CN110016734A - A kind of preparation method of near-infrared enhancing room temperature air sensing material - Google Patents
A kind of preparation method of near-infrared enhancing room temperature air sensing material Download PDFInfo
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- CN110016734A CN110016734A CN201910305691.9A CN201910305691A CN110016734A CN 110016734 A CN110016734 A CN 110016734A CN 201910305691 A CN201910305691 A CN 201910305691A CN 110016734 A CN110016734 A CN 110016734A
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- room temperature
- stannic oxide
- temperature air
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- 238000002360 preparation method Methods 0.000 title claims abstract description 28
- 239000011540 sensing material Substances 0.000 title claims abstract description 16
- 230000002708 enhancing effect Effects 0.000 title claims abstract description 12
- XOLBLPGZBRYERU-UHFFFAOYSA-N tin dioxide Chemical compound O=[Sn]=O XOLBLPGZBRYERU-UHFFFAOYSA-N 0.000 claims abstract description 95
- 239000007789 gas Substances 0.000 claims abstract description 34
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000002071 nanotube Substances 0.000 claims abstract description 23
- 239000010931 gold Substances 0.000 claims abstract description 22
- PAYRUJLWNCNPSJ-UHFFFAOYSA-N Aniline Chemical compound NC1=CC=CC=C1 PAYRUJLWNCNPSJ-UHFFFAOYSA-N 0.000 claims abstract description 20
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 claims abstract description 19
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 19
- 239000001257 hydrogen Substances 0.000 claims abstract description 19
- 229910052739 hydrogen Inorganic materials 0.000 claims abstract description 19
- 239000001301 oxygen Substances 0.000 claims abstract description 19
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 19
- ROOXNKNUYICQNP-UHFFFAOYSA-N ammonium persulfate Chemical compound [NH4+].[NH4+].[O-]S(=O)(=O)OOS([O-])(=O)=O ROOXNKNUYICQNP-UHFFFAOYSA-N 0.000 claims abstract description 18
- 239000000463 material Substances 0.000 claims abstract description 17
- 235000019441 ethanol Nutrition 0.000 claims abstract description 15
- 229920000767 polyaniline Polymers 0.000 claims abstract description 14
- 235000013855 polyvinylpyrrolidone Nutrition 0.000 claims abstract description 13
- 229920000036 polyvinylpyrrolidone Polymers 0.000 claims abstract description 13
- 239000001267 polyvinylpyrrolidone Substances 0.000 claims abstract description 13
- 238000009832 plasma treatment Methods 0.000 claims abstract description 10
- 235000012501 ammonium carbonate Nutrition 0.000 claims abstract description 9
- 229910001870 ammonium persulfate Inorganic materials 0.000 claims abstract description 9
- KHMOASUYFVRATF-UHFFFAOYSA-J tin(4+);tetrachloride;pentahydrate Chemical compound O.O.O.O.O.Cl[Sn](Cl)(Cl)Cl KHMOASUYFVRATF-UHFFFAOYSA-J 0.000 claims abstract description 6
- 239000002105 nanoparticle Substances 0.000 claims abstract description 5
- RJHLTVSLYWWTEF-UHFFFAOYSA-K gold trichloride Chemical class Cl[Au](Cl)Cl RJHLTVSLYWWTEF-UHFFFAOYSA-K 0.000 claims abstract description 4
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims abstract description 3
- 239000001099 ammonium carbonate Substances 0.000 claims abstract description 3
- 239000002994 raw material Substances 0.000 claims abstract description 3
- 239000000243 solution Substances 0.000 claims description 41
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 30
- 238000003756 stirring Methods 0.000 claims description 20
- 239000000835 fiber Substances 0.000 claims description 15
- 239000008367 deionised water Substances 0.000 claims description 9
- 229910021641 deionized water Inorganic materials 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- 239000007864 aqueous solution Substances 0.000 claims description 7
- 229910001887 tin oxide Inorganic materials 0.000 claims description 7
- 239000002243 precursor Substances 0.000 claims description 6
- 230000006698 induction Effects 0.000 claims description 5
- 238000000465 moulding Methods 0.000 claims description 5
- 238000012545 processing Methods 0.000 claims description 5
- 238000001354 calcination Methods 0.000 claims description 4
- 238000002525 ultrasonication Methods 0.000 claims description 4
- -1 H plasma treatment Substances 0.000 claims description 2
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 2
- 239000002253 acid Substances 0.000 claims description 2
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 claims 1
- 238000005660 chlorination reaction Methods 0.000 claims 1
- 230000036571 hydration Effects 0.000 claims 1
- 238000006703 hydration reaction Methods 0.000 claims 1
- 150000003839 salts Chemical class 0.000 claims 1
- 238000010792 warming Methods 0.000 claims 1
- 230000035945 sensitivity Effects 0.000 abstract description 11
- QGZKDVFQNNGYKY-UHFFFAOYSA-N Ammonia Chemical compound N QGZKDVFQNNGYKY-UHFFFAOYSA-N 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 8
- 229910021529 ammonia Inorganic materials 0.000 abstract description 5
- 238000010041 electrostatic spinning Methods 0.000 abstract description 5
- 230000008569 process Effects 0.000 abstract description 4
- 230000004044 response Effects 0.000 abstract description 3
- 238000005245 sintering Methods 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 description 8
- 238000001035 drying Methods 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- 229910021627 Tin(IV) chloride Inorganic materials 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
- 239000006193 liquid solution Substances 0.000 description 3
- 239000012299 nitrogen atmosphere Substances 0.000 description 3
- HPGGPRDJHPYFRM-UHFFFAOYSA-J tin(iv) chloride Chemical compound Cl[Sn](Cl)(Cl)Cl HPGGPRDJHPYFRM-UHFFFAOYSA-J 0.000 description 3
- 150000001875 compounds Chemical class 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000003795 desorption Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 229910010272 inorganic material Inorganic materials 0.000 description 2
- 239000011147 inorganic material Substances 0.000 description 2
- 239000006210 lotion Substances 0.000 description 2
- 230000001590 oxidative effect Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 239000013049 sediment Substances 0.000 description 2
- 238000005406 washing Methods 0.000 description 2
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 description 1
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 230000006978 adaptation Effects 0.000 description 1
- BFNBIHQBYMNNAN-UHFFFAOYSA-N ammonium sulfate Chemical compound N.N.OS(O)(=O)=O BFNBIHQBYMNNAN-UHFFFAOYSA-N 0.000 description 1
- 229910052921 ammonium sulfate Inorganic materials 0.000 description 1
- 235000011130 ammonium sulphate Nutrition 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 229910052799 carbon Inorganic materials 0.000 description 1
- 239000000919 ceramic Substances 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 238000002347 injection Methods 0.000 description 1
- 239000007924 injection Substances 0.000 description 1
- 238000007689 inspection Methods 0.000 description 1
- 230000003993 interaction Effects 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 239000011368 organic material Substances 0.000 description 1
- 229920000620 organic polymer Polymers 0.000 description 1
- 230000003647 oxidation Effects 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 238000004157 plasmatron Methods 0.000 description 1
- 230000001376 precipitating effect Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G73/00—Macromolecular compounds obtained by reactions forming a linkage containing nitrogen with or without oxygen or carbon in the main chain of the macromolecule, not provided for in groups C08G12/00 - C08G71/00
- C08G73/02—Polyamines
- C08G73/026—Wholly aromatic polyamines
- C08G73/0266—Polyanilines or derivatives thereof
-
- 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
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/02—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements ultrasonic or sonic; Corona discharge
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M10/00—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements
- D06M10/02—Physical treatment of fibres, threads, yarns, fabrics, or fibrous goods made from such materials, e.g. ultrasonic, corona discharge, irradiation, electric currents, or magnetic fields; Physical treatment combined with treatment with chemical compounds or elements ultrasonic or sonic; Corona discharge
- D06M10/025—Corona discharge or low temperature plasma
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- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/07—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof
- D06M11/11—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with halogens; with halogen acids or salts thereof; with oxides or oxyacids of halogens or salts thereof with halogen acids or salts thereof
- D06M11/13—Ammonium halides or halides of elements of Groups 1 or 11 of the Periodic System
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- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/32—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond
- D06M11/50—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with oxygen, ozone, ozonides, oxides, hydroxides or percompounds; Salts derived from anions with an amphoteric element-oxygen bond with hydrogen peroxide or peroxides of metals; with persulfuric, permanganic, pernitric, percarbonic acids or their salts
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- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- D06M15/37—Macromolecular compounds obtained otherwise than by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/61—Polyamines polyimines
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/3504—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light for analysing gases, e.g. multi-gas analysis
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01N—INVESTIGATING OR ANALYSING MATERIALS BY DETERMINING THEIR CHEMICAL OR PHYSICAL PROPERTIES
- G01N21/00—Investigating or analysing materials by the use of optical means, i.e. using sub-millimetre waves, infrared, visible or ultraviolet light
- G01N21/17—Systems in which incident light is modified in accordance with the properties of the material investigated
- G01N21/25—Colour; Spectral properties, i.e. comparison of effect of material on the light at two or more different wavelengths or wavelength bands
- G01N21/31—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry
- G01N21/35—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light
- G01N21/359—Investigating relative effect of material at wavelengths characteristic of specific elements or molecules, e.g. atomic absorption spectrometry using infrared light using near infrared light
Abstract
A kind of preparation method of near-infrared enhancing room temperature air sensing material is with Tin tetrachloride pentahydrate, N, dinethylformamide, ethyl alcohol, polyvinylpyrrolidone, ammonium carbonate, four water gold chlorides, aniline, hydrochloric acid, ammonium persulfate are raw material, successively include preparation, H plasma treatment, the load of Au nanoparticle, SnO of stannic oxide porous nanotube2The preparation of/Au/PANI and etc..The present invention can obtain the good porous SnO of crystallinity by electrostatic spinning and high temperature sintering2Nanotube, a large amount of Lacking oxygen will be generated in sample after hydrogen plasma process, gas sensing sensitivity is effectively improved, is at room temperature 17.32 to ammonia 100ppm concentration gases sensing sensitivity, the sensitivity under 40ppm concentration is 10.33, material overall performance is good, the present invention can effectively be anchored Lacking oxygen, can also respond near infrared light, lift gas sensing capabilities, gas response temperature can also be effectively reduced in the present invention simultaneously, realize gas sensing performance at room temperature.
Description
Technical field
The present invention relates to technical field of nano material, and in particular to a kind of system of near-infrared enhancing room temperature air sensing material
Preparation Method.
Background technique
On-site test has caused more and more to pay close attention to the gas that environmental and human health impacts constitute a threat to.Past several
In 10 years, based on the gas sensor of metal-oxide semiconductor (MOS) because of its excellent sensing capabilities, or even in rugged environment
Also extensive research has been obtained.Wherein, stannic oxide (SnO2) it is used as a kind of n-type semiconductor, with its excellent photoelectric properties, excellent
Different thermal stability (fusing point is 1127 DEG C), chemical inertness, low cost, it is nontoxic the advantages that be proved to that there is good gas sensing
Prospect.SnO2The sensor mechanism of gas sensor is the electron-transport based on sensor in different target gas.Work as SnO2Exposure
When in air, electrons are transferred in absorbed oxygen from its conductive strips, thus in SnO2Surface generates a large amount of oxygen (O2-、
O-Or O2-).Meanwhile in SnO2Surface forms the superficial layer that one layer of electronics is exhausted, conductivity is caused to decline.Reducing gas (such as
Ethyl alcohol, hydrogen and methanol) when, object gas will react with these oxygen, and electronics is released back into SnO2Surface causes sensor electric
Conductance increases.In oxidizing gas, more absorbed gas entrapments of electronics further reduced the conductance of sensor
Rate.
However, in practical applications, SnO2The optimum working temperature of sensing material is 400 DEG C or so, property at room temperature
Can be very poor, therefore, actually detected for many gases seems and is not suitable for that there is an urgent need to improve its detection at room temperature
Energy.At present improve room temperature sensing capabilities main path be exactly by inorganic material and high-molecular organic material progress it is compound, as PI,
PVA, PANI etc., these are compound to can effectively improve the sensing capabilities of inorganic material at room temperature, but due to organic polymer
The characteristic of material causes that the test returns time is long so that its difficult desorption for detected gas, affects the whole of material
Body performance.
Lacking oxygen is present in many N-shaped oxide semiconductor materials, and by providing very active surface location
It plays a significant role in its photovoltaic applications.The gas sensing of based oxide semiconductor material is a kind of oxide surface and mesh
Mark the surface interaction process between gas molecule.Hydrogen plasma process can make material surface generate Lacking oxygen.But oxygen
Vacancy is easy to react with Surface Oxygen and water etc., to lose effect, therefore, how to make to fix Lacking oxygen and play a role always is
One of problem urgently to be resolved.
To sum up, the preparation of current room temperature gas sensing material still remains the difficult desorption of detected gas, causes inspection
Survey turnaround time is long, affects the overall performance of material；On the other hand, room temperature air sensing material Lacking oxygen be easy and surface
The reaction such as oxygen and water, to lose the technical problems urgent need to resolve such as effect.
Summary of the invention
The purpose of the present invention is to provide a kind of preparation methods of near-infrared enhancing room temperature air sensing material.
The purpose of the present invention is what is realized by following technical measures:
A kind of preparation method of near-infrared enhancing room temperature air sensing material, which is characterized in that it be with Tin tetrachloride pentahydrate,
N,N-Dimethylformamide (DMF), ethyl alcohol, polyvinylpyrrolidone (PVP), ammonium carbonate, four water gold chlorides, aniline, hydrochloric acid, mistake
Ammonium sulfate is raw material, successively including the preparation of stannic oxide porous nanotube, H plasma treatment, Au nanoparticle it is negative
It carries, SnO2The preparation of/Au/PANI and etc..
Further, the preparation of the stannic oxide porous nanotube is by Tin tetrachloride pentahydrate, N, N- dimethyl formyl
Amine (DMF), ethyl alcohol are placed in conical flask, are stirred to being completely dissolved, and are added polyvinylpyrrolidone (PVP) and are stirred 8 ~ 15h, obtain
To mixed uniformly precursor sol liquid, precursor sol liquid is then subjected to high-pressure electrostatic molding, using syringe pump and No. 8 needles
High-pressure electrostatic is set as 12 ~ 18KV by head, and temperature is set as 50 ~ 70 DEG C, obtains colloidal sol fiber, and colloidal sol fiber is then placed in temperature
It is set as 70 ~ 90 DEG C of baking oven, dries 2 ~ 4h, takes out, then colloidal sol fiber is put into Muffle furnace, with the heating of 4 DEG C/min rate
2 ~ 3 h are roasted to 500 ~ 650 DEG C to get stannic oxide porous nanotube is arrived.
Further, above-mentioned Tin tetrachloride pentahydrate, n,N-Dimethylformamide (DMF), ethyl alcohol, polyvinylpyrrolidone
(PVP) mass ratio is 0.33 ~ 0.37:2.0 ~ 2.4:2.0 ~ 2.4:0.3 ~ 0.5.
Further, above-mentioned H plasma treatment is that stannic oxide porous nanotube obtained above is placed in hydrogen plasmatron
In formula induction furnace, hydrogen flow rate is set as 10 ~ 50ml/min, hydrogen purity 99.99%, and power setting is the condition of 80 ~ 150W
Lower carry out plasma treatment, processing time arrive the stannic oxide porous nanotube of oxygen-containing vacancy for 10 ~ 30min.
Further, the load of above-mentioned Au nanoparticle is stannic oxide to suspend in deionized water, the carbon of the 1M of addition
Acid ammonium solution stirring, is then added dropwise the four water aqueous solution of chloraurate of 0.4M, continues 0.5 ~ 2h of stirring, be washed with deionized
It is dry after 3 ~ 5 times, it is 60 ~ 80 DEG C of drying temperature, dry 4 ~ 6h, dry to terminate to be placed in 2 ~ 4h of calcining at 200 ~ 350 DEG C of temperature, then
It is passed through the H that volume ratio is 5:952And N2Mixed gas, can be obtained Au load tin oxide；Wherein, the stannic oxide with
The mass volume ratio of deionized water is 0.5 ~ 1:30 ~ 50, unit g/ml；The deionized water, sal volatile, four water gold chlorides
The volume ratio of aqueous solution is 30 ~ 50:25 ~ 50:20 ~ 30.
Further, above-mentioned SnO2The preparation of/Au/PANI is that 1M HCl is added in the Au-SnO2 sample of aniline sum together is molten
In liquid, ultrasonication 30 ~ 40 minutes, formed solution (1)；Meanwhile stirring ammonium persulfate and mixed in hydrochloric acid 30 minutes, and
It is pre-chilled, is formed solution (2) in ice bath；Then solution (2) is poured into solution (1), the material needed；Wherein, the Au
The tin oxide of load and the mass ratio of phenol solution are 1:0.1 ~ 0.4, the aniline solution, hydrochloric acid solution volume ratio be 0.1 ~
0.4:10~30；The concentration of the hydrochloric acid solution of ammonium persulfate is 13mmol/L ~ 20mmol/L, the solution in the solution (2)
It (1) is 1 ~ 3:10 ~ 15 with the volume ratio of solution (2).
The beneficial effects of the present invention are:
A kind of near-infrared of the present invention enhances room temperature air sensing material, can obtain crystallinity by electrostatic spinning and high temperature sintering
Good porous SnO2Nanotube will generate a large amount of Lacking oxygen in the sample after hydrogen plasma process, and effectively improve gas
Body sensing sensitivity is at room temperature 17.32 to ammonia 100ppm concentration gases sensing sensitivity, sensitive under 40ppm concentration
Degree is 10.33, and material overall performance is good, and the present invention can effectively be anchored Lacking oxygen, so as not to by the oxidizing gas of air
Oxidation, can also respond near infrared light, lift gas sensing capabilities, while gas response temperature can also be effectively reduced in the present invention
Degree, realizes gas sensing performance at room temperature.
Detailed description of the invention
Fig. 1 is the XRD diagram of original SnO2 nanotube prepared by embodiment 1 and SnO2/Au/PANI sample.
Fig. 2 is the SEM figure (high power) of SnO2/Au/PANI prepared by embodiment 1.
Fig. 3 is the SEM figure (low power) of SnO2/Au/PANI prepared by embodiment 1.
Fig. 4 is the TEM figure (low power × 50000) of SnO2/Au/PANI prepared by embodiment 1.
Fig. 5 is the TEM figure (high power × 500000) of SnO2/Au/PANI prepared by embodiment 1.
Fig. 6 is the XPS figure (O 1s) of SnO2/Au/PANI prepared by embodiment 1.
Fig. 7 is SnO2 prepared by embodiment 1 and SnO2/Au/PANI air-sensitive performance figure at room temperature.
Fig. 8 is selective performance map of the SnO2/Au/PANI to gas with various of the preparation of embodiment 1.
Specific embodiment
The present invention is specifically described below by embodiment, it is necessary to which indicated herein is that following embodiment is only used
In invention is further explained, it should not be understood as limiting the scope of the invention, person skilled in art can
To make some nonessential modifications and adaptations to the present invention according to aforementioned present invention content.
Embodiment 1
A kind of preparation of the tin oxide porous nanotube of oxygen-containing vacancy carries out as follows:
(1) stannic chloride pentahydrate 0.35g, n,N-Dimethylformamide 2.2g, ethyl alcohol 2.2g are weighed, stirring and dissolving in conical flask are added,
It takes 0.4gPVP to be added thereto again, stirs 12h, configured presoma.
(2) it takes precursor liquid to be placed in high-voltage electrostatic spinning molding equipment, is synthesized using high-pressure electrostatic forming technique, it is preceding
It drives liquid solution and is packed into syringe pump, high-pressure electrostatic is set as 16KV by syringe needle 0.8mm, and temperature is set as 60 DEG C, obtains colloidal sol fiber；It will
The fiber being collected into is placed in the baking oven that temperature is set as 80 DEG C, dries 3h；Fiber is finally put into Muffle furnace, with 4 DEG C/min rate
Heating, roasts 3h at 600 DEG C, obtains stannic oxide porous nanotube.
(3) stannic oxide porous nanotube is placed in hydrogen plasma tubular type induction furnace, hydrogen flow rate is set as 30ml/
Min, hydrogen purity 99.99%, power setting carry out plasma treatment under conditions of being 120W, and processing time setting is
20min。
(4) 0.8g stannic oxide is suspended in 40ml deionized water (18.2 M Ω), after stirring 15 minutes, 30ml is added
Then the four water aqueous solution of chloraurate 25ml of 0.4M are added dropwise in 1M sal volatile, stir 1h, distinguish centrifuge washing with water
Sediment 3 times, be put into 70 DEG C of dry 5h in drying box, then 5% H2250 DEG C are calcined under 95% nitrogen atmosphere protection,
3h is kept the temperature, Au-SnO2 sample is obtained.
(5) the Au-SnO2 sample of 0.03g aniline and 0.1g are added together in the 1M HCl solution of 2mL, ultrasonication
It 35 minutes, is formed solution (1).Meanwhile the hydrochloric acid solution of 0.2 mmol ammonium persulfate and 12ml being stirred 30 minutes, and in ice bath
Middle pre-cooling forms solution (2) and then pours into solution (2) in solution (1), the material needed.
The air-sensitive performance of material made from embodiment 1 is tested:
The gas sensing performance of sample is surveyed using intelligent gas sensor analysis system (CGS-8, Beijing Ai Lite)
Examination.The material of preparation is mixed with ethyl alcohol, forms uniform lotion.Lotion is coated on industrial ceramics pipe electrode with hairbrush,
It is prepared into gas sensor.Then, prepared sensor spontaneously dries a few hours in air to be tested, and uses
980 laser carry out second test as auxiliary irradiation on device.Gas sensitivity is defined as Ra/Rg, wherein Ra and Rg difference
Resistance when being exposed to air and ethyl alcohol for sensor.Sensor resistance rises to surely after response time is appointed as injection alcohol vapour
The time of definite value 90%.After turnaround time is defined as alcohol vapour removal, drop to the time of final resistance value 10%.It is right at room temperature
The test of different target gas concentration is tested, the test of further progress gas-selectively.At room temperature (20-30 degrees Celsius)
The sensitivity of lower test ammonia, sensitivity 10.33 under 40ppm concentration, sensitivity is 17.32. under 100ppm concentration
Embodiment 2
A kind of preparation of the tin oxide porous nanotube of oxygen-containing vacancy carries out as follows:
(1) stannic chloride pentahydrate 0.33g, n,N-Dimethylformamide 2.0g, ethyl alcohol 2.0g are weighed, stirring and dissolving in conical flask are added,
It takes 0.3gPVP to be added thereto again, stirs 8h, configured presoma.
(2) it takes precursor liquid to be placed in high-voltage electrostatic spinning molding equipment, is synthesized using high-pressure electrostatic forming technique, it is preceding
It drives liquid solution and is packed into syringe pump, high-pressure electrostatic is set as 12KV by syringe needle 0.8mm, and temperature is set as 50 DEG C, obtains colloidal sol fiber；It will
The fiber being collected into is placed in the baking oven that temperature is set as 70 DEG C, dries 4h；Fiber is finally put into Muffle furnace, with 4 DEG C/min rate
Heating, roasts 2h at 650 DEG C, obtains stannic oxide porous nanotube.
(3) stannic oxide porous nanotube is placed in hydrogen plasma tubular type induction furnace, hydrogen flow rate is set as 10ml/
Min, hydrogen purity 99.99%, power setting carry out plasma treatment under conditions of being 150W, and processing time setting is
30min。
(4) 0.5g stannic oxide is suspended in 30ml deionized water (18.2 M Ω), after stirring 15 minutes, 25ml is added
Then the four water aqueous solution of chloraurate 20ml of 0.4M are added dropwise in 1M sal volatile, stir 0.5h, take leave of the heart with moisture and wash
Wash sediment 3 times, be put into 60 DEG C of dry 4h in drying box, then 5% H2With calcining 200 under 95% nitrogen atmosphere protection
DEG C, 4h is kept the temperature, Au-SnO2 sample is obtained.
(5) the Au-SnO2 sample of 0.01g aniline and 0.1g are added together in the 1M HCl solution of 1mL, ultrasonication
It 30 minutes, is formed solution (1).Meanwhile the hydrochloric acid solution of 0.2 mmol ammonium persulfate and 10ml being stirred 30 minutes, and in ice bath
Middle pre-cooling is formed solution (2).Then, solution (2) is poured into solution (1), the material needed.
By the air-sensitive performance test for the material that experimental method made from embodiment 1 carries out, test result shows this product in room
It is high to ammonia detection sensitivity under the conditions of temperature.
Embodiment 3
A kind of preparation of the tin oxide porous nanotube of oxygen-containing vacancy carries out as follows:
(1) stannic chloride pentahydrate 0.37g, n,N-Dimethylformamide 2.4g, ethyl alcohol 2.4g are weighed, stirring and dissolving in conical flask are added,
It takes 0.5gPVP to be added thereto again, stirs 15h, configured presoma.
(2) it takes precursor liquid to be placed in high-voltage electrostatic spinning molding equipment, is synthesized using high-pressure electrostatic forming technique, it is preceding
It drives liquid solution and is packed into syringe pump, high-pressure electrostatic is set as 18KV by syringe needle 0.8mm, and temperature is set as 70 DEG C, obtains colloidal sol fiber；It will
The fiber being collected into is placed in the baking oven that temperature is set as 90 DEG C, dries 4h；Fiber is finally put into Muffle furnace, with 4 DEG C/min rate
Heating, roasts 3h at 650 DEG C, obtains stannic oxide porous nanotube.
(3) stannic oxide porous nanotube is placed in hydrogen plasma tubular type induction furnace, hydrogen flow rate is set as 50ml/
Min, hydrogen purity 99.99%, power setting carry out plasma treatment under conditions of being 150W, and processing time setting is
10min。
(4) 1g stannic oxide is suspended in 50ml deionized water (18.2 M Ω), after stirring 15 minutes, 50ml 1M is added
Then the four water aqueous solution of chloraurate 30ml of 0.4M are added dropwise in sal volatile, stir 2h, with water difference centrifuge washing precipitating
Object 3 times, be put into 80 DEG C of dry 6h in drying box, then 5% H2Lower 350 DEG C of the calcining of nitrogen atmosphere protection with 95%, keeps the temperature
4h obtains Au-SnO2 sample.
(5) the Au-SnO2 sample of 0.04g aniline and 0.1g are added together in the 1M HCl solution of 3 mL, at ultrasonic wave
Reason 40 minutes is formed solution (1).Meanwhile the hydrochloric acid solution of 0.2 mmol ammonium persulfate and 15ml being stirred 30 minutes, and in ice
It is pre-chilled, is formed solution (2) in bath.Then, solution (2) is poured into solution (1), the material needed.
By the air-sensitive performance test for the material that experimental method made from embodiment 1 carries out, test result shows this product in room
It is high to ammonia detection sensitivity under the conditions of temperature.
Claims (6)
1. a kind of preparation method of near-infrared enhancing room temperature air sensing material, which is characterized in that it is with five four chlorinations of hydration
Tin, n,N-Dimethylformamide (DMF), ethyl alcohol, polyvinylpyrrolidone (PVP), ammonium carbonate, four water gold chlorides, aniline, salt
Acid, ammonium persulfate are raw material, successively the preparation including stannic oxide porous nanotube, H plasma treatment, Au nanoparticle
Load, SnO2The preparation of/Au/PANI and etc..
2. a kind of preparation method of near-infrared enhancing room temperature air sensing material as described in claim 1, which is characterized in that institute
The preparation for stating stannic oxide porous nanotube is that Tin tetrachloride pentahydrate, n,N-Dimethylformamide (DMF), ethyl alcohol are placed in cone
It in shape bottle, stirs to being completely dissolved, adds polyvinylpyrrolidone (PVP) and stir 8 ~ 15h, before the colloidal sol being uniformly mixed
Liquid is driven, precursor sol liquid is then subjected to high-pressure electrostatic molding, using syringe pump and No. 8 syringe needles, high-pressure electrostatic is set as 12 ~
18KV, temperature are set as 50 ~ 70 DEG C, obtain colloidal sol fiber, and colloidal sol fiber is then placed in the baking oven that temperature is set as 70 ~ 90 DEG C, dry
Dry 2 ~ 4h, takes out, then colloidal sol fiber is put into Muffle furnace, is warming up at 500 ~ 650 DEG C with 4 DEG C/min rate and roasts 2 ~ 3
H to get arrive stannic oxide porous nanotube.
3. a kind of preparation method of near-infrared enhancing room temperature air sensing material as claimed in claim 2, which is characterized in that on
State Tin tetrachloride pentahydrate, n,N-Dimethylformamide (DMF), ethyl alcohol, polyvinylpyrrolidone (PVP) mass ratio be 0.33
~0.37:2.0~2.4:2.0~2.4:0.3~0.5。
4. a kind of preparation method of near-infrared enhancing room temperature air sensing material as claimed in claim 3, which is characterized in that on
Stating H plasma treatment is placed in stannic oxide porous nanotube obtained above in hydrogen plasma tubular type induction furnace, hydrogen stream
Speed is set as 10 ~ 50ml/min, hydrogen purity 99.99%, and power setting carries out plasma treatment under conditions of being 80 ~ 150W,
The processing time arrives the stannic oxide porous nanotube of oxygen-containing vacancy for 10 ~ 30min.
5. a kind of preparation method of near-infrared enhancing room temperature air sensing material as claimed in claim 4, which is characterized in that on
The load for stating Au nanoparticle is stannic oxide to suspend in deionized water, and the sal volatile of the 1M of addition stirs, then
The four water aqueous solution of chloraurate of 0.4M are added dropwise, continue 0.5 ~ 2h of stirring, it is dry after being washed with deionized 3 ~ 5 times, it is dry
60 ~ 80 DEG C of temperature, dry 4 ~ 6h, dry to terminate to be placed in 2 ~ 4h of calcining at 200 ~ 350 DEG C of temperature, then passing to volume ratio is 5:95
H2And N2Mixed gas, can be obtained Au load tin oxide；Wherein, the mass body of the stannic oxide and deionized water
Product is than being 0.5 ~ 1:30 ~ 50, unit g/ml；The deionized water, sal volatile, four water aqueous solution of chloraurate volume ratio be
30~50:25~50:20~30。
6. a kind of preparation method of near-infrared enhancing room temperature air sensing material as claimed in claim 5, which is characterized in that on
State SnO2The preparation of/Au/PANI is that the Au-SnO2 sample of aniline sum is added together in 1M HCl solution, ultrasonication 30 ~
It 40 minutes, is formed solution (1)；Meanwhile stirring ammonium persulfate and mixed in hydrochloric acid 30 minutes, and be pre-chilled in ice bath, it is formed molten
Liquid (2)；Then solution (2) is poured into solution (1), the material needed；Wherein, the tin oxide and phenol of the Au load
The mass ratio of solution is 1:0.1 ~ 0.4, and the aniline solution, hydrochloric acid solution volume ratio are 0.1 ~ 0.4:10 ~ 30；The solution
(2) concentration of the hydrochloric acid solution of ammonium persulfate is 13mmol/L ~ 20mmol/L, the volume ratio of the solution (1) and solution (2) in
For 1 ~ 3:10 ~ 15.
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