CN111533165A - High-sensitivity gas detection material and preparation method thereof - Google Patents

High-sensitivity gas detection material and preparation method thereof Download PDF

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CN111533165A
CN111533165A CN202010385701.7A CN202010385701A CN111533165A CN 111533165 A CN111533165 A CN 111533165A CN 202010385701 A CN202010385701 A CN 202010385701A CN 111533165 A CN111533165 A CN 111533165A
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李军
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Laixi Xingmai Advanced Material Technology Center
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Abstract

The invention relates to a graphene/metal oxide/metal sulfide high-sensitivity gas detection material and a preparation method thereof2The CdS ternary composite gas detection material overcomes the defects of the traditional single metal oxide semiconductor preparation method through the synergistic effect of the rapid response time of metal sulfide in gas detection, the good dispersibility of metal oxide nanoparticles and the large surface area of grapheneThe gas sensor has the problems of poor responsiveness, poor stability and short service life, and TiO is enabled to be added with the composite modifier2The nano particles have good dispersibility, so that the gas detection element prepared from the ternary composite gas detection material has higher sensitivity, selectivity and stability for gas detection.

Description

High-sensitivity gas detection material and preparation method thereof
Technical Field
The invention belongs to the technical field of gas detection material preparation processes, and particularly relates to a preparation method of a high-sensitivity gas detection material with sensitivity, responsiveness and selectivity superior to those of a common gas detection material.
Background
The gas detection material is one of functional materials, and when the material meets specific gas, the physical and chemical properties of the material change with the change of the type and concentration of the external gas under certain conditions, so that the material can be used as a gas sensor sensing device. The research on gas detection materials is started in the 30s of the 20 th century in China, and at present, with the increasing requirements of modern society on detection, control and alarm of flammable, explosive, toxic and harmful gases, the performance and the type of the gas detection materials are developed to a certain extent. The metal oxide semiconductor is the most common one of the gas detection materials, but the performance thereof has some problems, such as long response recovery time, poor stability, short life, and the like.
A metal sulfide semiconductor gas sensor is a gas sensor prepared by taking a metal sulfide material as a sensitive material, when a metal sulfide semiconductor device is contacted with a detected gas, surface adsorption or other physical and chemical adsorption actions can be generated, the actions can cause the resistance or work function of a gas detection material to change, namely, the resistance or work function is converted into electric signals, and related information such as the existence concentration of the detected gas can be known according to the strength change of the electric signals.
The metal oxide and the graphene are one of the most commonly used gas sensitive materials at present, and are suitable for being used as gas detection materials due to small size, large specific surface area and high surface activity of nanoparticles, for example, nano titanium dioxide can be used for preparing a gas detection element with high sensitivity, but a single nano material gas sensor has poor selectivity on gas, and meanwhile, the nano material is easy to agglomerate in a solvent and has poor dispersibility, so that the prepared nano material particles have non-uniform conditions, and the responsiveness and the sensitivity on gas detection are influenced.
The responsivity and sensitivity of gas detection materials are greatly dependent on the surface structure and catalytic activity of the materials, so that sensitive materials are often modified to improve the performance of sensors, and two methods are generally adopted: firstly, a gas detection material with a special shape and structure is synthesized, so that the specific surface area and the quantum size of the material are increased; and secondly, synthesizing a gas detection material containing a dopant.
Patent CN108181355A discloses a preparation method of a tin disulfide/graphene/tin dioxide ternary composite gas detection material for a nitrogen dioxide gas detection sensor, aiming at NO2The detection sensitivity of (2) is up to 10ppb, and NO can be detected at low temperature2High sensitivity, low detection limit gas detection response. However, SnO2The nano material has relatively high cost and poor chemical stability, and only oleic acid and oleylamine are added as the surfactant in the preparation process, so that SnO is not effectively improved2As the problem of easy agglomeration of the nano material, the prepared ternary composite nano material has the problem of uneven nano particles, thereby influencing the sensitivity and the responsiveness of gas detection.
Therefore, a novel composite gas detection material capable of effectively improving the nanoparticle aggregation effect and improving the sensitivity, selectivity, responsiveness and stability of the gas sensor is urgently needed.
Disclosure of Invention
The invention aims to provide a graphene/metal oxide/metal sulfide high-sensitivity gas detection material, which overcomes the problems of long response recovery time, poor stability and short service life of a gas sensor prepared by a traditional single metal oxide semiconductor, and solves the technical problem that a dispersion liquid of a nano material is easy to agglomerate by adding a composite modifier in the preparation process, so that the gas sensor prepared from the ternary composite gas detection material has better sensitivity and responsiveness to gas detection.
A high-sensitivity gas detection material is composed of graphene, metal oxide and metal sulfide, and is characterized in that: the metal oxide being TiO2The metal sulfide is CdS, and the specific preparation steps of the composite gas detection material comprise:
preparing graphene oxide by using an improved Hummer method and preparing a graphene oxide solution; and B: preparing a CdS nanowire material; and C: graphene and TiO2Compounding quantum wires; step D: graphene/TiO2And preparing the/CdS ternary composite gas detection material film.
The step A specifically comprises the following steps: the graphene oxide prepared by the Hummer method is placed in an oven at 200 ℃ to be heated for 2 hours to partially reduce the prepared graphene oxide, 30mg of graphene oxide is weighed and placed in a small beaker, 20ml of absolute ethyl alcohol is added to carry out ultrasonic oscillation, 8ml of concentrated HCL and 3ml of distilled water are added to continue oscillation for 3 hours, and graphene oxide solution is formed.
The step B specifically comprises the following steps: 20mmol of thiourea and 8mmol of cadmium nitrate were added in this order to 35ml of an ethylenediamine solution, magnetically stirred for one hour, and then the mixed solution was sonicated for 10min to form a uniform solution. Adding the solution into a polytetrafluoroethylene high-pressure autoclave, carrying out hydrothermal treatment for 36 hours at 180 ℃ in an electric oven, after the reaction is finished, naturally cooling the high-pressure autoclave to room temperature, washing a product by centrifugation, deionized water and absolute ethyl alcohol, drying the product by the oven at 50 ℃ to obtain yellow powder, adding 32.8g of the yellow powder into a 50ml conical flask, adding 30ml of deionized water and 10ml of absolute ethyl alcohol into the conical flask, stirring, carrying out ultrasonic treatment for 30min at 200W to obtain a CdS dispersion liquid, carrying out centrifugal collection, and mixing with the absolute ethyl alcohol to obtain an ethanol solution of CdS.
Further, the step C specifically comprises: adding 1.5-5ml of ethanol and 0.25-1.2ml of graphene oxide solution into a quartz microwave reaction tube, slowly adding 1.3mol of tetrabutyl titanate, stirring for 2 hours, adding a modifier I and a modifier II into the reaction tube to increase the dispersibility of the formed nanoparticles, putting the reaction tube into a microwave reactor, pre-stirring for 30 seconds, reacting for 1.5 hours at 260 ℃, washing a product for 3 times by using absolute ethyl alcohol and distilled water, finally centrifugally collecting, dispersing in ethyl alcohol to obtain graphene/TiO2The quantum wire ethanol solution comprises a modifier I:
Figure RE-GDA0002538165510000031
the modifier II is:
Figure RE-GDA0002538165510000032
further, step D specifically comprises: firstly, graphene and TiO are mixed2Ethanol solution coating of quantum wire on Al with finger electrode2O3Coating the CdS ethanol solution on the graphene/TiO ceramic wafer2The surface of the ethanol solution of the quantum wire reacts for 1.5h, and the aging is carried out for 100h at the temperature of 150 ℃ to obtain the graphene/TiO2the/CdS ternary composite gas detection material.
Furthermore, the mass ratio of the modifier I and the modifier II added in the step C in the preparation method is 1: 2.
Further, graphene/TiO in step D of the preparation method thereof2The volume ratio of the ethanol solution of the quantum wire to the ethanol solution of the CdS is as follows: 1: 3.5-5.
Further, the composition of the high-sensitivity gas detection material is graphene: 0.15-1.48% of TiO2: 13.40-17.23%, CdS: 82.36-85.12%, and the sum of the mass percentages of the three is 100%.
The invention has the beneficial effects that:
1. compared with the single metal oxide or metal sulfide or graphene which is independently used as the gas detection material, the ternary composite gas detection material has better sensitivity and selectivity.
2. The invention is used for preparing graphene/TiO2When the quantum wire ethanol solution is used, a modifier I and a modifier II are added to serve as composite modifiers, and the nano graphene/TiO is treated by the silicon-series composite modifiers2The dispersion system can improve lipophilicity of the formed nano material and effectively increase graphene/TiO2The quantum wires are used as the dispersibility of the nano material in ethanol, and are beneficial to the uniform coating with a CdS ethanol solution, so that the sensitivity and the responsiveness of the synthesized ternary composite gas detection material are further improved.
3. The modifier I and the modifier II are not optional, and not all dispersing agents or active agents can achieve the technical effect of the invention after being mixed, and the invention can effectively improve the dispersibility of the nano material in a solvent compared with a single modifier by greatly realizing the synergistic effect of the modifier I and the modifier II as the composite modifier, thereby being more beneficial to the sensitivity and the responsiveness of the composite gas detection material.
Drawings
FIG. 1 is a transmission electron microscope (SEM) picture of a ternary composite gas detection material prepared in example 1.
FIG. 2 is a graph showing the results of a gas sensor made of the ternary composite gas detecting material prepared in example 1 with respect to 30ppm of ethanol gas, 200ppm of toluene, 200ppm of acetone, and 200ppm of NO2200ppm NO gas.
FIG. 3 is a dynamic response curve of the ternary composite sensing material prepared in example 1 for 0.005ppm, 0.05ppm, 10ppm, 30ppm, 50ppm, 100pmm, 200ppm ethanol gas.
FIG. 4 is a graph showing the responsivity of the ternary complex gas detection materials prepared in example 1 and comparative examples 1 to 5 with respect to 200ppm of ethanol gas.
Detailed Description
Example 1: a high-sensitivity gas detection material is composed of graphene, metal oxide and metal sulfide, and is characterized in that: the metal sulfide is CdS, and the metal oxide is TiO2The specific preparation steps of the composite gas detection material comprise:
preparing graphene oxide by using an improved Hummer method and preparing a graphene oxide solution; and B: preparing a CdS nanowire material; and C: graphene and TiO2Compounding quantum wires; step D: graphene/TiO2And preparing the/CdS ternary composite gas detection material film.
The step A specifically comprises the following steps: the graphene oxide prepared by the Hummer method is placed in an oven at 200 ℃ to be heated for 2 hours to partially reduce the prepared graphene oxide, 30mg of graphene oxide is weighed and placed in a small beaker, 20ml of absolute ethyl alcohol is added to carry out ultrasonic oscillation, 8ml of concentrated HCL and 3ml of distilled water are added to continue oscillation for 3 hours, and graphene oxide solution is formed.
The step B specifically comprises the following steps: 20mmol of thiourea and 8mmol of cadmium nitrate were added in this order to 35ml of an ethylenediamine solution, magnetically stirred for one hour, and then the mixed solution was sonicated for 10min to form a uniform solution. Adding the solution into a polytetrafluoroethylene high-pressure autoclave, carrying out hydrothermal treatment for 36 hours at 180 ℃ in an electric oven, after the reaction is finished, naturally cooling the high-pressure autoclave to room temperature, washing a product by centrifugation, deionized water and absolute ethyl alcohol, drying the product by the oven at 50 ℃ to obtain yellow powder, adding 32.8g of the yellow powder into a 50ml conical flask, adding 30ml of deionized water and 10ml of absolute ethyl alcohol into the conical flask, stirring, carrying out ultrasonic treatment for 30min at 200W to obtain a CdS dispersion liquid, carrying out centrifugal collection, and mixing with the absolute ethyl alcohol to obtain an ethanol solution of CdS.
The step C is specifically as follows: adding 1.5ml of ethanol and 1.2ml of graphene oxide solution into a quartz microwave reaction tube, slowly adding 1.3mol of tetrabutyl titanate, stirring for 2 hours, adding 1.4ml of modifier I and 2.8ml of modifier II into the reaction tube, increasing the dispersibility of the formed nanoparticles, putting the reaction tube into a microwave reactor, pre-stirring for 30 seconds, reacting for 1.5 hours at 260 ℃, washing a product for 3 times by using absolute ethyl alcohol and distilled water, finally centrifugally collecting, dispersing in ethyl alcohol to obtain graphene/TiO2The quantum wire ethanol solution comprises a modifier I:
Figure RE-GDA0002538165510000051
the modifier II is:
Figure RE-GDA0002538165510000052
the mass ratio of the modifier I to the modifier II is 1: 2.
The step D is specifically as follows: firstly, graphene and TiO are mixed2Ethanol solution coating of quantum wire on Al with finger electrode2O3Coating the CdS ethanol solution on the graphene/TiO ceramic wafer2Reacting the surface of quantum wire with ethanol solution for 1.5 hr, and aging at 150 deg.CObtaining the graphene/TiO within 100h2/CdS ternary composite gas detection material, graphene/TiO2The volume ratio of the ethanol solution of the quantum wire to the ethanol solution of the CdS is as follows: 1:3.5.
The ternary composite gas detection material comprises the following components: 0.15%, TiO2: 17.23%, CdS: 82.62 percent, and the sum of the mass percentages of the three is 100 percent.
FIG. 2 is a graphene/TiO2For 30ppm ethanol gas, 200ppm toluene, 200ppm acetone and 200ppm NO of/CdS ternary composite gas detection material2200ppm NO gas, and FIG. 2 shows the response characteristics of graphene/TiO2the/CdS ternary composite gas detection material particularly shows good selectivity on ethanol gas.
FIG. 3 is a graphene/TiO2The sensitivity of the/CdS ternary composite gas detection material is detected for the detection of 0.005ppm, 0.05ppm, 10ppm, 30ppm, 50ppm, 100pmm and 200ppm ethanol gas, and the graphene/TiO can be seen from FIG. 32The lowest detection concentration of the/CdS ternary composite gas detection material is 0.005ppm, the response curve of the CdS ternary composite gas detection material is continuously increased along with the increase of the concentration, and a sensor made of the gas detection material has good repeatability.
The analysis results show that the formed TiO2The polarity of the middle Ti-O bond is larger, water adsorbed on the surface is dissociated due to polarization, hydroxyl is easy to generate, and the surface hydroxyl can improve TiO2As the adsorption performance, the nano graphene/TiO is treated by using silicon series modifier to provide convenience for surface modification2The dispersion system can improve lipophilicity of the formed nano material and effectively increase graphene/TiO2The quantum wires are used as the dispersibility of the nano material in ethanol, so that the quantum wires are beneficial to the uniform coating with a CdS ethanol solution, and the sensitivity and the responsiveness of the synthesized ternary composite gas detection material are further improved.
Example 2: a high-sensitivity gas detection material is composed of graphene, metal oxide and metal sulfide, and is characterized in that: the metal sulfide is CdS, and the metal oxide is TiO2The composite gas detecting materialThe preparation method comprises the following steps:
preparing graphene oxide by using an improved Hummer method and preparing a graphene oxide solution; and B: preparing a CdS nanowire material; and C: graphene and TiO2Compounding quantum wires; step D: graphene/TiO2And preparing the/CdS ternary composite gas detection material film.
The step A specifically comprises the following steps: the graphene oxide prepared by the Hummer method is placed in an oven at 200 ℃ to be heated for 2 hours to partially reduce the prepared graphene oxide, 30mg of graphene oxide is weighed and placed in a small beaker, 20ml of absolute ethyl alcohol is added to carry out ultrasonic oscillation, 8ml of concentrated HCL and 3ml of distilled water are added to continue oscillation for 3 hours, and graphene oxide solution is formed.
The step B specifically comprises the following steps: 20mmol of thiourea and 8mmol of cadmium nitrate were added in this order to 35ml of an ethylenediamine solution, magnetically stirred for one hour, and then the mixed solution was sonicated for 10min to form a uniform solution. Adding the solution into a polytetrafluoroethylene high-pressure autoclave, carrying out hydrothermal treatment for 36 hours at 180 ℃ in an electric oven, after the reaction is finished, naturally cooling the high-pressure autoclave to room temperature, washing a product by centrifugation, deionized water and absolute ethyl alcohol, drying the product by the oven at 50 ℃ to obtain yellow powder, adding 32.8g of the yellow powder into a 50ml conical flask, adding 30ml of deionized water and 10ml of absolute ethyl alcohol into the conical flask, stirring, carrying out ultrasonic treatment for 30min at 200W to obtain a CdS dispersion liquid, carrying out centrifugal collection, and mixing with the absolute ethyl alcohol to obtain an ethanol solution of CdS.
The step C is specifically as follows: adding 5ml of ethanol and 0.25ml of graphene oxide solution into a quartz microwave reaction tube, slowly adding 1.3mol of tetrabutyl titanate, stirring for 2 hours, adding 1.4ml of modifier I and 2.8ml of modifier II into the reaction tube, increasing the dispersibility of the formed nanoparticles, putting the reaction tube into a microwave reactor, pre-stirring for 30 seconds, reacting for 1.5 hours at 260 ℃, washing a product for 3 times by using absolute ethyl alcohol and distilled water, centrifugally collecting, dispersing in ethanol to obtain graphene/TiO2The quantum wire ethanol solution comprises a modifier I:
Figure RE-GDA0002538165510000061
the modifier II is:
Figure RE-GDA0002538165510000071
the mass ratio of the modifier I to the modifier II is 1: 2.
The step D is specifically as follows: firstly, graphene and TiO are mixed2Ethanol solution coating of quantum wire on Al with finger electrode2O3Coating the CdS ethanol solution on the graphene/TiO ceramic wafer2The surface of the ethanol solution of the quantum wire reacts for 1.5h, and the aging is carried out for 100h at the temperature of 150 ℃ to obtain the graphene/TiO2/CdS ternary composite gas detection material, graphene/TiO2The volume ratio of the ethanol solution of the quantum wire to the ethanol solution of the CdS is as follows: 1:5.
The ternary composite gas detection material comprises the following components: 1.48%, TiO2: 13.40%, CdS: 85.12 percent, and the sum of the mass percentages of the three is 100 percent.
Example 3: a high-sensitivity gas detection material is composed of graphene, metal oxide and metal sulfide, and is characterized in that: the metal sulfide is CdS, and the metal oxide is TiO2The specific preparation steps of the composite gas detection material comprise:
preparing graphene oxide by using an improved Hummer method and preparing a graphene oxide solution; and B: preparing a CdS nanowire material; and C: graphene and TiO2Compounding quantum wires; step D: graphene/TiO2And preparing the/CdS ternary composite gas detection material film.
The step A specifically comprises the following steps: the graphene oxide prepared by the Hummer method is placed in an oven at 200 ℃ to be heated for 2 hours to partially reduce the prepared graphene oxide, 30mg of graphene oxide is weighed and placed in a small beaker, 20ml of absolute ethyl alcohol is added to carry out ultrasonic oscillation, 8ml of concentrated HCL and 3ml of distilled water are added to continue oscillation for 3 hours, and graphene oxide solution is formed.
The step B specifically comprises the following steps: 20mmol of thiourea and 8mmol of cadmium nitrate were added in this order to 35ml of an ethylenediamine solution, magnetically stirred for one hour, and then the mixed solution was sonicated for 10min to form a uniform solution. Adding the solution into a polytetrafluoroethylene high-pressure autoclave, carrying out hydrothermal treatment for 36 hours at 180 ℃ in an electric oven, after the reaction is finished, naturally cooling the high-pressure autoclave to room temperature, washing a product by centrifugation, deionized water and absolute ethyl alcohol, drying the product by the oven at 50 ℃ to obtain yellow powder, adding 32.8g of the yellow powder into a 50ml conical flask, adding 30ml of deionized water and 10ml of absolute ethyl alcohol into the conical flask, stirring, carrying out ultrasonic treatment for 30min at 200W to obtain a CdS dispersion liquid, carrying out centrifugal collection, and mixing with the absolute ethyl alcohol to obtain an ethanol solution of CdS.
The step C is specifically as follows: adding 5ml of ethanol and 0.25ml of graphene oxide solution into a quartz microwave reaction tube, slowly adding 1.3mol of tetrabutyl titanate, stirring for 2 hours, adding 1.4ml of modifier I and 2.8ml of modifier II into the reaction tube, increasing the dispersibility of the formed nanoparticles, putting the reaction tube into a microwave reactor, pre-stirring for 30 seconds, reacting for 1.5 hours at 260 ℃, washing a product for 3 times by using absolute ethyl alcohol and distilled water, centrifugally collecting, dispersing in ethanol to obtain graphene/TiO2The quantum wire ethanol solution comprises a modifier I:
Figure RE-GDA0002538165510000081
the modifier II is:
Figure RE-GDA0002538165510000082
the mass ratio of the modifier I to the modifier II is 1: 2.
The step D is specifically as follows: firstly, graphene and TiO are mixed2Ethanol solution coating of quantum wire on Al with finger electrode2O3Coating the CdS ethanol solution on the graphene/TiO ceramic wafer2The surface of the ethanol solution of the quantum wire reacts for 1.5h, and the aging is carried out for 100h at the temperature of 150 ℃ to obtain the graphene/TiO2/CdS ternary composite gas detection material, graphene/TiO2The volume ratio of the ethanol solution of the quantum wire to the ethanol solution of the CdS is as follows: 1:4.
Ternary composite gasThe composition of the detection material is graphene: 0.41%, TiO2: 17.23%, CdS: 82.36 percent, and the sum of the mass percentages of the three is 100 percent.
Example 4: a high-sensitivity gas detection material is composed of graphene, metal oxide and metal sulfide, and is characterized in that: the metal sulfide is CdS, and the metal oxide is TiO2The specific preparation steps of the composite gas detection material comprise:
preparing graphene oxide by using an improved Hummer method and preparing a graphene oxide solution; and B: preparing a CdS nanowire material; and C: graphene and TiO2Compounding quantum wires; step D: graphene/TiO2And preparing the/CdS ternary composite gas detection material film.
The step A specifically comprises the following steps: the graphene oxide prepared by the Hummer method is placed in an oven at 200 ℃ to be heated for 2 hours to partially reduce the prepared graphene oxide, 30mg of graphene oxide is weighed and placed in a small beaker, 20ml of absolute ethyl alcohol is added to carry out ultrasonic oscillation, 8ml of concentrated HCL and 3ml of distilled water are added to continue oscillation for 3 hours, and graphene oxide solution is formed.
The step B specifically comprises the following steps: 20mmol of thiourea and 8mmol of cadmium nitrate were added in this order to 35ml of an ethylenediamine solution, magnetically stirred for one hour, and then the mixed solution was sonicated for 10min to form a uniform solution. Adding the solution into a polytetrafluoroethylene high-pressure autoclave, carrying out hydrothermal treatment for 36 hours at 180 ℃ in an electric oven, after the reaction is finished, naturally cooling the high-pressure autoclave to room temperature, washing a product by centrifugation, deionized water and absolute ethyl alcohol, drying the product by the oven at 50 ℃ to obtain yellow powder, adding 32.8g of the yellow powder into a 50ml conical flask, adding 30ml of deionized water and 10ml of absolute ethyl alcohol into the conical flask, stirring, carrying out ultrasonic treatment for 30min at 200W to obtain a CdS dispersion liquid, carrying out centrifugal collection, and mixing with the absolute ethyl alcohol to obtain an ethanol solution of CdS.
The step C is specifically as follows: adding 5ml of ethanol and 0.25ml of graphene oxide solution into a quartz microwave reaction tube, slowly adding 1.3mol of tetrabutyl titanate, stirring for 2 hours, adding 1.4ml of modifier I and 2.8ml of modifier II into the reaction tube, and enlargingForming the dispersibility of the nano particles, putting the reaction tube into a microwave reactor, pre-stirring for 30s, reacting for 1.5h at 260 ℃, washing the product with absolute ethyl alcohol and distilled water for 3 times, finally centrifugally collecting, dispersing in ethanol to obtain the graphene/TiO2The quantum wire ethanol solution comprises a modifier I:
Figure RE-GDA0002538165510000091
the modifier II is:
Figure RE-GDA0002538165510000092
the mass ratio of the modifier I to the modifier II is 1: 2.
The step D is specifically as follows: firstly, graphene and TiO are mixed2Ethanol solution coating of quantum wire on Al with finger electrode2O3Coating the CdS ethanol solution on the graphene/TiO ceramic wafer2The surface of the ethanol solution of the quantum wire reacts for 1.5h, and the aging is carried out for 100h at the temperature of 150 ℃ to obtain the graphene/TiO2/CdS ternary composite gas detection material, graphene/TiO2The volume ratio of the ethanol solution of the quantum wire to the ethanol solution of the CdS is as follows: 1:4.
The ternary composite gas detection material comprises the following components: 0.60% of TiO2: 16.80%, CdS: 82.60 percent, and the sum of the mass percentages of the three is 100 percent.
Comparative example 1: a high-sensitivity gas detection material is composed of graphene, metal oxide and metal sulfide, and is characterized in that: the metal sulfide is CdS, and the metal oxide is TiO2The specific preparation steps of the composite gas detection material comprise:
preparing graphene oxide by using an improved Hummer method and preparing a graphene oxide solution; and B: preparing a CdS nanowire material; and C: graphene and TiO2Compounding quantum wires; step D: graphene/TiO2And preparing the/CdS ternary composite gas detection material film.
The step A specifically comprises the following steps: the graphene oxide prepared by the Hummer method is placed in an oven at 200 ℃ to be heated for 2 hours to partially reduce the prepared graphene oxide, 30mg of graphene oxide is weighed and placed in a small beaker, 20ml of absolute ethyl alcohol is added to carry out ultrasonic oscillation, 8ml of concentrated HCL and 3ml of distilled water are added to continue oscillation for 3 hours, and graphene oxide solution is formed.
The step B specifically comprises the following steps: 20mmol of thiourea and 8mmol of cadmium nitrate were added in this order to 35ml of an ethylenediamine solution, magnetically stirred for one hour, and then the mixed solution was sonicated for 10min to form a uniform solution. Adding the solution into a polytetrafluoroethylene high-pressure autoclave, carrying out hydrothermal treatment for 36 hours at 180 ℃ in an electric oven, after the reaction is finished, naturally cooling the high-pressure autoclave to room temperature, washing a product by centrifugation, deionized water and absolute ethyl alcohol, drying the product by the oven at 50 ℃ to obtain yellow powder, adding 32.8g of the yellow powder into a 50ml conical flask, adding 30ml of deionized water and 10ml of absolute ethyl alcohol into the conical flask, stirring, carrying out ultrasonic treatment for 30min at 200W to obtain a CdS dispersion liquid, carrying out centrifugal collection, and mixing with the absolute ethyl alcohol to obtain an ethanol solution of CdS.
The step C is specifically as follows: adding 1.5ml of ethanol and 1.2ml of graphene oxide solution into a quartz microwave reaction tube, slowly adding 1.3mol of tetrabutyl titanate, stirring for 2 hours, adding a modifier I into the reaction tube to increase the dispersibility of the formed nanoparticles, putting the reaction tube into a microwave reactor, pre-stirring for 30 seconds, reacting for 1.5 hours at 260 ℃, washing a product with absolute ethyl alcohol and distilled water for 3 times, centrifugally collecting, dispersing in ethanol to obtain graphene/TiO2Quantum wire ethanol solution, 1.4ml modifier i:
Figure RE-GDA0002538165510000101
the step D is specifically as follows: firstly, graphene and TiO are mixed2Ethanol solution coating of quantum wire on Al with finger electrode2O3Coating the CdS ethanol solution on the graphene/TiO ceramic wafer2The surface of the ethanol solution of the quantum wire reacts for 1.5h, and the aging is carried out for 100h at the temperature of 150 ℃ to obtain the graphene/TiO2/CdS ternary composite gas detection material, graphene/TiO2The volume ratio of the ethanol solution of the quantum wire to the ethanol solution of the CdS is as follows: 1:3.5.
The ternary composite gas detection material comprises the following components: 0.15%, TiO2: 17.23%, CdS: 82.62 percent, and the sum of the mass percentages of the three is 100 percent.
Comparative example 2: a high-sensitivity gas detection material is composed of graphene, metal oxide and metal sulfide, and is characterized in that: the metal sulfide is CdS, and the metal oxide is TiO2The specific preparation steps of the composite gas detection material comprise:
preparing graphene oxide by using an improved Hummer method and preparing a graphene oxide solution; and B: preparing a CdS nanowire material; and C: graphene and TiO2Compounding quantum wires; step D: graphene/TiO2And preparing the/CdS ternary composite gas detection material film.
The step A specifically comprises the following steps: the graphene oxide prepared by the Hummer method is placed in an oven at 200 ℃ to be heated for 2 hours to partially reduce the prepared graphene oxide, 30mg of graphene oxide is weighed and placed in a small beaker, 20ml of absolute ethyl alcohol is added to carry out ultrasonic oscillation, 8ml of concentrated HCL and 3ml of distilled water are added to continue oscillation for 3 hours, and graphene oxide solution is formed.
The step B specifically comprises the following steps: 20mmol of thiourea and 8mmol of cadmium nitrate were added in this order to 35ml of an ethylenediamine solution, magnetically stirred for one hour, and then the mixed solution was sonicated for 10min to form a uniform solution. Adding the solution into a polytetrafluoroethylene high-pressure autoclave, carrying out hydrothermal treatment for 36 hours at 180 ℃ in an electric oven, after the reaction is finished, naturally cooling the high-pressure autoclave to room temperature, washing a product by centrifugation, deionized water and absolute ethyl alcohol, drying the product by the oven at 50 ℃ to obtain yellow powder, adding 32.8g of the yellow powder into a 50ml conical flask, adding 30ml of deionized water and 10ml of absolute ethyl alcohol into the conical flask, stirring, carrying out ultrasonic treatment for 30min at 200W to obtain a CdS dispersion liquid, carrying out centrifugal collection, and mixing with the absolute ethyl alcohol to obtain an ethanol solution of CdS.
The step C is specifically as follows: 1.5ml of ethanol and 1.2ml of graphene oxide solution are added into a quartz microwave reaction tubeSlowly adding 1.3mol of tetrabutyl titanate into the solution, stirring the solution for 2 hours, adding 2.8ml of modifier II into a reaction tube to increase the dispersibility of the formed nanoparticles, putting the reaction tube into a microwave reactor, pre-stirring the solution for 30 seconds, reacting the reaction tube for 1.5 hours at 260 ℃, washing the product for 3 times by using absolute ethyl alcohol and distilled water, centrifugally collecting the product, dispersing the product in the ethyl alcohol to obtain the graphene/TiO2The quantum wire ethanol solution and the modifier II are as follows:
Figure RE-GDA0002538165510000111
the step D is specifically as follows: firstly, graphene and TiO are mixed2Ethanol solution coating of quantum wire on Al with finger electrode2O3Coating the CdS ethanol solution on the graphene/TiO ceramic wafer2The surface of the ethanol solution of the quantum wire reacts for 1.5h, and the aging is carried out for 100h at the temperature of 150 ℃ to obtain the graphene/TiO2/CdS ternary composite gas detection material, graphene/TiO2The volume ratio of the ethanol solution of the quantum wire to the ethanol solution of the CdS is as follows: 1:3.5.
The ternary composite gas detection material comprises the following components: 0.15%, TiO2: 17.23%, CdS: 82.62 percent, and the sum of the mass percentages of the three is 100 percent.
Comparative example 3: a high-sensitivity gas detection material is composed of graphene, metal oxide and metal sulfide, and is characterized in that: the metal sulfide is CdS, and the metal oxide is TiO2The specific preparation steps of the composite gas detection material comprise:
preparing graphene oxide by using an improved Hummer method and preparing a graphene oxide solution; and B: preparing a CdS nanowire material; and C: graphene and TiO2Compounding quantum wires; step D: graphene/TiO2And preparing the/CdS ternary composite gas detection material film.
The step A specifically comprises the following steps: the graphene oxide prepared by the Hummer method is placed in an oven at 200 ℃ to be heated for 2 hours to partially reduce the prepared graphene oxide, 30mg of graphene oxide is weighed and placed in a small beaker, 20ml of absolute ethyl alcohol is added to carry out ultrasonic oscillation, 8ml of concentrated HCL and 3ml of distilled water are added to continue oscillation for 3 hours, and graphene oxide solution is formed.
The step B specifically comprises the following steps: 20mmol of thiourea and 8mmol of cadmium nitrate were added in this order to 35ml of an ethylenediamine solution, magnetically stirred for one hour, and then the mixed solution was sonicated for 10min to form a uniform solution. Adding the solution into a polytetrafluoroethylene high-pressure autoclave, carrying out hydrothermal treatment for 36 hours at 180 ℃ in an electric oven, after the reaction is finished, naturally cooling the high-pressure autoclave to room temperature, washing a product by centrifugation, deionized water and absolute ethyl alcohol, drying the product by the oven at 50 ℃ to obtain yellow powder, adding 32.8g of the yellow powder into a 50ml conical flask, adding 30ml of deionized water and 10ml of absolute ethyl alcohol into the conical flask, stirring, carrying out ultrasonic treatment for 30min at 200W to obtain a CdS dispersion liquid, carrying out centrifugal collection, and mixing with the absolute ethyl alcohol to obtain an ethanol solution of CdS.
The step C is specifically as follows: adding 1.5ml of ethanol and 1.2ml of graphene oxide solution into a quartz microwave reaction tube, slowly adding 1.3mol of tetrabutyl titanate, stirring for 2 hours, adding 1.4ml of modifier I and 2.8ml of oleic acid into the reaction tube, increasing the dispersibility of the formed nanoparticles, putting the reaction tube into a microwave reactor, pre-stirring for 30 seconds, reacting for 1.5 hours at 260 ℃, washing a product for 3 times by using absolute ethyl alcohol and distilled water, centrifugally collecting, dispersing in ethyl alcohol to obtain graphene/TiO2The mass ratio of the quantum wire ethanol solution, the modifier I and the oleic acid is 1: 2.
The step D is specifically as follows: firstly, graphene and TiO are mixed2Ethanol solution coating of quantum wire on Al with finger electrode2O3Coating the CdS ethanol solution on the graphene/TiO ceramic wafer2The surface of the ethanol solution of the quantum wire reacts for 1.5h, and the aging is carried out for 100h at the temperature of 150 ℃ to obtain the graphene/TiO2/CdS ternary composite gas detection material, graphene/TiO2The volume ratio of the ethanol solution of the quantum wire to the ethanol solution of the CdS is as follows: 1:3.5.
The ternary composite gas detection material comprises the following components: 0.15%, TiO2: 17.23%, CdS: 82.62 percent, and the sum of the mass percentages of the three is 100 percent.
Comparison ofExample 4: a high-sensitivity gas detection material is composed of graphene, metal oxide and metal sulfide, and is characterized in that: the metal sulfide is CdS, and the metal oxide is TiO2The specific preparation steps of the composite gas detection material comprise:
preparing graphene oxide by using an improved Hummer method and preparing a graphene oxide solution; and B: preparing a CdS nanowire material; and C: graphene and TiO2Compounding quantum wires; step D: graphene/TiO2And preparing the/CdS ternary composite gas detection material film.
The step A specifically comprises the following steps: the graphene oxide prepared by the Hummer method is placed in an oven at 200 ℃ to be heated for 2 hours to partially reduce the prepared graphene oxide, 30mg of graphene oxide is weighed and placed in a small beaker, 20ml of absolute ethyl alcohol is added to carry out ultrasonic oscillation, 8ml of concentrated HCL and 3ml of distilled water are added to continue oscillation for 3 hours, and graphene oxide solution is formed.
The step B specifically comprises the following steps: 20mmol of thiourea and 8mmol of cadmium nitrate were added in this order to 35ml of an ethylenediamine solution, magnetically stirred for one hour, and then the mixed solution was sonicated for 10min to form a uniform solution. Adding the solution into a polytetrafluoroethylene high-pressure autoclave, carrying out hydrothermal treatment for 36 hours at 180 ℃ in an electric oven, after the reaction is finished, naturally cooling the high-pressure autoclave to room temperature, washing a product by centrifugation, deionized water and absolute ethyl alcohol, drying the product by the oven at 50 ℃ to obtain yellow powder, adding 32.8g of the yellow powder into a 50ml conical flask, adding 30ml of deionized water and 10ml of absolute ethyl alcohol into the conical flask, stirring, carrying out ultrasonic treatment for 30min at 200W to obtain a CdS dispersion liquid, carrying out centrifugal collection, and mixing with the absolute ethyl alcohol to obtain an ethanol solution of CdS.
The step C is specifically as follows: adding 1.5ml ethanol and 1.2ml graphene oxide solution into a quartz microwave reaction tube, slowly adding 1.3mol tetrabutyl titanate, stirring for 2h, adding 2.8ml oleic acid and 0.4ml oleylamine into the reaction tube, increasing the dispersibility of the formed nanoparticles, putting the reaction tube into a microwave reactor, pre-stirring for 30s, reacting at 260 ℃ for 1.5h, washing the product with absolute ethyl alcohol and distilled water for 3 times, finally centrifugally collecting, dispersing and collectingObtaining graphene/TiO in ethanol2The mass ratio of the quantum wire ethanol solution, the oleic acid and the oleylamine is 1: 2.
The step D is specifically as follows: firstly, graphene and TiO are mixed2Ethanol solution coating of quantum wire on Al with finger electrode2O3Coating the CdS ethanol solution on the graphene/TiO ceramic wafer2The surface of the ethanol solution of the quantum wire reacts for 1.5h, and the aging is carried out for 100h at the temperature of 150 ℃ to obtain the graphene/TiO2/CdS ternary composite gas detection material, graphene/TiO2The volume ratio of the ethanol solution of the quantum wire to the ethanol solution of the CdS is as follows: 1:3.5.
The ternary composite gas detection material comprises the following components: 0.15%, TiO2: 17.23%, CdS: 82.62 percent, and the sum of the mass percentages of the three is 100 percent.
Comparative example 5: a high-sensitivity gas detection material is composed of graphene, metal oxide and metal sulfide, and is characterized in that: the metal sulfide is CdS, and the metal oxide is TiO2The specific preparation steps of the composite gas detection material comprise:
preparing graphene oxide by using an improved Hummer method and preparing a graphene oxide solution; and B: preparing a CdS nanowire material; and C: graphene and TiO2Compounding quantum wires; step D: graphene/TiO2And preparing the/CdS ternary composite gas detection material film.
The step A specifically comprises the following steps: the graphene oxide prepared by the Hummer method is placed in an oven at 200 ℃ to be heated for 2 hours to partially reduce the prepared graphene oxide, 30mg of graphene oxide is weighed and placed in a small beaker, 20ml of absolute ethyl alcohol is added to carry out ultrasonic oscillation, 8ml of concentrated HCL and 3ml of distilled water are added to continue oscillation for 3 hours, and graphene oxide solution is formed.
The step B specifically comprises the following steps: 20mmol of thiourea and 8mmol of cadmium nitrate were added in this order to 35ml of an ethylenediamine solution, magnetically stirred for one hour, and then the mixed solution was sonicated for 10min to form a uniform solution. Adding the solution into a polytetrafluoroethylene high-pressure autoclave, carrying out hydrothermal treatment for 36 hours at 180 ℃ in an electric oven, after the reaction is finished, naturally cooling the high-pressure autoclave to room temperature, washing a product by centrifugation, deionized water and absolute ethyl alcohol, drying the product by the oven at 50 ℃ to obtain yellow powder, adding 32.8g of the yellow powder into a 50ml conical flask, adding 30ml of deionized water and 10ml of absolute ethyl alcohol into the conical flask, stirring, carrying out ultrasonic treatment for 30min at 200W to obtain a CdS dispersion liquid, carrying out centrifugal collection, and mixing with the absolute ethyl alcohol to obtain an ethanol solution of CdS.
The step C is specifically as follows: adding 1.5ml of ethanol and 1.2ml of graphene oxide solution into a quartz microwave reaction tube, slowly adding 1.3mol of tetrabutyl titanate, stirring for 2 hours to increase the dispersibility of the formed nanoparticles, putting the reaction tube into a microwave reactor, pre-stirring for 30 seconds, reacting for 1.5 hours at 260 ℃, washing a product with absolute ethyl alcohol and distilled water for 3 times, finally centrifugally collecting, dispersing in ethanol to obtain graphene/TiO2Quantum wire ethanol solution.
The step D is specifically as follows: firstly, graphene and TiO are mixed2Ethanol solution coating of quantum wire on Al with finger electrode2O3Coating the CdS ethanol solution on the graphene/TiO ceramic wafer2The surface of the ethanol solution of the quantum wire reacts for 1.5h, and the aging is carried out for 100h at the temperature of 150 ℃ to obtain the graphene/TiO2/CdS ternary composite gas detection material, graphene/TiO2The volume ratio of the ethanol solution of the quantum wire to the ethanol solution of the CdS is as follows: 1:3.5.
The ternary composite gas detection material comprises the following components: 0.15%, TiO2: 17.23%, CdS: 82.62 percent, and the sum of the mass percentages of the three is 100 percent.
To further verify the effectiveness of modifier I and modifier II as composite modifiers, FIG. 4 shows the response of the ternary composite material prepared in example 1 to the sensitive materials prepared in comparative examples 1-5 to 200ppm of ethanol gas, as can be seen in FIG. 4: compared with a ternary composite gas detection material without a modifier, the ternary composite gas detection material has the advantages that the modifier is used in the preparation process of the ternary composite gas detection material, so that the sensitivity of the ternary composite gas detection material can be obviously improved; (2) compared with the ternary composite gas detection material taking oleic acid and oleylamine as surfactants in the prior art, the modifier I and the modifier II are used as composite modifiers, so that better responsiveness and sensitivity can be formed for ethanol gas; (2) compared with a single modifier I or a modifier II, the composite modifier forms a good synergistic effect, and the responsiveness and the sensitivity to ethanol gas are obviously improved.

Claims (8)

1. A high-sensitivity gas detection material is composed of graphene, metal oxide and metal sulfide, and is characterized in that: the metal oxide being TiO2The metal sulfide is CdS, and the specific preparation steps of the composite gas detection material comprise:
preparing graphene oxide by using an improved Hummer method and preparing a graphene oxide solution; and B: preparing a CdS nanowire material; and C: graphene and TiO2Compounding quantum wires; step D: graphene/TiO2And preparing the/CdS ternary composite gas detection material film.
2. The high-sensitivity gas detection material according to claim 1, wherein the step a is specifically as follows: the graphene oxide prepared by the Hummer method is placed in an oven at 200 ℃ to be heated for 2 hours to partially reduce the prepared graphene oxide, 30mg of graphene oxide is weighed and placed in a small beaker, 20ml of absolute ethyl alcohol is added to carry out ultrasonic oscillation, 8ml of concentrated HCL and 3ml of distilled water are added to continue oscillation for 3 hours, and graphene oxide solution is formed.
3. The high-sensitivity gas detection material according to claim 1, wherein the preparation method comprises the following specific steps: 20mmol of thiourea and 8mmol of cadmium nitrate were added in this order to 35ml of an ethylenediamine solution, magnetically stirred for one hour, and then the mixed solution was sonicated for 10min to form a uniform solution. Adding the solution into a polytetrafluoroethylene high-pressure autoclave, carrying out hydrothermal treatment for 36 hours at 180 ℃ in an electric oven, after the reaction is finished, naturally cooling the high-pressure autoclave to room temperature, washing a product by centrifugation, deionized water and absolute ethyl alcohol, drying the product by the oven at 50 ℃ to obtain yellow powder, adding 32.8g of the yellow powder into a 50ml conical flask, adding 30ml of deionized water and 10ml of absolute ethyl alcohol into the conical flask, stirring, carrying out ultrasonic treatment for 30min at 200W to obtain a CdS dispersion liquid, carrying out centrifugal collection, and mixing with the absolute ethyl alcohol to obtain an ethanol solution of CdS.
4. The high-sensitivity gas detection material according to claim 1, wherein the preparation method comprises the following specific steps: adding 1.5-5ml of ethanol and 0.25-1.2ml of graphene oxide solution into a quartz microwave reaction tube, slowly adding 1.3mol of tetrabutyl titanate, stirring for 2 hours, adding a modifier I and a modifier II into the reaction tube to increase the dispersibility of the formed nanoparticles, putting the reaction tube into a microwave reactor, pre-stirring for 30 seconds, reacting for 1.5 hours at 260 ℃, washing a product for 3 times by using absolute ethyl alcohol and distilled water, finally centrifugally collecting, dispersing in ethyl alcohol to obtain graphene/TiO2The quantum wire ethanol solution comprises a modifier I:
Figure FDA0002483719620000011
the modifier II is:
Figure FDA0002483719620000021
5. the high-sensitivity gas detection material according to claim 1, wherein the preparation method comprises the following specific steps: firstly, graphene and TiO are mixed2Ethanol solution coating of quantum wire on Al with finger electrode2O3Coating the CdS ethanol solution on the graphene/TiO ceramic wafer2The surface of the ethanol solution of the quantum wire reacts for 1.5h, and the aging is carried out for 100h at the temperature of 150 ℃ to obtain the graphene/TiO2the/CdS ternary composite gas detection material.
6. The highly sensitive gas detecting material according to claim 4, wherein the modifier I and the modifier II are added in the step C in a mass ratio of 1: 2.
7. The highly sensitive gas detecting material according to claim 5, wherein the graphene/TiO in step D of the preparation method2The volume ratio of the ethanol solution of the quantum wire to the ethanol solution of the CdS is as follows: 1: 3.5-5.
8. The highly sensitive gas detection material according to claim 5, wherein the composition of the highly sensitive gas detection material is graphene: 0.15-1.48% of TiO2: 13.40-17.23%, CdS: 82.36-85.12%, and the sum of the mass percentages of the three is 100%.
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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114014313A (en) * 2022-01-06 2022-02-08 河北化工医药职业技术学院 Graphene-based gas-sensitive material and preparation method thereof

Cited By (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN114014313A (en) * 2022-01-06 2022-02-08 河北化工医药职业技术学院 Graphene-based gas-sensitive material and preparation method thereof
CN114014313B (en) * 2022-01-06 2022-03-22 河北化工医药职业技术学院 Graphene-based gas-sensitive material and preparation method thereof

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