CN103323359B - A kind of detection method of Low Level Carbon Monoxide gas - Google Patents
A kind of detection method of Low Level Carbon Monoxide gas Download PDFInfo
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- CN103323359B CN103323359B CN201310231419.3A CN201310231419A CN103323359B CN 103323359 B CN103323359 B CN 103323359B CN 201310231419 A CN201310231419 A CN 201310231419A CN 103323359 B CN103323359 B CN 103323359B
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Abstract
The invention belongs to conductive polymer nanometer fiber gas field of sensing technologies, relate to a kind of detection method of Low Level Carbon Monoxide gas, poly-(the 3,4-rthylene dioxythiophene)-polystyrolsulfon acid spinning solution of first preparation; Prepare the responsive quartz crystal oscillator that surface deposits poly-(3,4-rthylene dioxythiophene)-polystyrolsulfon acid nano-fiber film again, be carbon monoxide gas sensor; Carbon monoxide gas sensor is adopted to be assembled into pick-up unit and to detect carbon monoxide gas concentration, first to air chamber purging, the frequency difference of reference quartz crystal oscillator and responsive quartz crystal oscillator and output frequency are stablized with nitrogen, CO gas is injected again in air chamber, resonance frequency changes, when frequency is stablized again, close CO gas, again use nitrogen sweep gas room, make output frequency recover stable, output frequency is gathered by computer over time and preserves; Its method of testing is simple, simple and efficient to handle, and principle is reliable, highly sensitive, and response is fast.
Description
Technical field:
The invention belongs to conductive polymer nanometer fiber gas field of sensing technologies, relate to conductive polymer nanometer fiber prepared by a kind of electrostatic spinning technique as sensitive material, utilize QCM (Quartz Crystal Microbalance) (QCM) principle to detect the processing step of CO gas, particularly a kind of detection method of Low Level Carbon Monoxide gas.
Background technology:
Compared with numerous traditional analytic system, gas sensor becomes the main testing tool of various organic and inorganic gas gradually, gas sensor comprises sensitive material and signal converting transmission system for detecting gas, sensitive material and tested gas react, the electricity obtained, calorifics or optical signalling are become digital signal through conversion, carry out follow-up study again, the selection of sensitive material is most important with the validity of synthesizing gas sensor, reliability and stability.In recent years, because nano material has the advantage that size is little, specific surface area is larger, people are devoted to the sensitive material preparing synthesis of nano structure gradually, and be applied in gas sensor, to improve its gas-sensitive property, the metal oxide of nanostructured and polymkeric substance, have the advantages such as size is controlled, biocompatibility, security, chemical stability, have many potential application in gas sensor.The metal oxide of the nanostructureds such as nano thin-film, nano particle, nanometer rods, nano wire, hollow-core construction, such as ZnO, SnO
2and TiO
2be conventional gas sensitive, its research and preparation method's comparative maturity, ZnO detects carbon monoxide (CO), ammonia (NH
3) and ethanol, SnO
2detect NO
x, NH
3and organic gas, TiO
2detect CO, NH
3all have been reported with formaldehyde etc.In order to improve susceptibility and the stability of Metal Oxide Gas Sensors, the method that many employings conductor is combined with semiconductor, as Au, Ag, Pt, carbon nano-tube etc. are combined with metal oxide, the response time of sensor can be shortened, although very short based on the gas sensor response time of metal oxide, stability is better, but still there are very large restraining factors---and test process needs certain high temperature to ensure test performance, which has limited the application of Metal Oxide Gas Sensors.And the gas sensor that sensitive material is functional polymer exactly solves this problem, at room temperature can carry out gas detect, but its response time and release time are usually long than metal oxide.
In recent years, due to conducting polymer show the advantage such as regulatable electric conductivity, pliability, diversity, stability and biocompatibility that doping-dedoping process is reversible, excellent, vast potential for future development is had in scientific research and industrial circle, conducting polymer also obtains people and more and more pays close attention in sensor, polyaniline, polypyrrole, polythiophene and derivant thereof are more typical conducting polymers, and the research report of its gas-sensitive property aspect is more and more.Except polyaniline, polypyrrole and polythiophene, a kind of conducting polymer comparing now concern is poly-(3,4-ethene dioxythiophene)-polystyrolsulfon acid (PEDOT-PSS), it is water miscible, can be used for organic thin film solar cell, its gas-sensitive property also obtains extensive concern recently.Mostly the gas-sensitive property research of current PEDOT-PSS film and nanostructured is the method adopting testing impedance, as the people such as Choi (Synth.Metals, 160 (2010) 1415-1421) prepare PEDOT-PSS nanofiber with method of electrostatic spinning, test its gas-sensitive property to organic gass such as ethanol, methyl alcohol and acetone; Recently, also have report to point out PEDOT-PSS can be combined with metal oxide (such as at ZnO(J.Alloy.Compd., 515 (2012) 80-85) or TiO
2(Sensor Actuat.B-Chem., 176 (2013) 390-398) nanofiber surface applies one deck PEDOT-PSS) after nano composite structure be used in room temperature under detect liquefied petroleum gas (LPG) and NO
2, and its air-sensitive impedance operator is tested.QCM (Quartz Crystal Microbalance) (Quartz Crystal Microbalance, QCM) ultimate principle is the piezoelectric property that make use of quartz-crystal resonator, the change of quartz crystal oscillator electrode surface quality is converted into the frequency change that quartz crystal oscillator circuit exports electric signal, theoretical research shows, the resonance frequency change of QCM (Quartz Crystal Microbalance) (QCM) is directly proportional to additional quality, QCM is a kind of very sensitive quality testing instrument, and its measuring accuracy can reach nanogram level (10
-9gram), can be used for gas, the constituent analysis of liquid, the measurement of micro-quality and the detection etc. of film thickness.Such as, Chinese patent (201220085010.6) discloses a kind of trace ammonia detection device of polyaniline film coated quartz crystal microbalance (QCM) crystal oscillator.The test of gas sensor generally adopts testing impedance method, and the method needs to make metal electrode on sensitive material, tiny for some, measure few nano material, also needs micro-processing technology processing metal microelectrode, cumbersome.
Summary of the invention:
The object of the invention is to the shortcoming overcoming prior art existence, seek to design the detection method that a kind of Low Level Carbon Monoxide gas is provided, electrostatic spinning technique and QCM (Quartz Crystal Microbalance) (QCM) technology are combined, electrostatic spinning technique is utilized to prepare a small amount of poly-(3, 4-ethene dioxythiophene)-polystyrolsulfon acid (PEDOT-PSS) nanofiber is as sensitive material, utilize the CO gas proving installation independently built to detect Low Level Carbon Monoxide (CO) gas, not be used on sensitive material and make metal electrode, have easy, quick and highly sensitive advantage.
To achieve these goals, concrete technology step of the present invention is:
(1), polyvinylpyrrolidone (PVP) powder is dissolved in absolute ethyl alcohol, by magnetic stirrer, obtains the settled solution that massfraction is 18wt%; To (3 be gathered again, 4-ethene dioxythiophene)-polystyrolsulfon acid (PEDOT-PSS) mixes with settled solution, stir, preparation obtains poly-(3,4-rthylene dioxythiophene)-polystyrolsulfon acid (PEDOT-PSS) spinning solution that massfraction is 10wt%;
(2), at ambient temperature, existing electrostatic spinning technique is utilized to prepare poly-(3, 4-ethene dioxythiophene)-polystyrolsulfon acid (PEDOT-PSS) nanofiber, quartz crystal oscillator in QCM (Quartz Crystal Microbalance) (QCM) is placed on collector aluminium foil, spinning distance and the distance between spinneret and aluminium foil are 10 centimetres, to prepare poly-(3, 4-ethene dioxythiophene)-polystyrolsulfon acid (PEDOT-PSS) spinning solution puts into syringe, apply 20 kilovolts of high-voltage DC power supplies, spinning 50-70 closes high-voltage DC power supply after second, take out surface deposition poly-(3, 4-ethene dioxythiophene) quartz crystal oscillator of-polystyrolsulfon acid (PEDOT-PSS) nano-fiber film, poly-(3 will be deposited, 4-ethene dioxythiophene) quartz crystal oscillator of-polystyrolsulfon acid (PEDOT-PSS) nano-fiber film places heating, drying 1 hour at 60 DEG C of temperature on hot plate, obtained surface deposition has a small amount of poly-(3, 4-ethene dioxythiophene) the responsive quartz crystal oscillator of-polystyrolsulfon acid (PEDOT-PSS) nano-fiber film, be carbon monoxide gas sensor,
(3), carbon monoxide gas sensor is adopted to be assembled into pick-up unit and to detect carbon monoxide gas concentration, first the frequency difference of reference quartz crystal oscillator and responsive quartz crystal oscillator and output frequency is made to be stabilized in 0Hz with nitrogen to air chamber purging, CO gas is injected again in air chamber, on responsive quartz crystal oscillator poly-(3, 4-ethene dioxythiophene)-polystyrolsulfon acid (PEDOT-PSS) nano-fiber film and CO gas interact, produce mass change, resonance frequency changes, when frequency is stablized again, close CO gas, again use nitrogen sweep gas room, output frequency is made to recover stable, output frequency is gathered by computer over time and preserves.
Cleaning Principle of the present invention is: apply certain alternating voltage and responsive quartz crystal oscillator is vibrated under certain frequency, when the sensitive material of responsive quartz crystal oscillator and gas to be measured interact, quality changes, impressed pressure makes it produce alternating electric field, thus changes the resonance frequency of responsive quartz crystal oscillator; During test, driving circuit makes reference quartz crystal oscillator and responsive quartz crystal oscillator vibrate under its resonance frequency, the oscillation frequency of frequency meter to reference quartz crystal oscillator and responsive quartz crystal oscillator is measured and is processed, obtain frequency difference signal and be output frequency, output frequency is outputted on computer, be spaced apart 0.1 second, computer is gathered output frequency by software, process and draw response curve.
The agent structure of the carbon monoxide gas sensor pick-up unit with the assembling of carbon monoxide gas sensor that the present invention relates to comprises admission line, admission line valve, nitrogen, CO gas, air chamber, reference quartz crystal oscillator, responsive quartz crystal oscillator, frequency meter, computer, gas exhaust duct and gas exhaust duct valve; Air chamber is connected with gas exhaust duct with admission line respectively, nitrogen and CO gas are respectively by admission line and air chamber pipeline communication, on admission line, corresponding nitrogen and CO gas place are shaped with admission line valve respectively, gas exhaust duct are shaped with gas exhaust duct valve; Reference quartz crystal oscillator and responsive quartz crystal oscillator is shaped with in air chamber, responsive quartz crystal oscillator surface deposition has poly-(3,4-ethene dioxythiophene)-polystyrolsulfon acid (PEDOT-PSS) nano-fiber film, unloaded reference quartz crystal oscillator is identical with the model/specification of responsive quartz crystal oscillator, reference quartz crystal oscillator and responsive quartz crystal oscillator are electrically connected with frequency meter, frequency meter is communicated with electric brain electric information, and computer carries out acquisition and processing by the frequency difference signal of software to reference quartz crystal oscillator and responsive quartz crystal oscillator.
The present invention compared with prior art, only needs very small amount of sensitive material to be used for test, does not need additionally to make metal electrode on sensitive material, also do not need to heat to sensitive material; Its method of testing is simple, simple and efficient to handle, and principle is reliable, highly sensitive, and response is fast, can on-line real time monitoring.
Accompanying drawing illustrates:
Fig. 1 is the stereoscan photograph of the nanofiber that the responsive quartz crystal oscillator that the present invention relates to deposits.
Fig. 2 is the carbon monoxide gas sensor pick-up unit agent structure principle schematic that the present invention relates to.
The resonse characteristic of CO gas of Fig. 3 to be the nano-fiber film of the responsive quartz crystal oscillator surface deposition that the present invention relates to concentration be 10,30 and 50ppm.
Embodiment:
Also be described further by reference to the accompanying drawings below by embodiment.
Embodiment:
The concrete technology step of the present embodiment is:
(1), polyvinylpyrrolidone (PVP) powder is dissolved in absolute ethyl alcohol, by magnetic stirrer, obtains the settled solution that massfraction is 18wt%; To gather (3,4-rthylene dioxythiophene)-polystyrolsulfon acid (PEDOT-PSS) again to mix with settled solution, and stir, preparation obtains the PEDOT-PSS spinning solution that massfraction is 10wt%;
(2), at ambient temperature, existing electrostatic spinning technique is utilized to prepare PEDOT-PSS nanofiber, quartz crystal oscillator in QCM (Quartz Crystal Microbalance) (QCM) is placed on collector aluminium foil, spinning distance and the distance between spinneret and aluminium foil are 10 centimetres, the PEDOT-PSS spinning solution prepared is put into syringe, apply 20 kilovolts of high-voltage DC power supplies, spinning 50-70 closes high-voltage DC power supply after second, take out the quartz crystal oscillator that surface deposition has PEDOT-PSS nano-fiber film, the quartz crystal oscillator depositing PEDOT-PSS nano-fiber film is placed heating, drying 1 hour at 60 DEG C of temperature on hot plate, obtained surface deposition has the responsive quartz crystal oscillator 7 of PEDOT-PSS nano-fiber film, be carbon monoxide gas sensor, the electron scanning micrograph of poly-(3,4-rthylene dioxythiophene)-polystyrolsulfon acid (PEDOT-PSS) nanofiber as shown in Figure 1,
(3), in the carbon monoxide gas sensor proving installation of self assembly, carbon monoxide gas concentration is detected, first purging with nitrogen 3 pairs of air chambers 5 makes the frequency difference of reference quartz crystal oscillator 6 and responsive quartz crystal oscillator 7 and output frequency be stabilized in 0Hz, CO gas 4 is injected again in air chamber 5, PEDOT-PSS nano-fiber film on responsive quartz crystal oscillator 7 and CO gas 4 interact, produce mass change, frequency changes, when frequency is stablized again, close CO gas 4, again purge air chamber 5 with nitrogen 3, output frequency is made to recover stable, output frequency is gathered by computer 9 over time and preserves.
The Cleaning Principle of the present embodiment is: apply certain alternating voltage and responsive quartz crystal oscillator 7 is vibrated under certain frequency, when the sensitive material of responsive quartz crystal oscillator 7 and gas to be measured interact, quality changes, impressed pressure makes it produce alternating electric field, thus changes the resonance frequency of responsive quartz crystal oscillator 7; During actual test, driving circuit makes reference quartz crystal oscillator 6 and responsive quartz crystal oscillator 7 vibrate under its resonance frequency, the oscillation frequency of frequency meter 8 pairs of reference quartz crystal oscillators 6 and responsive quartz crystal oscillator 7 is measured and is processed, obtain frequency difference signal and be output frequency, output frequency is outputted on computer 9, be spaced apart 0.1 second, computer is gathered output frequency by software, process and draw response curve.
The agent structure of the carbon monoxide gas sensor pick-up unit with the assembling of carbon monoxide gas sensor that the present embodiment relates to comprises admission line 1, admission line valve 2, nitrogen 3, CO gas 4, air chamber 5, reference quartz crystal oscillator 6, responsive quartz crystal oscillator 7, frequency meter 8, computer 9, gas exhaust duct 10 and gas exhaust duct valve 11; Air chamber 5 is connected with gas exhaust duct 10 with admission line 1 respectively, nitrogen 3 and CO gas 4 are respectively by admission line 1 and air chamber 5 pipeline communication, on admission line 1, corresponding nitrogen 3 and CO gas 4 place are shaped with admission line valve 2 respectively, gas exhaust duct 10 are shaped with gas exhaust duct valve 11; Reference quartz crystal oscillator 6 and responsive quartz crystal oscillator 7 is shaped with in air chamber 5, responsive quartz crystal oscillator 7 surface deposition has PEDOT-PSS nano-fiber film, unloaded reference quartz crystal oscillator 6 is identical with the model/specification of responsive quartz crystal oscillator 7, reference quartz crystal oscillator 6 and responsive quartz crystal oscillator 7 are electrically connected with frequency meter 8, frequency meter 8 and the electric information communication of computer 9, computer 9 carries out acquisition and processing by the frequency difference signal of software to reference quartz crystal oscillator 6 and responsive quartz crystal oscillator 7.
The present embodiment tests poly-(3 of responsive quartz crystal oscillator surface deposition, 4-ethene dioxythiophene)-polystyrolsulfon acid (PEDOT-PSS) nanofiber is to the response curve of variable concentrations CO gas (from 1ppm to 200ppm), wherein, after each test terminates, responsive quartz crystal oscillator 7 is put on heating plate and heats 30 minutes at 60 c, CO gas is made to obtain complete desorption, it is 10 that Fig. 3 gives PEDOT-PSS nano-fiber film to concentration, 30, the resonse characteristic of the CO gas of 50ppm, generally, the concentration of the frequency difference that QCM (Quartz Crystal Microbalance) (QCM) method records and tested gas is proportional, as can be seen from figure also, frequency difference increases along with the increase of concentration, illustrate within the scope of finite concentration, the concentration of frequency difference and gas to be measured is linear, under identical flow velocity, the concentration of CO gas raises, the carbon monoxide molecule entering air chamber accordingly increases, thus increase carbon monoxide molecule and poly-(3,4-ethene dioxythiophene) touch opportunity of-polystyrolsulfon acid (PEDOT-PSS) nano-fiber film, adsorbance increases, thus frequency difference increases, and test result shows that this sensor is only to concentration that the CO gas of 1ppm is existing quite significantly to be responded.
Claims (3)
1. a detection method for Low Level Carbon Monoxide gas, is characterized in that concrete technology step is:
(1), by polyvinylpyrrolidonepowder powder be dissolved in absolute ethyl alcohol, by magnetic stirrer, obtain the settled solution that massfraction is 18wt%; To gather (3,4-rthylene dioxythiophene)-polystyrolsulfon acid again to mix with settled solution, and stir, preparation obtains poly-(3,4-rthylene dioxythiophene)-polystyrolsulfon acid spinning solution that massfraction is 10wt%;
(2), at ambient temperature, existing electrostatic spinning technique is utilized to prepare poly-(3, 4-ethene dioxythiophene)-polystyrolsulfon acid nanofiber, quartz crystal oscillator in QCM (Quartz Crystal Microbalance) is placed on collector aluminium foil, spinning distance and the distance between spinneret and aluminium foil are 10 centimetres, to prepare poly-(3, 4-ethene dioxythiophene)-polystyrolsulfon acid spinning solution puts into syringe, apply 20 kilovolts of high-voltage DC power supplies, spinning 50-70 closes high-voltage DC power supply after second, take out surface deposition poly-(3, 4-ethene dioxythiophene) quartz crystal oscillator of-polystyrolsulfon acid nano-fiber film, poly-(3 will be deposited, 4-ethene dioxythiophene) quartz crystal oscillator of-polystyrolsulfon acid nano-fiber film places heating, drying 1 hour at 60 DEG C of temperature on hot plate, obtained surface deposition has poly-(3, 4-ethene dioxythiophene) the responsive quartz crystal oscillator of-polystyrolsulfon acid nano-fiber film, be carbon monoxide gas sensor,
(3), carbon monoxide gas sensor is adopted to be assembled into pick-up unit and to detect carbon monoxide gas concentration, first the frequency difference of reference quartz crystal oscillator and responsive quartz crystal oscillator is made to be stabilized in 0Hz with nitrogen to air chamber purging, CO gas is injected again in air chamber, on responsive quartz crystal oscillator poly-(3, 4-ethene dioxythiophene)-polystyrolsulfon acid nano-fiber film and CO gas interact, produce mass change, resonance frequency changes, when frequency is stablized again, close CO gas, again use nitrogen sweep gas room, the frequency difference of reference quartz crystal oscillator and responsive quartz crystal oscillator is made to recover stable, the frequency difference of reference quartz crystal oscillator and responsive quartz crystal oscillator is gathered by computer over time and preserves.
2. the detection method of Low Level Carbon Monoxide gas according to claim 1, it is characterized in that Cleaning Principle is: apply alternating voltage and responsive quartz crystal oscillator is vibrated, when the sensitive material of responsive quartz crystal oscillator and gas to be measured interact, quality changes, impressed pressure makes it produce alternating electric field, thus changes the resonance frequency of responsive quartz crystal oscillator; During test, driving circuit makes reference quartz crystal oscillator and responsive quartz crystal oscillator vibrate under its resonance frequency, the oscillation frequency of frequency meter to reference quartz crystal oscillator and responsive quartz crystal oscillator is measured and is processed, obtain frequency difference signal and be output frequency, output frequency is outputted on computer, be spaced apart 0.1 second, computer is gathered output frequency by software, process and draw response curve.
3. the detection method of Low Level Carbon Monoxide gas according to claim 1, is characterized in that the agent structure of the pick-up unit of the employing carbon monoxide gas sensor assembling related to comprises admission line, admission line valve, nitrogen, CO gas, air chamber, reference quartz crystal oscillator, responsive quartz crystal oscillator, frequency meter, computer, gas exhaust duct and gas exhaust duct valve; Air chamber is connected with gas exhaust duct with admission line respectively, nitrogen and CO gas are respectively by admission line and air chamber pipeline communication, on admission line, corresponding nitrogen and CO gas place are shaped with admission line valve respectively, gas exhaust duct are shaped with gas exhaust duct valve; Reference quartz crystal oscillator and responsive quartz crystal oscillator is shaped with in air chamber, responsive quartz crystal oscillator surface deposition has poly-(3,4-ethene dioxythiophene)-polystyrolsulfon acid nano-fiber film, unloaded reference quartz crystal oscillator is identical with the model/specification of responsive quartz crystal oscillator, reference quartz crystal oscillator and responsive quartz crystal oscillator are electrically connected with frequency meter, frequency meter is communicated with electric brain electric information, and computer carries out acquisition and processing by the frequency difference signal of software to reference quartz crystal oscillator and responsive quartz crystal oscillator.
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| CN105136984A (en) * | 2015-08-12 | 2015-12-09 | 浙江工商大学 | Detection device and method for volatile methanol in experimental environment |
| CN105242006A (en) * | 2015-09-17 | 2016-01-13 | 浙江工商大学 | Detection apparatus for carbon monoxide in laboratory environment and detection method |
| CN105588918A (en) * | 2015-09-17 | 2016-05-18 | 浙江工商大学 | System and method for detecting nitric oxide in experimental environment |
| CN105527375A (en) * | 2015-09-17 | 2016-04-27 | 浙江工商大学 | Device and method for detecting sulfur dioxide in experiment environment |
| CN105606657B (en) * | 2015-12-26 | 2018-10-09 | 靳职雄 | Pass in and out the online test method of toxic gas carbon monoxide in mouth plastic products |
| CN114965872B (en) * | 2022-04-27 | 2023-10-13 | 重庆科技学院 | Electronic nose and method for multi-sensor data fusion |
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