CN102636552A - Methane gas sensor on basis of organic thin film transistor and preparation method of methane gas sensor - Google Patents
Methane gas sensor on basis of organic thin film transistor and preparation method of methane gas sensor Download PDFInfo
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Abstract
The invention discloses a methane gas sensor on the basis of an organic thin film transistor and a preparation method of the methane gas sensor, and belongs to the field of application of gas sensors. A novel methane gas detection method is characterized by low cost and simple preparation process. The methane gas sensor adopts a bottom gate bottom contact structure of the organic thin film transistor and comprises a substrate, gate electrodes positioned on the substrate, an insulating layer positioned on the gate electrodes, and source electrodes and drain electrodes positioned on the gate-electrode insulting layer, wherein an organic layer with a gas detection function is arranged above the source and drain electrodes. The methane gas sensor is used for detecting methane in the environment.
Description
Technical field
The invention belongs to the gas sensor technical field, be specifically related to a kind of based on machine thin film transistor (TFT) methane gas sensor and preparation method thereof.
Background technology
Methane is very wide in distributed in nature, is one of principal ingredient of rock gas, biogas, hole gas and coal gas.Production industry has caused great harm to the accident that the methane gas blast causes in the ore deposit.Methane explodes as one of main threat of mine safety problem, causes enormous economic loss and staff's sacrifice.Methane is nontoxic basically to the people, belongs to micro-virus kind, and the methane of skin contact liquefaction can cause frostbite.But during excessive concentration, oxygen content can obviously reduce in the air, causes the people to suffocate.When methane reaches 25%-30% in the air, can cause headache, dizziness, weak, absent minded, breathe and palpitate quickly etc.If untimely away from, can cause death by suffocation.The burning-point of methane has only about 63 ℃, when content is 5%-15% in air, meets naked light and will produce blast, and blast is the strongest when content reaches 9.5%.Therefore, the concentration that detects surrounding environment methane exactly has crucial meaning to protection staff's life security.
At present; The method that methane commonly used detects has interference of light detection method (such as Chinese patent CN 201984032 U, CN 201780268 U, CN 1010957318 A, CN 201844973 U, CN 101915123 A, 200520033421.0 etc.); Production by Catalytic Combustion Process (Chinese patent CN 101695658), and vapor-phase chromatography etc.Wherein, interference of light detection method and Production by Catalytic Combustion Process all have the high shortcoming of cost consumption in various degree; Optical interferometry can not carry out continuous coverage, and is not directly perceived to the gas concentration indication; Though the Production by Catalytic Combustion Process response sensitivity is high, good to the selectivity of gas, measured value poor stability, precision are lower, and its response signal is interfered easily, have the variation of zero point drift and output sensitivity.
Organic material is cheap, material source is extensive, with flexible substrates mutually characteristics such as compatibility OTFT is made in development aspect the gas sensor and application caused people's extensive concern.But OTFT gas sensor response speed is fast, selectivity, good reversibility working and room temperature, and can microminiaturized, array.OTFT has special advantages; It can provide the response of multiparameter; Such as: under the methane environment, measure; Can observe the variation of switch current ratio, the drift of threshold voltage, variation of mobility or the like, from low price, low-power consumption, the aspect that can be mass-produced, the OTFT gas sensor is a new development visual angle.
Summary of the invention
The object of the invention is to overcome the shortcoming of traditional detection methane transducer, provides a kind of preparation technology simple, low production cost, be used to detect methane and can the multiparameter response a kind of based on machine thin film transistor (TFT) methane gas sensor and preparation method thereof.
A kind of based on machine thin film transistor (TFT) methane gas sensor; The organic layer 6 that comprise glass substrate 1, gate electrode 2, gate insulator 3, drain electrode 4 source electrodes 5, has a detection of gas function is formed; It is characterized in that: gate insulator 3 is positioned on the substrate 1 that is etched with grid 2; Source electrode 5 is positioned on the gate insulator 3 with drain electrode 6; Organic layer 6 connection source electrodes 5 and drain electrode 4, organic layer 6 is not only as the basic structure ingredient of organic film FET device but also as the sensitive function layer.
Further say; Said organic layer 6 is a raw material with p type, semiconductor material acene class, by anthracene, aphthacene, pentacene, 6, and the silica-based acetylene pentacene of 13-two or three isopropyl esters, 3; 4-benzopyrene, coronene, 6, at least a formation in 13-five and the benzoquinones.
Say that further the thickness of said organic layer 6 is 5-500 nm.
Say that further said substrate 1 is processed by silicon chip, glass, thin polymer film or metal forming.
Say that further said gate electrode 2, source electrode 5 and drain electrode 4 are processed by low-resistance metal and alloy material, metal oxide or conducing composite material, the thickness of source electrode 5 and drain electrode 4 is 10-300 nm.
Say that further the thickness of said gate insulator 3 is 20-2000 nm.
A kind of preparation method based on machine thin film transistor (TFT) methane gas sensor may further comprise the steps:
1. earlier substrate (1) is cleaned completely, it is dry to clean the back;
2. prepare gate electrode (2) at substrate surface;
3. handle at gate electrode (2) above-prepared gate insulator (3) and to insulation course;
4. go up preparation source electrode (5) and drain electrode (4) at said gate insulator (3);
5. between source electrode (5) and drain electrode (4), prepare the organic layer (6) that is used to survey methane gas.
Furtherly, gate electrode described in the preparation method (2), source electrode (5), drain electrode (4) are through the arbitrary method preparation in chemical vapor deposition, serigraphy, printing or the spin coating of vacuum thermal evaporation, magnetron sputtering, plasma enhancing.
Furtherly, gate insulator described in the preparation method (3) is through the arbitrary method preparation in chemical vapor deposition, thermal oxide, spin coating or the vacuum evaporation of plasma enhancing.
Furtherly, organic layer described in the preparation method (6) is through the arbitrary method preparation in chemical vapor deposition, thermal oxide, spin coating, vacuum evaporation, spin coating, a film, impression, printing or the gas blowout of plasma enhancing.
Furtherly, spin coating proceeding described in the preparation method is that 1000 rev/mins speed spin coating gate insulator (3) is changeed in 400 rev/mins of preceding commentaries on classics, back, and thickness is 20-2000nm; Said annealing temperature is 150 ℃, and the time is 1 hour.
Furtherly, the organic layer of vapor deposition described in the preparation method (6) speed is the 0.01-0.03 nm/sec, and thickness is the 5-500 nanometer.
Furtherly, speed is in the 0.1-0.6 nm/sec during institute's described vapor deposition source electrode (5) and drain electrode (6) among the preparation method, and thickness is the 10-300 nanometer.
The present invention has following beneficial effect:
One, adopt multiple preparation technology, simplify device greatly and prepare process, device can be integrated, array, microminiaturization, is fit to large-scale production.
Two, but acene class and acene analog derivative organic material large tracts of land with low cost forms film, and can be compatible mutually with flexible substrate.
Three, other organic semiconducting materials relatively, the OTFT device of acene class material preparation have good electrology characteristic, can produce bigger response current, are convenient to realize the detection to analyte.
Four, can make response to methane gas fast based on the methane gas sensor of OTFT.
Five, can produce the multiparameter response to measured analyte.
Description of drawings
Fig. 1 is the synoptic diagram of gas sensor of the present invention;
Fig. 2 is exposed to source-drain current and the response curve of time in the 100ppm methane gas for methane transducer of the present invention;
1 is substrate among the figure, and 2 is grid, and 3 is gate insulator, and 4 is drain electrode, and 5 is the source electrode, and 6 is organic layer.
Embodiment
Principle:, therefore good current response characteristic is arranged based on the prepared OTFT of this type of material because also benzene material can form the characteristics of polycrystalline state and higher carrier mobility.The OTFT gas sensor with organic layer as sensitive layer; When work; OTFT organic layer adsorption analysis thing; Make to produce physics or chemisorption between analyte and the organic layer, change film morphology generation potential barrier or charge carrier and fall into into, thereby make the parameter of device change.Obtain the information of institute's detected gas through the variation of detection means parameter (field-effect mobility of threshold voltage, switching current or organic layer conducting polymer materials).
A kind of based on machine thin film transistor (TFT) methane gas sensor; The organic layer composition that comprises glass substrate, gate electrode, gate insulator, drain electrode, source electrode, has the detection of gas function; It is characterized in that: gate insulator is positioned on the substrate that is etched with grid; Source electrode and drain electrode are positioned on the gate insulator, and organic layer connects source electrode and drain electrode, and organic layer is not only as the basic structure ingredient of organic film FET device but also as the sensitive function layer.
Substrate can adopt rigid substrate or flexible substrate, a kind of as in silicon chip, glass, thin polymer film and the metal forming, and the present invention adopts cheap film-substrate.
Gate insulator adopts the material with excellent dielectric properties, comprise inorganic insulating material such as silicon dioxide (SiO2), silicon nitride (Si3N4), aluminium oxide (Al2O3), etc.; Organic insulation such as polymethylmethacrylate (PMMA), polyvinylpyrrolidone (PVP), polyvinyl alcohol (PVA) (PVA), polystyrene (PS) etc., the preparation method can be various film build methods such as vacuum thermal evaporation, spin coating, spraying, magnetron sputtering.The thickness of said gate insulator 3 is 20-2000 nm.
Organic layer adopts acene class and acene analog derivative organic material to process; Comprise anthracene (anthracene), aphthacene, pentacene or rubrene, 6; 13-five and benzoquinones, 3,4-acene pyrene etc., the preparation method can be various film build methods such as vacuum thermal evaporation, spin coating, spraying, magnetron sputtering.The thickness of said methane gas organic semiconductor detecting layer is 5-500 nm.
The OTFT gas sensor is made up of glass substrate, gate electrode, gate insulator, drain electrode, source electrode, organic layer; Gate insulator is positioned on the substrate that is etched with grid; Source electrode and drain electrode are positioned on the gate insulator, and organic layer connects source electrode and drain electrode.Organic layer is a raw material with p type organic semiconducting materials pentacene.
Glass substrate to the good gate electrode ITO of sputter is cleaned; After at first utilizing clean-out system to clean, ultrasonic 10 minutes of detergent solution is cleaned substrate with washing agent again; Use deionized water rinsing; Ultrasonic 10 minutes of deionized water solution was used acetone soln ultrasonic 10 minutes again, was placed in the ethanolic solution ultrasonic 10 minutes at last.Clean the back and dry up substrate with nitrogen; Transfer 500 rev/mins, the back speed spin coating insulation course PMMA that changes 1000 rev/mins before the setting to, thickness is 500 nanometers; Under 150 ℃ of temperature, annealed 1 hour then; Utilize vacuum deposition method then, vapor deposition source electrode and drain electrode, source-drain electrode are the Au electrode, vapor deposition speed 0.1-0.3 nm/sec, and thickness is 50 nanometers; Last vapor deposition organic layer pentacene, speed is the 0.01-0.02 nm/sec, thickness reaches 50 nanometers.
The above-mentioned gas sensor as for saturated, is reached when stablizing, be exposed in the methane gas that same concentration is 100ppm; (referring to Fig. 2) can know by response curve, and the source-drain current of device sharply reduces in the time of in being exposed to methane gas, and this is because when methane absorption and organic thin film layer; Methane shows as weak reductant and the two generation electric charge of organic layer film shifts, and produces potential barrier or trap; Make the organic layer holoe carrier reduce, therefore make source-drain current reduce.
Glass substrate to the good gate electrode ITO of sputter is cleaned; After at first utilizing clean-out system to clean, ultrasonic 10 minutes of detergent solution is cleaned substrate with washing agent again; Use deionized water rinsing; Ultrasonic 10 minutes of deionized water solution was used acetone soln ultrasonic 10 minutes again, was placed in the ethanolic solution ultrasonic 10 minutes at last.Clean the back and dry up substrate with nitrogen; Transfer 500 rev/mins, the back speed spin coating insulation course PS that changes 1000 rev/mins before the setting to, thickness is 20 nanometers; Under 150 ℃ of temperature, annealed 1 hour then; Utilize vacuum deposition method then, vapor deposition source electrode and drain electrode, source-drain electrode are the Au electrode, vapor deposition speed 0.1-0.3 nm/sec, and thickness is 50 nanometers; Last vapor deposition organic layer pentacene, speed is the 0.01-0.02 nm/sec, thickness reaches 25 nanometers; Promptly get gas sensor.
Glass substrate to the good gate electrode ITO of sputter is cleaned; After at first utilizing clean-out system to clean, ultrasonic 15 minutes of detergent solution is cleaned substrate with washing agent again; Use deionized water rinsing; Ultrasonic 15 minutes of deionized water solution was used acetone soln ultrasonic 15 minutes again, was placed in the ethanolic solution ultrasonic 15 minutes at last.Clean the back and dry up substrate with nitrogen; Transfer 500 rev/mins, the back speed spin coating insulation course PVA that changes 1000 rev/mins before the setting to, thickness is 2000 nanometers; Under 150 ℃ of temperature, annealed 1 hour then; Utilize vacuum deposition method then, vapor deposition source electrode and drain electrode, source-drain electrode are the Au electrode, vapor deposition speed 0.1-0.3 nm/sec, and thickness is 50 nanometers; Last vapor deposition organic layer pentacene, speed is the 0.01-0.02 nm/sec, thickness reaches 25 nanometers; Promptly get gas sensor.
Glass substrate to the good gate electrode ITO of sputter is cleaned; After at first utilizing clean-out system to clean, ultrasonic 15 minutes of detergent solution is cleaned substrate with washing agent again; Use deionized water rinsing; Ultrasonic 15 minutes of deionized water solution was used acetone soln ultrasonic 15 minutes again, was placed in the ethanolic solution ultrasonic 15 minutes at last.Clean the back and dry up substrate with nitrogen; Transfer 500 rev/mins, the back speed spin coating insulation course PMMA that changes 1000 rev/mins before the setting to, thickness is 2000 nanometers; Under 150 ℃ of temperature, annealed 1 hour then; Utilize vacuum deposition method then, vapor deposition source electrode and drain electrode, source-drain electrode are the Au electrode, vapor deposition speed 0.1-0.3 nm/sec, and thickness is 50 nanometers; Last vapor deposition organic layer pentacene, speed is the 0.01-0.02 nm/sec, thickness reaches 50 nanometers; Promptly get gas sensor.
Glass substrate to the good gate electrode ITO of sputter is cleaned; After at first utilizing clean-out system to clean, ultrasonic 15 minutes of detergent solution is cleaned substrate with washing agent again; Use deionized water rinsing; Ultrasonic 15 minutes of deionized water solution was used acetone soln ultrasonic 10 minutes again, was placed in the ethanolic solution ultrasonic 15 minutes at last.Clean the back and dry up substrate with nitrogen; Transfer 500 rev/mins, the back speed spin coating insulation course PMMA that changes 1000 rev/mins before the setting to, thickness is 250 nanometers; Under 150 ℃ of temperature, annealed 1 hour then; Utilize vacuum deposition method then, vapor deposition source electrode and drain electrode, source-drain electrode are the Au electrode; Vapor deposition speed 0.1-0.6 nm/sec, thickness is 50 nanometers, preceding 100 nanometer vapor deposition speed are the 0.1-0.3 nm/sec; Back 150 nanometer vapor deposition speed are the 0.3-0.6 nm/sec; Last vapor deposition organic layer pentacene, speed is the 0.01-0.03 nm/sec, and thickness reaches 50 nanometers, and preceding 20nm speed is 0.01 nm/sec, and back 30nm is the 0.02-0.03 nm/sec; Promptly get gas sensor.
Glass substrate to the good gate electrode ITO of sputter is cleaned; After at first utilizing clean-out system to clean, ultrasonic 15 minutes of detergent solution is cleaned substrate with washing agent again; Use deionized water rinsing; Ultrasonic 15 minutes of deionized water solution was used acetone soln ultrasonic 15 minutes again, was placed in the ethanolic solution ultrasonic 15 minutes at last.Clean the back and dry up substrate with nitrogen; Transfer 500 rev/mins, the back speed spin coating insulation course PVA that changes 1000 rev/mins before the setting to, thickness is 250 nanometers; Under 150 ℃ of temperature, annealed 1 hour then; Utilize vacuum deposition method then, vapor deposition source electrode and drain electrode, source-drain electrode are the Au electrode, vapor deposition speed 0.1-0.3 nm/sec, and thickness is 50 nanometers; Last vapor deposition organic layer aphthacene, speed is the 0.01-0.02 nm/sec, thickness reaches 5 nanometers; Promptly get gas sensor.
Embodiment 7
Glass substrate to the good gate electrode ITO of sputter is cleaned; After at first utilizing clean-out system to clean, ultrasonic 15 minutes of detergent solution is cleaned substrate with washing agent again; Use deionized water rinsing; Ultrasonic 15 minutes of deionized water solution was used acetone soln ultrasonic 15 minutes again, was placed in the ethanolic solution ultrasonic 15 minutes at last.Clean the back and dry up substrate with nitrogen; Transfer 500 rev/mins, the back speed spin coating insulation course PVA that changes 1000 rev/mins before the setting to, thickness is 250 nanometers; Under 150 ℃ of temperature, annealed 1 hour then; Utilize vacuum deposition method then, vapor deposition source electrode and drain electrode, source-drain electrode are the Au electrode, vapor deposition speed 0.1-0.3 nm/sec, and thickness is 50 nanometers; Last vapor deposition organic layer anthracene, speed is the 0.01-0.02 nm/sec, thickness reaches 500 nanometers; Promptly get gas sensor.
Embodiment 8
Glass substrate to the good gate electrode ITO of sputter is cleaned; After at first utilizing clean-out system to clean, ultrasonic 10 minutes of detergent solution is cleaned substrate with washing agent again; Use deionized water rinsing; Ultrasonic 10 minutes of deionized water solution was used acetone soln ultrasonic 10 minutes again, was placed in the ethanolic solution ultrasonic 10 minutes at last.Clean the back and dry up substrate with nitrogen; Transfer 500 rev/mins, the back speed spin coating insulation course PMMA that changes 1000 rev/mins before the setting to, thickness is 200 nanometers; Under 150 ℃ of temperature, annealed 1 hour then; Utilize vacuum deposition method then, vapor deposition source electrode and drain electrode, source-drain electrode are the Cu electrode, vapor deposition speed 0.1-0.3 nm/sec, and thickness is 10 nanometers; Last vapor deposition organic layer pentacene, speed is the 0.01-0.02 nm/sec, thickness reaches 50 nanometers; Promptly get gas sensor.
Embodiment 9
Glass substrate to the good gate electrode ITO of sputter is cleaned; After at first utilizing clean-out system to clean, ultrasonic 10 minutes of detergent solution is cleaned substrate with washing agent again; Use deionized water rinsing; Ultrasonic 10 minutes of deionized water solution was used acetone soln ultrasonic 10 minutes again, was placed in the ethanolic solution ultrasonic 10 minutes at last.Clean the back and dry up substrate with nitrogen; Transfer 500 rev/mins, the back speed spin coating insulation course PS that changes 1000 rev/mins before the setting to, thickness is 200 nanometers; Under 150 ℃ of temperature, annealed 1 hour then; Utilize vacuum deposition method then, vapor deposition source electrode and drain electrode, source-drain electrode are the Al electrode, vapor deposition speed 0.1-0.3 nm/sec, and thickness is 300 nanometers; Last vapor deposition organic layer pentacene, speed is the 0.01-0.02 nm/sec, thickness is 25 nanometers; Promptly get gas sensor.
Claims (10)
1. one kind based on machine thin film transistor (TFT) methane gas sensor; Organic layer (6) composition that comprises glass substrate (1), gate electrode (2), gate insulator (3), drain electrode (4) source electrode (5), has the detection of gas function; It is characterized in that: gate insulator (3) is positioned on the substrate (1) that is etched with grid (2); Source electrode (5) and drain electrode (6) are positioned on the gate insulator (3), and organic layer (6) connects source electrode (5) and drain electrode (4).
2. according to claim 1 a kind of based on machine thin film transistor (TFT) methane gas sensor; It is characterized in that: said organic layer (6) is by anthracene, aphthacene, pentacene, 6; The silica-based acetylene pentacene of 13-two or three isopropyl esters, 3; 4-benzopyrene, coronene, 6, at least a formation in 13-five and the benzoquinones.
3. according to each described methane gas sensor based on OTFT of claim 1～2, it is characterized in that: the thickness of said organic layer (6) is 5-500 nm.
4. according to claim 1 a kind of based on machine thin film transistor (TFT) methane gas sensor, it is characterized in that: said substrate (1) is processed by silicon chip, glass, thin polymer film or metal forming.
5. according to claim 1 a kind of based on machine thin film transistor (TFT) methane gas sensor; It is characterized in that: said gate electrode (2), source electrode (5) and drain electrode (4) are processed by low-resistance metal and alloy material, metal oxide or conducing composite material, and the thickness of source electrode (5) and drain electrode (4) is 10-300 nm.
6. according to claim 1 a kind of based on machine thin film transistor (TFT) methane gas sensor, it is characterized in that: the thickness of said gate insulator (3) is 20-2000 nm.
7. preparation method based on machine thin film transistor (TFT) methane gas sensor may further comprise the steps:
1. earlier substrate (1) is cleaned completely, it is dry to clean the back;
2. prepare gate electrode (2) at substrate surface;
3. handle at gate electrode (2) above-prepared gate insulator (3) and to insulation course;
4. go up preparation source electrode (5) and drain electrode (4) at said gate insulator (3);
5. between source electrode (5) and drain electrode (4), prepare the organic layer (6) that is used to survey methane gas.
8. a kind of preparation method based on machine thin film transistor (TFT) methane gas sensor according to claim 8 is characterized in that: said gate electrode (2), source electrode (5), drain electrode (4) are through the arbitrary method preparation in chemical vapor deposition, serigraphy, printing or the spin coating of vacuum thermal evaporation, magnetron sputtering, plasma enhancing.
9. a kind of preparation method based on machine thin film transistor (TFT) methane gas sensor according to claim 8 is characterized in that: said gate insulator (3) is through the arbitrary method preparation in chemical vapor deposition, thermal oxide, spin coating or the vacuum evaporation of plasma enhancing.
10. a kind of preparation method based on machine thin film transistor (TFT) methane gas sensor according to claim 8 is characterized in that: the arbitrary method preparation in the chemical vapor deposition that said organic layer (6) strengthens through plasma, thermal oxide, spin coating, vacuum evaporation, spin coating, a film, impression, printing or the gas blowout.
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| CN108896717A (en) * | 2018-07-24 | 2018-11-27 | 京东方科技集团股份有限公司 | A kind of chemical sensitisation unit and chemical sensor, chemical sensing devices |
| CN110501385A (en) * | 2019-08-29 | 2019-11-26 | 电子科技大学 | A kind of Organic Thin Film Transistors nitrogen dioxide sensor and preparation method thereof based on air dielectric layer |
| CN114646675A (en) * | 2022-04-02 | 2022-06-21 | 西安电子科技大学杭州研究院 | Hydrogen sensor based on thin film transistor/preparation method and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108447915A (en) * | 2018-03-02 | 2018-08-24 | 华中科技大学 | A kind of thin film field effect transistor type gas sensor and preparation method thereof |
| CN108896717A (en) * | 2018-07-24 | 2018-11-27 | 京东方科技集团股份有限公司 | A kind of chemical sensitisation unit and chemical sensor, chemical sensing devices |
| US10976281B2 (en) | 2018-07-24 | 2021-04-13 | Hefei Xinsheng Optoelectronics Technology Co., Ltd. | Chemical sensing unit, chemical sensor, and chemical sensing device electrically coupled to light emitting diode |
| CN110501385A (en) * | 2019-08-29 | 2019-11-26 | 电子科技大学 | A kind of Organic Thin Film Transistors nitrogen dioxide sensor and preparation method thereof based on air dielectric layer |
| CN114646675A (en) * | 2022-04-02 | 2022-06-21 | 西安电子科技大学杭州研究院 | Hydrogen sensor based on thin film transistor/preparation method and application thereof |
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Application publication date: 20120815 |