CN111122666A - Ag-SnO2Preparation method of-rGO aerogel gas-sensitive material - Google Patents
Ag-SnO2Preparation method of-rGO aerogel gas-sensitive material Download PDFInfo
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Abstract
The invention relates to Ag-SnO2The invention discloses a preparation method of an-rGO aerogel gas-sensitive material, which comprises the steps of firstly preparing Ag-SnO2-rGO sol, then aged and freeze-dried, finally the primary formed Ag-SnO2Putting rGO aerogel into vacuum drying to obtain Ag-SnO2-rGO aerogel gas sensitive material. SnO using graphene as a network skeleton structure2Coating on the lamellar structure, and taking the Ag simple substance as a metal catalyst, the overall sensitivity and recovery rate of the material can be improved. Ag as catalyst of material can enhance reaction activity and reduceActivating energy and improving the preparation efficiency. The aerogel sample is prepared by adopting a one-step method and a hydrothermal reduction method, the process is simple in material consumption and convenient and fast to operate, the negative effect caused by impurities can be reduced, the purity of the sample can be improved, and the selectivity of the material is improved.
Description
Technical Field
The invention belongs to the field of preparation processes of nano-porous composite materials, and particularly relates to Ag-SnO2A preparation method of an rGO aerogel gas-sensitive material, relating to a preparation method of a gas sensing material with high specific surface area, high porosity and high electron mobility.
Background
As a three-dimensional network-like material having a high specific surface area, high porosity, high electron mobility, and chemical stability, graphene may be used to support metal oxide particles in the nanometer order. Metal oxide SnO2Is a typical n-type wide bandgap semiconductor with an energy band gap of 3.6eV at a temperature of 300K, is one of the main choices as a gas-sensitive material, and is widely applied to H2S、SOx、NOxEtc. sensing of the gas. In previous research work, we have attempted to combine graphene with SnO2The recombination forms aerogel materials with p-n heterojunctions, which are used for detecting NOx in air. However, SnO has been known to have problems of large power consumption, high temperature of operating environment, long response time and the like2Graphene aerogels still have a large research space.
Ag is used as a high-conductivity metal material, has stable physicochemical properties, can be used as a catalyst in a gas-sensitive material due to high electron mobility, and improves the reaction activity and finally the gas-sensitive performance by increasing the electron mobility in the material. In order to realize the detection technology of gas sensitivity under the condition of room temperature, Ag-simple-substance-doped SnO2The graphene composite aerogel can effectively prevent the agglomeration of metal oxides and the overlapping of graphene layers, and can improve the electrical, chemical and physical properties of materials, thereby being a novel gas sensing deviceAnd (5) feeding.
The Xiaoguo of the university of technology in southwest utilizes the self redox reaction between graphene oxide and stannous chloride dihydrate to prepare SnO by ultrasonically dispersing graphene oxide and ultrasonically mixing two substances2rGO composites with 50ppm NO concentration2The response reaches 35%, but the reaction is gentle due to the small specific surface area, and the sensitivity is low. Zusasai et al, university of Henan industry, propose an Ag/SnO2The novel gas-sensitive material with good responsiveness to trimethylamine gas at 220 ℃ is obtained from the/rGO nano composite material, and the electron mobility of the material is improved by adding the metal Ag simple substance, so that the overall sensitivity is improved, but the powder material has a compact structure, so that the recovery time is too long, and practical application is difficult to carry out. Therefore, the improvement of the specific surface area and the porosity is a research object for preparing the gas-sensitive material with high sensitivity, high recovery performance and high cycle rate.
Disclosure of Invention
The invention aims to improve the defects of the prior art and provides Ag-SnO2-preparation method of rGO aerogel gas sensitive material.
The technical scheme of the invention is as follows: in the preparation of SnO2On the basis of the graphene composite material, simple substance Ag nano particles are doped, and the activation energy of the reaction is reduced by adding a metal catalyst, so that the sensing effect of the gas sensitive material is improved. The doping of the simple substance Ag not only improves the gas-sensitive property of the material, but also avoids SnO caused by undersize particles2Agglomeration and graphene layer overlap. The reducing agent of the aerogel is introduced into the graphene oxide, so that the reduction of the graphene oxide can be effectively promoted, and a three-dimensional porous network structure is formed.
The specific technical scheme of the invention is as follows: a preparation method of an Ag-SnO2-rGO aerogel gas-sensitive material comprises the following specific steps:
(1) preparation of the Sol
Weighing a tin source, a silver source and a reducing agent, adding the tin source, the silver source and the reducing agent into deionized water, stirring for a period of time, adding an alcohol solution and a graphene oxide solution for crosslinking, adding an alkaline reagent for regulating the pH value, performing ultrasonic treatment, and finally putting the mixture into a hydrothermal reaction kettle for reaction to obtain Ag-SnO2-rGO sol;
(2) aging of
Taking out the prepared Ag-SnO2-rGO sol, putting the sol into a container, standing for complete gelation, pouring an aging solution, and aging for 3-5 days;
(3) freeze drying
Putting the Ag-SnO2-rGO sol obtained in the step (2) into a freeze dryer, wherein the drying temperature is-55 to-60 ℃, the pressure is 1 to 5Pa, the sol is maintained for 36 to 72 hours under the constant temperature and pressure state, and a sample is taken out after the temperature of the freeze dryer is raised to the room temperature;
(4) drying at elevated temperature
And (4) putting the Ag-SnO2-rGO aerogel preliminarily formed in the step (3) into a vacuum drying box for continuous drying to obtain the Ag-SnO2-rGO aerogel gas-sensitive material. -
Preferably, the tin source in the step (1) is tin tetrachloride pentahydrate (SnCl4 & 5H2O) or tin tetrachloride; the silver source is silver nitrate (AgNO3) or silver chloride (AgCl); the concentration of the graphene oxide solution is 3-8 mg/mL; the reducing agent is urea or ascorbic acid (VC); the alcoholic solution is methanol or ethanol; the alkaline reagent is ammonia water or sodium hydroxide solution.
Preferably, in the step (1), the tin source, the graphene, the silver source, the reducing agent and the deionized water are mixed according to the weight ratio of 1: (0.13-0.35): (0.19-0.20): (0.41-1.61): (19-58) in mass ratio; stirring for 30-60 min, and then mixing according to the volume ratio of alcohol to water of 1: (3-8) adding an alcohol solution; and continuously stirring for 10-30 min, adding the graphene oxide solution, stirring for 2-3 h, adding an alkaline reagent to adjust the pH value to 10-12, stirring for 10-30 min, and then performing ultrasonic treatment.
Preferably, the stirring speed in the step (1) is 500-700 rpm. Preferably, the speed of adding the alkaline reagent in the step (1) is controlled to be 0.1-0.2 mL/s. Preferably, in the step (1), the ultrasonic frequency is 80-120 Hz, the ultrasonic time is 30-60 min, and the ultrasonic temperature is 40-60 ℃. Preferably, the reaction temperature of the sol in the step (1) in the hydrothermal reaction kettle is 120-200 ℃, and the reaction time is 10-14 h.
Preferably, in the step (2), a mixed solution of ethanol and water with a volume ratio of 1 (4-6) is used as an aging liquid; the aging time is 3-5 days.
Preferably, in the step (4), the drying temperature is 40-60 ℃, and the drying time is 5-8 h.
The density of the Ag-SnO2-rGO aerogel gas-sensitive material prepared by the method is 0.11-0.18 g/cm3, the specific surface area is 231-256 m2/g, and the responsiveness is 31-47%.
Has the advantages that:
(1) compared with Ag/SnO2Ag-SnO researched by the invention2The rGO composite aerogel has larger specific surface area and porosity, and provides a favorable basis for the adsorption performance of the gas-sensitive material.
(2) Compared with SnO2Graphene aerogel sample and Ag-SnO prepared by using same2the/rGO composite aerogel sample has good gas-sensitive performance and NOxThe method has the advantages of high selectivity, strong response and high sensitivity, and can be primarily used for a gas detection system.
(3) Compared with the traditional metal oxide/graphene composite material, the Ag-SnO prepared by the invention2the/rGO composite aerogel has higher electron mobility and better conductivity.
(4) Compared with the traditional composite aerogel product, the invention adopts a one-step method and a hydrothermal reduction method to crosslink the aerogel on the basis of ensuring the product performance, thereby reducing impurities in the reaction process and improving the product purity.
Drawings
FIG. 1 is Ag-SnO prepared in example 12-XRD pattern of rGO composite aerogel material.
FIG. 2 is Ag-SnO prepared in example 12-fourier-infrared spectrum of rGO composite aerogel material.
FIG. 3 is Ag-SnO prepared in example 12SEM images of rGO composite aerogel materials at multiples of (a)500(b)1000(c)5000(d) 20000.
FIG. 4 is Ag-SnO prepared in example 12-mapping profile and EDS energy spectrum of rGO aerogel (a).
FIG. 5 is Ag-SnO prepared in example 12-rGO composite aerogel materialBET test pattern of (a).
Detailed Description
The invention is further illustrated by the following examples, without limiting the scope of protection.
Example 1
Adding 10mL of deionized water into a beaker, then weighing 0.5259g of tin pentahydrate, 0.1019g of silver nitrate and 0.216g of urea by using an electronic balance, stirring the solution for 30min at the rotating speed of 500rpm, adding 2mL of ethanol, stirring for 10min, then adding 14.4mL of 5mg/mL graphene oxide solution, stirring for 2h, then dropwise adding ammonia water at the speed of 0.1mL/s to adjust the pH value to 11, continuously stirring for 30min, carrying out ultrasonic treatment for 30min under the conditions that the temperature is 50 ℃ and the frequency is 100Hz, then pouring into a hydrothermal reaction kettle with the volume of 50mL, and reacting for 12h at 180 ℃. And (3) taking out the gel after the reaction kettle is cooled to room temperature, soaking the gel into a mixed solution with the alcohol-water ratio of 1:5 for aging, and replacing the aging solution on time every day, wherein the aging process is 5 days. The sample is placed in a small 10mL beaker and is put into a freeze dryer for drying, the drying temperature is set to be-60 ℃, the drying time is set to be 48h, and the drying pressure is set to be 1 Pa. After the freeze drying is finished, the sample is put into a vacuum drying oven to be dried for 6 hours at the temperature of 50 ℃, and the Ag-SnO can be obtained after the drying is finished2The density of the prepared material is 0.11g/cm3A specific surface area of 256m2The responsivity was 47%.
FIG. 1 shows Ag-SnO2-XRD patterns of rGO aerogel materials. In the figure, the peaks at 26.6 degrees, 38.4 degrees and 51.8 degrees respectively correspond to SnO2The (110), (101) and (211) planes of the material conform to a tetragonal rutile structure, peaks at 38.1 degrees, 44.3 degrees, 64.4 degrees, 77.4 degrees and 81.5 degrees respectively correspond to (111), (200), (220), (311) and (222) planes of the simple substance Ag, and the peak shapes are sharp, so that the material has good crystallinity.
FIG. 2 shows Ag-SnO2-fourier-ir spectrum of rGO aerogel material. In the figure at a wavelength of 1570cm-1Where is the characteristic peak of C ═ C bond; 1240cm-1Is a characteristic peak of C-O-C bond, which is due to the existence of graphene, 624cm-1Is a characteristic peak of Sn-O bond, and confirms SnO2Is present.
FIG. 3 is Ag-SnO prepared in example 12SEM images of rGO composite aerogel materials at multiples of (a)500(b)1000(c)5000(d) 20000. As is apparent from the graph (a), the graphene is reduced to form a three-dimensional network structure, the surface of the graphene has clearly visible folds, and SnO in the graph (c)2And Ag is attached to the surface of the graphene sheet layer in a large amount, and tetragonal graphene can be observed in fig. (d).
FIG. 4 is Ag-SnO prepared in example 12-mapping profile and EDS energy spectrum of rGO aerogel (a). Fig. 4(a) is a mapping surface scan of the material, and it can be observed that each element is uniformly distributed, but irregular growth of part of the simple substance of Ag occurs, and fig. 4(b) analyzes the content of each element, and the content is consistent with the XRD test.
FIG. 5 is Ag-SnO2BET test pattern of rGO aerogel material, belonging to class IV isotherms, H4 hysteresis loop, with specific surface area up to 256m2The/g is a material with high porosity, the pore diameter of the material is mostly distributed in the range of 2-5nm, and the material belongs to the range of mesoporous materials.
Example 2
Adding 15mL of deionized water into a beaker, then weighing 0.4207g of stannic chloride, 0.0815g of silver nitrate and 0.634g of ascorbic acid by using an electronic balance, stirring the solution for 35min at the rotating speed of 500rpm, adding 2mL of methanol, stirring for 15min, then adding 9mL of 8mg/mL graphene oxide solution, stirring for 2.5h, then dropwise adding ammonia water at the speed of 0.15mL/s to adjust the pH value to 10, continuously stirring for 10min, carrying out ultrasonic treatment for 40min under the conditions that the temperature is 40 ℃ and the frequency is 120Hz, then pouring into a hydrothermal reaction kettle with the volume of 50mL, and reacting for 10h at the temperature of 120 ℃. And (3) taking out the gel after the reaction kettle is cooled to room temperature, soaking the gel into a mixed solution with the alcohol-water ratio of 1:4 for aging, and replacing the aging solution on time every day, wherein the aging process is 3 days. The sample is placed in a small 10mL beaker and is put into a freeze dryer for drying, the drying temperature is set to be-55 ℃, the drying time is set to be 36h, and the drying pressure is set to be 3 Pa. After the freeze drying is finished, the sample is put into a vacuum drying oven to be dried for 5 hours at the temperature of 40 ℃, and the Ag-SnO can be obtained after the drying is finished2-rGO composite aerogel material, saidThe density of the prepared material is 0.15g/cm3A specific surface area of 226m2The responsivity was 34%.
Example 3
Adding 10mL of deionized water into a beaker, then weighing 0.3506g of stannic chloride pentahydrate, 0.0679g of silver chloride and 0.324g of urea by using an electronic balance, stirring the solution for 40min at the rotation speed of 550rpm, adding 3mL of ethanol, stirring for 20min, then adding 24mL of 3mg/mL graphene oxide solution, stirring for 3h, then dropwise adding ammonia water at the speed of 0.2mL/s to adjust the pH value to 12, continuously stirring for 15min, carrying out ultrasonic treatment for 45min under the conditions that the temperature is 60 ℃ and the frequency is 80Hz, then pouring into a hydrothermal reaction kettle with the volume of 50mL, and reacting for 12h at the temperature of 140 ℃. And (3) taking out the gel after the reaction kettle is cooled to room temperature, soaking the gel into a mixed solution with the alcohol-water ratio of 1:6 for aging, and replacing the aging solution on time every day, wherein the aging process is 4 days. The sample is placed in a 10mL small beaker and is put into a freeze dryer for drying, the drying temperature is set to be-55 ℃, the drying time is set to be 42h, and the drying pressure is set to be 5 Pa. After the freeze drying is finished, the sample is put into a vacuum drying oven to be dried for 7 hours at the temperature of 55 ℃, and Ag-SnO can be obtained after the drying is finished2-rGO composite aerogel material prepared with a density of 0.13g/cm3A specific surface area of 241m2The responsivity was 39%.
Example 4
Adding 15mL of deionized water into a beaker, then weighing 0.2629g of stannic chloride, 0.0509g of silver nitrate and 0.4227g of ascorbic acid by using an electronic balance, stirring the solution for 50min at the rotating speed of 600rpm, adding 3mL of methanol, stirring for 25min, then adding 12mL of 6mg/mL of graphene oxide solution, stirring for 2.5h, then dropwise adding ammonia water at the speed of 0.15mL/s to adjust the pH value to 10, continuously stirring for 20min, carrying out ultrasonic treatment for 50min at the temperature of 50 ℃ and the frequency of 100Hz, then pouring into a hydrothermal reaction kettle with the volume of 50mL, and reacting for 13h at the temperature of 160 ℃. And (3) taking out the gel after the reaction kettle is cooled to room temperature, soaking the gel into a mixed solution with the alcohol-water ratio of 1:4 for aging, and replacing the aging solution on time every day, wherein the aging process is 3 days. Placing the sample in a small 10mL beaker, and drying in a freeze dryer at-60 deg.C for 6 deg.C0h and the drying pressure is 3 Pa. After the freeze drying is finished, the sample is put into a vacuum drying oven to be dried for 8 hours at the temperature of 60 ℃, and the Ag-SnO can be obtained after the drying is finished2-rGO composite aerogel material prepared with a density of 0.17g/cm3A specific surface area of 231m2The responsivity was 31%.
Example 5
Adding 10mL of deionized water into a beaker, then weighing 0.2104g of stannic chloride pentahydrate, 0.0408g of silver chloride and 0.216g of urea by using an electronic balance, stirring the solution at the rotating speed of 700rpm for 60min, then adding 2mL of ethanol, stirring for 30min, then adding 14.4mL of 5mg/mL graphene oxide solution, stirring for 3h, then dropwise adding ammonia water at the speed of 0.1mL/s to adjust the pH value to 11, continuously stirring for 30min, then carrying out ultrasonic treatment for 60min under the conditions of the temperature of 50 ℃ and the frequency of 100Hz, then pouring into a hydrothermal reaction kettle with the volume of 50mL, and reacting for 14h at the temperature of 180 ℃. And (3) taking out the gel after the reaction kettle is cooled to room temperature, soaking the gel into a mixed solution with the alcohol-water ratio of 1:5 for aging, and replacing the aging solution on time every day, wherein the aging process is 5 days. The sample is placed in a small 10mL beaker and is put into a freeze dryer for drying, the drying temperature is set to be-60 ℃, the drying time is set to be 72h, and the drying pressure is set to be 1 Pa. After the freeze drying is finished, the sample is put into a vacuum drying oven to be dried for 6 hours at the temperature of 50 ℃, and the Ag-SnO can be obtained after the drying is finished2-rGO composite aerogel material prepared with a density of 0.18g/cm3Specific surface area of 239m2The responsivity was 42%.
Claims (10)
1. Ag-SnO2The preparation method of the rGO aerogel gas-sensitive material comprises the following specific steps:
(1) preparation of the Sol
Weighing a tin source, a silver source and a reducing agent, adding the tin source, the silver source and the reducing agent into deionized water, stirring for a period of time, adding an alcohol solution and a graphene oxide solution for crosslinking, adding an alkaline reagent for regulating the pH value, performing ultrasonic treatment, and finally placing the mixture into a hydrothermal reaction kettle for reaction to obtain Ag-SnO2-rGO sol;
(2) aging of
The prepared Ag-SnO2-rGO sol extractionPutting the mixture into a container, standing the mixture completely for gelation, and pouring the aging solution into the container;
(3) freeze drying
The Ag-SnO obtained in the step (2)2Putting the rGO sol into a freeze dryer, drying at the temperature of-55 to-60 ℃ under the pressure of 1 to 5Pa, maintaining the temperature for 36 to 72 hours under the constant temperature and pressure state, and taking out a sample after the temperature of the freeze dryer is raised to the room temperature;
(4) drying at elevated temperature
The Ag-SnO preliminarily formed in the step (3)2Putting the rGO aerogel into a vacuum drying oven for continuous drying to obtain Ag-SnO2-rGO aerogel gas sensitive material. -
2. The production method according to claim 1, characterized in that the tin source in step (1) is tin tetrachloride pentahydrate or tin tetrachloride; the silver source is silver nitrate or silver chloride; the concentration of the graphene oxide solution is 3-8 mg/mL; the reducing agent is urea or ascorbic acid; the alcoholic solution is methanol or ethanol; the alkaline reagent is ammonia water or sodium hydroxide solution.
3. The method according to claim 1, wherein in step (1), the ratio of the tin source, the graphene source, the silver source, the reducing agent and the deionized water is 1: (0.13-0.35): (0.19-0.20): (0.41-1.61): (19-58) in mass ratio; stirring for 30-60 min, and then mixing according to the volume ratio of alcohol to water of 1: (3-8) adding an alcohol solution; and continuously stirring for 10-30 min, adding the graphene oxide solution, stirring for 2-3 h, adding an alkaline reagent to adjust the pH value to 10-12, stirring for 10-30 min, and then performing ultrasonic treatment.
4. The method according to claim 1, wherein the stirring speed in the step (1) is 500 to 700 rpm.
5. The method according to claim 1, wherein the rate of the addition of the alkali agent in the step (1) is controlled to 0.1 to 0.2 mL/s.
6. The preparation method according to claim 1, wherein the ultrasonic frequency in the step (1) is 80-120 Hz, the ultrasonic time is 30-60 min, and the ultrasonic temperature is 40-60 ℃.
7. The preparation method according to claim 1, wherein the reaction temperature of the sol in the hydrothermal reaction kettle in the step (1) is 120-200 ℃ and the reaction time is 10-14 h.
8. The preparation method according to claim 1, wherein a mixed solution of ethanol and water in a volume ratio of 1 (4-6) is used as the aging liquid in the step (2); the aging time is 3-5 days.
9. The method according to claim 1, wherein the drying temperature in the step (4) is 40 to 60 ℃ and the drying time is 5 to 8 hours.
10. The production method according to claim 1, wherein the Ag-SnO produced in the step (4)2The density of the-rGO aerogel gas-sensitive material is 0.11-0.18 g/cm3The specific surface area is 231-256 m2The responsivity is 31-47%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111982981A (en) * | 2020-08-17 | 2020-11-24 | 合肥微纳传感技术有限公司 | SnO (stannic oxide)2Gas-sensitive material, preparation method and application thereof |
| CN113019324A (en) * | 2021-03-12 | 2021-06-25 | 南京工业大学 | Preparation method of silver-titanium dioxide-graphene composite aerogel |
| CN114324498A (en) * | 2022-01-06 | 2022-04-12 | 吉林大学 | Based on Au-SnO2Ppb level NO of nanoflower sensitive materials2Gas sensor and preparation method thereof |
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| CN111982981A (en) * | 2020-08-17 | 2020-11-24 | 合肥微纳传感技术有限公司 | SnO (stannic oxide)2Gas-sensitive material, preparation method and application thereof |
| CN111982981B (en) * | 2020-08-17 | 2022-09-30 | 微纳感知(合肥)技术有限公司 | SnO (stannic oxide) 2 Gas-sensitive material, preparation method and application thereof |
| CN113019324A (en) * | 2021-03-12 | 2021-06-25 | 南京工业大学 | Preparation method of silver-titanium dioxide-graphene composite aerogel |
| CN114324498A (en) * | 2022-01-06 | 2022-04-12 | 吉林大学 | Based on Au-SnO2Ppb level NO of nanoflower sensitive materials2Gas sensor and preparation method thereof |
| CN114324498B (en) * | 2022-01-06 | 2024-02-27 | 吉林大学 | Au-SnO-based 2 Ppb level NO of nanoflower sensitive materials 2 Gas sensor and preparation method thereof |
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