CN109470744B - Acetone sensor based on composite sensitive material, preparation method and application thereof - Google Patents
Acetone sensor based on composite sensitive material, preparation method and application thereof Download PDFInfo
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- 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
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Abstract
Based on MoO3/In2O3The acetone sensor of composite sensitive material is a indirectly heated structure, which is composed of a ceramic tube substrate with two parallel, annular and mutually separated gold electrodes on the outer surface, and MoO coated on the outer surface of the ceramic tube and the gold electrodes3/In2O3The composite sensitive material and a nickel-chromium alloy heating coil arranged in the ceramic tube. When the sensor works, direct current is supplied to the nichrome heating coil to provide the working temperature of the sensor, and the work of measuring the concentration of acetone is realized by measuring the direct current resistance value between two gold electrodes in different atmospheres. In MoO3Compounding In on the basis of solid spheres2O3The hollow sphere structure is realized, the sensitivity to acetone is improved, the response recovery speed is high, the repeatability is good, and the method has a wide application prospect in the aspect of gas detection. The invention has the advantages of simple synthesis method, small volume, easy production and the like.
Description
Technical Field
The invention belongs to the technical field of semiconductor oxide gas sensors, and particularly relates to MoO based on one-step hydrothermal synthesis3/In2O3Composite sensitivityAn acetone sensor of material, a preparation method and application thereof.
Background
Acetone is one of the most representative Volatile Organic Compounds (VOCs) commonly used in explosives, plastics, paints, fibers, rubber, and other fields. However, due to its volatility, toxicity and flammability, acetone, when released in the atmosphere, pollutes the environment and causes harm to humans. When the acetone concentration is higher than 450mg/m3(173ppm), damage to the eyes, nose and central nervous system of the human body occurs. Therefore, in order to create a friendly environment and ensure human health, it is necessary to develop a gas sensor with rapid and selective acetone detection.
Gas sensors are receiving increasing attention for monitoring and detecting acetone gas in the atmospheric environment. They are considered to be excellent detection methods due to their ease of manufacture, low power consumption and low cost. Semiconductor oxides are increasingly used in gas sensors as an important gas sensitive material due to their unique physical and chemical properties. The sensing mechanism of a chemically-resistant gas sensor is related to the interaction between the oxygen species adsorbed on the surface of the gas-sensitive material and the target gas, and a change in its resistance occurs therewith. Various factors at the surface of the material, including crystal size, surface morphology and microstructure of the oxide semiconductor material, may play a particularly important role in affecting their sensing performance. In addition, the two gas-sensitive materials are combined, and the gas-sensitive materials can be further modified by utilizing the synergistic effect between the two gas-sensitive materials, so that better gas-sensitive characteristics are obtained.
Disclosure of Invention
The invention aims to provide a method based on MoO3/In2O3Acetone sensor made of composite sensitive material, preparation method of acetone sensor and MoO3/In2O3The composite sensitive material is in a hollow sphere structure.
In the invention, the MoO-based3/In2O3The acetone sensor of composite sensitive material is a indirectly heated structure, and its external surface is equipped with two parallel stripsAnd annular and mutually separated gold electrodes2O3Ceramic tube substrate coated with Al2O3MoO on the outer surface of ceramic tube and gold electrode3/In2O3Composite sensitive material and Al-doped composite material2O3A nichrome heating coil in the ceramic tube. When the sensor works, direct current is supplied to the nichrome heating coil to provide the working temperature of the sensor, and the function of measuring the concentration of acetone is realized by measuring the direct current resistance value between two gold electrodes in different atmospheres. The sensor with the tubular structure is simple in manufacturing process, small in size and beneficial to industrial mass production, and therefore has important application value. Wherein, MoO3/In2O3The composite sensitive material is prepared by the following steps:
(1) dissolving 0.48-0.5 g of sodium molybdate dihydrate, 0.38-1.52 g of indium nitrate hydrate, 0.6-0.7 g of thiourea and 0.45-0.5 g of citric acid in 70mL of mixed solution containing 50mL of deionized water and 20mL of absolute ethyl alcohol, and violently stirring for 30-60 min to form uniform solution;
(2) then transferring the solution obtained in the step (1) into a high-pressure hydrothermal kettle, and carrying out hydrothermal reaction for 20-30 h at the temperature of 180-200 ℃;
(3) after the reaction in the step (2) is finished, naturally cooling the high-pressure hydrothermal kettle to room temperature, collecting a reaction product, washing the reaction product with water, centrifugally washing the reaction product with deionized water and ethanol to remove impurity ions, drying the reaction product in the air at 70-90 ℃ for 10-20 hours, and finally calcining the reaction product at 450-500 ℃ for 2-5 hours to obtain MoO3/In2O3A composite sensitive material;
the invention relates to a method based on MoO3/In2O3The preparation method of the acetone sensor of the composite sensitive material comprises the following steps:
(1) get MoO3/In2O3The composite sensitive material and ethanol are mixed according to the mass ratio of 0.25-0.5 mg: 1mg of the mixture was mixed homogeneously to form a paste, and the paste was dipped with a fine brush to coat Al with two parallel, annular and mutually discrete gold electrodes on the surface2O3Outer surface of ceramic tube, making itCompletely covering the gold electrode, wherein the thickness of the obtained composite sensitive material is 15-30 mu m; al (Al)2O3The inner diameter of the ceramic tube is 0.6-0.8 mm, the outer diameter is 1.0-1.5 mm, and the length is 4-5 mm; the width of a single gold electrode is 0.4-0.5 mm, and the distance between two gold electrodes is 0.5-0.6 mm; a platinum wire lead is led out of the gold electrode, and the length of the platinum wire lead is 4-6 mm;
(2) al coated with composite sensitive material2O3Sintering the ceramic tube at 350-450 ℃ for 3-5 h, and then enabling a nichrome heating coil (with 50-60 turns) with the resistance value of 30-40 omega to penetrate through Al2O3The ceramic tube is internally provided with a direct current to provide a proper working temperature for the sensor; finally, Al is led through a platinum wire2O3The ceramic tube is welded on the indirectly heated hexagonal tube seat;
(3) finally, aging the sensor obtained in the step (2) in an air environment at 200-400 ℃ for 5-7 days to obtain MoO3/In2O3Composite-based oxide semiconductor acetone sensors.
The working principle is as follows:
when MoO3/In2O3When the composite material-based acetone sensor is placed in the air, oxygen molecules in the air are adsorbed on the surface of the sensor and come from MoO3/In2O3Ionization of conduction band electrons of composite sensitive material to form adsorbed oxygen ions and O2-，O-Or O2-The method of (1) exists. And a depletion layer is formed on the surface of the composite sensitive material, so that the measuring resistance of the sensor is increased. When the sensor contacts acetone gas at a suitable temperature, a reaction occurs between the oxygen species and the target gas, resulting in the release of electrons trapped in the ionized oxygen species back into the MoO3/In2O3The composite sensitive material is in a conduction band. The depletion layer barrier is reduced and the conductance of the sensor is increased, thereby decreasing the measurement resistance. Here we define the sensitivity S of the sensor: r ═ Sa/RgWherein R isaIs the resistance of the sensor in air, RgResistance after the sensor was exposed to acetone.
Prepared by the inventionBased on MoO3/In2O3The acetone sensor made of the composite sensitive material has the following advantages:
(1) the composite material with the hollow structure can be prepared by a simple one-step hydrothermal method, the synthesis method is simple, the cost is low, and an effective sensitive material and a preparation method are provided for developing a high-performance acetone sensor.
(2)MoO3/In2O3The composite material sensor has the advantages of high response speed, good selectivity, good stability to acetone and strong reliability.
(3) The tube sensor is commercially available, and the device has simple process and small volume and is suitable for mass production.
Drawings
FIG. 1: MoO3/In2O3The structure schematic diagram of the composite sensitive material acetone sensor;
FIG. 2: comparative examples of the present invention (a) low resolution SEM images, (b) single sphere SEM images, (c) single broken sphere SEM images; (d-f) low resolution SEM pictures of inventive samples of example 1, example 2 and example 3, wherein the inset is the SEM picture of its corresponding single broken sphere; (g-i) SEM images of individual spheres of samples of example 1, example 2 and example 3 of the invention.
FIG. 3: the response value of the samples of the comparative example, the example 1, the example 2 and the example 3 to 100ppm of acetone gas at 175-250 ℃ is plotted against the working temperature.
FIG. 4: comparative, example 1, example 2 and example 3 samples are plotted against the response of 100ppm of 8 test gases.
FIG. 5: the samples of comparative example, example 1, example 2 and example 3 had (a) a relationship of response values and (b) a dynamic response curve for different concentrations of acetone gas at the optimum operating temperature.
As shown in fig. 1, the names of the respective components are: annular gold electrode 1, MoO3/In2O3Composite sensitive material 2, hexagonal base 3, nichrome heating coil 4 and Al2O3A ceramic tube 5 and a platinum wire 6;
as shown in FIG. 2(a), the obtained MoO3The spheres are uniform in size but have high adhesiveness, and as can be seen from fig. 2(b) a single sphere and fig. 2(c) a broken sphere, the comparative example is a solid sphere having a surface formed by stacking a plurality of nanosheets. Fig. 2(d-f) shows that all 3 embodiments are spherical structures with uniform size, and the hollow internal structure can be seen from the interpolation diagram. As shown In FIG. 2(g-i), the particle size of the hollow sphere slightly increased and the surface blocking was reduced as the In content increased.
FIG. 3 is a graph showing the response of the test sample to 100ppm acetone gas versus the operating temperature for comparative example, example 1, example 2 and example 3. As can be seen from the figure, the optimum working temperature for the four groups of samples is 250 ℃. Wherein the sensitivity of the comparative example is 2.8, the sensitivity of example 1 is 14.1, the sensitivity of example 2 is 38.1, and the sensitivity of example 3 is 5.5. At the optimum operating temperature, the sensitivity of example 2 was the highest, about 13.6 times the sensitivity of the comparative example. It can be seen that by compounding In2O3The reaction efficiency of the sensitive material and the acetone can be improved, and the composite oxide semiconductor acetone sensor with high sensitivity is obtained.
As shown in fig. 4, the response values of the comparative example, example 1, example 2 and example 3 samples are compared to 100ppm of 8 test gases. It can be seen from the figure that the response values of the examples are improved to some extent compared with the comparative examples, and only the response value of the examples is improved to the greatest extent. In addition, in 3 embodiments, the response value of embodiment 2 is most significantly improved.
As shown in fig. 5, the response value relationship and the dynamic response curve of the samples of the comparative example, the example 1, the example 2 and the example 3 to the acetone gas with different concentrations at the optimal working temperature. The sensitivity test method comprises the following steps: firstly, the sensor is put into a gas box, the resistance at the moment is measured by an ammeter connected with the sensor, and the resistance value of the sensor in the air, namely R, is obtaineda(ii) a Then injecting 1-100 ppm acetone into the gas tank by using a microsyringe, and measuring to obtain the resistance value R of the sensor in acetone with different concentrationsgAccording to the definition of sensitivity S, formula S ═ Ra/RgAnd finally obtaining the standard working curve of the acetone concentration-sensitivity by calculating the sensitivity of the sensor under different concentrations. It can be seen from the figure that the response values of the comparative example and the example each linearly increase with the increase of the acetone concentration, and the sensitivities of the comparative example and the example 2 are 2.8 and 38.1, respectively, when the acetone concentration is 100 ppm.
Detailed Description
Comparative example:
with MoO3The solid ball is used as a sensitive material to manufacture the indirectly heated acetone sensor, and the specific manufacturing process comprises the following steps:
(1) 0.48g of sodium molybdate dihydrate, 0.65g of thiourea and 0.45g of citric acid were dissolved in 70mL of a mixed solution containing 50mL of deionized water and 20mL of anhydrous ethanol. Stirring vigorously for 30min to form a uniform solution;
(2) then transferring the obtained solution into a hydrothermal kettle, and then putting the hydrothermal kettle into a hydrothermal oven, wherein the oven parameters are set to be 180 ℃ and 22 h;
(3) after the reaction time was over, the autoclave was naturally cooled to room temperature, and the black precipitate adhering to the inner wall of the liner was carefully collected. The precipitate was washed with water and centrifuged several times with deionized water and ethanol to remove impurity ions, and dried in air at 80 ℃ for 12 h. After drying, calcining the product at 450 ℃ for 3h to obtain MoO3A solid sphere sensitive material;
(4) get MoO3The solid sphere sensitive material is mixed with ethanol according to the mass ratio of 0.4 mg: 1mg were mixed homogeneously to form a slurry. Coating Al with two parallel, annular and mutually separated gold electrodes on the surface by dipping slurry with a fine hairbrush2O3The outer surface of the ceramic tube is completely covered with a gold electrode (Al)2O3The inner diameter of the ceramic tube is 0.7mm, the outer diameter is 1.1mm, and the length is 4.5 mm; the width of a single gold electrode is 0.4mm, and the distance between two gold electrodes is 0.5 mm; a platinum wire lead is led out of the gold electrode, and the length of the platinum wire lead is 5 mm).
(5) Sintering the coated ceramic tube at 400 ℃ for 3h, and then passing a nichrome heating coil having a resistance value of 35 Ω through Al2O3The ceramic tube is internally provided with direct current to provide the sensorAnd finally, welding the ceramic tube on the universal indirectly heated hexagonal tube seat through a platinum wire at a proper working temperature.
(6) Finally, the sensor is aged for 7 days in an air environment at 250 ℃, so that MoO-based sensor is obtained3An oxide semiconductor acetone sensor of solid sphere sensitive material.
Example 1:
in a Mo/In molar ratio of 2: 1 MoO3/In2O3The acetone sensor is made of the hollow ball material, and the making process comprises the following steps:
(1) 0.48g of sodium molybdate dihydrate, 0.38g of indium nitrate hydrate, 0.65g of thiourea and 0.45g of citric acid were dissolved in 70mL of a mixed solution containing 50mL of deionized water and 20mL of anhydrous ethanol. Stirring vigorously for 30min to form a uniform solution;
(2) then transferring the obtained solution into a hydrothermal kettle, and then putting the hydrothermal kettle into a hydrothermal oven, wherein the oven parameters are set to be 180 ℃ and 22 h;
(3) after the reaction time was completed, the autoclave was naturally cooled to room temperature, and the precipitate adhering to the inner wall of the reactor liner was carefully collected. The precipitate was washed with water and centrifuged several times with deionized water and ethanol to remove impurity ions, and dried in air at 80 ℃ for 12 h. After drying, calcining the product at 450 ℃ for 3h to obtain MoO3/In2O3Hollow sphere composite sensitive material;
(4) get MoO3/In2O3The hollow sphere sensitive material is mixed with ethanol according to the mass ratio of 0.4 mg: 1mg were mixed homogeneously to form a slurry. Coating Al with two parallel, annular and mutually separated gold electrodes on the surface by dipping slurry with a fine hairbrush2O3Outer surface of ceramic tube (Al)2O3The inner diameter of the ceramic tube is 0.7mm, the outer diameter is 1.1mm, and the length is 4.5 mm; the width of a single gold electrode is 0.4mm, and the distance between two gold electrodes is 0.5 mm; a platinum wire lead is led out of the gold electrode, and the length of the platinum wire lead is 5 mm).
(5) Sintering the coated ceramic tube at 400 ℃ for 3h, and then passing a nichrome heating coil having a resistance value of 35 Ω through Al2O3The ceramic tube is internally provided with a direct current to provide a sensorProper working temperature. And finally, welding the ceramic tube on the universal indirectly heated hexagonal tube seat through a platinum wire.
(6) Finally, aging the sensor in an air environment at 250 ℃ for 7 days to obtain MoO3/In2O3The hollow ball material is based on an oxide semiconductor acetone sensor.
Example 2:
in a Mo/In molar ratio of 1: 1 MoO3/In2O3The acetone sensor is made of the hollow ball material, and the making process comprises the following steps:
(1) 0.48g of sodium molybdate dihydrate, 0.76g of indium nitrate hydrate, 0.65g of thiourea and 0.45g of citric acid were dissolved in 70mL of a mixed solution containing 50mL of deionized water and 20mL of anhydrous ethanol. Stirring vigorously for 30min to form a uniform solution;
(2) then transferring the obtained solution into a hydrothermal kettle, and then putting the hydrothermal kettle into a hydrothermal oven, wherein the oven parameters are set to be 180 ℃ and 22 h;
(3) after the reaction time was completed, the autoclave was naturally cooled to room temperature, and the precipitate adhering to the inner wall of the reactor liner was carefully collected. The precipitate was washed with water and centrifuged several times with deionized water and ethanol to remove impurity ions, and dried in air at 80 ℃ for 12 h. After drying, calcining the product at 450 ℃ for 3h to obtain MoO3/In2O3Hollow sphere composite sensitive material;
(4) get MoO3/In2O3The hollow sphere sensitive material is mixed with ethanol according to the mass ratio of 0.4 mg: 1mg were mixed homogeneously to form a slurry. Coating Al with two parallel, annular and mutually separated gold electrodes on the surface by dipping slurry with a fine hairbrush2O3Outer surface of ceramic tube (Al)2O3The inner diameter of the ceramic tube is 0.7mm, the outer diameter is 1.1mm, and the length is 4.5 mm; the width of a single gold electrode is 0.4mm, and the distance between two gold electrodes is 0.5 mm; a platinum wire lead is led out of the gold electrode, and the length of the platinum wire lead is 5 mm).
(5) Sintering the coated ceramic tube at 400 ℃ for 3h, and then passing a nichrome heating coil having a resistance value of 35 Ω through Al2O3The inside of the ceramic tube is communicated with direct currentThe sensor provides the appropriate operating temperature. And finally, welding the ceramic tube on the universal indirectly heated hexagonal tube seat through a platinum wire.
(6) Finally, aging the sensor in an air environment at 250 ℃ for 7 days to obtain MoO3/In2O3The hollow ball material is based on an oxide semiconductor acetone sensor.
Example 3:
in a Mo/In molar ratio of 1: 2 MoO3/In2O3The acetone sensor is made of the hollow ball material, and the making process comprises the following steps:
(1) 0.48g of sodium molybdate dihydrate, 1.52g of indium nitrate hydrate, 0.65g of thiourea and 0.45g of citric acid were dissolved in 70mL of a mixed solution containing 50mL of deionized water and 20mL of anhydrous ethanol. Stirring vigorously for 30min to form a uniform solution;
(2) then transferring the obtained solution into a hydrothermal kettle, and then putting the hydrothermal kettle into a hydrothermal oven, wherein the oven parameters are set to be 180 ℃ and 22 h;
(3) after the reaction time was completed, the autoclave was naturally cooled to room temperature, and the precipitate adhering to the inner wall of the reactor liner was carefully collected. The precipitate was washed with water and centrifuged several times with deionized water and ethanol to remove impurity ions, and dried in air at 80 ℃ for 12 h. After drying, calcining the product at 450 ℃ for 3h to obtain MoO3/In2O3Hollow sphere composite sensitive material;
(4) get MoO3/In2O3The hollow sphere sensitive material is mixed with ethanol according to the mass ratio of 0.4 mg: 1mg were mixed homogeneously to form a slurry. Coating Al with two parallel, annular and mutually separated gold electrodes on the surface by dipping slurry with a fine hairbrush2O3Outer surface of ceramic tube (Al)2O3The inner diameter of the ceramic tube is 0.7mm, the outer diameter is 1.1mm, and the length is 4.5 mm; the width of a single gold electrode is 0.4mm, and the distance between two gold electrodes is 0.5 mm; a platinum wire lead is led out of the gold electrode, and the length of the platinum wire lead is 5 mm).
(5) Sintering the coated ceramic tube at 400 ℃ for 3h, and then passing a nichrome heating coil having a resistance value of 35 Ω through Al2O3The interior of the ceramic tube is communicated with a straight tubeGalvanic electricity is used to provide the proper operating temperature for the sensor. And finally, welding the ceramic tube on the universal indirectly heated hexagonal tube seat through a platinum wire.
(6) Finally, aging the sensor in an air environment at 250 ℃ for 7 days to obtain MoO3/In2O3The hollow ball material is based on an oxide semiconductor acetone sensor.
Claims (5)
1. Based on MoO3/In2O3The acetone sensor of hollow ball composite sensitive material is formed from Al whose external surface is equipped with two parallel, ring-shaped and mutually-separated gold electrodes2O3Ceramic tube substrate coated with Al2O3Composite sensitive material on the outer surface of the ceramic tube and the gold electrode, Al2O3A nickel-chromium alloy heating coil in the ceramic tube, and a platinum wire is led out of the gold electrode; the method is characterized in that: the composite sensitive material is MoO3/In2O3The hollow sphere composite sensitive material is prepared by the following steps,
(1) dissolving 0.48-0.5 g of sodium molybdate dihydrate, 0.38-1.52 g of indium nitrate hydrate, 0.6-0.7 g of thiourea and 0.45-0.5 g of citric acid in 70mL of mixed solution containing 50mL of deionized water and 20mL of absolute ethyl alcohol, and violently stirring for 30-60 min to form uniform solution;
(2) then transferring the solution obtained in the step (1) into a high-pressure hydrothermal kettle, and carrying out hydrothermal reaction for 20-30 h at the temperature of 180-200 ℃;
(3) after the reaction in the step (2) is finished, naturally cooling the high-pressure hydrothermal kettle to room temperature, collecting a reaction product, washing the reaction product with water, centrifugally washing the reaction product with deionized water and ethanol to remove impurity ions, drying the reaction product in the air at 70-90 ℃ for 10-20 hours, and finally calcining the reaction product at 450-500 ℃ for 2-5 hours to obtain MoO3/In2O3The hollow sphere composite sensitive material.
2. A MoO-based composition according to claim 13/In2O3The acetone sensor of the hollow sphere composite sensitive material is characterized in that: composite sensitivityThe thickness of the material is 15-30 μm.
3. A MoO-based composition according to claim 13/In2O3The acetone sensor of the hollow sphere composite sensitive material is characterized in that: al (Al)2O3The inner diameter of the ceramic tube is 0.6-0.8 mm, the outer diameter is 1.0-1.5 mm, and the length is 4-5 mm; the width of a single gold electrode is 0.4-0.5 mm, and the distance between two gold electrodes is 0.5-0.6 mm; and a platinum wire lead is led out of the gold electrode, and the length of the platinum wire lead is 4-6 mm.
4. MoO-based according to any of claims 1 to 33/In2O3The preparation method of the acetone sensor of the hollow sphere composite sensitive material comprises the following steps:
(1) get MoO3/In2O3The composite sensitive material and ethanol are mixed according to the mass ratio of 0.25-0.5 mg: 1mg of the mixture was mixed homogeneously to form a paste, and the paste was dipped with a fine brush to coat Al with two parallel, annular and mutually discrete gold electrodes on the surface2O3The outer surface of the ceramic tube is completely covered with the gold electrode;
(2) al coated with composite sensitive material2O3Sintering the ceramic tube at 350-450 ℃ for 3-5 h, and then enabling a nickel-chromium alloy heating coil with a resistance value of 30-40 omega to penetrate through Al2O3The ceramic tube is internally provided with a direct current to provide a proper working temperature for the sensor; finally, Al is led through a platinum wire2O3The ceramic tube is welded on the indirectly heated hexagonal tube seat;
(3) finally, aging the sensor obtained in the step (2) in an air environment at 200-400 ℃ for 5-7 days to obtain the sensor based on MoO3/In2O3The acetone sensor is made of hollow ball composite sensitive material.
5. MoO-based according to any of claims 1 to 33/In2O3The acetone sensor made of the hollow sphere composite sensitive material is applied to the aspect of detecting acetone gas in the atmospheric environment.
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