CN101915787A - Inorganic nanoporous titanium dioxide fibrous membrane gas sensor and manufacturing method thereof - Google Patents
Inorganic nanoporous titanium dioxide fibrous membrane gas sensor and manufacturing method thereof Download PDFInfo
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- CN101915787A CN101915787A CN 201010231182 CN201010231182A CN101915787A CN 101915787 A CN101915787 A CN 101915787A CN 201010231182 CN201010231182 CN 201010231182 CN 201010231182 A CN201010231182 A CN 201010231182A CN 101915787 A CN101915787 A CN 101915787A
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Abstract
The invention provides an inorganic nanoporous titanium dioxide fibrous membrane gas sensor and a manufacturing method thereof. The sensor comprises a ceramic matrix, an interdigital platinum electrode, a lead and a circuit, wherein the interdigital platinum electrode, the lead and the circuit are formed on the surface of the ceramic matrix. The sensor is characterized in that an inorganic nanoporous titanium dioxide fibrous membrane is deposited on the interdigital platinum electrode. The preparation method of the sensor is characterized by comprising the following concrete steps of: dissolving a hydrophobic polymer into a solvent, adding titanium dioxide nanoparticles or soluble titanium salt, and stirring to form a uniform solution; carrying out electrostatic spinning, and directly depositing spun fibers onto the interdigital platinum electrode; immerging the interdigital platinum electrode into the solvent, immediately taking out and putting into a vacuum drying box for drying; and carrying out heat pressing, subsequently calcining, and removing organic components in the hybrid fibers to obtain a high-sensitivity gas sensor coated with the inorganic nanoporous titanium dioxide fibrous membrane. The invention has the advantages of higher stability and longer service life.
Description
Technical field
The present invention relates to a kind of inorganic nano poriferous titanium dioxide fiber film gas transducer and preparation method thereof, belong to the new textile material applied technical field.
Background technology
Along with developing rapidly of industry, the various harmful gases that discharge in the industrial processes (as ammonia, sulfuretted hydrogen, nitrogen monoxide, nitrogen dioxide etc.), endangering people's life health day by day, therefore detect the toxic gas that discharges in the industrial processes how fast, efficiently and accurately, it is an important research work, human beings'health there is significance, the optimum development of social environment is had very positive meaning.
The character of the gas sensor that the use metal-oxide semiconductor is made is subjected to the influence of gas flow and surface reaction.At present some researchers use oxide nano thread to attempt to address these problems, for example tin ash sensor, zinc paste sensor etc., but there is the problem of the less stable of oxidation film on the sensor.
Summary of the invention
The purpose of this invention is to provide a kind of oxidation film good stability and have gas sensor of higher detection sensitivity and preparation method thereof.
In order to achieve the above object, the invention provides a kind of inorganic nano poriferous titanium dioxide fiber film gas transducer, form by interdigital platinum electrode, lead-in wire and circuit that ceramic matrix, ceramic matrix surface form, during test interdigital platinum electrode is connected into circuit by lead-in wire, it is characterized in that, deposit inorganic nano poriferous titanium dioxide fiber film on the described interdigital platinum electrode.
The present invention also provides the preparation method of above-mentioned inorganic nano poriferous titanium dioxide fiber film gas transducer, it is characterized in that, the concrete steps that deposit inorganic nano poriferous titanium dioxide fiber film on interdigital platinum electrode are:
The first step is dissolved in hydrophobic polymer in the solvent, adds titania nanoparticles or solubility titanium salt, stirs to form uniform solution;
In second step, the solution that the first step is obtained carries out electrostatic spinning, the fiber that is spun into is directly deposited on the interdigital platinum electrode form tunica fibrosa;
In the 3rd step, in the interdigital platinum electrode immersion solvent with the second step gained, it is dry to take out and put into vacuum drying chamber immediately, and described solvent is identical with solvent for use in the first step;
The 4th step, the interdigital platinum electrode of the 3rd step gained under 90-120 ℃, 1-10MPa pressure, hot pressing 20-60 minute, is carried out 400-500 ℃ of calcining subsequently, remove the organic principle in the hybridized fiber, thereby obtain being coated with the highly sensitive gas sensor of inorganic nano poriferous titanium dioxide fiber film.
Hydrophobic polymer in the described first step is ethyl cellulose, acetyl cellulose, polyacrylonitrile, polystyrene, zein, polymethylmethacrylate, polycarbonate, polyvinyl acetate (PVA), PLA, Polyvinylchloride, polyacrylonitrile, polycaprolactone, poly butylene succinate, poly-succinic acid-butanediol-be total to-mutual-phenenyl two acid bromide two alcohol ester, poly-hydroxyl valerate or polyamide.
Solvent in the described first step is N, dinethylformamide, N,N-dimethylacetamide, tetrahydrofuran, methylene chloride, ethylene dichloride, methenyl choloride, monochloro methane, acetone, formic acid, benzene, toluene, cyclohexane, the potpourri of one or more in hexafluoroisopropanol and the trifluoroethanol.
Solubility titanium salt in the described first step is a tetraisopropoxy titanium.
Inorganic nano poriferous titanium dioxide fiber film, be to pile up the nonwoven fabrics that forms at random by the inorganic nano poriferous titanium dioxide fiber of diameter in the 100-500 nanometer range, fiber itself has the duct and the micro fiber of 1-100 nanometer and forms, and makes fiber have the specific surface area than the high several magnitude of common solid fibers.In addition, titania is with a kind of N-type semiconductor metal oxide, have the continuous band structure different with metal, generally constitute by low energy valence band of filling up electronics (valence band hole concentration) and empty high energy conduction band (conduction band electron concentration), have the forbidden band between valence band and the conduction band, its conduction is by the migration in " hole " electronic conduction to be achieved.When the electrode that deposits inorganic nano poriferous titanium dioxide fiber film adsorbs some oxidizing gas, semiconductor carriers will be reduced, and resistance value is increased; When reducibility gas was adsorbed onto on the electrode, then charge carrier increased, and the semi-conductor electricity resistance is descended.If gas concentration changes, its resistance will change thereupon.According to this characteristic, can learn the kind and the concentration of adsorbed gas from the variation of resistance.The semiconductor air-sensitive time (response time) generally is no more than 1min.Inorganic nano poriferous titanium dioxide fiber film gas transducer utilizes the absorption of gas and the resistivity of semiconductor this mechanism that changes itself is detected.
Advantage of the present invention is to have advantages of higher stability and serviceable life.
Embodiment
Specify the present invention below in conjunction with embodiment.
Embodiment 1
A kind of inorganic nano poriferous titanium dioxide fiber film gas transducer, form by interdigital platinum electrode, lead-in wire and circuit that ceramic matrix, ceramic matrix surface form, during test interdigital platinum electrode is connected into circuit by lead-in wire, it is characterized in that, deposit inorganic nano poriferous titanium dioxide fiber film on the described interdigital platinum electrode.
The first step is dissolved in N with acetyl cellulose (Mn 40000), in dinethylformamide/acetone (mass ratio 2/1) solution, is mixed with concentration and is 10% solution (calculating with mass percent); Then 1 gram tetraisopropoxy titanium and 0.5 gram acetate are added in the 5 cellulose acetate ester solutions that prepare in advance of gram, stir and form uniform solution.
Second step, the solution that the first step is prepared at room temperature carries out electrostatic spinning, the spinning condition that is adopted is that voltage is 17 kilovolts, the fiber receiving range is 16 centimetres, injection of solution speed is 1.5 milliliters/hour, and the prepared fiber of electrostatic spinning directly deposits on the preprepared interdigital platinum electrode.
The 3rd step prepared the interdigital platinum electrode that has the titaniferous hybridized fiber with second step and is immersed in N, and in about three seconds in dinethylformamide/acetone (mass ratio 2/1) solution, it is dry to take out and put into vacuum drying chamber immediately.Temperature is about 80 degrees centigrade in the vacuum drying chamber, 5 hours drying times.
In the 4th step, the organic/inorganic titania hybrid fiber that the 3rd step was prepared is heated to 120 ℃, and keeps 20 minutes, applies the pressure of 8MPa then; Then the tunica fibrosa for preparing was calcined one hour under 400 ℃ in muffle furnace, remove the organic principle in the hybridized fiber, thereby obtain being coated with the highly sensitive gas sensor of inorganic nano poriferous titanium dioxide fiber film, its using method is identical with common metal-oxide semiconductor gas sensor, the inorganic nano poriferous titanium dioxide fiber sensor of preparation reaches 100ppb to the detection limit of nitrogen dioxide, and the response time is 5 seconds.
Embodiment 2
A kind of inorganic nano poriferous titanium dioxide fiber film gas transducer, form by interdigital platinum electrode, lead-in wire and circuit that ceramic matrix, ceramic matrix surface form, during test interdigital platinum electrode is connected into circuit by lead-in wire, it is characterized in that, deposit inorganic nano poriferous titanium dioxide fiber film on the described interdigital platinum electrode.
The first step is dissolved in ethyl cellulose (Mn 97000) in dimethyl formamide/tetrahydrofuran (mass ratio 3/1) solution, is mixed with concentration and is 9% solution (calculating with mass percent); Add 2 gram titania nanoparticles (particle diameter is the 10-100 nanometer, and Aladdin net commercial form is bought) to 20 then and restrain in the ethyl cellulose solution for preparing in advance, stir and form uniform solution.
Second step, the solution that the first step is prepared at room temperature carries out electrostatic spinning, the spinning condition that is adopted is that voltage is 18 kilovolts, the fiber receiving range is 15 centimetres, injection of solution speed is 2 milliliters/hour, and the prepared fiber of electrostatic spinning directly deposits on the preprepared interdigital platinum electrode.
The 3rd step prepared the interdigital platinum electrode that has the titaniferous hybridized fiber with second step and is immersed in about three seconds in dimethyl formamide/tetrahydrofuran (mass ratio 3/1) solution, and it is dry to take out and put into vacuum drying chamber immediately.Temperature is about 80 degrees centigrade in the vacuum drying chamber, 5 hours drying times.
In the 4th step, the organic/inorganic titania hybrid fiber that the 3rd step was prepared is heated to 90 ℃, and keeps 60 minutes, applies the pressure of 1MPa then; Then the tunica fibrosa for preparing was calcined one hour under 500 ℃ in muffle furnace, remove the organic principle in the hybridized fiber, thereby obtain being coated with the highly sensitive gas sensor of inorganic nano poriferous titanium dioxide fiber film, its using method is identical with common metal-oxide semiconductor gas sensor, the inorganic nano poriferous titanium dioxide fiber sensor of preparation reaches 200ppb to the detection limit of nitrogen dioxide, and the response time is 10 seconds.
Embodiment 3
A kind of inorganic nano poriferous titanium dioxide fiber film gas transducer, form by interdigital platinum electrode, lead-in wire and circuit that ceramic matrix, ceramic matrix surface form, during test interdigital platinum electrode is connected into circuit by lead-in wire, it is characterized in that, deposit inorganic nano poriferous titanium dioxide fiber film on the described interdigital platinum electrode.
The first step is dissolved in poly butylene succinate (Mn 20000) in methylene chloride/methenyl choloride (mass ratio 3/1) solution, is mixed with concentration and is 12% solution (calculating with mass percent); Add 2 gram titania nanoparticles (particle diameter is the 10-100 nanometer, and Aladdin net commercial form is bought) to 20 then and restrain in the ethyl cellulose solution for preparing in advance, stir and form uniform solution.
Second step, the solution that the first step is prepared at room temperature carries out electrostatic spinning, the spinning condition that is adopted is that voltage is 20 kilovolts, the fiber receiving range is 15 centimetres, injection of solution speed is 2 milliliters/hour, and the prepared fiber of electrostatic spinning directly deposits on the preprepared interdigital platinum electrode.
The 3rd step prepared the interdigital platinum electrode that has the titaniferous hybridized fiber with second step and is immersed in about three seconds in methylene chloride/methenyl choloride (mass ratio 3/1) solution, and it is dry to take out and put into vacuum drying chamber immediately.Temperature is about 80 degrees centigrade in the vacuum drying chamber, 5 hours drying times.
In the 4th step, the organic/inorganic titania hybrid fiber that the 3rd step was prepared is heated to 120 ℃, and keeps 30 minutes, applies the pressure of 9MPa then; Then the tunica fibrosa for preparing was calcined one hour under 500 ℃ in muffle furnace, remove the organic principle in the hybridized fiber, thereby obtain being coated with the highly sensitive gas sensor of inorganic nano poriferous titanium dioxide fiber film, its using method is identical with common metal-oxide semiconductor gas sensor, the inorganic nano poriferous titanium dioxide fiber sensor of preparation reaches 500ppb to the detection limit of nitrogen dioxide, and the response time is 15 seconds.
Embodiment 4
A kind of inorganic nano poriferous titanium dioxide fiber film gas transducer, form by interdigital platinum electrode, lead-in wire and circuit that ceramic matrix, ceramic matrix surface form, during test interdigital platinum electrode is connected into circuit by lead-in wire, it is characterized in that, deposit inorganic nano poriferous titanium dioxide fiber film on the described interdigital platinum electrode.
The first step is dissolved in polyvinyl acetate (PVA) (Mn 500000) in the dimethyl formamide solution, is mixed with concentration and is 11.5% solution (calculating with mass percent); Add 2 gram titania nanoparticles (particle diameter is the 10-100 nanometer, and Aladdin net commercial form is bought) to 20 then and restrain in the polyvinyl acetate ester solution for preparing in advance, stir and form uniform solution.
Second step, the solution that the first step is prepared at room temperature carries out electrostatic spinning, the spinning condition that is adopted is that voltage is 20 kilovolts, the fiber receiving range is 15 centimetres, injection of solution speed is 2 milliliters/hour, and the prepared fiber of electrostatic spinning directly deposits on the preprepared interdigital platinum electrode.
The 3rd step prepared the interdigital platinum electrode that has the titaniferous hybridized fiber with second step and is immersed in about three seconds in the dimethyl formamide solution, and it is dry to take out and put into vacuum drying chamber immediately.Temperature is about 80 degrees centigrade in the vacuum drying chamber, 5 hours drying times.
In the 4th step, the organic/inorganic titania hybrid fiber that the 3rd step was prepared is heated to 120 ℃, and keeps 30 minutes, applies the pressure of 9MPa then; Then the tunica fibrosa for preparing was calcined one hour under 500 ℃ in muffle furnace, remove the organic principle in the hybridized fiber, thereby obtain being coated with the highly sensitive gas sensor of inorganic nano poriferous titanium dioxide fiber film, its using method is identical with common metal-oxide semiconductor gas sensor, the inorganic nano poriferous titanium dioxide fiber sensor of preparation reaches 800ppb to the detection limit of nitrogen dioxide, and the response time is 20 seconds.
Embodiment 5
A kind of inorganic nano poriferous titanium dioxide fiber film gas transducer, form by interdigital platinum electrode, lead-in wire and circuit that ceramic matrix, ceramic matrix surface form, during test interdigital platinum electrode is connected into circuit by lead-in wire, it is characterized in that, deposit inorganic nano poriferous titanium dioxide fiber film on the described interdigital platinum electrode.
The first step, polyacrylonitrile (Mn 80000) is dissolved in the dimethyl formamide solution, is mixed with concentration and is 15% solution (calculating with mass percent); Add 2 gram titania nanoparticles (particle diameter is the 10-100 nanometer, and Aladdin net commercial form is bought) to 20 then and restrain in the polyacrylonitrile solution for preparing in advance, stir and form uniform solution.
Second step, the solution that the first step is prepared at room temperature carries out electrostatic spinning, the spinning condition that is adopted is that voltage is 20 kilovolts, the fiber receiving range is 15 centimetres, injection of solution speed is 1 milliliter/hour, and the prepared fiber of electrostatic spinning directly deposits on the preprepared interdigital platinum electrode.
The 3rd step prepared the interdigital platinum electrode that has the titaniferous hybridized fiber with second step and is immersed in about three seconds in the dimethyl formamide solution, and it is dry to take out and put into vacuum drying chamber immediately.Temperature is about 80 degrees centigrade in the vacuum drying chamber, 5 hours drying times.
In the 4th step, the organic/inorganic titania hybrid fiber that the 3rd step was prepared is heated to 120 ℃, and keeps 30 minutes, applies the pressure of 9MPa then; Then the tunica fibrosa for preparing was calcined one hour under 500 ℃ in muffle furnace, remove the organic principle in the hybridized fiber, thereby obtain being coated with the highly sensitive gas sensor of inorganic nano poriferous titanium dioxide fiber film, its using method is identical with common metal-oxide semiconductor gas sensor, the inorganic nano poriferous titanium dioxide fiber sensor of preparation reaches 1000ppb to the detection limit of nitrogen dioxide, and the response time is 25 seconds.
Claims (5)
1. inorganic nano poriferous titanium dioxide fiber film gas transducer, form by interdigital platinum electrode, lead-in wire and circuit that ceramic matrix, ceramic matrix surface form, during test interdigital platinum electrode is connected into circuit by lead-in wire, it is characterized in that, deposit inorganic nano poriferous titanium dioxide fiber film on the described interdigital platinum electrode.
2. the preparation method of the described inorganic nano poriferous titanium dioxide fiber of claim 1 film gas transducer is characterized in that, the concrete steps that deposit inorganic nano poriferous titanium dioxide fiber film on interdigital platinum electrode are:
The first step is dissolved in hydrophobic polymer in the solvent, adds titania nanoparticles or solubility titanium salt, stirs to form uniform solution;
In second step, the solution that the first step is obtained carries out electrostatic spinning, the fiber that is spun into is directly deposited on the interdigital platinum electrode form tunica fibrosa;
In the 3rd step, in the interdigital platinum electrode immersion solvent with the second step gained, it is dry to take out and put into vacuum drying chamber immediately, and described solvent is identical with solvent for use in the first step;
The 4th step, the interdigital platinum electrode of the 3rd step gained under 90-120 ℃, 1-10MPa pressure, hot pressing 20-60 minute, is carried out 400-500 ℃ of calcining subsequently, remove the organic principle in the hybridized fiber, thereby obtain being coated with the highly sensitive gas sensor of inorganic nano poriferous titanium dioxide fiber film.
3. the preparation method of inorganic nano poriferous titanium dioxide fiber film gas transducer as claimed in claim 2, it is characterized in that the hydrophobic polymer in the described first step is ethyl cellulose, acetyl cellulose, polyacrylonitrile, polystyrene, zein, polymethylmethacrylate, polycarbonate, polyvinyl acetate (PVA), PLA, Polyvinylchloride, polyacrylonitrile, polycaprolactone, poly butylene succinate, poly-succinic acid-butanediol-be total to-mutual-phenenyl two acid bromide two alcohol ester, poly-hydroxyl valerate, polyethylene terephthalate or polyamide.
4. the preparation method of inorganic nano poriferous titanium dioxide fiber film gas transducer as claimed in claim 2 is characterized in that, the solvent in the described first step is N, dinethylformamide, N,N-dimethylacetamide, tetrahydrofuran, methylene chloride, ethylene dichloride, methenyl choloride, monochloro methane, acetone, formic acid, benzene, toluene, cyclohexane, the potpourri of one or more in hexafluoroisopropanol and the trifluoroethanol.
5. the preparation method of inorganic nano poriferous titanium dioxide fiber film gas transducer as claimed in claim 2 is characterized in that, the solubility titanium salt in the described first step is a tetraisopropoxy titanium.
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Cited By (7)
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| CN102441375A (en) * | 2011-11-03 | 2012-05-09 | 华东理工大学 | Homogeneous mesoporous rhodium oxide / alumina composite catalysis material, preparation method and application thereof |
| CN102759525A (en) * | 2012-06-11 | 2012-10-31 | 江苏大学 | Method for making gas sensor based on natural color-sensitive material and porous TiO2 film |
| CN102953059A (en) * | 2012-08-28 | 2013-03-06 | 河北工业大学 | Manufacture method of acetone gas sensitive sensor based on titanium dioxide doped by zinc oxide |
| CN105675663A (en) * | 2016-01-19 | 2016-06-15 | 武汉工程大学 | Gas sensor on basis of polyaniline/titanium dioxide composite nano-fibers and method for manufacturing gas sensor |
| CN109870488A (en) * | 2017-12-04 | 2019-06-11 | 中国科学院大连化学物理研究所 | A kind of preparation method of alcohol gas sensor |
| CN112816451A (en) * | 2021-01-08 | 2021-05-18 | 山东省科学院新材料研究所 | AIE type high-stability flexible fiber, gas sensor, preparation method and application thereof |
| CN114835209A (en) * | 2022-04-26 | 2022-08-02 | 北京交通大学 | Electrochemical membrane contact ozone catalytic device based on titanium fiber electrode and water treatment method |
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| CN102441375A (en) * | 2011-11-03 | 2012-05-09 | 华东理工大学 | Homogeneous mesoporous rhodium oxide / alumina composite catalysis material, preparation method and application thereof |
| CN102441375B (en) * | 2011-11-03 | 2013-04-10 | 华东理工大学 | Homogeneous mesoporous rhodium oxide/alumina composite catalysis material, preparation method and application thereof |
| CN102759525A (en) * | 2012-06-11 | 2012-10-31 | 江苏大学 | Method for making gas sensor based on natural color-sensitive material and porous TiO2 film |
| CN102759525B (en) * | 2012-06-11 | 2014-08-20 | 江苏大学 | Method for making gas sensor based on natural color-sensitive material and porous TiO2 film |
| CN102953059A (en) * | 2012-08-28 | 2013-03-06 | 河北工业大学 | Manufacture method of acetone gas sensitive sensor based on titanium dioxide doped by zinc oxide |
| CN102953059B (en) * | 2012-08-28 | 2015-03-11 | 河北工业大学 | Manufacture method of acetone gas sensitive sensor based on titanium dioxide doped by zinc oxide |
| CN105675663A (en) * | 2016-01-19 | 2016-06-15 | 武汉工程大学 | Gas sensor on basis of polyaniline/titanium dioxide composite nano-fibers and method for manufacturing gas sensor |
| CN105675663B (en) * | 2016-01-19 | 2019-03-08 | 武汉工程大学 | Gas sensor and preparation method thereof based on polyaniline/titanium dioxide composite nano fiber |
| CN109870488A (en) * | 2017-12-04 | 2019-06-11 | 中国科学院大连化学物理研究所 | A kind of preparation method of alcohol gas sensor |
| CN112816451A (en) * | 2021-01-08 | 2021-05-18 | 山东省科学院新材料研究所 | AIE type high-stability flexible fiber, gas sensor, preparation method and application thereof |
| CN112816451B (en) * | 2021-01-08 | 2023-06-09 | 山东省科学院新材料研究所 | AIE (air-assisted polyethylene) high-stability flexible fiber, gas sensor and preparation methods and application of AIE high-stability flexible fiber and gas sensor |
| CN114835209A (en) * | 2022-04-26 | 2022-08-02 | 北京交通大学 | Electrochemical membrane contact ozone catalytic device based on titanium fiber electrode and water treatment method |
| CN114835209B (en) * | 2022-04-26 | 2024-04-09 | 北京交通大学 | Electrochemical membrane contact ozone catalytic device based on titanium fiber electrode and water treatment method |
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Application publication date: 20101215 |