CN110044970B - Application of flower-shaped ZnO nano material loaded with Ru nano particles in acetone gas sensor - Google Patents
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Abstract
The invention provides an application of a flower-shaped ZnO nano material loaded with Ru nano particles in an acetone gas sensor, wherein crystals of the flower-shaped ZnO nano material loaded with the Ru nano particles are flower-shaped, the average grain diameter of the crystal particles is 5 mu m, the Ru nano particles are uniformly loaded on the surfaces of the ZnO nano particles, and the flower-shaped ZnO nano material loaded with the Ru nano particles is used as a sensitive material to be coated on a sensitive element, has good gas-sensitive response to acetone gas, and has important application value as the acetone gas sensor.
Description
Technical Field
The invention belongs to the technical field of gas sensors, and particularly relates to a flower-shaped ZnO nano material loaded with Ru nano particles as a gas sensitive material, a preparation method of the flower-shaped ZnO nano material and application of the flower-shaped ZnO nano material in an acetone gas sensor.
Background
The acetone is mainly used as a solvent in industries such as explosives, plastics, rubber, fibers, leather, grease, paint spraying and the like, and can also be used as an important raw material for synthesizing substances such as ketene, acetic anhydride, iodoform, polyisoprene rubber, methyl methacrylate, chloroform, epoxy resin and the like. Acetone has great health hazard to human body, and acute poisoning is mainly manifested by anesthesia to central nervous system, manifested by debilitation, nausea, headache, dizziness, and easy excitation. Vomiting, shortness of breath, spasm and even coma occur in severe cases. It has irritation to eyes, nose and throat. The chronic effects include vertigo, burning sensation, pharyngitis, bronchitis, asthenia, and excitement. Repeated exposure of the skin for a long period of time can cause dermatitis. And acetone itself has extremely flammable and explosive characteristics. The rapid and intelligent detection of acetone necessitates the development of high performance acetone gas sensors.
Among gas sensors, the metal oxide semiconductor type gas sensor has the advantages of high sensitivity, good selectivity, quick response recovery, low cost, convenience in carrying and the like, and is one of the most widely used gas sensors at present. The metal oxide semiconductor gas sensor directly adsorbs detection gas by using a sensitive material, so that the electrical property and the like of the material are changed, and the gas concentration is detected by detecting the change of an output signal of a sensitive element of a peripheral circuit. Oxide semiconductor sensitive materials with different morphologies have great influence on the gas-sensitive performance, so that the gas-sensitive performance is often improved by synthesizing the sensitive materials with different morphologies. In addition to this, the catalytic material has an influence on the gas-sensitive properties of the sensitive material.
Disclosure of Invention
In order to solve the technical problems, the invention provides a flower-shaped ZnO nano material loaded with Ru (ruthenium) nano particles.
The invention also aims to provide a preparation method of the flower-shaped ZnO nano material loaded with the Ru nano particles.
The invention further aims to provide application of the flower-shaped ZnO nano material loaded with the Ru nano particles in an acetone gas sensor.
The crystal of the flower-shaped ZnO nano material loaded with the Ru nano particles is flower-shaped, the average grain diameter of the crystal particles is 5 mu m, and the Ru nano particles are uniformly loaded on the surfaces of the ZnO nano particles.
The preparation method of the flower-shaped ZnO nano material loaded with the Ru nano particles comprises the following steps:
step one, preparing flower-shaped ZnO
The flower-like ZnO can be prepared by a plurality of methods, such as a hydrothermal method, a thermal zinc powder evaporation method, a microwave heating method and the like, and the invention provides the following preparation method:
s11 dissolving 4-8 g of sodium hydroxide in 100-120 ml of water to prepare solution A;
s12 dissolving 2-3 g of zinc sulfate in 35-45 ml of water to prepare a solution B;
placing the S13A solution in 55-70oC, under a water bath, dropwise adding the solution B into the solution A while stirring; after the dropwise addition is finished, placing the mixed solution in a temperature range of 55-70 DEGoC, drying in a drying oven for 4-8 hours; centrifuging and washing the mixed solution, and then precipitating the precipitate at 60-80 DEG CoDrying for 12-24 hours under C, taking out and grinding to obtain flower-shaped crystal ZnO white powder;
step two, preparation of flower-shaped ZnO nano material loaded with Ru nano particles
S21, adding 0.01-0.1 g of flower-shaped crystal ZnO white powder prepared in the step one into 30-60 ml of ethylene glycol to completely dissolve the flower-shaped crystal ZnO white powder;
s22 mixing 100-150 μ L of water with concentration of 15-30mmol/L RuCl3Adding the solution to the solution prepared in S21 and dissolving completely;
s23 dissolving the solution prepared in S22 in 120-150%oAnd C, reacting for 3-5 hours, centrifuging the obtained product to obtain an off-white precipitate, and grinding the precipitate for 20-30 min to obtain the flower-shaped ZnO nano material loaded with the Ru nano particles.
Further, the solvent water used in the above steps is deionized water.
Further, in the step S13, the dropping speed of the solution B to the solution a is 1 drop/second, the dropping speed is controlled to completely react the zinc sulfate with the sodium hydroxide, and the flower-like crystal ZnO required by the target can be prepared by controlling the reactant ratio, the reaction temperature and the drying parameter.
Further, the solution is subjected to ultrasonic treatment for 15-30 min after being dissolved in the step S22, so that the substance dispersion effect in the solution is better.
The flower-shaped ZnO nano material loaded with the Ru nano particles is applied to an acetone gas sensor, and the flower-shaped ZnO nano material loaded with the Ru nano particles is coated on a sensitive element of the sensor.
Furthermore, the thickness of a sensitive layer formed by the flower-shaped ZnO nano material loaded with the Ru nano particles is 20-40 mu m.
Furthermore, the acetone gas sensor comprises an explosion-proof cover, a sensitive element coated with flower-shaped ZnO nano material loaded with Ru nano particles and a six-pin tube seat.
Further, the preparation method of the acetone gas sensor comprises the following steps:
(1) preparing a flower-shaped ZnO nano material loaded with Ru nano particles into slurry, and uniformly coating the slurry on Al with an annular Au electrode2O3Forming a sensitive layer with the thickness of 20-40 mu m on the outer surface of the ceramic tube, wherein the sensitive layer completely covers the annular Au electrode;
(2) the element obtained in the step (1) is 60-80%oC, drying for 1-3 hours;
(3) passing the Ni-Cr alloy heating wire with the resistance value of 35-40 omega through Al2O3The ceramic tube is used as a heating wire to obtain a sensitive element;
(4) and welding the sensitive element on a six-pin tube seat and packaging.
Further, the preparation method of the slurry in the step (1) comprises the steps of putting the dried flower-shaped ZnO nano material loaded with the Ru nano particles into a mortar, and grinding for 20-30 minutes; and then dripping water into the mortar and continuing to grind for 20-30 minutes to obtain viscous slurry.
Furthermore, the mass ratio of the flower-shaped ZnO nano material loaded with the Ru nano particles to water in the slurry preparation is 5: 1-3.
The invention has the advantages and beneficial effects that: the flower-shaped ZnO nano material loaded with the Ru nano particles has a high specific surface area, and meanwhile, the sensitivity of the Ru-modified ZnO to acetone gas is improved, so that the flower-shaped ZnO nano material loaded with the Ru nano particles is used as a sensitive material, the high specific surface area is applied, and the gas sensitive response can be improved by effectively utilizing the catalytic action of Ru on the surface of ZnO and the acetone gas; in addition, the acetone gas sensor is an improvement on the existing structure, and the flower-shaped ZnO nano material loaded with the Ru nano particles is coated on a sensitive element, so that the acetone gas sensor has the characteristics of simple preparation method, low cost, excellent quick response recovery characteristic and large-scale production, and has good detection performance on acetone gas. Generally, the invention has simple process, small volume of the manufactured device and suitability for mass production, thereby having important application value.
Drawings
FIG. 1 shows SEM (a) and TEM (b) morphologies of flower-like ZnO nanomaterial loaded with Ru nanoparticles according to the present invention;
FIG. 2 is a schematic diagram of the device structure of the acetone sensor prepared by the present invention;
FIG. 3 is an XRD pattern of flower-like ZnO nanomaterial loaded with Ru nanoparticles prepared by the invention;
FIG. 4 shows an acetone sensor of the present invention operating at 172 deg.CoC, a sensitivity-acetone concentration characteristic curve of the device;
FIG. 5 shows an acetone sensor of the present invention operating at 172 deg.CoC. Acetone concentration of 100ppmThe response recovery curve of the device;
FIG. 6 shows an acetone sensor of the present invention operating at 172 deg.CoC. The gas concentration is 100ppm, the selective characteristics of the device.
Detailed Description
The present invention will be further described with reference to the following embodiments.
Example 1
The flower-shaped ZnO nano material loaded with Ru nano particles is used as a sensitive material to manufacture an indirectly heated acetone sensor, and as shown in figure 2, the sensor consists of an explosion-proof protective cover 1, a sensitive element 2 coated with the flower-shaped ZnO nano material loaded with Ru nano particles and a six-pin tube seat 3.
The specific manufacturing steps are as follows:
(1) adding 6g of NaOH into 112.5ml of deionized water, and stirring for 5 minutes by magnetic force to completely dissolve the NaOH, wherein the solution is marked as A solution;
(2) 2.1567g of ZnSO4•7H2Dissolving O in 37.5ml of deionized water, and stirring for 5 minutes by magnetic force to completely dissolve the O, wherein the solution is marked as solution B;
(3) slowly dropwise adding the solution B to a solution placed at 60oC, in the solution A of the water bath, keeping magnetic stirring, and after the dropwise addition is finished, placing the mixed solution in a 60-degree mixeroC, drying in an oven for 6 hours;
(4) the mixed solution is washed for a plurality of times by centrifugation with deionized water, and the precipitate is 80 DEGoDrying for 12 hours at C, taking out and grinding to obtain flower-shaped ZnO white powder;
(5) adding 0.05g of flower-shaped ZnO powder into 50ml of ethylene glycol, and uniformly dispersing under magnetic stirring;
(6) taking 124 mu L of RuCl3Adding the solution (with the concentration of 20 mmol/L) into the solution obtained in the step (5), magnetically stirring at room temperature to completely dissolve the solution, and performing ultrasonic treatment for 20 minutes;
(7) the solution is at 140oC, reacting for 4 hours, washing and centrifuging the obtained product for multiple times by using deionized water to obtain offwhite precipitate, and placing the offwhite precipitate at 60 DEG CoC, drying in an oven for 6 hours completely, grinding for 25 minutes to obtain the Ru loaded nanoFlower-like ZnO nano-materials of rice grains;
(8) putting the dried flower-shaped ZnO nano material powder loaded with the Ru nano particles into a mortar, and grinding for 30 minutes; then, dropping deionized water (the mass ratio of the nano material to the water is 5: 2) into the mortar, and continuously grinding for 30 minutes to obtain viscous slurry; uniformly coating the paste on Al with annular Au electrode by using a brush2O3Forming a sensitive layer with the thickness of 30 microns on the outer surface of the ceramic tube, wherein the sensitive layer completely covers the annular Au electrode;
(9) coating flower-like ZnO nano material Al loaded with Ru nano particles2O3The ceramic tube is at 70oC, drying for 1 hour; then, a Ni-Cr alloy heating wire with the resistance value of 38 omega is penetrated through Al2O3And finally welding the sensitive element on a six-pin tube seat and packaging to obtain the acetone gas sensor loaded with the flower-shaped ZnO nano material powder of the Ru nano particles.
Example 2
The flower-shaped ZnO nano material loaded with Ru nano particles is used as a sensitive material to manufacture an indirectly heated acetone sensor, and as shown in figure 2, the sensor consists of an explosion-proof protective cover 1, a sensitive element 2 coated with the flower-shaped ZnO nano material loaded with Ru nano particles and a six-pin tube seat 3.
The specific manufacturing steps are as follows:
(1) adding 4.10g of NaOH into 100.5 ml of deionized water, and stirring for 5 minutes by magnetic force to completely dissolve the NaOH, wherein the solution is marked as solution A;
(2) 2.5679 g of ZnSO4•7H2Dissolving O in 40.6 ml of deionized water, and stirring for 5 minutes by magnetic force to completely dissolve the O, and marking as a solution B;
(3) slowly dropwise adding the solution B to the mixture placed in a container 55oC, in the solution A of the water bath, keeping magnetic stirring, and after the dropwise addition is finished, placing the mixed solution in a 65-degree mixeroC, drying in an oven for 6 hours;
(4) the mixed solution is washed by deionized water for a plurality of times through centrifugation, and the precipitate is 60 DEGoDrying for 24 hours under C, taking out and grinding to obtain flower-shaped ZnOA white powder;
(5) adding 0.02 g of flower-shaped ZnO powder into 40 ml of ethylene glycol, and uniformly dispersing under magnetic stirring;
(6) taking 140 mu L of RuCl3Adding the solution (with the concentration of 15 mmol/L) into the solution obtained in the step (5), magnetically stirring at room temperature to completely dissolve the solution, and then performing ultrasonic treatment for 20 minutes;
(7) the solution is at 120oC, reacting for 5 hours, washing the obtained product with deionized water for many times, centrifuging to obtain an off-white precipitate, and placing the off-white precipitate at 60 DEG CoC, drying in an oven for 6 hours completely, and grinding for 20 minutes to obtain a flower-shaped ZnO nano material loaded with Ru nano particles;
(8) putting the dried powder of the flower-shaped ZnO nano material loaded with the Ru nano particles into a mortar, and grinding for 30 minutes; then, dropping deionized water (the mass ratio of the nano material to the water is 5: 1) into the mortar, and continuously grinding for 30 minutes to obtain viscous slurry; uniformly coating the paste on Al with annular Au electrode by using a brush2O3Forming a sensitive layer with the thickness of 30 microns on the outer surface of the ceramic tube, wherein the sensitive layer completely covers the annular Au electrode;
(9) coating flower-like ZnO nano material Al loaded with Ru nano particles2O3The ceramic tube is at 70oC, drying for 1 hour; then, a Ni-Cr alloy heating wire with the resistance value of 38 omega is penetrated through Al2O3And finally welding the sensitive element on a six-pin tube seat and packaging to obtain the acetone gas sensor loaded with the flower-shaped ZnO nano material powder of the Ru nano particles.
Example 3
The flower-shaped ZnO nano material loaded with Ru nano particles is used as a sensitive material to manufacture an indirectly heated acetone sensor, and as shown in figure 2, the sensor consists of an explosion-proof protective cover 1, a sensitive element 2 coated with the flower-shaped ZnO nano material loaded with Ru nano particles and a six-pin tube seat 3.
The specific manufacturing steps are as follows:
(1) 7.5780g of NaOH is added into 120.0ml of deionized water, and the mixture is magnetically stirred for 5 minutes to be completely dissolved and marked as solution A;
(2) 2.7786g of ZnSO4•7H2Dissolving O in 43.8ml of deionized water, and stirring for 5 minutes by magnetic force to completely dissolve the O, wherein the solution is marked as solution B;
(3) slowly dropwise adding the solution B to a container 70oC, in the solution A of the water bath, keeping magnetic stirring, and after the dropwise addition is finished, placing the mixed solution in a place of 70oC, drying in an oven for 8 hours;
(4) the mixed solution is washed for a plurality of times by centrifugation with deionized water, and the precipitate is 80 DEGoDrying for 12 hours at C, taking out and grinding to obtain flower-shaped ZnO white powder;
(5) adding 0.1g of flower-shaped ZnO powder into 60ml of ethylene glycol, and uniformly dispersing under magnetic stirring;
(6) taking 150 mu L of RuCl3Adding the solution (with the concentration of 30 mmol/L) into the solution obtained in the step (5), magnetically stirring at room temperature to completely dissolve the solution, and then performing ultrasonic treatment for 20 minutes;
(7) the solution is at 150oC, reacting for 3 hours, washing and centrifuging the obtained product for multiple times by using deionized water to obtain offwhite precipitate, and placing the offwhite precipitate at 60 DEG CoC, drying in an oven for 6 hours completely, and grinding for 20 minutes to obtain a flower-shaped ZnO nano material loaded with Ru nano particles;
(8) putting the dried powder of the flower-shaped ZnO nano material loaded with the Ru nano particles into a mortar, and grinding for 30 minutes; then, dropping deionized water (the mass ratio of the nano material to the water is 5: 3) into the mortar, and continuously grinding for 30 minutes to obtain viscous slurry; uniformly coating the paste on Al with annular Au electrode by using a brush2O3Forming a sensitive layer with the thickness of 40 mu m on the outer surface of the ceramic tube, wherein the sensitive layer completely covers the annular Au electrode;
(9) coating flower-like ZnO nano material Al loaded with Ru nano particles2O3The ceramic tube is at 70oC, drying for 1 hour; then, a Ni-Cr alloy heating wire with a resistance value of 38 omega is passed through Al2O3The ceramic tube is used as a heating wire, and finally the sensitive element is welded on the six-pin tube seat and is carried outAnd packaging to finally obtain the acetone gas sensor loaded with the powder of the flower-shaped ZnO nano material of the Ru nano particles.
The ZnO nanocrystals obtained in the above examples were observed, and the results of the examples are similar, so only example 1 will be described. As shown in fig. 1, (a) the flower-like ZnO nanocrystals supporting Ru nanoparticles are seen as flower-like crystals, and (b) the particle size of the flower-like ZnO nanomaterial supporting Ru nanoparticles is seen as 5 μm; as shown in fig. 3, the XRD spectrum of the sample showed characteristic peaks of ZnO, indicating that the sample contains ZnO crystals.
The performance of the acetone sensor manufactured in each of the above examples was measured, and the results of each example were similar, so that the description will be given by only referring to example 1. As shown in fig. 4, when the device is at an operating temperature of 172 foUnder C, the sensitivity of the device is increased along with the increase of the concentration of acetone, and a curve shows a good linear relation in the range of the concentration of the acetone of 1-5 ppm; as shown in fig. 5, when the device is at an operating temperature of 172 foC. At an acetone concentration of 100ppm, the response time of the device was 1 second and the recovery time of the device was 52 seconds. The excellent response recovery characteristic is shown, and the acetone gas is well detected; as shown in fig. 6, when the device is at an operating temperature of 172 foC. Under the condition that the gas concentration is 100ppm, the sensitivity of the device to acetone is higher than that of other detection gases, and the device shows good selectivity.
Materials, reagents and experimental equipment related to the embodiment of the invention are all commercial products in the field of sensor materials if no special description is provided.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, modifications and decorations can be made without departing from the core technology of the present invention, and these modifications and decorations shall also fall within the protection scope of the present invention. Any changes which come within the meaning and range of equivalency of the claims are to be embraced within their scope.
Claims (9)
1. The application of the flower-shaped ZnO nano material loaded with the Ru nano particles in the acetone gas sensor is characterized in that the method for preparing the flower-shaped ZnO nano material loaded with the Ru nano particles comprises the following steps:
step one, preparing flower-shaped ZnO by adopting a hydrothermal method to obtain flower-shaped crystal ZnO white powder, and specifically comprises the following steps:
s11 dissolving 4-8 g of sodium hydroxide in 100-120 ml of water to prepare solution A;
s12 dissolving 2-3 g of zinc sulfate in 35-45 ml of water to prepare a solution B;
placing the S13A solution in a water bath at 55-70 ℃, dropwise adding the B solution into the A solution while stirring; after the dropwise adding is finished, placing the mixed solution in an oven at 55-70 ℃ for 4-8 hours; centrifuging and washing the mixed solution, drying the precipitate at the temperature of 60-80 ℃ for 12-24 hours, taking out and grinding to obtain flower-shaped crystal ZnO white powder;
step two, preparing the flower-shaped ZnO nano material loaded with Ru nano particles, which comprises the following specific steps:
s21, adding 0.01-0.1 g of flower-shaped crystal ZnO white powder prepared in the step one into 30-60 ml of ethylene glycol to completely dissolve the flower-shaped crystal ZnO white powder;
s22 RuCl with concentration of 15-30 mmol/L and 100-150 mu L3Adding the solution into the solution prepared in S21 and dissolving completely;
s23, reacting the solution prepared in S22 at 120-150 ℃ for 3-5 hours, centrifuging the obtained product to obtain an off-white precipitate, grinding the precipitate for 20-30 min to obtain a flower-shaped ZnO nano material loaded with Ru nanoparticles, wherein the average particle size of crystal particles of the flower-shaped ZnO nano material loaded with the Ru nanoparticles is 5 mu m, and the Ru nanoparticles are uniformly loaded on the surfaces of the ZnO nanoparticles, and the specific application process is as follows:
and coating the flower-shaped ZnO nano material loaded with the Ru nano particles on a sensitive element of a sensor.
2. The application of the flower-like ZnO nanomaterial loaded with Ru nanoparticles in the acetone gas sensor as claimed in claim 1, wherein in the first step, the solvent water used is deionized water.
3. The use of the Ru nanoparticle-supported flower-like ZnO nanomaterial in an acetone gas sensor according to claim 1, wherein the dropping speed of the B solution into the a solution in step S13 is 1 drop/sec.
4. The application of the flower-like ZnO nanomaterial loaded with Ru nanoparticles in the acetone gas sensor, according to claim 1, is characterized in that in step S22, the solution is subjected to ultrasonic treatment for 15-30 min after dissolution.
5. The application of the flower-shaped ZnO nano material loaded with the Ru nanoparticles in the acetone gas sensor as claimed in any one of claims 1-4, wherein the thickness of a sensitive layer formed on the sensitive element by the flower-shaped ZnO nano material loaded with the Ru nanoparticles is 20-40 μm.
6. The application of the flower-shaped ZnO nanomaterial loaded with Ru nanoparticles to the acetone gas sensor as claimed in claim 5, wherein the acetone gas sensor comprises an explosion-proof cover, a sensitive element coated with the flower-shaped ZnO nanomaterial loaded with Ru nanoparticles and a six-pin tube seat.
7. The application of the flower-like ZnO nanomaterial loaded with Ru nanoparticles to the acetone gas sensor as claimed in claim 5, wherein the preparation method of the acetone gas sensor comprises the following steps:
(1) preparing a flower-shaped ZnO nano material loaded with Ru nano particles into slurry, and uniformly coating the slurry on Al with an annular Au electrode2O3Forming a sensitive layer with the thickness of 20-40 mu m on the outer surface of the ceramic tube, wherein the sensitive layer completely covers the annular Au electrode;
(2) drying the element obtained in the step (1) at the temperature of 60-80 ℃ for 1-3 hours;
(3) passing the Ni-Cr alloy heating wire with the resistance value of 35-40 omega through Al2O3The ceramic tube is used as a heating wire to obtain a sensitive element;
(4) and welding the sensitive element on a six-pin tube seat and packaging.
8. The application of the flower-shaped ZnO nanomaterial loaded with Ru nanoparticles in the acetone gas sensor according to claim 7, wherein in the step (1), the slurry is prepared by putting the dried flower-shaped ZnO nanomaterial loaded with Ru nanoparticles into a mortar and grinding for 20-30 minutes; and then dripping water into the mortar and continuing to grind for 20-30 minutes to obtain viscous slurry.
9. The application of the flower-shaped ZnO nanomaterial loaded with Ru nanoparticles to the acetone gas sensor according to claim 8, wherein the mass ratio of the flower-shaped ZnO nanomaterial loaded with Ru nanoparticles to water during slurry preparation is 5: 1-3.
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