CN111426728A - Preparation and application of VOCs gas sensor based on core-shell layered structure tin dioxide-copper oxide composite nano material - Google Patents
Preparation and application of VOCs gas sensor based on core-shell layered structure tin dioxide-copper oxide composite nano material Download PDFInfo
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Abstract
The invention discloses a preparation method and application of a VOCs gas sensor based on a core-shell layered structure tin dioxide-copper oxide composite nanomaterial, belonging to the technical field of nano functional materials and environmental monitoring, wherein the preparation method comprises the following steps: s1: processing a Pd metal interdigital electrode; s2: preparing a core-shell layered structure tin dioxide-copper oxide composite nano material; s3: and coating a gas sensitive material, and using the VOCs gas sensor for detecting VOCs gases with different concentrations. The preparation method is simple, low in cost, easy to control in operation and high in production efficiency; the volume of the sensor is reduced; the method has the characteristics of high sensitivity, good stability and high detection speed for VOCs gas.
Description
Technical Field
The invention relates to the technical field of nano functional materials and environmental monitoring, in particular to preparation and application of a VOCs gas sensor based on a core-shell layered structure tin dioxide-copper oxide composite nano material.
Background
Air pollution, water pollution and soil pollution are three major pollutions threatening the normal life of human beings, and in recent years, along with the development of industry and the increase of population, the air pollution becomes more and more serious, especially the pollution of indoor VOCs, and in addition, the exceeding of the VOCs in the room of people for most of time seriously threatens the healthy life of common people. In the VOCs pollution, the content of formaldehyde exceeds the standard, and medical research shows that the formaldehyde concentration is higher than 0.1mg/m after long-term exposure3Ring ofIn the environment, the probability of the human body suffering from leukemia is increased. Therefore, it is an urgent and significant matter to realize accurate monitoring of the content of VOCs in the environment where life is generated.
The 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 concentration of the gas is detected by detecting the change of an output signal of a sensitive element of a peripheral circuit. Since there are many materials used for gas sensing, oxide semiconductor sensitive materials are mainly used at present. 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 structure of the sensitive material also has an effect on the gas-sensing properties.
Based on the above, the invention designs the preparation and application of the VOCs gas sensor based on the core-shell layered structure tin dioxide-copper oxide composite nano material, so as to solve the above mentioned problems.
Disclosure of Invention
The invention aims to provide preparation and application of a VOCs gas sensor based on a core-shell layered structure tin dioxide-copper oxide composite nano material, so as to solve the problems in the background technology.
In order to achieve the purpose, the invention provides the following technical scheme: a preparation method of a VOCs gas sensor based on a core-shell layered structure tin dioxide-copper oxide composite nano material comprises the following steps:
s1: treatment of Pd metal interdigital electrode
Firstly, wiping Al with a pd metal interdigital electrode prepared by a screen printing technology by using acetone and ethanol cotton balls respectively2O3Cleaning the substrate, and adding Al2O3Sequentially placing the substrate in acetone, ethanol and deionized water, respectively ultrasonically cleaning for 5-10 minutes, and finally drying at 100-120 ℃;
s2: preparation of core-shell layered structure stannic oxide-copper oxide composite nano material
S2.1: copper acetylacetonate and tin tetrachloride are weighed according to a certain molar ratio, then are put into methanol for full dissolution, and the obtained mixed solution is subjected to solvothermal reaction at a certain temperature.
S2.2: and (4) after the solvothermal reaction is finished, naturally cooling to room temperature, filtering and washing a product obtained by the reaction, and then putting the product into an oven for drying.
S2.3: and after the drying, directly calcining the obtained product in a muffle furnace, and naturally cooling to obtain the core-shell layered structure tin dioxide-copper oxide composite nano material.
S3: coating of gas sensitive materials
Putting the dried tin dioxide-copper oxide composite nano material with the core-shell layered structure into a mortar, and grinding for 20-30 minutes; then, dripping deionized water into the mortar, and continuously grinding for 20-30 minutes to obtain viscous slurry; dipping a small amount of slurry by using a small hairbrush, coating the slurry on a Pd metal finger electrode, and drying the Pd metal finger electrode at the temperature of 60-80 ℃ to obtain a tin dioxide-copper oxide composite nano material gas-sensitive layer with a core-shell layered structure and a thickness of 2-4 mu m; and finally, aging the prepared device for 24-72 hours under direct current of 40-80 mA in an environment with the relative humidity of 40% RH and the temperature of 20-35 ℃ to obtain the VOCs gas sensor based on the core-shell layered structure tin dioxide-copper oxide composite nano material.
Preferably, the preparation method of the Pd metal interdigital electrode comprises the following steps:
preparing a pd metal interdigital electrode by adopting a screen printing technology, and printing ink: pd powder: the mass ratio of the diluent is 1: 1: 2, stirring to prepare paste; and then injecting the paste onto a silk screen plate with the interdigital electrode pattern, scraping the paste under the conditions of an inclination angle of 30-45 degrees and a pressure of 5-10N, printing the electrodes, drying, and curing by ultraviolet light to complete the preparation of the metal interdigital electrode.
Preferably, the ink model is Jiahua JX 07500487.
Preferably, the width and the electrode spacing of the pd metal interdigital electrode are both 0.15-0.20 mm, and the thickness is 100-150 nm.
Preferably, the solvothermal reaction temperature is 110-220 ℃, and the solvothermal reaction time is 6-48 hours.
Preferably, the molar ratio of the copper acetylacetonate to the tin tetrachloride is 1:1, and the molar concentration of the copper acetylacetonate is 0.01 to 0.1 mol/L.
Preferably, the oven drying conditions are as follows: drying for 1-5 hours at the temperature of 60-120 ℃, wherein the temperature programming rate is 2-10 ℃/min.
Preferably, the temperature rise rate of the temperature programming in the muffle furnace is in the range of 2-20 ℃/min, the calcination time is 2-8 hours, and the calcination temperature is 500-800 ℃.
Preferably, the mass ratio of the nano microspheres to the deionized water is 5: 1 to 3.
The application of the core-shell layered structure tin dioxide-copper oxide composite nanomaterial-based VOCs gas sensor is characterized in that the core-shell layered structure tin dioxide-copper oxide composite nanomaterial-based VOCs gas sensor prepared by the method according to any one of claims 1 to 9 is used for detecting VOCs gases with different concentrations.
Compared with the prior art, the invention has the beneficial effects that: the VOCs gas sensor of the core-shell layered structure tin dioxide-copper oxide composite nanomaterial prepared by the invention has the advantages of simple preparation method, low cost, easiness in operation control and higher production efficiency; the tin dioxide/copper oxide composite nanomaterial with the core-shell structure for the VOCs gas sensor enhances the catalytic conversion effect on VOCs gas, thereby improving the detection sensitivity on VOCs and reducing the volume of the sensor; the method has the characteristics of high sensitivity, good stability and high detection speed for VOCs gas.
Drawings
In order to more clearly illustrate the technical solutions of the embodiments of the present invention, the drawings used in the description of the embodiments will be briefly introduced below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a flow chart of the preparation method of the present invention;
FIG. 2 is a schematic diagram of the structure of a VOCs gas sensor made in accordance with the present invention;
FIG. 3 is a graph showing the sensitivity-VOCs concentration characteristics of the VOCs gas sensor of the present invention at a working temperature of 220 ℃;
FIG. 4 is a diagram showing the selective characteristics of the VOCs gas sensor of the present invention at a working temperature of 220 deg.C and a VOCs gas concentration of 100 ppm.
In the drawings, the components represented by the respective reference numerals are listed below:
1、Al2O3a substrate; 2. pd metal interdigital electrodes; 3. and (3) a composite nano material gas-sensitive layer.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Referring to fig. 1-2, the present invention provides a technical solution: a preparation method of a VOCs gas sensor based on a core-shell layered structure tin dioxide-copper oxide composite nano material comprises the following steps:
s1: treatment of Pd metal interdigital electrode
Firstly, wiping Al with a pd metal interdigital electrode prepared by a screen printing technology by using acetone and ethanol cotton balls respectively2O3Cleaning the substrate, and adding Al2O3Sequentially placing the substrate in acetone, ethanol and deionized water, respectively ultrasonically cleaning for 5-10 minutes, and finally drying at 100-120 ℃;
the preparation method of the Pd metal interdigital electrode comprises the following steps:
preparing a pd metal interdigital electrode by adopting a screen printing technology, and preparing a Pd metal interdigital electrode according to an ink (the ink type adopts Jiahua JX 07500487): pd powder: the mass ratio of the diluent is 1: 1: 2, stirring to prepare paste; and then injecting the paste onto a silk screen plate with the interdigital electrode pattern, scraping the paste under the conditions of an inclination angle of 30-45 degrees and a pressure of 5-10N, printing the electrodes, drying, and curing by ultraviolet light to complete the preparation of the metal interdigital electrode. The width and the electrode spacing of the pd metal interdigital electrode are both 0.15-0.20 mm, and the thickness is 100-150 nm.
S2: preparation of core-shell layered structure stannic oxide-copper oxide composite nano material
S2.1: weighing copper acetylacetonate and tin tetrachloride according to a certain molar ratio, fully dissolving in methanol, and carrying out a solvothermal reaction on the obtained mixed solution at a certain temperature, wherein the solvothermal reaction temperature is 110-220 ℃, and the solvothermal reaction time is 6-48 hours.
Wherein the molar ratio of the copper acetylacetonate to the tin tetrachloride is 1:1, and the molar concentration of the copper acetylacetonate is 0.01-0.1 mol/L.
S2.2: after the solvothermal reaction is finished, naturally cooling to room temperature, filtering and washing a product obtained by the reaction, and then putting the product into an oven for drying, wherein the oven drying conditions are as follows: drying for 1-5 hours at the temperature of 60-120 ℃, wherein the temperature programming rate is 2-10 ℃/min.
S2.3: and after the drying, directly calcining the obtained product in a muffle furnace, wherein the temperature rise rate of the temperature programming in the muffle furnace is 2-20 ℃/min, the calcining time is 2-8 hours, the calcining temperature is 500-800 ℃, and the core-shell layered structure tin dioxide-copper oxide composite nano material is prepared after natural cooling.
S3: coating of gas sensitive materials
Putting the dried tin dioxide-copper oxide composite nano material with the core-shell layered structure into a mortar, and grinding for 20-30 minutes; and then, dropping deionized water into the mortar, wherein the mass ratio of the nano microspheres to the deionized water is 5: 1-3, and then continuously grinding for 20-30 minutes to obtain viscous slurry; dipping a small amount of slurry by using a small hairbrush, coating the slurry on a Pd metal finger electrode, and drying the Pd metal finger electrode at the temperature of 60-80 ℃ to obtain a tin dioxide-copper oxide composite nano material gas-sensitive layer with a core-shell layered structure and a thickness of 2-4 mu m; and finally, aging the prepared device for 24-72 hours under direct current of 40-80 mA in an environment with the relative humidity of 40% RH and the temperature of 20-35 ℃ to obtain the VOCs gas sensor based on the core-shell layered structure tin dioxide-copper oxide composite nano material.
Tin dioxide (SnO)2) The n-type semiconductor material has wide band gap and direct band gap of 3.6-3.8eV, excellent flame retarding and conducting performance, infrared radiation reflecting, light shielding, adsorption, stable chemical performance, high photocatalytic activity, etc. Because the band gap of tin dioxide is wider and the response visible spectrum is less, the related research on the photocatalytic degradation of pollutants by directly using tin dioxide is less. In order to improve the catalytic performance of tin dioxide, it is one of the most effective methods to select a compound with other semiconductors with smaller band gap. Because the tin dioxide is an n-type semiconductor, the tin dioxide is selected to be compounded with a p-type semiconductor copper oxide (0.96eV) with a smaller band gap, and a novel p-n heterojunction compound semiconductor tin dioxide/copper oxide nano material is prepared.
The invention successfully prepares the tin dioxide/copper oxide composite nano material with the spherical hierarchical structure with higher purity at low temperature by utilizing a solvothermal-calcination two-step method. The yield of the target product is high (99.0-99.9 percent), and the requirement of the industrial application field on the stannic oxide/copper oxide composite nano material product can be met. The purity of the product is high (99.95-99.98%), the content of impurities is low, and the dispersibility is good.
Example 2
The invention provides a technical scheme that: the application of the core-shell layered structure tin dioxide-copper oxide composite nanomaterial-based VOCs gas sensor is characterized in that the core-shell layered structure tin dioxide-copper oxide composite nanomaterial-based VOCs gas sensor prepared by the method according to any one of claims 1 to 9 is used for detecting VOCs gases with different concentrations. Referring to fig. 3-4, when the operating temperature of the VOCs gas sensor is 220 ℃, the sensitivity of the device increases with increasing VOCs gas concentration, and the curve shows a good linear relationship in the range of 10-100 ppm of VOCs gas concentration. When the working temperature of the VOCs gas sensor is 220 ℃ and the concentration of the VOCs gas is 100ppm, the sensitivity of the device to formaldehyde is higher than that of other detection gases. The device showed good selectivity. The gas-sensitive performance indexes of the VOCs gas sensor are as follows:
sensitivity was 14.8(100ppm formaldehyde);
VOCs gas test range: 10 to 500 ppm.
In the description herein, references to the description of "one embodiment," "an example," "a specific example" or the like are intended to mean that a particular feature, structure, material, or characteristic described in connection with the embodiment or example is included in at least one embodiment or example of the invention. In this specification, the schematic representations of the terms used above do not necessarily refer to the same embodiment or example. Furthermore, the particular features, structures, materials, or characteristics described may be combined in any suitable manner in any one or more embodiments or examples.
The preferred embodiments of the invention disclosed above are intended to be illustrative only. The preferred embodiments are not intended to be exhaustive or to limit the invention to the precise embodiments disclosed. Obviously, many modifications and variations are possible in light of the above teaching. The embodiments were chosen and described in order to best explain the principles of the invention and the practical application, to thereby enable others skilled in the art to best utilize the invention. The invention is limited only by the claims and their full scope and equivalents.
Claims (10)
1. A preparation method of a VOCs gas sensor based on a core-shell layered structure tin dioxide-copper oxide composite nano material is characterized by comprising the following steps:
s1: treatment of Pd metal interdigital electrode
Firstly, wiping Al with a pd metal interdigital electrode prepared by a screen printing technology by using acetone and ethanol cotton balls respectively2O3Cleaning the substrate, and adding Al2O3The substrate is sequentially placed in acetone, ethanol and deionized water, and is respectively cleaned by ultrasonic waves in the range of 5 toDrying for 10 minutes at the temperature of 100-120 ℃;
s2: preparation of core-shell layered structure stannic oxide-copper oxide composite nano material
S2.1: weighing copper acetylacetonate and stannic chloride according to a certain molar ratio, fully dissolving in methanol, and carrying out solvothermal reaction on the obtained mixed solution at a certain temperature;
s2.2: after the solvothermal reaction is finished, naturally cooling to room temperature, filtering and washing a product obtained by the reaction, and then putting the product into an oven for drying;
s2.3: after the drying, directly calcining the obtained product in a muffle furnace, and naturally cooling to obtain the core-shell layered structure tin dioxide-copper oxide composite nano material;
s3: coating of gas sensitive materials
Putting the dried tin dioxide-copper oxide composite nano material with the core-shell layered structure into a mortar, and grinding for 20-30 minutes; then, dripping deionized water into the mortar, and continuously grinding for 20-30 minutes to obtain viscous slurry; dipping a small amount of slurry by using a small hairbrush, coating the slurry on a Pd metal finger electrode, and drying the Pd metal finger electrode at the temperature of 60-80 ℃ to obtain a tin dioxide-copper oxide composite nano material gas-sensitive layer with a core-shell layered structure and a thickness of 2-4 mu m; and finally, aging the prepared device for 24-72 hours under direct current of 40-80 mA in an environment with the relative humidity of 40% RH and the temperature of 20-35 ℃ to obtain the VOCs gas sensor based on the core-shell layered structure tin dioxide-copper oxide composite nano material.
2. The preparation method of the VOCs gas sensor based on the core-shell layered structure tin dioxide-copper oxide composite nanomaterial according to claim 1, characterized by comprising the following steps: the preparation method of the Pd metal interdigital electrode comprises the following steps:
preparing a pd metal interdigital electrode by adopting a screen printing technology, and printing ink: pd powder: the mass ratio of the diluent is 1: 1: 2, stirring to prepare paste; and then injecting the paste onto a silk screen plate with the interdigital electrode pattern, scraping the paste under the conditions of an inclination angle of 30-45 degrees and a pressure of 5-10N, printing the electrodes, drying, and curing by ultraviolet light to complete the preparation of the metal interdigital electrode.
3. The preparation method of the VOCs gas sensor based on the core-shell layered structure tin dioxide-copper oxide composite nanomaterial according to claim 1, characterized by comprising the following steps: the ink type adopts Jiahua JX 07500487.
4. The preparation method of the VOCs gas sensor based on the core-shell layered structure tin dioxide-copper oxide composite nanomaterial according to claim 1, characterized by comprising the following steps: the width and the electrode spacing of the pd metal interdigital electrode are both 0.15-0.20 mm, and the thickness is 100-150 nm.
5. The preparation method of the VOCs gas sensor based on the core-shell layered structure tin dioxide-copper oxide composite nanomaterial according to claim 1, characterized by comprising the following steps: the solvothermal reaction temperature is 110-220 ℃, and the solvothermal reaction time is 6-48 hours.
6. The preparation method of the VOCs gas sensor based on the core-shell layered structure tin dioxide-copper oxide composite nanomaterial is characterized in that the molar ratio of copper acetylacetonate to tin tetrachloride is 1:1, and the molar concentration of the copper acetylacetonate is 0.01-0.1 mol/L.
7. The preparation method of the VOCs gas sensor based on the core-shell layered structure tin dioxide-copper oxide composite nanomaterial according to claim 1, characterized by comprising the following steps: the drying conditions of the oven are as follows: drying for 1-5 hours at the temperature of 60-120 ℃, wherein the temperature programming rate is 2-10 ℃/min.
8. The preparation method of the VOCs gas sensor based on the core-shell layered structure tin dioxide-copper oxide composite nanomaterial according to claim 1, characterized by comprising the following steps: the temperature rise rate of the temperature programming in the muffle furnace is in the range of 2-20 ℃/min, the calcination time is 2-8 hours, and the calcination temperature is 500-800 ℃.
9. The preparation method of the VOCs gas sensor based on the core-shell layered structure tin dioxide-copper oxide composite nanomaterial according to claim 1, characterized by comprising the following steps: the mass ratio of the nano microspheres to the deionized water is 5: 1 to 3.
10. The application of the VOCs gas sensor based on the core-shell layered structure tin dioxide-copper oxide composite nano material is characterized in that: the VOCs gas sensor based on the tin dioxide-copper oxide composite nanomaterial with the core-shell layered structure, which is prepared by the method according to any one of claims 1 to 9, is used for detecting VOCs gases with different concentrations.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114166899A (en) * | 2021-11-24 | 2022-03-11 | 上海大学 | PdRh-based loaded SnO2Formaldehyde MEMS gas sensor with multi-shell structure and preparation method thereof |
| CN115072772A (en) * | 2022-06-14 | 2022-09-20 | 山西农业大学 | Preparation method, product and application of spherical core-shell structure tin-titanium oxide |
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2020
- 2020-05-11 CN CN202010393552.9A patent/CN111426728A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114166899A (en) * | 2021-11-24 | 2022-03-11 | 上海大学 | PdRh-based loaded SnO2Formaldehyde MEMS gas sensor with multi-shell structure and preparation method thereof |
| CN115072772A (en) * | 2022-06-14 | 2022-09-20 | 山西农业大学 | Preparation method, product and application of spherical core-shell structure tin-titanium oxide |
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