble metal nanoparticles supported In2O3Can promote the conversion of oxygen molecules and the reaction rate between oxygen ions and the molecules of the gas to be detected, and finally can improve the gas-sensitive performance
Fig. 1 is a flow chart illustrating steps of a method for manufacturing a porous indium oxide-based ethanol gas sensor according to an embodiment of the present invention, and as shown in fig. 1, the method for manufacturing a porous indium oxide-based ethanol gas sensor according to the present invention includes the following steps:
step S1: preparing a gold nanoparticle-loaded porous indium oxide nano composite ethanol sensitive material;
step S2: preparing a gas sensor element with an indirectly heated ceramic tube structure, wherein the ceramic tube structure is provided with a gold electrode;
step S3: and coating the porous indium oxide nano composite ethanol sensitive material on a gold electrode with a ceramic tube structure, thereby forming the gold nanoparticle-loaded porous indium oxide-based ethanol gas sensor.
The preparation of the gold nanoparticle-loaded porous indium oxide nano composite ethanol sensitive material comprises the following steps:
pure In2O3Preparing porous nano microspheres: 1mmol (0.293g) of InCl3·4H2Dissolving O in 35ml of deionized water, stirring for 15 minutes to form a uniform mixed solution, adjusting the pH value of the mixed solution to 11 by dropwise adding ammonia water and hydrochloric acid during stirring, and magnetically stirring for 2 hours. The uniformly stirred mixed solution was charged into a 50 ml teflon-lined stainless steel autoclave, reacted at 180 ℃ for 24 hours under hydrothermal conditions, the autoclave was naturally cooled to room temperature, and then the prepared precipitate was collected by centrifugation and washed with deionized water and absolute ethanol several times to remove unreacted raw materials. The obtained precipitate was dried at 80 ℃ for 2 hours to obtain white in (OH)3And (3) precursor. Finally, in (OH)3Calcining the precursor In a tube furnace at 300 ℃ for 2 hours In the air atmosphere to obtain light yellow pure In2O3And (3) nano materials.
In accordance with2O3The preparation of the indium oxide nano composite ethanol sensitive material loaded with gold by the porous nano microspheres comprises the following steps:
50mg of the pure In obtained2O3Powder, 1mL of chloroauric acid (HAuCl) at a concentration of 0.01mol/L4) Solution, a certain amount of polyvinylpyrrolidoneKetone (PVP) was dispersed by sonication into 15 mL of deionized water for 15 minutes, and 0.1mL of 0.1mol/L sodium citrate solution was slowly added dropwise to the above solution under continuous stirring to reduce chloroauric acid to gold nanoparticles. Then, stirring was continued with heating for 30 minutes, and the precipitate was collected by centrifugation, washed several times with water and ethanol, and dried at 80 ℃. And finally, calcining the obtained sample in air at 300 ℃ for 30 minutes to obtain the gold nanoparticle-loaded porous indium oxide gas-sensitive material.
The method for preparing the ethanol gas sensor with the indirectly heated ceramic tube structure comprises the following steps
Mixing and grinding 0.15g of gold nanoparticle-loaded porous indium oxide nano powder and 0.3ml of terpineol in an agate mortar to form homogeneous paste; uniformly coating a layer of paste on the outer surface of a ceramic tube core with two annular gold electrodes and four Pt leads, and putting the ceramic tube core into a muffle furnace for annealing at 100 ℃ for 20 min; and (3) passing an Ni-Cr heating wire through the inside of the ceramic tube, welding the Ni-Cr heating wire and four Pt electrode wires on the six-pin base together, installing an outer cover net cap on the six-pin base, and aging the prepared element by using an aging table for at least 24 hours to prepare the indirectly heated ceramic tube gas sensor element.
To prepare pure In2O3The results of X-ray diffraction, scanning electron microscope, transmission electron microscope and BET test on the porous nano-microsphere and gold-loaded indium oxide nanocomposite are shown in FIGS. 1 to 4, wherein the gold-loaded indium oxide nanoparticles have a size of 50 to 150nm and a specific surface area of 31.9m2The primary pore size is concentrated at 14nm and the size of the gold nanoparticles is 19 nm.
Detection dynamic sensitivity curves for different concentrations of ethanol gas at the optimum operating temperature as shown in fig. 5, the gas response for 100ppm of ethanol gas at the optimum operating temperature of 220 ℃ was 85.7.
The preparation method of the high-sensitivity gold nanoparticle-loaded porous indium oxide-based ethanol gas sensor provided by the embodiment of the invention comprises two steps of synthesis, and the specific steps comprise: firstly, preparing a porous indium oxide nano microsphere gas-sensitive material by taking indium chloride as a raw material and ammonia water and hydrochloric acid as solution pH value regulators through hydrothermal reaction and calcination treatment; and secondly, loading gold nanoparticles on the surface of the porous indium oxide nanospheres through in-situ reduction reaction by using the prepared porous indium oxide and chloroauric acid as raw materials and sodium citrate as a surfactant, and finally obtaining the gold nanoparticle-loaded porous indium oxide nanosphere gas-sensitive material. Through reasonable regulation and control of the hydrothermal temperature and the calcining temperature and the loading of the gold nanoparticles, the ethanol gas sensor has ultrahigh sensitivity to ethanol gas at a lower working temperature, and the selectivity and the stability are relatively excellent. The response value of the ethanol gas sensor to 100ppm of ethanol gas at the optimal working temperature is 85.7. The method has the advantages that the catalytic action of noble metal is utilized, the surface porous morphology of the prepared pure indium oxide nano material is combined, the sensitivity of the pure indium oxide nano material to ethanol gas is improved, and meanwhile, the selectivity of the pure indium oxide nano material to the ethanol gas is enhanced by the loading of gold nano particles.
The foregoing description of specific embodiments of the present invention has been presented. It is to be understood that the present invention is not limited to the specific embodiments described above, and that various changes and modifications may be made by one skilled in the art within the scope of the appended claims without departing from the spirit of the invention.
Claims (10)
1. A preparation method of a porous indium oxide-based ethanol gas sensor is characterized by comprising the following steps:
step S1: preparing a gold nanoparticle-loaded porous indium oxide nano composite ethanol sensitive material;
step S2: preparing a gas sensor element with an indirectly heated ceramic tube structure, wherein the ceramic tube structure is provided with a gold electrode;
step S3: and coating the porous indium oxide nano composite ethanol sensitive material on a gold electrode with a ceramic tube structure, thereby forming the gold nanoparticle-loaded porous indium oxide-based ethanol gas sensor.
2. The method for preparing a porous indium oxide-based ethanol gas sensor according to claim 1, wherein the preparation of the porous indium oxide composite ethanol sensitive material comprises the following steps:
In2O3preparing porous nano microspheres;
in accordance with2O3And preparing the gold-loaded indium oxide nano composite structure by using the porous nano microspheres.
3. The method of manufacturing a porous indium oxide-based ethanol gas sensor according to claim 2, wherein the In is2O3The preparation of the porous nano-microsphere comprises the following steps:
adding InCl3·4H2Dissolving O in deionized water, stirring to form a mixed solution, and dropwise adding ammonia water and hydrochloric acid to adjust the pH value of the mixed solution in the stirring process;
loading the mixed solution into an autoclave, reacting under a hydrothermal condition, naturally cooling the autoclave to room temperature, collecting the prepared precipitate by centrifugation, and washing with deionized water and absolute ethyl alcohol for several times to remove unreacted InCl3·4H2O；
Drying the obtained precipitate to obtain white in (OH)3A precursor;
finally, in (OH)3And calcining the precursor in a tubular furnace in the air atmosphere to obtain the indium oxide nano material.
4. The method of manufacturing a porous indium oxide-based ethanol gas sensor according to claim 2, wherein the In-based gas sensor is manufactured according to In2O3The preparation of the indium oxide nano composite ethanol sensitive material loaded with gold by the porous nano microspheres comprises the following steps:
in is mixed with2O3Dispersing the powder, the chloroauric acid solution and polyvinylpyrrolidone into deionized water by ultrasonic, and slowly dripping the sodium citrate solution into the solution under continuous stirring to reduce the chloroauric acid into gold nanoparticles;
then continuously heating and stirring, collecting precipitate by centrifugation, washing with deionized water and ethanol, and drying;
and calcining the obtained sample in air to obtain the gold nanoparticle-loaded porous indium oxide ethanol sensitive material.
5. The method for manufacturing a porous indium oxide-based ethanol gas sensor according to claim 3, wherein the In is2O3InCl in preparation of porous nano-microsphere3·4H2The concentration of O is 1 mmol/L; the pH of the mixed solution was adjusted to 11 by ammonia and hydrochloric acid.
6. The method for preparing a porous indium oxide-based ethanol gas sensor according to claim 4, wherein the chloroauric acid solution is 0.01mol/L in the preparation of the indium oxide nanocomposite ethanol sensitive material.
7. The method of claim 4, wherein Au is added to In at a mass fraction of 0.5 wt% In the preparation of the gold-loaded indium oxide nanocomposite ethanol-sensitive material2O3The substrate is loaded.
8. The method for manufacturing a porous indium oxide-based ethanol gas sensor according to claim 1, wherein the step S3 includes the steps of:
mixing the synthesized porous indium oxide nano composite ethanol sensitive material and terpineol in a mortar to form homogeneous paste, and then coating the homogeneous paste on the surface of a ceramic tube structure to form a film;
after the film is dried at room temperature, inserting a Ni-Cr alloy coil as a heater into a ceramic tube and aging at 300 ℃ for at least 24 hours;
and finally, fixing the ceramic tube and the hexagonal base by welding to finish the preparation of the ethanol gas sensor based on the indirectly heated ceramic tube.
9. The method of claim 8, wherein the thin film coated on the surface of the ceramic tube structure has a thickness of 50-70 μm, a core of the ceramic tube has a length of 7 mm and an outer diameter of 1.5 mm; a pair of gold electrodes is attached to two ends of the surface of the ceramic tube, and each electrode is provided with a platinum wire.
10. An ethanol gas sensor, characterized by being produced by the production method for a porous indium oxide-based ethanol gas sensor according to any one of claims 1 to 9.
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