CN112903751A - Xylene gas sensor based on gold-palladium alloy modified SnS2 sensitive layer and preparation method thereof - Google Patents

Xylene gas sensor based on gold-palladium alloy modified SnS2 sensitive layer and preparation method thereof Download PDF

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CN112903751A
CN112903751A CN202110000519.XA CN202110000519A CN112903751A CN 112903751 A CN112903751 A CN 112903751A CN 202110000519 A CN202110000519 A CN 202110000519A CN 112903751 A CN112903751 A CN 112903751A
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palladium alloy
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卢洋
阮圣平
刘大力
周敬然
刘彩霞
李昕
温善鹏
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Jilin University
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Abstract

SnS based on gold-palladium alloy modification2A xylene gas sensor of a sensitive layer and a preparation method thereof belong to the technical field of gas sensors. The sensor is sequentially composed of Al from bottom to top2O3Substrate, Pd metal interdigital electrode, and Al with Pd metal interdigital electrode2O3SnS decorated by gold-palladium alloy and prepared by coating technology on substrate2And (4) forming a sensitive layer. When the gold-palladium alloy is modified in SnS2The gas sensor has good gas response and excellent gas selectivity due to the synergistic effect of the bimetal. Meanwhile, the method has simple process, and the prepared xylene gas sensor has small volume and is suitable for mass production, thereby having important application value. The method has the characteristics of simple preparation method, low cost, high response recovery speed and hopeful large-scale production, and has good detection performance on the dimethylbenzene gas.

Description

SnS based on gold-palladium alloy modification2Xylene gas sensor of sensitive layer and preparation method thereof
Technical Field
The invention belongs to the technical field of gas sensors, and particularly relates to gold-palladium alloy modified SnS2A xylene gas sensor of a sensitive layer and a preparation method thereof.
Background
With the rapid development of industrial technology and the increasing awareness of human safety, health problems caused by volatile organic compounds have become a focus of social attention. People are more and more frequently exposed to dangerous gases, such as natural gas with methane and carbon monoxide as main components, organic volatile toxic gases such as formaldehyde, benzene and xylene released from decoration materials, sulfur dioxide and nitrogen oxides in coal combustion and automobile exhaust, and the like. Once the flammable and explosive, toxic and harmful gases are generated or leaked, the health and life of people are threatened. Therefore, it is necessary to develop a gas sensor having high sensitivity and high detection speed.
Xylene is an important chemical raw material, and the main sources of xylene in the atmospheric environment are paint, dye, synthetic fiber, synthetic rubber, petroleum processing industry and the like. In addition, accidental leakage during transportation, storage, etc. can also cause contamination of the xylene. Besides a series of pollution to air, the xylene gas also has great harm to human bodies, such as stimulation to eyes and upper respiratory tract of people, anesthesia to central system and the like. Therefore, it has been important to design and manufacture a gas sensor having high sensitivity and high selectivity to detect xylene in air.
There are many materials used for gas sensors, such as the more traditional oxide semiconductor sensitive materials. But nowadays more and more new materials are being soughtOf wide interest, the two-dimensional material SnS as used in the present invention2. There are many methods for improving the response of the sensitive material, such as modifying the noble metal, changing the morphology of the sensitive material or changing the structure of the sensitive material. The modification with noble metals is a common and simple method, and is widely used in gas detection, energy storage and photocatalysis.
SnS used in the invention and based on gold-palladium alloy modification2The two-dimensional sheet structure material has very good application potential due to low energy consumption and small pollution. The gas sensor manufactured by the method utilizes the sensitive material to directly adsorb and detect gas, so that the electrical property and the like of the material are changed, and the gas concentration is detected by testing the change of the output signal of the sensitive element.
Disclosure of Invention
The invention aims to provide SnS modified based on gold-palladium alloy2A xylene gas sensor of a sensitive layer and a preparation method thereof. The method is simple and easy to implement, few in working procedures, low in cost and low in equipment requirement, can improve the gas-sensitive response of the gas sensor to the dimethylbenzene gas, is suitable for mass production, and has important application value. As shown in figure 1, the SnS based on the gold-palladium alloy modification is disclosed by the invention2The xylene gas sensor of the sensitive layer is sequentially composed of Al from bottom to top2O3Substrate, Pd metal interdigital electrode, and Al with Pd metal interdigital electrode2O3SnS decorated by gold-palladium alloy and prepared by coating technology on substrate2A sensitive layer of a two-dimensional sheet-like structural material; SnS2The diameter of the two-dimensional sheet structure material is 550-650 nm, the width and the spacing of the Pd metal interdigital electrodes are 0.15-0.20 mm, and the thickness is 100-150 nm.
SnS2As a typical two-dimensional material, the excellent semiconductor performance of the material enables the material to play a good role in the field of gas sensors, such as large surface area/volume ratio, high thermal stability, excellent adsorption capacity and the like, which is beneficial to improving the gas-sensitive performance of the material; the common modification of the gold-palladium alloy plays a role of the synergy of bimetal and promotes gasThe adsorption of molecules on the surface of the material greatly improves the gas-sensitive performance of the material. Meanwhile, the method has simple process, and the prepared device has small volume and is suitable for mass production, thereby having important application value.
The invention provides a method for preparing the xylene gas sensor, which comprises the following steps:
1. treatment of Pd metal interdigital electrode
Wiping Al with Pd metal interdigital electrode (prepared by screen printing technology) with acetone and ethanol cotton balls respectively2O3A substrate, and Al with Pd metal interdigital electrode2O3Sequentially placing the substrate in acetone, ethanol and deionized water, respectively ultrasonically cleaning for 5-10 minutes, and finally drying at 100-120 ℃;
the invention uses the silk-screen printing technology to print Al2O3Preparing Pd metal interdigital electrodes on the substrate. The specific method comprises the following steps: mixing the ink [ Jiahua JX07500487]: 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 interdigital electrode patterns, scraping the paste under the conditions of an inclination angle of 30-45 degrees and a pressure of 5-10N, printing electrodes, drying, and curing by ultraviolet light to finish the preparation of the Pd metal interdigital electrode, wherein the width and the electrode spacing of the Pd metal interdigital electrode are 0.15-0.20 mm, and the thickness of the Pd metal interdigital electrode is 100-150 nm.
2. SnS modified by gold-palladium alloy2Preparation of two-dimensional sheet-like structural material
(1) Preparation of SnS2Two-dimensional sheet structure material: SnS2Prepared by a simple hydrothermal method, and specifically 0.5-1 mmol of SnCl4·5H2O and 2.5-3.5 mmol CH4N2S (thiourea) is added into 20-50 mL of deionized water, and the mixture is stirred for 0.5-1 h at the rotating speed of 300-400 rpm by strong magnetic force until the mixture is uniformly mixed; then transferring the obtained mixed solution into a 50mL stainless steel high-pressure reaction kettle with polytetrafluoroethylene as an inner lining, carrying out hydrothermal reaction at 170-210 ℃ for 16-24 h, and obtaining SnS2Washing with deionized water and ethanol, and drying at 60-80 deg.C for 12-24Hour(s) to obtain SnS2A two-dimensional sheet structure material;
(2) preparation of gold-palladium alloy modified SnS2Two-dimensional sheet structure material: the gold and palladium simple substances are obtained by reducing chloroauric acid and chloropalladic acid by ascorbic acid, and a chloroauric acid solution (20mM) and a chloropalladic acid solution (20mM) are prepared firstly. 0.34g of HAuCl4·4H2Dissolving O in 50mL of deionized water, and stirring until the O is completely dissolved to obtain a 20mM chloroauric acid solution; 0.177g of PdCl2Dissolving in 1.5mL hydrochloric acid with mass fraction of 37%, stirring to completely dissolve, and adding deionized water to 50mL to obtain 20mM chloropalladate solution; the specific modification ratio is as follows: au and SnS2In a molar ratio of 0.15 to 0.25: 1; pd and SnS2In a molar ratio of 0.15 to 0.25: 1; AuPd alloy and SnS2In a molar ratio of 0.15 to 0.25: 1. the specific modification scheme is as follows: adding 0.01-0.1 g of SnS2Dispersing the two-dimensional sheet structure material into 20-40 mL of deionized water, stirring for 2-5 h to form uniformly dispersed suspension, adding 2000-3000 mu L of chloroauric acid solution into the suspension, and stirring; adding 0.01-0.1 g of SnS2Dispersing the two-dimensional sheet structure material into 20-40 mL of deionized water, stirring for 2-5 h to form uniformly dispersed suspension, adding 2000-3000 mu L of chloropalladate solution into the suspension, and stirring; adding 0.01-0.1 g of SnS2Dispersing the two-dimensional sheet structure material into 20-40 mL of deionized water, stirring for 2-5 h to form uniformly dispersed suspension, respectively adding 1000-2000 mu L of chloroauric acid solution and equal volume of chloropalladate solution, and stirring; after uniformly stirring, adding 1-5 mL of ascorbic acid solution (0.1M), continuously stirring for 2-5 h to obtain Au-modified SnS2Au modified SnS2And SnS modified by AuPd alloy2Centrifuging by using ethanol and deionized water, and drying at 60-80 ℃ for 6-12 hours to finally form Au and SnS respectively2In a molar ratio of 0.15 to 0.25: 1.pd and SnS2In a molar ratio of 0.15 to 0.25: 1 and AuPd alloy and SnS2The molar ratio of the nano-materials is 0.15-0.25: 1; for convenience, the materials obtained by the preparation are respectively marked as SnS2、Au-SnS2、Pd-SnS2、AuPd-SnS2
3. SnS based on gold-palladium alloy modification2Preparing a gas sensor of a sensitive layer of a two-dimensional sheet-like structure material: SnS modified by the prepared gold-palladium alloy2Putting the two-dimensional sheet structure material into a mortar, and grinding for 5-10 minutes to obtain a powdery material; then, dropping deionized water into the mortar, and grinding for 5-10 minutes to obtain viscous slurry; dipping a small amount of slurry by using a hairbrush, and coating the slurry on Al with Pd metal interdigital electrodes2O3Drying the substrate at room temperature to obtain the SnS modified by the gold-palladium alloy with the thickness of 2-4 mu m2A sensitive layer of a two-dimensional sheet-like structural material; finally, aging the product for 20 to 24 hours under the direct current of 80 to 100mA in the environment with the relative humidity of 30 to 56 percent RH and the temperature of 20 to 35 ℃, thereby obtaining the SnS based on the gold-palladium alloy modification2And the gas sensor of the sensitive layer.
After the gas sensor was prepared, the xylene gas-sensitive performance of the gas sensor was tested (CGS-1 TP type gas-sensitive performance tester, erlite technologies ltd, beijing).
The invention has the advantages and positive effects that:
when the gold-palladium alloy is modified on SnS, the xylene gas sensor of the invention2When the nano-sheet is used, the gas-sensitive performance is obviously improved due to the synergistic effect of the bimetal. More importantly, SnS modified based on gold-palladium alloy2The response of the gas sensor to benzene, toluene and xylene gases is obviously different, and further shows that the gas sensor has good capacity of distinguishing the benzene, toluene and xylene gases. Meanwhile, the method has simple process, and the prepared xylene gas sensor has small volume and is suitable for mass production, thereby having important application value. The sensor of the invention has the characteristics of high response, low working temperature, simple preparation method, low cost and being expected to be produced in a large scale.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to these drawings without creative efforts.
FIG. 1 is a schematic diagram of the structure of a xylene gas sensor prepared according to the present invention;
as shown in fig. 1, the xylene gas sensor prepared by the invention comprises the following components in sequence from bottom to top: al (Al)2O3Substrate 1, Pd metal interdigital electrode 3 and Al coated2O3Gold-palladium alloy modified SnS on substrate 12A sensitive layer 2 of two-dimensional sheet-like structured material. SnS modified by gold-palladium alloy2The thickness of the sensitive layer 2 of the two-dimensional sheet-shaped structural material is 2-4 mu m, the width and the interval of the Pd metal interdigital electrode 3 are both 0.15-0.20 mm, and the thickness is 100-150 nm.
FIG. 2 shows SnS modified by Au-Pd alloy2Scanning electron microscope (a) and transmission electron microscope (b) of the two-dimensional sheet structure material; FIG. 2(a) is a scanning electron microscope image, and it can be seen that the prepared material has a sheet-like hexagonal structure and the size of the material is 550-650 nm; FIG. 2(b) is a transmission electron microscope image showing that the lattice fringe spacing of 0.277nm corresponds to SnS2The lattice fringe spacing of 0.227nm corresponds to the (111) crystal face of Pd, the lattice fringe spacing of 0.236nm corresponds to the (111) crystal face of Au, and the result shows that the SnS modified by the Au-Pd alloy2And (4) successfully synthesizing.
FIG. 3 shows pure SnS2Gold modified SnS2(Au-SnS2) Palladium modified SnS2 Pd-SnS2) And SnS modified by gold-palladium alloy2(AuPd-SnS2) XRD pattern of the material; diffraction peaks in the XRD map correspond to those of a standard card, and no other impurity peaks exist, which indicates the successful synthesis of the material.
FIG. 4 is based on pure SnS2Gold modified SnS2(Au-SnS2) Palladium modified SnS2(Pd-SnS2) And SnS modified by gold-palladium alloy2(AuPd-SnS2) The device working temperature made of the sensitive layer and the corresponding responsivity relation curve; wherein responsivity is expressed as the device being emptyThe ratio of the resistance value in the gas to be measured. As shown in FIG. 4, the SnS modified based on the Au-Pd alloy2The response value of the device made of the sensitive layer is far higher than that of the other 3 devices.
FIG. 5 shows SnS based on Au-Pd alloy modification2(AuPd-SnS2) A selectivity test chart of a device made of the sensitive layer; as shown in fig. 5, when the gas sensor has a working temperature of 160 ℃ and a gas concentration of 100ppm, the gas sensor has higher response to xylene than other detection gases, and the gas sensor shows good selectivity;
FIG. 6 shows pure SnS2Gold modified SnS2Palladium modified SnS2And SnS modified by gold-palladium alloy2XPS test pattern of material.
As can be seen from the figure, there are no other impurity elements except the Au, Pd, Sn, S and O elements; FIG. 6(a) is an XPS spectrum of Sn 3d in pure SnS2In the material, the peaks at 487.25eV and 495.75eV correspond to Sn 3d, respectively3/2And 3d5/2This is SnS2Middle Sn4+But in gold-palladium alloy modified SnS2The diffraction peak is slightly shifted to the right in the spectrum of Sn (A), because of the combination of Au-Pd alloy and SnS2There is electron transfer, which explains the SnS modified by AuPd alloy2There is a significant reason for the improvement in response. FIG. 6(b) is an XPS spectrum of S2 p, with peaks at 153.15eV and 161.95eV corresponding to S2 p3/2 and S2 p1/2, respectively. The two peaks at 83.6eV and 87.2eV in FIG. 6(c) correspond to 4f of metallic Au, respectively7/2And 4f5/2Two peaks at 336.75eV and 341.95eV in FIG. 6(d) correspond to 3d of metallic Pd, respectively5/2And 3d3/2The results indicate successful synthesis of gold palladium alloy, fig. 6(e) is XPS spectrum corresponding to O1s, the peak at 532eV corresponds to the presence of adsorbed oxygen, and no lattice oxygen and oxygen vacancies are detected.
FIG. 7 shows SnS based on Au-Pd alloy modification2Response time and recovery time test patterns of devices made of the sensitive layer; as shown in fig. 7, when the gas sensor is at the operating temperatureSnS based on gold-palladium alloy modification at 160 ℃ and xylene concentration of 100ppm2The response of the gas sensor of (1) is about 4s and the recovery time of the gas sensor is about 5 s. Corresponding to example 4;
FIG. 8 shows SnS based on Au-Pd alloy modification2The responsivity-xylene concentration characteristic curve of a device prepared by the sensitive layer at the working temperature of 160 ℃; as can be seen, the devices produced also respond at lower xylene concentrations, with lower detection limits.
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 from the embodiments of the present invention by a person skilled in the art without any creative effort, should be included in the protection scope of the present invention.
Examples 1 to 4:
processing a Pd metal interdigital electrode:
firstly, wiping Al with Pd metal interdigital electrodes with the width of 3mm and the length of 4mm prepared by a screen printing technology by using acetone and ethanol cotton balls respectively2O3Cleaning the substrate, and then putting Al with Pd metal interdigital electrode2O3The substrate is sequentially placed in acetone, ethanol and deionized water, respectively ultrasonically cleaned for 5 minutes, and finally dried at 100 ℃ for later use.
The invention uses screen printing technology to prepare Pd metal interdigital electrode. The specific method comprises the following steps: ink [ jiahua JX07500487 ]: pd powder: mixing the diluents in a mass ratio of 1: 2, and 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 degrees and a pressure of 5 newtons, printing the electrode, drying, and curing by ultraviolet light to complete the preparation of the Pd metal interdigital electrode. The width and the electrode spacing of the Pd metal interdigital electrode are both 0.15mm, and the thickness is 150 nm.
2. Pure SnS2Gold-modified SnS2Palladium-modified SnS2And SnS modified by Au-Pd alloy2Preparing a gas sensitive material:
(1) preparation of SnS2Two-dimensional sheet structure material: SnS2Prepared by a simple hydrothermal method. Specifically, 1mmol of SnCl4·5H2O and 3mmol CH4N2S (thiourea) is added into 30mL of deionized water to be mixed, and the mixture is stirred for 30min by strong magnetic force at the rotating speed of 350rpm until the mixture is uniformly mixed. The mixed solution was then transferred to a 50mL stainless steel autoclave lined with polytetrafluoroethylene and subjected to hydrothermal reaction at 190 ℃ for 18 hours. The obtained SnS2Washing with deionized water and ethanol, and drying at 60 deg.C for 12 hr to obtain SnS2Two-dimensional sheet-like structured material (example 1).
(2) Preparation of gold-modified SnS2Two-dimensional sheet structure material: the gold and palladium simple substances are obtained by reducing chloroauric acid and chloropalladic acid with ascorbic acid. A solution of chloroauric acid (20mM) and a solution of chloropalladate (20mM) were first prepared. 0.34g of HAuCl4·4H2Dissolving O in 50mL of deionized water, and stirring until the O is completely dissolved to prepare a corresponding chloroauric acid solution; 0.177g of PdCl2Dissolving the mixture in 1.5mL of hydrochloric acid with the mass fraction of 37%, stirring the mixture until the hydrochloric acid is completely dissolved, and then adding a proper amount of deionized water to 50mL to prepare the corresponding chloropalladate solution. This example is for SnS2Performing Au and SnS on two-dimensional sheet structure material2The molar ratio is 0.2: 1. The modification scheme is as follows: 0.05g of SnS2Dispersing a two-dimensional sheet structure material into 30mL of deionized water, stirring for 3h to form uniformly dispersed suspension, adding 2730 muL of chloroauric acid solution into the suspension, stirring uniformly, adding 2mL of ascorbic acid solution (0.1M), continuously stirring for 3h to obtain Au-modified SnS2Centrifuging with ethanol and deionized water, and drying at 60 deg.C for 12 hr to obtain Au and SnS2Au modified SnS with molar ratio of 0.2: 12Two-dimensional sheet-like structured material (example 2).
(3) Preparation of Palladium-modified SnS2Two-dimensional sheet structure material: the embodiment pairSnS2Pd and SnS carried out on two-dimensional sheet structure material2The molar ratio is 0.2: 1. The specific modification scheme is as follows: 0.05g of SnS2Dispersing a two-dimensional sheet structure material into 30mL of deionized water, stirring for 3h to form uniformly dispersed suspension, adding 2730 muL of chloropalladate solution into the suspension, stirring uniformly, adding 2mL of ascorbic acid solution (0.1M), continuously stirring for 3h to obtain Pd modified SnS2Centrifuging with ethanol and deionized water, and drying at 60 deg.C for 12 hr to obtain Pd and SnS2The molar ratio is 0.2: 1 Pd-modified SnS2Two-dimensional sheet-like structured material (example 3).
(4) Preparation of gold-palladium alloy modified SnS2Two-dimensional sheet structure material: this example is for SnS2AuPd alloy and SnS are carried out on two-dimensional sheet structure material2Modification in a molar ratio of 0.2: 1. The specific modification scheme is as follows: 0.05g of SnS2Dispersing a two-dimensional sheet structure material into 30mL of deionized water, stirring for 3h to form uniformly dispersed suspension, respectively adding 1365 mu L of chloroauric acid solution and chloropalladate solution into the suspension, stirring uniformly, adding 2mL of ascorbic acid solution (0.1M), continuing stirring for 3h to obtain the AuPd alloy modified SnS2Centrifuging with ethanol and deionized water, and drying at 60 deg.C for 12 hr to obtain AuPd alloy and SnS2AuPd alloy modified SnS with molar ratio of 0.2: 12Two-dimensional sheet-like structured material (example 4).
(5) SnS based on gold-palladium alloy modification2Preparing a gas sensor of a sensitive layer of a two-dimensional sheet-like structure material: SnS modified by gold-palladium alloy2Putting the two-dimensional sheet structure material into a mortar, and grinding for 10 minutes to obtain powder; then, dropping deionized water into the mortar, and grinding for 10 minutes to obtain viscous slurry; dipping a small amount of slurry by using a hairbrush, and coating the slurry on Al with Pd metal interdigital electrodes2O3Drying the substrate at room temperature to obtain SnS modified by palladium-gold alloy with thickness of 3 μm2Sensitive coating of two-dimensional sheet structure material; finally aging under 100mA direct current for 24 hours in an environment with relative humidity of 40% RH and temperature of 25 deg.C to obtainSnS based on gold-palladium alloy modification2The two-dimensional sheet structure material is a gas sensor with a sensitive layer.
The same preparation method is used for obtaining the product based on SnS2Gas sensor as sensitive layer, and SnS based on gold modification2Gas sensor as sensitive layer and SnS based on palladium modification2A gas sensor which is a sensitive layer.
After the gas sensor was prepared, the xylene gas-sensitive performance of the gas sensor was tested (CGS-1 TP type gas-sensitive performance tester, erlite technologies ltd, beijing).
SnS modified by Au-Pd alloy prepared in the above examples2The gas-sensitive performance of the gas sensor taking the two-dimensional sheet structure material as the sensitive layer and the Pd as the metal interdigital electrode is tested by a CGS-1TP type gas-sensitive performance tester of Elite technologies, Inc. of Beijing. The gas-sensitive performance indexes are as follows:
example 1:
sensitivity was 2.49(100ppm xylene);
the response time was 6 seconds and the recovery time was 8 seconds.
Example 2:
sensitivity was 7.62(100ppm xylene);
the response time was 5 seconds and the recovery time was 7 seconds.
Example 3:
sensitivity was 3.92(100ppm xylene);
the response time was 6 seconds and the recovery time was 7 seconds.
Example 4:
sensitivity was 27.7(100ppm xylene);
the response time was 4 seconds and the recovery time was 5 seconds.
The above description is only an embodiment of the present invention, and the scope of the present invention should not be limited thereto, but all equivalent changes and modifications made within the scope of the present invention should still fall within the scope covered by the present invention.

Claims (2)

1. SnS based on gold-palladium alloy modification2Of the sensitive layerThe preparation method of the xylene gas sensor comprises the following steps:
(1) treatment of Pd metal interdigital electrode
Respectively wiping Al with Pd metal interdigital electrode by using acetone and ethanol cotton balls2O3A substrate, and Al with Pd metal interdigital electrode2O3Sequentially placing the substrate in acetone, ethanol and deionized water, respectively ultrasonically cleaning for 5-10 minutes, and finally drying at 100-120 ℃;
(2) SnS modified by gold-palladium alloy2Preparation of two-dimensional sheet-like structural material
Firstly, adding 0.5-1 mmol of SnCl4·5H2O and 2.5-3.5 mmol CH4N2S is added into 20-50 mL of deionized water, and the mixture is stirred for 0.5-1 h at the rotating speed of 300-400 rpm by strong magnetic force until the mixture is uniformly mixed; then transferring the obtained mixed solution into a stainless steel high-pressure reaction kettle with polytetrafluoroethylene as an inner lining, carrying out hydrothermal reaction for 16-24 h at 170-210 ℃, and obtaining SnS2Washing with deionized water and ethanol, and drying at 60-80 ℃ for 12-24 hours to obtain SnS2A two-dimensional sheet structure material;
② 0.34g of HAuCl4·4H2Dissolving O in 50mL of deionized water, and stirring until the O is completely dissolved to obtain a 20mM chloroauric acid solution; 0.177g of PdCl2Dissolving in 1.5mL hydrochloric acid with mass fraction of 37%, stirring to completely dissolve, and adding deionized water to 50mL to obtain 20mM chloropalladate solution;
③ 0.01-0.1 g of SnS obtained in the step I2Dispersing the two-dimensional sheet structure material into 20-40 mL of deionized water, stirring for 2-5 h to form uniformly dispersed suspension, then respectively adding 1000-2000 mu L of chloroauric acid solution obtained in the step II and equal volume of chloropalladate solution, stirring uniformly, adding 1-5 mL of 0.1M ascorbic acid solution, and continuing stirring for 2-5 h; SnS modified by the obtained AuPd alloy2Centrifuging the solution by using ethanol and deionized water, and drying the solution at the temperature of between 60 and 80 ℃ for 6 to 12 hours to obtain the SnS modified by the gold-palladium alloy2Two-dimensional sheet structure material of AuPd alloy and SnS2In a molar ratio of 0.15 to 0.25: 1;
(3) SnS modified by the gold-palladium alloy prepared in the step (2)2Putting the two-dimensional sheet structure material into a mortar, and grinding for 5-10 minutes to obtain a powdery material; then, dropping deionized water into the mortar, and grinding for 5-10 minutes to obtain viscous slurry; dipping a small amount of slurry by using a hairbrush, and coating the slurry on Al with Pd metal interdigital electrodes2O3Drying the substrate at room temperature to obtain the SnS modified by the gold-palladium alloy with the thickness of 2-4 mu m2A sensitive layer of a two-dimensional sheet-like structural material; finally, aging the product for 20 to 24 hours under the direct current of 80 to 100mA in the environment with the relative humidity of 30 to 56 percent RH and the temperature of 20 to 35 ℃, thereby obtaining the SnS based on the gold-palladium alloy modification2And the gas sensor of the sensitive layer.
2. SnS based on gold-palladium alloy modification2The xylene gas sensor of sensitive layer, its characterized in that: is prepared by the method of claim 1.
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