CN113213528A - SnO/SnO synthesized by adopting hydrothermal method2Method for preparing nano composite gas-sensitive material - Google Patents

SnO/SnO synthesized by adopting hydrothermal method2Method for preparing nano composite gas-sensitive material Download PDF

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CN113213528A
CN113213528A CN202110464018.7A CN202110464018A CN113213528A CN 113213528 A CN113213528 A CN 113213528A CN 202110464018 A CN202110464018 A CN 202110464018A CN 113213528 A CN113213528 A CN 113213528A
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李聪
陆雨晴
张鸿飞
张庆磊
孙庆枫
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Civil Aviation University of China
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    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
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    • C01G19/00—Compounds of tin
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    • B82Y40/00—Manufacture or treatment of nanostructures
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    • G01N27/00—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means
    • G01N27/02—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance
    • G01N27/04—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance
    • G01N27/12—Investigating or analysing materials by the use of electric, electrochemical, or magnetic means by investigating impedance by investigating resistance of a solid body in dependence upon absorption of a fluid; of a solid body in dependence upon reaction with a fluid, for detecting components in the fluid
    • G01N27/125—Composition of the body, e.g. the composition of its sensitive layer
    • G01N27/127—Composition of the body, e.g. the composition of its sensitive layer comprising nanoparticles
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    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/01—Particle morphology depicted by an image
    • C01P2004/03—Particle morphology depicted by an image obtained by SEM
    • C—CHEMISTRY; METALLURGY
    • C01—INORGANIC CHEMISTRY
    • C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2004/00—Particle morphology
    • C01P2004/60—Particles characterised by their size
    • C01P2004/64—Nanometer sized, i.e. from 1-100 nanometer

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Abstract

The invention adopts a one-step hydrothermal method of calcination post-treatment to prepare SnO/SnO with good dispersibility2Composite nanoparticles. By varying the reaction medium and the reaction temperature, the composition of the product can be adjusted. The structure, morphology and chemical properties of the product are characterized by adopting characterization technologies such as X-ray diffraction (XRD), Scanning Electron Microscope (SEM), X-ray photoelectron spectroscopy (XPS) and the like. In order to explore the application prospect of the material, the gas-sensitive test of the system is carried out. The results show that at lower temperatures, due to SnO2And SnO in the product coexists, so that the ethanol gas-sensitive performance of the sensor is enhanced.

Description

SnO/SnO synthesized by adopting hydrothermal method2Method for preparing nano composite gas-sensitive material
Technical Field
The invention relates to the technical field of nano materials, in particular to a method for preparing SnO/SnO with good dispersibility by adopting a hydrothermal synthesis method2A method of compounding nanoparticles.
Background
The rapid growth of industrialized and urban populations has led to air pollution, mainly from factory and automotive emissions. Such contamination threatens the survival of animals and plants; therefore, there is an urgent need to improve the level of atmospheric pollution to maintain the ecosystem. Furthermore, explosive and combustible gas leaks pose a considerable risk to the population, and accurate real-time gas detection sensors are therefore critical to protect humans and residential environments.
A low cost, reliable, low operating temperature, high sensitivity, small gas sensor is the best way to avoid accidents caused by toxic, explosive gases. Metal Oxide Semiconductor (MOS) based gas sensors have been extensively studied over the past several decades because of their many characteristics of ideal gas sensors. SnO2The gas sensor has the advantages of good sensitivity response, simple preparation, low cost, no toxicity, good chemical stability and the like, and is widely applied in many fields. For SnO2A great deal of research has been conducted on base gas sensors, some of which have been directed to improving the gas sensing performance requirements of metal oxide sensors, and thus improving the selectivity and response of the sensors. By the reaction in SnO2The surface of the sensor is coated with noble metal nano particles such as palladium, platinum, gold, silver and the like, so that the gas-sensitive property of the sensor can be improved; this improves SnO2The gas response of the sensor, but also increases its cost. Previous research reports that SnO can be combined in the process of preparing composite sensor2Other compounds co-ordinating, e.g. SnS2、ZnSnO3NiO, ZnO and the like.
SnO/SnO is prepared by a simple hydrothermal method by changing a solvent (distilled water, ethanolamine or triethanolamine is used as a reaction medium)2Hybrid nanoparticles. The results show that varying the reaction medium and the reaction temperature can vary the composition of the final product. The prepared SnO/SnO2The composite material is prepared into an ethanol gas detection sensor and shows good gas-sensitive performance.
Disclosure of Invention
The invention aims to provide a hydrothermal synthesis method for preparing SnO/SnO with good dispersibility2Composite nanoparticles. The composition of the product is adjusted by changing the reaction medium and the reaction temperature. At lower temperatures due to SnO2And the coexistence of SnO in the product realizes the enhancement of the ethanol gas-sensitive performance of the sensor at a lower temperature.
To achieve the above object, the present invention providesThe following technical scheme is as follows: SnO prepared by hydrothermal synthesis method2A method of nano gas sensitive material, characterized by comprising the steps of:
step 1: preparation of the precursor
Dissolving 8.0g of tin dichloride dihydrate in 60mL of deionized water, continuously and violently stirring for 2 hours at room temperature to form a uniform white emulsion, then transferring the white emulsion into a 100 mL polytetrafluoroethylene lining, putting the polytetrafluoroethylene lining into a stainless steel autoclave, heating at the constant temperature of 160 ℃ for 16 hours, cooling to room temperature, centrifuging, washing and drying to obtain a precursor;
step 2: SnO2Preparation of the Material
Drying the precursor at 80 ℃ for 12 hours, SnO2The sample (S1) was obtained after heating at a rate of 2 deg.C/min and calcining in air at 500 deg.C for 2 hours. Obtaining a second sample by replacing water with ethanolamine while keeping other conditions unchanged (S2);
SnCl2·2H2o is insoluble in triethanolamine, so 60mL of distilled water and 60mL of triethanolamine were magnetically stirred at room temperature for 2h to obtain a homogeneous solvent. Other samples were prepared at 160 ℃ as above for other experimental procedures, resulting in samples S3-160. The samples obtained at 100 ℃ and 130 ℃ were designated S3-100 and S3-130, respectively, with the other conditions unchanged.
And step 3: gas sensing performance testing
SnO to be prepared2And SnO/SnO2Grinding the powder into paste with distilled water, and coating the paste powder on Al2O3A pair of gold electrodes is arranged at two ends of the ceramic tube, and four platinum wires are attached to the electrodes. Passing Ni-Cr heating wire through Al2O3The ceramic tube formed an indirect thermal device (as shown in fig. 1), and was aged at 180mA for 120h to improve its repeatability and stability. And then performing gas-sensitive test on the CGS-8 intelligent gas-sensitive analysis system.
Further, the temperature of the sensing test in the step 3 is 160 ℃.
Further, in step 3, the gas sensitivity is defined as R ═ Ra/Rg, the response time T1 is the time required for the resistance change value of the sensing material to fall to 90% of the maximum difference value after the sensing gas enters, and the recovery time T2 is the time required for the resistance change value of the sensing material to rise to 90% of the maximum difference value after the sensing gas is turned off.
Further, Ra is the resistance value of the sensing material under the air condition, and Rg is the resistance value of the sensing material under the air condition.
Compared with the prior art, the invention has the beneficial effects that: SnO/SnO with good dispersibility is prepared by adopting a hydrothermal synthesis method2Composite nanoparticles. By varying the reaction medium and the reaction temperature, the composition of the product can be adjusted. At lower temperatures due to SnO2And the coexistence of SnO in the product realizes the enhancement of the ethanol gas-sensitive performance of the sensor at a lower temperature.
Drawings
FIG. 1 is a schematic diagram of a gas sensor used in the present invention, including a ceramic tube, a platinum wire, a gold electrode, and a nickel-chromium heater;
FIG. 2 is a powder X-ray powder diffraction pattern of a sample obtained by the present invention, which is analyzed by XRD, a series of SnO particles formed in different solvents2The crystalline phase structure of the sample was characterized as shown in fig. 2 a. The XRD pattern shows that all diffraction peaks of the S1 sample (water is used as a solvent) are SnO2(JCPDS No.41-1445) in the tetragonal rutile structure. Apparent peaks centered at 26.6 °, 33.9 °, 37.9 ° and 51.8 ° correspond to crystalline SnO2Reflection of the (110), (101), (200) and (211) planes of the pure tetragonal phase. No peak caused by impurities exists in the sample, and the purity of the sample is high. The diffraction peak of S1 was broad, indicating SnO2The product consisted of small particles.
SnO prepared from ethanolamine and triethanolamine2The sample has new peaks at 29.8 °, 33.3 ° and 37.1 ° (fig. 2a is marked with an inverted triangle) which are defined by regular tetragonal SnO2And positive tetragonal SnO production (JCPDS card number. 06-0395), indicating coexistence in the second stage. As shown in FIG. 2b, the samples obtained at different temperatures by using triethanolamine aqueous solution as solvent are SnO/SnO2Composite materials, SnO, when reaction temperatures are above 100 DEG C2The diffraction peaks are more pronounced.
FIG. 3 is SnO prepared according to example two of the present invention2Scanning electron micrographs of the nanocomposites, a general morphological analysis of the samples with a field emission electron microscope, are shown in FIGS. 3 a-e. As shown in FIG. 3a, the S1 sample had a non-uniform spherical structure consisting of SnO having a diameter of about 30nm2Nano-particle composition, and SnO2The nanoparticles are tightly aggregated. The S2 sample shown in fig. 3b consists of irregular nanoparticles distributed relatively uniformly, with a particle size of about 20 nm. As can be seen from FIG. 3c, the irregular spherical product with uniform particle size and good dispersibility is obtained by using the triethanolamine aqueous solution as the solvent. The sample was produced at 160 ℃ and the nanoparticles in S3-160 were about 30nm in diameter. As the hydrothermal reaction temperature was decreased, the particle sizes of the S3-130 and S3-100 samples gradually increased and the morphologies became irregular, as shown in FIGS. 3 d-e.
Fig. 4 is a graph of the response of a gas-sensitive device to operating temperature. As shown in FIG. 5a, SnO was expressed2Response of series (S1, S2, and S3-160) nanoparticle gas sensors to operating temperature when exposed to 50ppm ethanol gas. The responses of S1, S2, and S3-160 tended to increase in the initial phase, reached a maximum at the same optimum operating temperature of 160 ℃ and then began to decrease. The maximum response values at 160 ℃ for the sensor based on S1 and the sensor based on S2 were 21.3 and 7.6, respectively. The response of the S3-160 sample to 50ppm ethanol gas increased from 2.6 to 39.1 at operating temperatures of 100-160 ℃, indicating that the sensitivity of the S3-160 based sensor was much higher at the same operating temperature. The influence of experimental synthesis conditions on the response of product gas is further examined by changing the hydrothermal reaction temperature to 100, 130 and 160 ℃ and taking the triethanolamine aqueous solution as a solvent. The obtained samples were fabricated into sensors and their gas response was studied. FIG. 5b is a graph of the response of nanoparticle gas sensors S3-100, S3-130, and S3-160 to 50ppm ethanol gas, reaching a maximum at the respective optimum operating temperature and then falling as the operating temperature increases. SnO/SnO prepared at 100 ℃ and 130 ℃2The maximum response values of the samples were 19.2 and 8.3, respectively, which are lower than that of SnO/SnO prepared at 160 DEG C2The response of the composite. The results are substantially consistent with the SEM test results。SnO/SnO2The small particle size of the product increases the specific surface area of the product, and is beneficial to increasing the adsorption capacity of surface gas, so that the gas response of the product is improved;
FIG. 5 shows representative dynamic responses of S3-160-based sensors at 160 ℃ to ethanol gas concentrations of 5, 10, 20, 30, 40, 50, 100, and 200 ppm. The response amplitude gradually increases with increasing gas concentration. FIGS. 5b and 5c show the gas response of the S3-160 based sensor at an optimum temperature of 160 ℃ and an ethanol concentration of 5-200 ppm. The gas response increased linearly at 100ppm ethanol gas (FIG. 5b) and decreased slightly at 200ppm (FIG. 5 c). Testing the S3-160 sensor at 1000ppm ethanol gas showed an unsaturated absorption capacity, meaning a wide detection range. Experimental data from 5 to 40ppm were fitted, as shown in FIG. 5 c. Coefficient of correlation R2Reaching 0.980, which shows a good linear correlation at low ethanol concentrations. Therefore, the S3-160 material has potential application prospect in quantitative detection of low-concentration ethanol gas.
Fig. 6 shows that the reproducibility of the ethanol detection is better when the response value is kept around 39.1. Subsequently, a series of SnO-based materials were tested2The sensors of the samples responded to 50ppm of gas from different gases (ethanol, acetone, benzene, n-butanol and dry ammonia).
Fig. 7 shows that the sensors respond to different gases to the lowest extent, among which ammonia. The S1, S3-100, and S3-160 sensors responded similarly to ethanol and n-butanol gas, with the S3-160 sensors responding more to ethanol than n-butanol. In contrast, the S3-160 sensor was less selective for ethanol and n-butanol gases.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
The first embodiment is as follows:
(1) preparation of the precursor
Dissolving 8.0g of tin dichloride dihydrate in 60mL of deionized water, continuously and violently stirring for 2 hours at room temperature to form a uniform white emulsion, then transferring the white emulsion into a 100 mL polytetrafluoroethylene lining, putting the polytetrafluoroethylene lining into a stainless steel autoclave, heating at the constant temperature of 160 ℃ for 16 hours, cooling to room temperature, centrifuging, washing and drying to obtain a precursor;
(2)SnO2preparation of the Material
Drying the precursor at 80 ℃ for 12 hours, SnO2The sample (S1) was obtained after heating at a rate of 2 c/min and calcining in air at 500 c for 2 hours. Obtaining a second sample by replacing water with ethanolamine while keeping other conditions unchanged (S2);
SnCl2·2H2o is insoluble in triethanolamine, so 60mL of distilled water and 60mL of triethanolamine were magnetically stirred at room temperature for 2h to obtain a homogeneous solvent. Other samples were prepared at 160 ℃ as above for other experimental procedures, resulting in samples S3-160. The samples obtained at 100 ℃ and 130 ℃ were designated S3-100 and S3-130, respectively, with the other conditions unchanged.
Example two:
(1) preparation of the precursor
Dissolving 8.0g of tin dichloride dihydrate in 60mL of deionized water, continuously and violently stirring for 2 hours at room temperature to form a uniform white emulsion, then transferring the white emulsion into a 100 mL polytetrafluoroethylene lining, putting the polytetrafluoroethylene lining into a stainless steel autoclave, heating at the constant temperature of 160 ℃ for 16 hours, cooling to room temperature, centrifuging, washing and drying to obtain a precursor;
(2)SnO2preparation of the Material
Drying the precursor at 80 ℃ for 12 hours, SnO2The sample (S1) was obtained after heating at a rate of 2 c/min and calcining in air at 500 c for 2 hours. Obtaining a second sample by replacing water with ethanolamine while keeping other conditions unchanged (S2);
SnCl2·2H2o insolubilityIn triethanolamine, 60mL of distilled water and 60mL of triethanolamine were magnetically stirred at room temperature for 2 hours to obtain a homogeneous solvent. Other samples were prepared at 160 ℃ as above for other experimental procedures, resulting in samples S3-160. The samples obtained at 100 ℃ and 130 ℃ were designated S3-100 and S3-130, respectively, with the other conditions unchanged.
(3) Gas sensing performance testing
SnO to be prepared2And SnO/SnO2Grinding the powder into paste with distilled water, and coating the paste powder on Al2O3A pair of gold electrodes is arranged at two ends of the ceramic tube, and four platinum wires are attached to the electrodes. Passing Ni-Cr heating wire through Al2O3The ceramic tube formed an indirect thermal device (as shown in fig. 1), and was aged at 180mA for 120h to improve its repeatability and stability. And then performing gas-sensitive test on the CGS-8 intelligent gas-sensitive analysis system.
It is noted that, herein, relational terms such as first and second, and the like may be used solely to distinguish one entity or action from another entity or action without necessarily requiring or implying any actual such relationship or order between such entities or actions. Also, the terms "comprises," "comprising," or any other variation thereof, are intended to cover a non-exclusive inclusion, such that a process, method, article, or apparatus that comprises a list of elements does not include only those elements but may include other elements not expressly listed or inherent to such process, method, article, or apparatus.
Although embodiments of the present invention have been shown and described, it will be appreciated by those skilled in the art that changes, modifications, substitutions and alterations can be made in these embodiments without departing from the principles and spirit of the invention, the scope of which is defined in the appended claims and their equivalents.

Claims (3)

1. A series of SnO prepared by hydrothermal synthesis method2A method of gas sensing materials, characterized by the steps of:
step 1: preparation of the precursor
Dissolving 8.0g of tin dichloride dihydrate in 60mL of deionized water, continuously and violently stirring for 2 hours at room temperature to form a uniform white emulsion, then transferring the white emulsion into a 100 mL polytetrafluoroethylene lining, putting the polytetrafluoroethylene lining into a stainless steel autoclave, heating at the constant temperature of 160 ℃ for 16 hours, cooling to room temperature, centrifuging, washing and drying to obtain a precursor;
step 2: SnO2Preparation of the Material
Drying the precursor at 80 ℃ for 12 hours, SnO2The sample (S1) was obtained after heating at a rate of 2 c/min and calcining in air at 500 c for 2 hours. Obtaining a second sample by replacing water with ethanolamine while keeping other conditions unchanged (S2);
SnCl2·2H2o is insoluble in triethanolamine, so 60mL of distilled water and 60mL of triethanolamine were magnetically stirred at room temperature for 2h to obtain a homogeneous solvent. Other samples were prepared at 160 ℃ as above for other experimental procedures, resulting in samples S3-160. The samples obtained at 100 ℃ and 130 ℃ were designated S3-100 and S3-130, respectively, with the other conditions unchanged;
and step 3: gas sensing performance testing
The gas sensor is made into an indirectly heated sintered element by a traditional method. Welding a ceramic tube on a base, then heating a nickel-chromium wire (Ni-Cr), supplying an element with proper working temperature to penetrate through the ceramic tube and also welding the element on the base, and re-welding a detection welding point without an indication number by using a universal meter 2K ohm measuring range to measure resistance. After the number is indicated, a small amount of sample is taken by a medicine spoon, continuously ground and blended into paste. Then coating the Pt lead wire outside the ceramic tube by using a coating pen; until the gold electrode is completely covered, each sample is numbered after the step is finished, and finally the sample is naturally volatilized and solidified at room temperature, and a layer of uniform gas-sensitive material-thick film is formed on the outer layer of the ceramic tube. Aging at 180mA for 120h to improve the repeatability and stability. And then performing gas-sensitive test on the CGS-8 intelligent gas-sensitive analysis system.
2. The method for preparing Sn according to claim 1 by hydrothermal synthesisO2A method of producing nanomaterials, comprising: and the sensing test temperature in the step 3 is 100-160 ℃.
3. SnO prepared by hydrothermal synthesis method according to claim 12A method of gas sensing materials, characterized by: in the step 3, the gas sensitivity is defined as R ═ Ra/Rg, the response time T1 is the time required for the resistance change value of the sensing material to fall to 90% of the maximum difference value after the sensing gas enters, and the recovery time T2 is the time required for the resistance change value of the sensing material to rise to 90% of the maximum difference value after the sensing gas is turned off.
CN202110464018.7A 2021-04-29 2021-04-29 SnO/SnO synthesized by adopting hydrothermal method2Method for preparing nano composite gas-sensitive material Pending CN113213528A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115676873A (en) * 2022-10-08 2023-02-03 电子科技大学长三角研究院(湖州) Defect-state tin oxide normal-temperature sensing material, preparation method and application

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN115676873A (en) * 2022-10-08 2023-02-03 电子科技大学长三角研究院(湖州) Defect-state tin oxide normal-temperature sensing material, preparation method and application

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