CN115262034B - Chain bead-shaped tin oxide-based heterogeneous nanofiber gas-sensitive material, and preparation and application thereof - Google Patents
Chain bead-shaped tin oxide-based heterogeneous nanofiber gas-sensitive material, and preparation and application thereof Download PDFInfo
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- CN115262034B CN115262034B CN202210847330.9A CN202210847330A CN115262034B CN 115262034 B CN115262034 B CN 115262034B CN 202210847330 A CN202210847330 A CN 202210847330A CN 115262034 B CN115262034 B CN 115262034B
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- 239000000463 material Substances 0.000 title claims abstract description 93
- 239000002121 nanofiber Substances 0.000 title claims abstract description 57
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 229910001887 tin oxide Inorganic materials 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title abstract description 11
- BDERNNFJNOPAEC-UHFFFAOYSA-N propan-1-ol Chemical compound CCCO BDERNNFJNOPAEC-UHFFFAOYSA-N 0.000 claims abstract description 48
- 238000001523 electrospinning Methods 0.000 claims abstract description 24
- 238000010041 electrostatic spinning Methods 0.000 claims abstract description 18
- 238000001354 calcination Methods 0.000 claims abstract description 17
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims abstract description 9
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical class [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims abstract description 7
- 239000011324 bead Substances 0.000 claims abstract description 7
- 229920000642 polymer Polymers 0.000 claims abstract description 7
- 238000005516 engineering process Methods 0.000 claims abstract description 6
- 230000002194 synthesizing effect Effects 0.000 claims abstract description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 39
- 238000003756 stirring Methods 0.000 claims description 19
- 238000001027 hydrothermal synthesis Methods 0.000 claims description 15
- XEEYBQQBJWHFJM-UHFFFAOYSA-N iron Substances [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 11
- -1 iron ions Chemical class 0.000 claims description 10
- 238000010438 heat treatment Methods 0.000 claims description 8
- 229910052742 iron Inorganic materials 0.000 claims description 8
- 238000000034 method Methods 0.000 claims description 8
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims description 8
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims description 8
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims description 8
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 4
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 claims description 4
- 239000003960 organic solvent Substances 0.000 claims description 4
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 4
- TXUICONDJPYNPY-UHFFFAOYSA-N (1,10,13-trimethyl-3-oxo-4,5,6,7,8,9,11,12,14,15,16,17-dodecahydrocyclopenta[a]phenanthren-17-yl) heptanoate Chemical compound C1CC2CC(=O)C=C(C)C2(C)C2C1C1CCC(OC(=O)CCCCCC)C1(C)CC2 TXUICONDJPYNPY-UHFFFAOYSA-N 0.000 claims description 2
- OQBLGYCUQGDOOR-UHFFFAOYSA-L 1,3,2$l^{2}-dioxastannolane-4,5-dione Chemical compound O=C1O[Sn]OC1=O OQBLGYCUQGDOOR-UHFFFAOYSA-L 0.000 claims description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 claims description 2
- WQZGKKKJIJFFOK-GASJEMHNSA-N Glucose Natural products OC[C@H]1OC(O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-GASJEMHNSA-N 0.000 claims description 2
- 239000004793 Polystyrene Substances 0.000 claims description 2
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 claims description 2
- 235000019253 formic acid Nutrition 0.000 claims description 2
- 239000008103 glucose Substances 0.000 claims description 2
- 239000002245 particle Substances 0.000 claims description 2
- 229920002239 polyacrylonitrile Polymers 0.000 claims description 2
- 229920002223 polystyrene Polymers 0.000 claims description 2
- 235000011150 stannous chloride Nutrition 0.000 claims description 2
- 239000001119 stannous chloride Substances 0.000 claims description 2
- RCIVOBGSMSSVTR-UHFFFAOYSA-L stannous sulfate Chemical compound [SnH2+2].[O-]S([O-])(=O)=O RCIVOBGSMSSVTR-UHFFFAOYSA-L 0.000 claims description 2
- 229910000375 tin(II) sulfate Inorganic materials 0.000 claims description 2
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 claims description 2
- 239000012855 volatile organic compound Substances 0.000 abstract description 9
- 229910021645 metal ion Inorganic materials 0.000 abstract description 7
- 238000001514 detection method Methods 0.000 abstract description 6
- 230000007774 longterm Effects 0.000 abstract description 2
- 239000007789 gas Substances 0.000 description 129
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 43
- 229910006404 SnO 2 Inorganic materials 0.000 description 17
- 239000006228 supernatant Substances 0.000 description 17
- 230000004044 response Effects 0.000 description 16
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 15
- 229910052799 carbon Inorganic materials 0.000 description 15
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 13
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 12
- ZMANZCXQSJIPKH-UHFFFAOYSA-N Triethylamine Chemical compound CCN(CC)CC ZMANZCXQSJIPKH-UHFFFAOYSA-N 0.000 description 12
- 229910052782 aluminium Inorganic materials 0.000 description 12
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 12
- 239000011888 foil Substances 0.000 description 12
- 238000001291 vacuum drying Methods 0.000 description 12
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 11
- 238000004140 cleaning Methods 0.000 description 11
- 235000019441 ethanol Nutrition 0.000 description 11
- 230000035945 sensitivity Effects 0.000 description 9
- LRHPLDYGYMQRHN-UHFFFAOYSA-N N-Butanol Chemical compound CCCCO LRHPLDYGYMQRHN-UHFFFAOYSA-N 0.000 description 8
- DNJIEGIFACGWOD-UHFFFAOYSA-N ethanethiol Chemical compound CCS DNJIEGIFACGWOD-UHFFFAOYSA-N 0.000 description 8
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 7
- 230000000052 comparative effect Effects 0.000 description 7
- 239000008367 deionised water Substances 0.000 description 7
- 229910021641 deionized water Inorganic materials 0.000 description 7
- 229960001031 glucose Drugs 0.000 description 7
- 238000001000 micrograph Methods 0.000 description 7
- 238000012360 testing method Methods 0.000 description 7
- 239000012295 chemical reaction liquid Substances 0.000 description 6
- 229910044991 metal oxide Inorganic materials 0.000 description 6
- 150000004706 metal oxides Chemical class 0.000 description 6
- 239000000203 mixture Substances 0.000 description 6
- 229920003023 plastic Polymers 0.000 description 6
- 239000004033 plastic Substances 0.000 description 6
- 229920001343 polytetrafluoroethylene Polymers 0.000 description 6
- 239000004810 polytetrafluoroethylene Substances 0.000 description 6
- 239000002244 precipitate Substances 0.000 description 6
- 229910001220 stainless steel Inorganic materials 0.000 description 6
- 239000010935 stainless steel Substances 0.000 description 6
- 238000011084 recovery Methods 0.000 description 5
- 239000011701 zinc Substances 0.000 description 5
- 238000005457 optimization Methods 0.000 description 4
- 238000011160 research Methods 0.000 description 4
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 3
- 239000010949 copper Substances 0.000 description 3
- 230000036541 health Effects 0.000 description 3
- 239000011159 matrix material Substances 0.000 description 3
- 229910052725 zinc Inorganic materials 0.000 description 3
- 238000004458 analytical method Methods 0.000 description 2
- 239000000919 ceramic Substances 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 238000012544 monitoring process Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 206010010071 Coma Diseases 0.000 description 1
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 description 1
- 229910002554 Fe(NO3)3·9H2O Inorganic materials 0.000 description 1
- 208000019693 Lung disease Diseases 0.000 description 1
- 206010028813 Nausea Diseases 0.000 description 1
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 description 1
- 239000003905 agrochemical Substances 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 229910001429 cobalt ion Inorganic materials 0.000 description 1
- XLJKHNWPARRRJB-UHFFFAOYSA-N cobalt(2+) Chemical compound [Co+2] XLJKHNWPARRRJB-UHFFFAOYSA-N 0.000 description 1
- 229910001431 copper ion Inorganic materials 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 201000010099 disease Diseases 0.000 description 1
- 208000037265 diseases, disorders, signs and symptoms Diseases 0.000 description 1
- 208000002173 dizziness Diseases 0.000 description 1
- 239000000975 dye Substances 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000003205 fragrance Substances 0.000 description 1
- 238000004868 gas analysis Methods 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 230000008693 nausea Effects 0.000 description 1
- 229910001453 nickel ion Inorganic materials 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 238000011056 performance test Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 238000005036 potential barrier Methods 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 238000004445 quantitative analysis Methods 0.000 description 1
- 238000011897 real-time detection Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 238000003892 spreading Methods 0.000 description 1
- 230000007480 spreading Effects 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
Classifications
-
- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F9/00—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments
- D01F9/08—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material
- D01F9/10—Artificial filaments or the like of other substances; Manufacture thereof; Apparatus specially adapted for the manufacture of carbon filaments of inorganic material by decomposition of organic substances
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N33/00—Investigating or analysing materials by specific methods not covered by groups G01N1/00 - G01N31/00
- G01N33/0004—Gaseous mixtures, e.g. polluted air
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02A—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE
- Y02A50/00—TECHNOLOGIES FOR ADAPTATION TO CLIMATE CHANGE in human health protection, e.g. against extreme weather
- Y02A50/20—Air quality improvement or preservation, e.g. vehicle emission control or emission reduction by using catalytic converters
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Health & Medical Sciences (AREA)
- Life Sciences & Earth Sciences (AREA)
- Food Science & Technology (AREA)
- Analytical Chemistry (AREA)
- Textile Engineering (AREA)
- General Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- Medicinal Chemistry (AREA)
- Physics & Mathematics (AREA)
- Combustion & Propulsion (AREA)
- Biochemistry (AREA)
- General Health & Medical Sciences (AREA)
- General Physics & Mathematics (AREA)
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- Pathology (AREA)
- Investigating Or Analyzing Materials By The Use Of Fluid Adsorption Or Reactions (AREA)
Abstract
The invention discloses a chain bead tin oxide-based heterogeneous nanofiber gas-sensitive material and preparation and application thereof, wherein the preparation method of the gas-sensitive material comprises the following steps: synthesizing nano fibers by using an electrostatic spinning technology, and calcining in air to obtain the heterogeneous nano fiber gas-sensitive material; among them, the electrospinning solution required for electrospinning includes tin salt, carbonaceous spheres adsorbing metal ions, and polymer. When the gas-sensitive material is applied to a gas-sensitive sensor, high-selectivity, high-sensitivity and long-term stable detection of various Volatile Organic Compounds (VOCs) such as n-propanol can be realized.
Description
Technical Field
The invention belongs to the technical field of nano materials, and particularly relates to a chain bead-shaped tin oxide-based heterogeneous nanofiber gas-sensitive material, and preparation and application thereof.
Background
Research shows that high concentration of Volatile Organic Compounds (VOCs) can cause serious pollution to the environment and simultaneously harm human health. For example, n-propanol is not only a colorless transparent liquid, but also a toxic volatile organic compound, and is widely used in pharmaceutical, clinical laboratory, agricultural products, and in the production of dyes, cosmetics, fragrances, and agricultural chemicals. If the human body stays in the high-concentration n-propanol environment, dizziness, nausea or coma can be caused, and even the possibility of pulmonary diseases is increased. Thus, health and safety issues require highly sensitive and highly selective detection and quantitative analysis of n-propanol, early identification and real-time detection of n-propanol concentration being critical for protecting people from diseases, and the great risk of n-propanol gas has led to great interest in its detection.
Meanwhile, the emission of other VOCs gases such as acetone, triethylamine, ethanethiol, n-butanol and the like can cause the problems of human body harm, environmental pollution and the like, and the material has great significance in the aspects of human health, environmental monitoring, food safety and the like for the analysis and detection of the gases.
Tin dioxide (SnO 2) was the metal oxide gas-sensitive material of earliest research and commercialization. In 1962, taguchi et al studied the gas-sensitive properties of SnO 2, and opened the way for gas sensing technology; in 1968, the fei-plus company developed a Pt and Pb-doped SnO 2 gas sensor for the first time, which marks that the gas sensing technology formally enters the practical and commercialized stage. In the last decades, semiconductor gas sensors using SnO 2 as a matrix material have been one of the research hotspots of a large number of researchers. In 2004, eramiat et al analyzed documents related to metal oxide gas sensitive materials, and found that SnO 2 material was present in a proportion of up to 35% and was the first of all metal oxide gas sensitive materials. Therefore, snO 2 material is used as a gas-sensitive material, and the realization of monitoring of relevant information such as identification and concentration of VOCs gas such as n-propanol and the like is a great theoretical basis.
However, as with most metal oxide-based gas sensors, snO 2 -based gas sensors also suffer from high operating temperatures, poor selectivity and stability, longer response/recovery times, sensitivity to be further improved, and the like, and are currently mainly addressed by means of component optimization and structural optimization. A great deal of research shows that after a small amount of other metal oxides are doped in the SnO 2 matrix material, a series of changes can occur in the properties of the material, such as catalytic activity, carrier concentration, physical and chemical properties, surface electrical properties, grain size, surface potential barriers, grain boundary barriers and the like, and certain influence is exerted on the properties of the material. Therefore, component optimization is one of effective ways for improving and enhancing the performance of the gas-sensitive material, and is mainly realized by doping, surface modification to form p-n junction, p-p junction, n-n junction and other methods. And how to use component optimization to solve the problems of low sensitivity, poor selectivity and the like of the SnO 2 gas-sensitive material in measuring various volatile organic compounds such as n-propanol and the like is a hot spot problem in the prior VOCs gas analysis and detection.
Disclosure of Invention
Based on the technical problems in the background art, the invention provides a chain bead tin oxide-based heterogeneous nanofiber gas-sensitive material, and preparation and application thereof, wherein when the gas-sensitive material is applied to a gas sensor, high-selectivity, high-sensitivity and long-term stable detection of various atmospheric pollutants such as n-propanol can be realized.
The invention provides a preparation method of a chain bead tin oxide-based heterogeneous nanofiber gas-sensitive material, which comprises the following steps: synthesizing nano fibers by using an electrostatic spinning technology, and calcining in air to obtain the heterogeneous nano fiber gas-sensitive material;
Wherein the electrospinning solution comprises a tin salt, carbonaceous spheres that adsorb metal ions, and a polymer.
Preferably, in the electrospinning solution, the tin salt is preferably at least one of stannous chloride, stannous oxalate, stannic chloride or stannous sulfate; the metal ion is preferably at least one of iron ion, cobalt ion, copper ion, nickel ion or zinc ion; the polymer is preferably at least one of polyvinylpyrrolidone, polyvinyl alcohol, polyacrylonitrile or polystyrene.
Preferably, the carbonaceous ball for adsorbing metal ions is obtained by adding the carbonaceous ball into a solution containing metal ions and stirring and adsorbing;
Preferably, the carbonaceous spheres are obtained by subjecting glucose to a hydrothermal reaction;
Preferably, the carbonaceous spheres have a particle size of 700-800nm.
Preferably, in the electrospinning solution, the mass ratio of the tin salt to the carbonaceous balls adsorbing metal ions to the polymer is 1:0.4-2:3-5.
Preferably, the electrospinning solution further comprises an organic solvent;
Preferably, the organic solvent is at least one of N, N-dimethylformamide, polyvinyl alcohol, or formic acid.
Preferably, the voltage of the electrostatic spinning is 14-16kV, the distance between the needle head and the collector is 10-20cm, and the feeding speed is 0.0002-0.0004mm/s.
Preferably, the calcination temperature is 450-550 ℃, the time is 1-3h, and the heating rate is 1-3 ℃/min.
The invention provides a chain bead-shaped tin oxide-based heterogeneous nanofiber gas-sensitive material, which is prepared by the preparation method.
The invention also provides application of the chain bead-shaped tin oxide-based heterogeneous nanofiber gas-sensitive material in a gas sensor.
Preferably, the gas sensor is an n-propanol, acetone, triethylamine, ethanethiol or n-butanol gas sensor.
The beneficial effects of the invention are as follows:
SnO 2, a typical n-type semiconductor, exhibits the unique characteristics required for an ideal gas sensor, with a wide band gap of 3.5eV, high electron mobility, photoelectric response, excellent chemical and thermal stability; meanwhile, snO 2 has the advantages of low cost, no toxicity, easy preparation and suitability for large-scale production;
According to the tin oxide-based heterogeneous nanofiber gas-sensitive material, a carbonaceous ball absorbing metal ions is used as a template, and a small amount of other metal oxides are doped in the obtained SnO 2 matrix material after electrostatic spinning and calcination to obtain the SnO 2/MO (Fe, co, cu, ni or Zn) heterogeneous nanofiber with a specific configuration; MO (Fe, co, cu, ni or Zn) in the heterogeneous nanofiber presents a hollow structure, snO 2 is wrapped outside the MO (Fe, co, cu, ni or Zn) to form a heterojunction, and finally the tin oxide-based heterogeneous nanofiber gas-sensitive material with a chain bead-like microstructure is obtained; tests show that the gas-sensitive performance of the obtained tin oxide-based heterogeneous nanofiber gas-sensitive material is obviously improved, particularly, the response to n-propanol, acetone, triethylamine, ethanethiol or n-butanol is better, the gas-sensitive performance is obviously improved when the tin oxide-based heterogeneous nanofiber gas-sensitive material is applied to a gas-sensitive sensor, and the gas-sensitive performance reaches a higher level; meanwhile, the one-dimensional nanofiber structure promotes the adsorption and analysis of the gas, and the performance of the gas sensor is further effectively improved.
Drawings
FIG. 1 is a flow chart of the preparation of the beaded tin oxide based heterogeneous nanofiber gas sensitive material of examples 1-5;
FIG. 2 is a scanning electron microscope image of a gas sensitive material doped with 100mg carbonaceous spheres obtained in examples 1-5;
FIG. 3 is a graph showing the sensitivity test of 100ppm n-propanol when the gas-sensitive material obtained in example 1 and comparative example 1 is used in a gas-sensitive sensor;
FIG. 4 is a graph showing the selectivity of the gas sensor for different gases when the gas sensor material with the optimal carbon sphere doping amount obtained in examples 2-5 is used.
Detailed Description
The present invention will be described in detail by way of specific examples, which should be clearly set forth for the purpose of illustration and are not to be construed as limiting the scope of the present invention.
Example 1
The embodiment provides a chain bead-shaped tin oxide-based heterogeneous nanofiber gas-sensitive material, which is prepared by the following method:
(1) 5.9451g of glucose monohydrate (C 6H12O6·H2 O), 0.1822g of Cetyl Trimethyl Ammonium Bromide (CTAB) and 30mL of deionized water are mixed and stirred for 1.5h at 50 ℃ to be uniformly mixed, the mixture is transferred into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, the hydrothermal reaction is carried out for 300min at 180 ℃, the obtained reaction liquid is subjected to supernatant removal by a pipette, and the obtained precipitate is subjected to centrifugal cleaning by adopting ethanol and water in sequence until the supernatant is colorless and transparent, so that Carbonaceous Spheres (CSs) are obtained;
(2) Dispersing 100mg of the carbonaceous balls in 8mL of absolute ethyl alcohol, stirring for 60min to obtain a carbonaceous ball solution, dissolving 808mg of Fe (NO 3)3·9H2 O (2 mmol) in 2mL of absolute ethyl alcohol, dropwise adding the obtained solution into the carbonaceous ball solution under stirring, stirring for 12h, transferring into a 50mL centrifuge tube, and centrifugally cleaning the supernatant with ethanol and DMF to be colorless and transparent to obtain the carbonaceous balls adsorbed with Fe 3+;
(3) 0mg, 25mg, 50mg, 75mg, 100mg, 200mg of the carbonaceous spheres adsorbed with Fe 3+ and 113mg of SnCl 2·2H2 O (0.5 mmol), 0.45g of polyvinylpyrrolidone were added to 2.25mL of N-N Dimethylformamide (DMF), and stirred at a rate of 100rpm for 12 hours at room temperature to obtain an electrospinning solution;
(4) Placing the electrospinning solution into a 5mL plastic injector with a 19G blunt stainless steel needle for electrostatic spinning, applying 15kV voltage between the needle tip and an aluminum foil collector, wherein the distance between the needle tip and the aluminum foil collector is fixed to be 15cm, and the feeding speed is 0.0003mm/s, so as to obtain the nanofiber after electrostatic spinning;
(5) Placing the electrospun nanofiber in a vacuum drying oven for vacuum drying for 9 hours, and then calcining in air at the temperature of 500 ℃ for 2 hours at the heating rate of 2 ℃/min to obtain the chain bead-shaped tin oxide-based heterogeneous nanofiber gas-sensitive material with different carbon sphere doping amounts, which are respectively abbreviated as SnO 2, sn/Fe-25, sn/Fe-50, sn/Fe-75, sn/Fe-100 and Sn/Fe-200; wherein the gas sensitive material with the optimal carbon sphere doping amount is Sn/Fe-50.
Example 2
The embodiment provides a chain bead-shaped tin oxide-based heterogeneous nanofiber gas-sensitive material, which is prepared by the following method:
(1) 5.9451g of glucose monohydrate (C 6H12O6·H2 O), 0.1822g of Cetyl Trimethyl Ammonium Bromide (CTAB) and 30mL of deionized water are mixed and stirred for 1.5h at 50 ℃ to be uniformly mixed, the mixture is transferred into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, the hydrothermal reaction is carried out for 300min at 180 ℃, the obtained reaction liquid is subjected to supernatant removal by a pipette, and the obtained precipitate is subjected to centrifugal cleaning by adopting ethanol and water in sequence until the supernatant is colorless and transparent, so that Carbonaceous Spheres (CSs) are obtained;
(2) Dispersing 100mg of the carbonaceous balls in 8mL of absolute ethyl alcohol, stirring for 60min to obtain a carbonaceous ball solution, dissolving 582mg of Co (NO 3)2·6H2 O (2 mmol) in 2mL of absolute ethyl alcohol, dropwise adding the obtained solution into the carbonaceous ball solution under stirring, stirring for 12h, transferring into a 50mL centrifuge tube, and sequentially centrifugally cleaning with ethanol and DMF to obtain a colorless transparent supernatant, thereby obtaining the carbonaceous balls adsorbed with Co 2+;
(3) 0mg, 25mg, 50mg, 75mg, 100mg, 200mg of Co 2+ -adsorbed carbonaceous spheres and 113mg of SnCl 2·2H2 O (0.5 mmol), 0.45g of polyvinylpyrrolidone were added to 2.25mL of N-N Dimethylformamide (DMF), and stirred at a rate of 100rpm for 12 hours at room temperature to obtain an electrospinning solution, respectively;
(4) Placing the electrospinning solution into a 5mL plastic injector with a 19G blunt stainless steel needle for electrostatic spinning, applying 15kV voltage between the needle tip and an aluminum foil collector, wherein the distance between the needle tip and the aluminum foil collector is fixed to be 15cm, and the feeding speed is 0.0003mm/s, so as to obtain the nanofiber after electrostatic spinning;
(5) And (3) placing the electrospun nanofiber in a vacuum drying oven for vacuum drying for 9 hours, and then calcining in air at the temperature of 500 ℃ for 2 hours at the heating rate of 2 ℃/min to obtain the chain bead-shaped tin oxide-based heterogeneous nanofiber gas-sensitive material with different carbon sphere doping amounts, which are respectively abbreviated as SnO 2, sn/Co-25, sn/Co-50, sn/Co-75, sn/Co-100 and Sn/Co-200, wherein the gas-sensitive material with the optimal carbon sphere doping amount is Sn/Co-100.
Example 3
The embodiment provides a chain bead-shaped tin oxide-based heterogeneous nanofiber gas-sensitive material, which is prepared by the following method:
(1) 5.9451g of glucose monohydrate (C 6H12O6·H2 O), 0.1822g of Cetyl Trimethyl Ammonium Bromide (CTAB) and 30mL of deionized water are mixed and stirred for 1.5h at 50 ℃ to be uniformly mixed, the mixture is transferred into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, the hydrothermal reaction is carried out for 300min at 180 ℃, the obtained reaction liquid is subjected to supernatant removal by a pipette, and the obtained precipitate is subjected to centrifugal cleaning by adopting ethanol and water in sequence until the supernatant is colorless and transparent, so that Carbonaceous Spheres (CSs) are obtained;
(2) Dispersing 100mg of the carbonaceous balls in 8mL of absolute ethyl alcohol, stirring for 60min to obtain a carbonaceous ball solution, dissolving 475mgNiCl 2·6H2 O (2 mmol) in 2mL of absolute ethyl alcohol, dropwise adding the obtained solution into the carbonaceous ball solution under the stirring condition, stirring for 12h, transferring into a 50mL centrifuge tube, and sequentially adopting ethanol and DMF for centrifugal cleaning until the supernatant is colorless and transparent to obtain the carbonaceous balls adsorbed with Ni 2+;
(3) 0mg, 25mg, 50mg, 75mg, 100mg, 200mg of Ni 2+ -adsorbed carbonaceous spheres and 113mg of SnCl 2·2H2 O (0.5 mmol), respectively, and 0.45g of polyvinylpyrrolidone were added to 2.25mL of N-N Dimethylformamide (DMF), followed by stirring at a rate of 100rpm for 12 hours at room temperature to obtain an electrospinning solution;
(4) Placing the electrospinning solution into a 5mL plastic injector with a 19G blunt stainless steel needle for electrostatic spinning, applying 15kV voltage between the needle tip and an aluminum foil collector, wherein the distance between the needle tip and the aluminum foil collector is fixed to be 15cm, and the feeding speed is 0.0003mm/s, so as to obtain the nanofiber after electrostatic spinning;
(5) And (3) placing the electrospun nanofiber in a vacuum drying oven for vacuum drying for 9 hours, and then calcining in air at the temperature of 500 ℃ for 2 hours at the heating rate of 2 ℃/min to obtain the chain bead-shaped tin oxide-based heterogeneous nanofiber gas-sensitive material with different carbon sphere doping amounts, which are respectively abbreviated as SnO 2, sn/Ni-25, sn/Ni-50, sn/Ni-75, sn/Ni-100 and Sn/Ni-200, wherein the gas-sensitive material with the optimal carbon sphere doping amount is Sn/Ni-50.
Example 4
The embodiment provides a chain bead-shaped tin oxide-based heterogeneous nanofiber gas-sensitive material, which is prepared by the following method:
(1) 5.9451g of glucose monohydrate (C 6H12O6·H2 O), 0.1822g of Cetyl Trimethyl Ammonium Bromide (CTAB) and 30mL of deionized water are mixed and stirred for 1.5h at 50 ℃ to be uniformly mixed, the mixture is transferred into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, the hydrothermal reaction is carried out for 300min at 180 ℃, the obtained reaction liquid is subjected to supernatant removal by a pipette, and the obtained precipitate is subjected to centrifugal cleaning by adopting ethanol and water in sequence until the supernatant is colorless and transparent, so that Carbonaceous Spheres (CSs) are obtained;
(2) Dispersing 100mg of the carbonaceous balls in 8mL of absolute ethyl alcohol, stirring for 60min to obtain a carbonaceous ball solution, dissolving 483mg of Cu (NO 3)2·3H2 O (2 mmol) in 2mL of absolute ethyl alcohol, dropwise adding the obtained solution into the carbonaceous ball solution under stirring, stirring for 12h, transferring into a 50mL centrifuge tube, and sequentially centrifugally cleaning with ethanol and DMF until the supernatant is colorless and transparent to obtain the carbonaceous balls adsorbed with Cu 2+;
(3) 0mg, 25mg, 50mg, 75mg, 100mg, 200mg of Cu 2+ -adsorbed carbonaceous spheres and 113mg of SnCl 2·2H2 O (0.5 mmol), respectively, and 0.45g of polyvinylpyrrolidone were added to 2.25mL of N-N Dimethylformamide (DMF), and stirred at a rate of 100rpm for 12 hours at room temperature to obtain an electrospinning solution;
(4) Placing the electrospinning solution into a 5mL plastic injector with a 19G blunt stainless steel needle for electrostatic spinning, applying 15kV voltage between the needle tip and an aluminum foil collector, wherein the distance between the needle tip and the aluminum foil collector is fixed to be 15cm, and the feeding speed is 0.0003mm/s, so as to obtain the nanofiber after electrostatic spinning;
(5) And (3) placing the electrospun nanofiber in a vacuum drying oven for vacuum drying for 9 hours, and then calcining in air, wherein the calcining temperature is 500 ℃, the calcining time is 2 hours, and the heating rate is 2 ℃/min, so that the chain bead-shaped tin oxide-based heterogeneous nanofiber gas-sensitive materials with different carbon sphere doping amounts are obtained, which are respectively abbreviated as SnO 2, sn/Cu-25, sn/Cu-50, sn/Cu-75, sn/Cu-100 and Sn/Cu-200, wherein the gas-sensitive material with the optimal carbon sphere doping amount is Sn/Cu-50.
Example 5
The embodiment provides a chain bead-shaped tin oxide-based heterogeneous nanofiber gas-sensitive material, which is prepared by the following method:
(1) 5.9451g of glucose monohydrate (C 6H12O6·H2 O), 0.1822g of Cetyl Trimethyl Ammonium Bromide (CTAB) and 30mL of deionized water are mixed and stirred for 1.5h at 50 ℃ to be uniformly mixed, the mixture is transferred into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, the hydrothermal reaction is carried out for 300min at 180 ℃, the obtained reaction liquid is subjected to supernatant removal by a pipette, and the obtained precipitate is subjected to centrifugal cleaning by adopting ethanol and water in sequence until the supernatant is colorless and transparent, so that Carbonaceous Spheres (CSs) are obtained;
(2) Dispersing 100mg of the carbonaceous balls in 8mL of absolute ethyl alcohol, stirring for 60min to obtain a carbonaceous ball solution, dissolving 595mgZn (NO 3)2·6H2 O (2 mmol) in 2mL of absolute ethyl alcohol, dropwise adding the obtained solution into the carbonaceous ball solution under stirring, stirring for 12h, transferring into a 50mL centrifuge tube, and sequentially centrifugally cleaning with ethanol and DMF until the supernatant is colorless and transparent to obtain the carbonaceous balls adsorbed with Zn 2+;
(3) 0mg, 25mg, 50mg, 75mg, 100mg, 200mg of Zn 2+ -adsorbed carbonaceous spheres and 113mg of SnCl 2·2H2 O (0.5 mmol), respectively, and 0.45g of polyvinylpyrrolidone were added to 2.25mL of N-N Dimethylformamide (DMF), followed by stirring at a rate of 100rpm for 12 hours at room temperature to obtain an electrospinning solution;
(4) Placing the electrospinning solution into a 5mL plastic injector with a 19G blunt stainless steel needle for electrostatic spinning, applying 15kV voltage between the needle tip and an aluminum foil collector, wherein the distance between the needle tip and the aluminum foil collector is fixed to be 15cm, and the feeding speed is 0.0003mm/s, so as to obtain the nanofiber after electrostatic spinning;
(5) And (3) placing the electrospun nanofiber in a vacuum drying oven for vacuum drying for 9 hours, and then calcining in air, wherein the calcining temperature is 500 ℃, the calcining time is 2 hours, and the heating rate is 2 ℃/min, so that the chain bead-shaped tin oxide-based heterogeneous nanofiber gas-sensitive material with the optimal carbon sphere doping amount is obtained, which is respectively abbreviated as SnO 2, sn/Zn-25, sn/Zn-50, sn/Zn-75, sn/Zn-100 and Sn/Zn-200, wherein the gas-sensitive material with the optimal carbon sphere doping amount is Sn/Zn-75.
Comparative example 1
The comparative example proposes a tin oxide-based heterogeneous nanofiber gas-sensitive material, which is prepared by the following method:
(1) 5.9451g of glucose monohydrate (C 6H12O6·H2 O), 0.1822g of Cetyl Trimethyl Ammonium Bromide (CTAB) and 30mL of deionized water are mixed and stirred for 1.5h at 50 ℃ to be uniformly mixed, the mixture is transferred into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, the hydrothermal reaction is carried out for 300min at 180 ℃, the obtained reaction liquid is subjected to supernatant removal by a pipette, and the obtained precipitate is subjected to centrifugal cleaning by adopting ethanol and water in sequence until the supernatant is colorless and transparent, so that Carbonaceous Spheres (CSs) are obtained;
(2) 50mg of carbonaceous spheres and 113mg of SnCl 2·2H2 O (0.5 mmol), 0.45g of polyvinylpyrrolidone were added to 2.25mL of N-N Dimethylformamide (DMF), and stirred at 100rpm for 12 hours at room temperature to obtain an electrospinning solution;
(3) Placing the electrospinning solution into a 5mL plastic injector with a 19G blunt stainless steel needle for electrostatic spinning, applying 15kV voltage between the needle tip and an aluminum foil collector, wherein the distance between the needle tip and the aluminum foil collector is fixed to be 15cm, and the feeding speed is 0.0003mm/s, so as to obtain the nanofiber after electrostatic spinning;
(4) And (3) placing the electrospun nanofiber in a vacuum drying oven for vacuum drying for 9 hours, and then calcining in air at the calcining temperature of 500 ℃ for 2 hours at the heating rate of 2 ℃/min to obtain the tin oxide-based heterogeneous nanofiber gas-sensitive material, namely SnO 2/CSs-50.
FIG. 1 is a flow chart of the preparation of the beaded tin oxide based hetero-nanofiber gas-sensitive material of examples 1-5. As can be seen from fig. 1, after synthesizing carbonaceous balls by hydrothermal reaction and ion adsorption, the tin oxide-based heterogeneous nanofiber gas-sensitive material using the carbonaceous balls as a template is formed by using an electrostatic spinning technology and high-temperature calcination in air.
FIG. 2 is a scanning electron micrograph of a gas sensitive material with 100mg carbonaceous spheres doping obtained in examples 1-5: FIG. 2 (a) is a scanning electron microscope image of a SnO 2 gas sensitive material; FIG. 2 (b) is a scanning electron microscope image of Sn/Fe-100 gas sensitive material; FIG. 2 (c) is a scanning electron microscope image of Sn/Co-100 gas sensitive material; FIG. 2 (d) is a scanning electron microscope image of Sn/Ni-100 gas sensitive material; FIG. 2 (e) is a scanning electron microscope image of Sn/Cu-100 gas sensitive material; FIG. 2 (f) is a scanning electron microscope image of Sn/Zn-100 gas sensitive material; the insets in fig. 2 are transmission electron microscope pictures corresponding to the gas sensitive material, respectively. As can be seen from fig. 2, the fiber structure of the obtained gas-sensitive material has a structure with a plurality of heterojunctions, and the microstructure of the chain beads is shown in the whole.
Performance test:
uniformly spreading the films of the tin oxide-based heterogeneous nanofiber gas-sensitive materials obtained in the examples 1-5 and the comparative example 1 on the surface of a ceramic wafer, dropwise adding one drop of deionized water, and airing the ceramic wafer to obtain the gas-sensitive element of the gas-sensitive material in the examples and the gas-sensitive element of the gas-sensitive material in the comparative example.
The gas sensor is subjected to gas-sensitive test, and specifically the manufactured gas sensor is placed into a gas-sensitive test air chamber, and is connected with a Pian meter to apply 10V bias voltage to a material, and the voltmeter is used for controlling temperature; after circuit connection is completed, dry air is introduced into the air chamber, quantitative air to be tested is introduced after the baseline to be tested, the dry air is introduced again after the test is completed to recover the baseline, and meanwhile, response/recovery time is recorded, and test results are shown in fig. 3-4:
FIG. 3 is a graph showing the sensitivity test of 100ppm n-propanol when the gas-sensitive material obtained in example 1 and comparative example 1 is used in a gas-sensitive sensor; FIG. 3 (a) is a graph showing the response of the gas-sensitive materials obtained in example 1 and comparative example 1 to 100ppm n-propanol at different operating temperatures for a gas-sensitive sensor, wherein the optimal doping amount of the carbonaceous ball is 50mg, and the optimal response temperature is 250 ℃; FIG. 3 (b) is a graph showing the response and recovery time of the gas sensor to 100ppm n-propanol at 250℃of the optimal working temperature for the gas sensor using the gas-sensitive material with optimal carbon sphere doping amount obtained in example 1, wherein the response time is 25s and the recovery time is 37s, which indicates that the gas-sensitive element has better response and recovery characteristics; FIG. 3 (c) is a graph showing the real-time response of the optimum carbon sphere doping amount of the gas sensitive material obtained in example 1 to 1-100ppm n-propanol gas at an optimum working temperature of 250℃for the gas sensitive sensor; the inset is a linear fitting curve, and the linearity of the response of the nanofiber to 1-100ppm of n-propanol is better; FIG. 3 (d) is a graph showing the selectivity of the gas-sensitive material of example 1 for different gases when the gas-sensitive material of example 1 is used in a gas sensor, and shows that the gas-sensitive material of example 1 has good selectivity and sensitivity to n-propanol gas, and relatively weak response to other gases, which may be related to the synergistic effect of the nano-scale n-n junction formed by the material.
FIG. 4 is a graph showing the selectivity of the gas sensor for different gases when the gas sensor material with the optimal carbon sphere doping amount obtained in examples 2-5 is used; FIG. 4 (a) is a graph showing the selectivity of the gas-sensitive material with the optimal carbon sphere doping amount obtained in example 2 to different gases when the gas-sensitive material is used in a gas sensor, wherein the gas-sensitive material obtained in example 2 has good selectivity and sensitivity to acetone, and relatively weak response to other gases; FIG. 4 (b) is a graph showing the selectivity of the gas-sensitive material of example 3 to different gases when the gas-sensitive material is used in a gas sensor, wherein the gas-sensitive material of example 3 has good selectivity and sensitivity to triethylamine, and relatively weak response to other gases; FIG. 4 (c) is a graph showing the selectivity of the gas-sensitive material of example 4 to different gases when the gas-sensitive material is used in a gas sensor, wherein the gas-sensitive material of example 4 has good selectivity and sensitivity to ethanethiol, and relatively weak response to other gases; FIG. 4 (d) is a graph showing the selectivity of the gas-sensitive material of example 5 to different gases when the gas-sensitive material of example 5 is used in a gas sensor, wherein the gas-sensitive material of example 5 has good selectivity and sensitivity to n-butanol and relatively weak response to other gases.
The foregoing is only a preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art, who is within the scope of the present invention, should make equivalent substitutions or modifications according to the technical scheme of the present invention and the inventive concept thereof, and should be covered by the scope of the present invention.
Claims (6)
1. The application of the chain bead tin oxide based heterogeneous nanofiber gas-sensitive material in the n-propanol gas-sensitive sensor is characterized in that the chain bead tin oxide based heterogeneous nanofiber gas-sensitive material is prepared by the following method: synthesizing nano fibers by using an electrostatic spinning technology, and calcining in air to obtain the heterogeneous nano fiber gas-sensitive material;
wherein, the electrospinning solution required by the electrospinning comprises tin salt, carbonaceous balls for adsorbing iron ions and polymer;
In the electrospinning solution, the tin salt is at least one of stannous chloride, stannous oxalate, stannic chloride or stannous sulfate; the polymer is at least one of polyvinylpyrrolidone, polyvinyl alcohol, polyacrylonitrile or polystyrene; the carbonaceous ball for adsorbing the iron ions is obtained by adding the carbonaceous ball into a solution containing the iron ions and stirring and adsorbing.
2. The application of the chain bead tin oxide based heterogeneous nanofiber gas-sensitive material in an n-propanol gas-sensitive sensor, wherein the carbonaceous ball is obtained by carrying out a hydrothermal reaction on glucose;
The particle size of the carbonaceous ball is 700-800nm.
3. Use of a beaded tin oxide based hetero-nanofiber gas-sensitive material according to claim 1 or 2 in an n-propanol gas-sensitive sensor, characterized in that the mass ratio of tin salt, iron ion-adsorbing carbonaceous spheres and polymer in the electrospinning solution is 1:0.4-2:3-5.
4. Use of a beaded tin oxide based hetero-nanofiber gas-sensitive material according to claim 1 or 2 in an n-propanol gas-sensitive sensor, characterized in that the electrospinning solution further comprises an organic solvent;
the organic solvent is at least one of N, N-dimethylformamide, polyvinyl alcohol or formic acid.
5. The use of a beaded tin oxide based hetero-nanofiber gas-sensitive material according to claim 1 or 2 in an n-propanol gas-sensitive sensor, wherein the voltage of the electrospinning is 14-16kV, the distance of the needle from the collector is 10-20cm, and the feeding speed is 0.0002-0.0004mm/s.
6. The use of a beaded tin oxide based heterogeneous nanofiber gas-sensitive material according to claim 1 or 2 in an n-propanol gas-sensitive sensor, wherein the calcination temperature is 450-550 ℃, the time is 1-3h, and the heating rate is 1-3 ℃/min.
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