CN102928473A - Low-voltage flexible OTFT ammonia gas sensor and manufacturing method thereof - Google Patents
Low-voltage flexible OTFT ammonia gas sensor and manufacturing method thereof Download PDFInfo
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Abstract
The invention discloses a low-voltage flexible OTFT ammonia gas sensor and a manufacturing method thereof, wherein the sensor is a bottom-gate bottom contact device configuration and is provided with a source S, a drain D, a gate G, a three-pole electrode, an insulating layer and an active layer. The grid electrode is made of Indium Tin Oxide (ITO) thin film material and is plated on the flexible plastic substrate; a terpolymer P (VDF-TrFE-CTFE) of vinylidene fluoride (VDF), trifluoroethylene (TrFE) and Chlorotrifluoroethylene (CTFE) is used as an insulating layer; a gold film with certain flexibility is used as a source drain electrode layer; an organic sensitive film P3HT or P3 HT/nano oxide composite film and the like with good response to ammonia gas are prepared between the source electrode and the drain electrode. The invention utilizes the vinylidene fluoride terpolymer with higher dielectric constant to replace SiO2The organic insulating layer which is well matched with the organic sensitive film is manufactured, so that the working voltage of the sensor is reduced, and the working current is improved; and meanwhile, the flexibility of the device is improved.
Description
Technical field
The present invention relates to flexible electronic sensor and organic polymer material field, be specifically related to a kind of based on P (VDF-TrFE-CTFE) terpolymer as flexible OTFT ammonia gas sensor of the low pressure of insulation course and preparation method thereof.
Background technology
Ammonia is widely toxic gas of a kind of commercial Application, and is colourless, and the pungency foul smell is arranged, and it has the upper respiratory tract of animal or human's body stimulates and corrosive attack, often be attracted to mucocutaneous and the eye conjunctiva on, stimulate and inflammation thereby produce, if the people sucks 700mg m
-3Lasting 30min can poison, if suck 1750～4000mgm
-3But threat to life, the ammonia allowable concentration of employment security administration of health office of Department of Labor (OSHA) regulation is 50ppm (10
-6, lower same), and U.S. professional safety and health research institute (NIOSH) set upper limit is 25ppm.The gas sensor that detects at present ammonia mainly contains metal semiconductor sensor, electrochemical sensor, conduction high polymer sensor, nano material sensor, Electronic Nose etc.
The metal semiconductor material is a class material that is applied to the earliest ammonia gas sensor.This material mainly is to rely on the conductivity variations of contact ammonia front and back to detect.But the temperature application range of most of metal semiconductor sensor is at 200～500 ℃, and poor selectivity is the greatest drawback that the metal semiconductor material is used, and this has brought difficulty for its application.
Electrochemical ammonia sensor is to determine the concentration of ammonia can be divided into electric potential type, Direct Current type and capacitor type by the variation of current potential, electric current before and after the ammonia by detecting electrode.Traditional electrochemical sensor uses liquid electrolyte, electrolytical evaporation or pollute and cause easily sensor signal to decline falling, affect the accuracy of detection of sensor, and reduced the serviceable life of sensor.
In recent years, conduction high polymer, nano material etc. has become the study hotspot of ammonia gas sensor, and it has the advantages such as preparation is simple, cheap, application restric-tion lacks than original sensor.When gas passes through, produce the electronics give and accept relation between the gas of absorption and the sensitive material, learn the information that gas molecule exists that detects by detecting the physical property variation (such as the conductance variation) that causes that interacts.And aspect the ammonia gas sensor Patents, most employing coating type or the resistor-type structure reported are there are no the ammonia gas sensor patent report based on the OTFT device architecture.
In recent years, the OTFT gas sensor has extraordinary application prospect also having received increasing concern aspect chemical gas and the biochemical detection.Compare with traditional gas sensor, based on the gas sensor of OTFT structure except have selectivity good, highly sensitive, can use at normal temperatures etc. the advantage, also have following remarkable advantage: the high resistance that utilizes the fundamental characteristics of field effect transistor to be difficult to detect changes the curent change that is converted into easy detection; Can regulate by the grid operating voltage of suitable selector the sensitivity of sensor; The multiparameter model such as mobility, threshold voltage more is conducive to identification and the analysis of gaseous species, concentration; By can regulate easily the electrical property of sensor to the chemical modification of organic molecule, improve sensitivity; Be easy to integratedly, can prepare the large tracts of land sensor array.But traditional OTFT gas sensor is mainly used the structure of inorganic field effect pipe, adopts SiO
2As insulation course, had a strong impact on the pliability of device; Source-drain current is less, 10
-7The A magnitude is difficult to detect; And inorganic insulation layer contacts with not mating of organic sensitive thin film device had relatively high expectations to grid voltage, need reach-40V about, the back-end processing circuit is complicated, has limited to a certain extent the range of application of sensors with auxiliary electrode were.
The scientific research institutions such as Cambridge University, Tokyo University, the University of Pennsylvania, Princeton University and Bell Laboratory, IBM, Xerox, Epson have all carried out the work of OTFT and application facet thereof.Domestic aspect, should change chemistry institute of institute, the Chinese Academy of Sciences, Tsing-Hua University, Northern Transportation University, 26 in middle electric group, Jilin University and University of Electronic Science and Technology etc. take Changchun and in succession carry out the research work of OTFT as the research unit of representative, but it is then few that OTFT is applied to the research of sensor field.
Aspect the OTFT ammonia gas sensor, the present OTFT device of reporting has been useful on the detection of ammonia.As,
,
Utilize spin-coating method the P3HT film to be plated in the SiO of thermal oxide Deng the people
2On/Si the base, for detection of ammonia; The people such as Liu Bo, Fu Songqi has prepared based on SiO
2The OTFT device of insulation course, and be used for the detection of ammonia, response is good.But its structure is mainly taked inorganic field effect pipe die formula, utilizes SiO
2As insulating layer material, technique is complicated, and pliability is poor, and inorganic insulation layer contacts with organic sensitive thin film and have certain defect, requires the device operating voltage higher, and electric current is less, is difficult to detection, can not satisfy the practicality requirement of OTFT gas sensor.Taiwan university of communications wears people such as inscription will etc. and utilizes polyvinylphenol PVP to make insulation course, pentacene is made the bottom gate top contact OTFT device of organic sensitive membrane, response to ammonia is unsatisfactory, but after adding the diameter polystyrene spheres particle of diameter 200nm between insulation course and active layer, performance is necessarily promoted, and can detect the ammonia of 0.5ppm, but grid voltage is still higher, electric current is on the low side, has also improved the complicacy of device preparation simultaneously, and practicality is bad.
Summary of the invention
For above-mentioned prior art, the technical problem to be solved in the present invention is: there are the problems such as poor selectivity, cost height, complex process, practicality be relatively poor in existing ammonia gas sensor.
Purpose of the present invention is: OTFT ammonia gas sensor of a kind of low pressure flexibility and preparation method thereof is provided, the preparation technology of this ammonia gas sensor is simple, cost is low, selectivity is good, but condition of work requires low working and room temperature, is with a wide range of applications in real time environment monitoring field.
In order to solve the problems of the technologies described above, the present invention adopts following technical scheme:
A kind of OTFT ammonia gas sensor of low pressure flexibility is characterized in that: contact devices configuration at the bottom of the bottom gate, be provided with source electrode, drain electrode, grid, and grid adopts the ITO organic material; Wherein source electrode and drain electrode are done electrode layer with gold copper-base alloy; Arrange between source electrode and the drain electrode ammonia is responded the preferably sensitive thin film such as P3HT organic semiconductor thin-film or P3HT/ nanometer oxidate compound film; Insulation course between source-drain electrode and grid adopts dielectric coefficient higher and contact preferably P (VDF-TrFE-CTFE) terpolymer with organic sensitive thin film.
The grid voltage that described device need to provide is lower, for-3V ~-5V, and electric current is larger, is easy to detect.
Described device all adopts organic material except source-drain electrode, pliability is better, and environmental suitability is stronger; And technique is simple, has reduced cost.
The organic sensitive thin film thickness of described device is 50～150nm, and the insulating layer material of employing is P (VDF-TrFE-CTFE) terpolymer, and thickness is 50～200nm.
Method for making according to the flexible OTFT ammonia gas sensor of low pressure provided by the present invention is characterized in that, may further comprise the steps:
1), adopt the ITO flexiplast as substrate, the column criterion of going forward side by side is cleaned;
2), utilize three kinds of monomers to synthesize P (VDF-TrFE-CTFE) terpolymer;
3), take the method for spin coating to utilize 2) in synthetic material prepare organic insulator;
4), preparation source-drain electrode mask plate;
5), in conjunction with mask plate, the vacuum evaporation source-drain electrode;
6), adopt flexiplast to encapsulate, draw measurement circuit at the source drain-gate three end utmost points respectively with 60 μ m Si-Al wires, adopt the method for pressure welding to realize connection;
7), utilize spin-coating method to prepare organic semiconductor P3HT or P3HT/ nano-oxide film.
Be P (VDF-TrFE-CTFE) terpolymer according to the described organic insulation layer material of step 3), thickness is 50～200nm, and relative dielectric constant is up to 50, grid voltage can be dropped to-3V about.In addition, insulating layer material can also be selected other terpolymers of the same type, such as P (VDF-TrFE-CFE) etc.
Be 50～150 nm according to the organic sensitive thin film thickness in the step 7), better to susceptibility, the selectivity of ammonia.
According to the above step, except source-drain electrode is toughness preferably the gold coated films, all the other materials all adopt organic material, make device have higher pliability, can realize the variation of sensor outward appearance, have enlarged the range of application of sensor.
Compared with prior art, the present invention has following beneficial effect:
1, adopt the ammonia gas sensor of OTFT structure, but but have that technique is simple, volume is little, an advantage such as work under the low integrated array room temperature of cost;
2, the inorganic insulation layer material is changed into the organic ternary multipolymer of high-k, reduced the operating voltage of device, improved source-drain current, strengthened the practicality of device;
3, except source-drain electrode adopted gold thin film, other structures of device were all taked organic material, have improved the pliability of device, have enlarged the range of application of device;
When 4, making insulation course and sensitive membrane, only require simple process such as using spin coating, gas blowout, compare with traditional inorganic material, reduced membrance casting condition and cost, be applicable to fairly large production;
5, the OTFT sensor has the advantages that the multiparameters such as leakage current, threshold voltage, switch current ratio and mobility detect, and is easier to determine component and the concentration of gas; Polynary organic copolymer material is combined with thin-film technique, simplified device preparation technology, improved device performance, for new approach has been opened up in the preparation and application of OTFT ammonia gas sensor.
Description of drawings
Fig. 1 is OTFT ammonia gas sensor structural section figure provided by the present invention;
Fig. 2 is the synthetic chemistry reaction equation of insulation course terpolymer provided by the present invention.
Embodiment
Adopt the flexible OTFT ammonia gas sensor of low pressure of material and thin film technique preparation, in conjunction with shown in Figure 1, get the ITO(tin indium oxide) flexible substrate, utilize vinylidene (VDF), trifluoro-ethylene (TrFE), synthetic P (VDF-TrFE-CTFE) terpolymer of chlorotrifluoroethylene (CTFE) to prepare insulation course, gold thin film is as source-drain electrode, and source S, drain D and grid G three-end electrode have respectively the outer lead for test.
In conjunction with shown in Figure 2, it is the synthetic reaction formula of terpolymer P (VDF-TrFE-CTFE).Add quantitative distilled water, an amount of initiating agent and emulsifying agent in reactor, to-150 ℃, pass into VDF, TrFE, the CTFE monomer of gaseous state with cooled with liquid nitrogen again, every kind of monomer is controlled with mass flowmeter.Keep constant temperature after subsequently reactor being warming up to initiation temperature, and begin to stir with the rotating speed of 250 r/min from normal temperature.Total reaction time needs about 4 h, take top pressure as benchmark, stops reaction when the conversion ratio that reaches 20%.The terpolymer that obtains is respectively with distilled water washing 3 times, and 60 ℃ of dryings are one day in vacuum drying chamber, obtain final terpolymer.But owing to test all with certain error at every turn, finally all synthetic terpolymer must be carried out component analysis, determine the ratio of various materials.
Before the insulation course preparation, at first to prepared ITO substrate surface pre-service.Successively ultrasonic cleaning in deionized water, acetone and absolute ethyl alcohol, dry for standby.At first, synthetic terpolymer is dissolved in D, in the D-dimethyl formamide (DMF), utilizes spin-coating method film forming on the ITO substrate, then dry, remove the DMF of remained on surface.Secondly, preparation source-drain electrode mask plate, and in conjunction with mask plate vacuum evaporation Au electrode, do again contact conductor, encapsulation.At last, the polymer P 3HT of 3-hexyl thiophene is dissolved in the methenyl choloride solvent that concentration is 5mg/ml, adopts gas blowout technique, prepare one deck P3HT film at device surface; Perhaps respectively the polymer P 3HT of 3-hexyl thiophene is dissolved in the methenyl choloride solvent that concentration is 5mg/ml, nano-oxide solution is dissolved in the anhydrous ethanol solvent that concentration is 5mg/ml, get again two kinds of solution of equivalent and be made into mixed liquor, preparation P3HT/ nanometer oxidate compound film, solvent, test are removed in oven dry.
Claims (6)
1. the flexible OTFT ammonia gas sensor of low pressure is characterized in that: for contact devices configuration at the bottom of the bottom gate, be provided with source electrode, drain electrode, grid, grid employing ITO flexible substrate; Wherein make source electrode and drain electrode layer with gold thin film; Preparation responds the preferably organic sensitive thin film of P3HT or P3HT/ nano-oxide composite membrane etc. to ammonia between source electrode and the drain electrode; Insulation course between source-drain electrode and grid adopts dielectric coefficient higher and contact preferably P (VDF-TrFE-CTFE) terpolymer with organic sensitive membrane.
2. the flexible OTFT ammonia gas sensor of low pressure according to claim 1 is characterized in that, grid voltage is-and 3V ~-5V.
3. the flexible OTFT ammonia gas sensor of low pressure according to claim 1, it is characterized in that, described P3HT or P3HT/ nano-oxide composite sensing film thickness are 50～150nm, and the insulating layer material of employing is P (VDF-TrFE-CTFE) terpolymer, and thickness is 50～200nm.
4. the method for making of the flexible OTFT ammonia gas sensor of low pressure is characterized in that, may further comprise the steps:
Utilize three kinds of monomer chemosynthesis P (VDF-TrFE-CTFE) terpolymer;
Method with spin coating will
In synthetic material prepare organic insulator;
5. the method for making of the flexible OTFT ammonia gas sensor of low pressure according to claim 4 is characterized in that, wherein step
Described organic insulation layer material is P (VDF-TrFE-CTFE) terpolymer, and thickness is 50～200nm, and relative dielectric constant is 50, grid voltage can be dropped to-3V ~-5V.In addition, insulating layer material can also be selected other terpolymers of the same type, such as P (VDF-TrFE-CFE) etc.
6. the method for making of the flexible OTFT ammonia gas sensor of low pressure according to claim 4 is characterized in that described step
In ammonia is responded preferably the P3HT organic semiconductor thin-film or P3HT/ nanometer oxidate compound film equal thickness is 50～150 nm.
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| CN104132988A (en) * | 2014-07-28 | 2014-11-05 | 南京邮电大学 | Preparation method of flexible organic ion-sensitive field effect transistor |
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| CN110806429A (en) * | 2019-08-08 | 2020-02-18 | 杭州市富阳区浙工大银湖创新创业研究院 | Resistance-type flexible gas sensor with resistance compensation function in bending state and preparation method thereof |
| CN117723095A (en) * | 2024-02-08 | 2024-03-19 | 电子科技大学 | Flexible capacitance strain sensor with length of variable electrode and preparation method thereof |
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| CN104132988A (en) * | 2014-07-28 | 2014-11-05 | 南京邮电大学 | Preparation method of flexible organic ion-sensitive field effect transistor |
| CN108365096A (en) * | 2018-02-02 | 2018-08-03 | 合肥工业大学 | The block copolymer semiconductor nanowires preparation method and its usage of helical structure |
| CN108365096B (en) * | 2018-02-02 | 2021-11-12 | 合肥工业大学 | Preparation method and application of block copolymer semiconductor nanowire with spiral structure |
| CN110806429A (en) * | 2019-08-08 | 2020-02-18 | 杭州市富阳区浙工大银湖创新创业研究院 | Resistance-type flexible gas sensor with resistance compensation function in bending state and preparation method thereof |
| CN117723095A (en) * | 2024-02-08 | 2024-03-19 | 电子科技大学 | Flexible capacitance strain sensor with length of variable electrode and preparation method thereof |
| CN117723095B (en) * | 2024-02-08 | 2024-04-26 | 电子科技大学 | Flexible capacitance strain sensor with length of variable electrode and preparation method thereof |
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