CN106840483A - Carbon nano-tube/poly aniline laminated film flexible force sensitive sensor and preparation method thereof - Google Patents
Carbon nano-tube/poly aniline laminated film flexible force sensitive sensor and preparation method thereof Download PDFInfo
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- CN106840483A CN106840483A CN201710205510.6A CN201710205510A CN106840483A CN 106840483 A CN106840483 A CN 106840483A CN 201710205510 A CN201710205510 A CN 201710205510A CN 106840483 A CN106840483 A CN 106840483A
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/20—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress
- G01L1/22—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress using resistance strain gauges
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Abstract
The invention discloses carbon nano-tube/poly aniline laminated film flexible force sensitive sensor and preparation method thereof.It includes：Dimethyl silicone polymer (PDMS) insulating protective layer and metal interdigital electrode flexible substrates on the upper and lower surface of carbon nano-tube/poly aniline laminated film；Insulating protective layer is attached to carbon nano-tube/poly aniline laminated film upper surface；Interdigital electrode flexible substrates are located at below carbon nano-tube/poly aniline laminated film；Interdigital electrode flexible substrates and carbon nano-tube/poly aniline laminated film constitute the quick unit of flexible force sensitive sensor power.The features such as carbon nano-tube/poly aniline laminated film has good, reproducible pliability, stable performance and long service life in the flexible force sensitive sensor.
Description
Technical field
The invention belongs to nanometer technology and field of sensing technologies, more particularly to a kind of carbon nano-tube/poly aniline laminated film
Flexible force sensitive sensor and preparation method.
Background technology
Flexible sensor is because have excellent bendability and unrestricted with testee face shaping, and wide
General application.Flexible force sensitive sensor is mainly used in the measurement of shearing force and extruding force.In conductive material, polyaniline is due to original
The advantages of expecting simple cheap, synthesis, good environment temperature, high temperature resistant and good conductance and physical and chemical performance,
By the widely studied of researcher and application.CNT has also been opened up because of its superior mechanics, electricity and chemical property
Open globalization research.Application of the composite of research and development CNT and polyaniline on force-sensing sensor, design one
Kind of polyaniline and the composite of CNT its resistance can occur the sensor of significant change with the change of stress degree,
With good significance of scientific research and application prospect.Existing flexible force sensitive sensor utilizes CNT/non-conductive polymer (two
Methylsiloxane or SBS) as force-sensitive material (application number
201010260505.3), such composite is mainly, using carbon nanotube conducting as signal transmission, unavoidably to occur
The problems such as conduction time delay, stability difference, these shortcomings limit the quick conductive material of non-conductive polymer power in high-performance flexible power
Application on dependent sensor.
The content of the invention
Regarding to the issue above, the present invention is in order to avoid CNT/non-conductive polymer (dimethyl siloxane or benzene second
Alkene-butadiene-styrene block copolymer) deficiency existing for force-sensing sensor, there is provided one kind is based on carbon nano-tube/poly aniline
Laminated film flexible force sensitive sensor and preparation method, with pliability is good, reproducible, the spy such as stable performance and long service life
Point.
To achieve the above object, the present invention takes following technical scheme：
The present invention provides carbon nano-tube/poly aniline laminated film flexible force sensitive sensor, and it includes：
(1) carbon nano-tube/poly aniline laminated film；
(2) dimethyl silicone polymer (PDMS) insulating protective layer of carbon nano-tube/poly aniline laminated film upper surface；
(3) carbon nano-tube/poly aniline laminated film lower surface Ti-Au interdigital electrode flexible substrates.
The Ti-Au interdigital electrodes be direct plating on a flexible substrate, the part and carbon nano-tube/poly aniline THIN COMPOSITE
Film constitutes the quick unit of power of flexible force sensitive sensor；It is characterized in that：
The carbon nano-tube/poly aniline laminated film is evenly coated on CNT for polyaniline, the composite wood of formation
The film that material is made；
The flexible base material is polyimides (PI).
Described carbon nano-tube/poly aniline laminated film flexible force sensitive sensor, it is characterised in that described CNT
It is carboxylated SWCN or functionalized multi-wall carbonnanotubes.
The carbon nano-tube/poly aniline laminated film flexible force sensitive sensor preparation method that the present invention is provided, its step is as follows：
1) metal interdigital electrode flexible substrates manufacture craft is used, carbon nano-tube/poly aniline laminated film lower surface is made
Metal interdigital electrode flexible substrates, the thickness is 75~150 μm of flexible polyimide (PI) substrate oxygen plasma treatment,
Design parameter：Vacuum 0.1Pa, is passed through oxygen, and 10~20sccm of oxygen flow makes operating pressure reach 20~120Pa, radio frequency
60~100W of power, processes 5min at room temperature；
2) design such as Fig. 2 interdigital electrodes, the 100 μm of metallic tines in interval are plated using photoetching technique in polyimides (PI) substrate
Refer to electrode.Design parameter is as follows, uv-exposure parameter：110 DEG C of front baking 3min of AZ5214 glue, expose 1s, and 2min is dried after 120 DEG C,
Exposure 20s, develop 1min；Electron beam evaporation plating parameter：Vacuum 5 × 10-6Mbar, Ti, Au thickness are respectively 10nm, 100nm；
3) carbon nano tube dispersion liquid：20mg CNTs are taken, concentrated nitric acid and 27mL that 9mL mass fractions are 68% is dispersed in
During mass fraction is 98% concentrated sulfuric acid, 45~90min are stirred in 110 DEG C of oil baths, and CNT is washed till into neutrality, dried carbon
Nanotube is made into 0.2mg/mL mixed liquors, is added in mixed liquor also comprising neopelex, neopelex
SDBS mass is the 1% of mixed liquor solution quality, and in 30~60min of 300W ultrasonic disperses；
4) 60mg ammonium persulfates (APS) is added in 40mL concentration is for the HCl of 1mol/L, adds 300 μ L steps 3) system
Standby concentration is 0.2mg/mL CNT mixed liquors, and ultrasound 5~30 minutes stirs 20min, is eventually adding 43 μ L benzene at 5 DEG C
Amine, controlling reaction temperature stirs 3~12h at 5 DEG C, that is, be made the composite of carbon nano-tube/poly aniline；
5) in step 2) in the interdigital flexible substrates that prepare, composite in 4) is uniformly coated with spraying process, at room temperature
Dry；After solvent volatilizees completely, in interdigital flexible electrode 2) on to form uniform carbon nano-tube/poly aniline composite thin
Film；The carbon nano-tube/poly aniline composite material film controls 100~200 μm of thickness；
6) in step 5) one strata dimethyl siloxane of uniform coating on carbon nano-tube/poly aniline composite material film
(PDMS) insulating protective layer, resulting carbon nano-tube/poly aniline laminated film flexible force sensitive sensor.
Operation principle of the invention is：Carbon nano-tube/poly aniline film lower surface arrangement interdigital electrode flexible substrates are constituted
The quick unit of power of force-sensing sensor；Carbon nano-tube/poly aniline film upper surface coats one layer of insulating protective layer；Sensor surface
Pressure transmission on carbon nano-tube/poly aniline film when, contact condition between carbon nano-tube/poly aniline composite and
Gap changes therewith, causes composite material resistance to change；Can just be reflected by the size for measuring interdigital electrode two ends resistance
Go out the size of pressure.
Electrode is made up of metal interdigital electrode in the present invention, can be using the soft of standard with attachment insulating protective layer thereon
Property circuit-board processes make.
Carbon nano-tube/poly aniline composite is prepared using in-situ polymerization in the present invention.CNT can select carboxylic
Base SWCN or functionalized multi-wall carbonnanotubes, the raw material of synthesized polyaniline is aniline.Carbon nano-tube/poly aniline is answered
The principle of conjunction is to ensure that CNT is uniformly dispersed in synthetic system.
The preparation process of carbon nano-tube/poly aniline composite membrane is：20mg CNTs are taken, 9mL mass point is dispersed in
Number is in 68% concentrated nitric acid and the concentrated sulfuric acid that 27mL mass fractions are 98%, 45min are stirred in 110 DEG C of oil baths, by CNT
Neutrality is washed till, dried CNT is made into 0.2mg/mL mixed liquors, is added in mixed liquor also comprising DBSA
Sodium, neopelex SDBS mass is the 1% of mixed liquor solution quality, and in 300~1000W ultrasonic disperses 30~60
Minute；40mL concentration for 1mol/L HCl in add 60mg ammonium persulfates (APS), add 300 μ L steps 3) prepare it is dense
It is 0.2mg/mL CNT mixed liquors to spend, ultrasound 5~30 minutes, and 20min is stirred at 5 DEG C, is eventually adding 43 μ L aniline, is controlled
Reaction temperature stirs 3~12h at 5 DEG C, that is, be made the composite of polyaniline and CNT.With spraying process by composite
It is coated uniformly in interdigital flexible substrates, dries at room temperature；After solvent volatilizees completely, the shape on the interdigital flexible electrodes of Ti-Au
Into uniform carbon nano-tube/poly aniline composite material film.
The one strata dimethyl silica of uniform coating on the above-mentioned carbon nano-tube/poly aniline composite material film surface being made
Alkane (PDMS) insulating protective layer, resulting carbon nano-tube/poly aniline laminated film flexible force sensitive sensor.
Excellent effect of the invention is：In conductive material, polyaniline has that raw material is cheap, synthesis is simple, environment temperature
The advantages of good, high temperature resistant of property and good conductance and physical and chemical performance；CNT have superior mechanics, electricity and
Chemical property；CNT is prepared using in-situ polymerization and the composite of polyaniline its resistance can be with the change of stress degree
And there is significant change；The composite of CNT and polyaniline has good flexility；Carbon nano-tube/poly aniline is answered
Mutual distance between condensation material can change with material strain, and carbon nano-tube/poly aniline composite will not be made because of pressure
With and damage, thus force-sensitive property shows significant stability；By repeated ultrasonic decentralized processing, CNT is in whole body
It is uniformly dispersed in system, it is compound with polyaniline good.
2V constant voltages are passed through in test process, after after the resistance stabilization of force-sensing sensor, in the middle of flexible sensor
Position quickly applies pressure bends it, then removes pressure, after it is restored to the original state, more than quick repetition acts again several
Cycle, while the curent change on monitoring computer, draws electric current and the change curve of time, such as Fig. 4.As can be seen from the figure
By the bending after stress, electric current there occurs obvious change to flexible sensor, and peaking can be arrived in 0.03s.
Brief description of the drawings
Fig. 1 flexible force sensitive sensor generalized sections, including dimethyl silicone polymer (PDMS) insulating protective layer 1,
Carbon nano-tube/poly aniline composite material film 2 is interdigital electrode position, metal interdigital electrode 3, PI flexible substrates 4.
Fig. 2 flexible force sensitive sensor interdigitated electrode structure schematic diagrames.
Fig. 3 sensing material scanning electron microscope (SEM) photographs
The quick response curve of Fig. 4 power
Fig. 5 bend tests influence on sensitivities
Specific embodiment
It is described further below by embodiment and with reference to accompanying drawing.
Embodiment 1：
1) Ti-Au metal interdigital electrode flexible substrates manufacture crafts are used, is made under carbon nano-tube/poly aniline laminated film
Surface 50nm thick Ti-Au metal interdigital electrode flexible substrates, the thickness is 75 μm of flexible polyimide (PI) substrate oxygen
Corona treatment, design parameter：Vacuum 0.1Pa, is passed through oxygen, and oxygen flow 10sccm makes operating pressure reach 20Pa,
Radio-frequency power 60W, processes 5min at room temperature；
2) design such as Fig. 2 interdigital electrodes, the 100 μm of metallic tines in interval are plated using photoetching technique in polyimides (PI) substrate
Refer to electrode.Design parameter is as follows, uv-exposure parameter：110 DEG C of front baking 3min of AZ5214 glue, expose 1s, and 2min is dried after 120 DEG C,
Exposure 20s, develop 1min；Electron beam evaporation plating parameter：Vacuum 5 × 10-6Mbar, Ti, Au thickness are respectively 10nm, 100nm；
3) carbon nano tube dispersion liquid：20mg CNTs are taken, concentrated nitric acid and 27mL that 9mL mass fractions are 65% is dispersed in
During mass fraction is 98% concentrated sulfuric acid, 45min are stirred in 110 DEG C of oil baths, and CNT is washed till into neutrality, dried carbon nanometer
Pipe is made into 0.2mg/mL mixed liquors, is added in mixed liquor also comprising neopelex, neopelex SDBS
Quality is the 1% of mixed liquor solution quality, and in 300W ultrasonic disperses 30 minutes；
4) 60mg ammonium persulfates (APS) is added in 40mL concentration is for the HCl of 1mol/L, adds 300 μ L steps 3) system
Standby concentration is 0.2mg/mL CNT mixed liquors, and ultrasound 10 minutes stirs 20min, is eventually adding 43 μ L aniline at 5 DEG C,
Controlling reaction temperature stirs 8h at 5 DEG C, that is, be made the composite of polyaniline and CNT；
5) in step 2) in the metal interdigital electrode flexible substrates that prepare, composite in 4) is uniformly applied with spraying process
Cover, dry at room temperature；After solvent volatilizees completely, in interdigital flexible electrode 2) on formed uniform carbon nano-tube/poly aniline answer
Condensation material film；The carbon nano-tube/poly aniline composite material film controls 150 μm of thickness；
6) in step 5) one strata dimethyl siloxane of uniform coating on carbon nano-tube/poly aniline composite material film
(PDMS) insulating protective layer, resulting carbon nano-tube/poly aniline laminated film flexible force sensitive sensor.
Embodiment 2：
1) Al metal interdigital electrode flexible substrates manufacture crafts are used, carbon nano-tube/poly aniline laminated film following table is made
Face 200nm thick Al metal interdigital electrode flexible substrates, the thickness be 75 μm of flexible polyimide (PI) substrate oxygen etc. from
Daughter is processed, design parameter：Vacuum 0.1Pa, is passed through oxygen, and oxygen flow 10sccm makes operating pressure reach 20Pa, radio frequency
Power 60W, processes 5min at room temperature；
2) design such as Fig. 2 interdigital electrodes, the 100 μm of metallic tines in interval are plated using photoetching technique in polyimides (PI) substrate
Refer to electrode.Design parameter is as follows, uv-exposure parameter：110 DEG C of front baking 3min of AZ5214 glue, expose 1s, and 2min is dried after 120 DEG C,
Exposure 20s, develop 1min；Electron beam evaporation plating parameter：Vacuum 5 × 10-6Mbar, Ti, Au thickness are respectively 10nm, 100nm；
3) carbon nano tube dispersion liquid：20mg CNTs are taken, concentrated nitric acid and 27mL that 9mL mass fractions are 65% is dispersed in
During mass fraction is 98% concentrated sulfuric acid, 45min are stirred in 110 DEG C of oil baths, and CNT is washed till into neutrality, dried carbon nanometer
Pipe is made into 0.2mg/mL mixed liquors, is added in mixed liquor also comprising neopelex, neopelex SDBS
Quality is the 1% of mixed liquor solution quality, and in 300W ultrasonic disperses 30 minutes；
4) 60mg ammonium persulfates (APS) is added in 40mL concentration is for the HCl of 1mol/L, adds 300 μ L steps 3) system
Standby concentration is 0.2mg/mL CNT mixed liquors, and ultrasound 10 minutes stirs 20min, is eventually adding 43 μ L aniline at 5 DEG C,
Controlling reaction temperature stirs 8h at 5 DEG C, that is, be made the composite of polyaniline and CNT；
5) in step 2) in the metal interdigital electrode flexible substrates that prepare, composite in 4) is uniformly applied with spraying process
Cover, dry at room temperature；After solvent volatilizees completely, in interdigital flexible electrode 2) on formed uniform carbon nano-tube/poly aniline answer
Condensation material film；The carbon nano-tube/poly aniline composite material film controls 150 μm of thickness；
6) in step 5) one strata dimethyl siloxane of uniform coating on carbon nano-tube/poly aniline composite material film
(PDMS) insulating protective layer, resulting carbon nano-tube/poly aniline laminated film flexible force sensitive sensor.
2V constant voltages are passed through in test process, after after the resistance stabilization of force-sensing sensor, in the middle of flexible sensor
Position quickly applies pressure bends it, then removes pressure, after it is restored to the original state, more than quick repetition acts again several
Cycle, while the curent change on monitoring computer, draws electric current and the change curve of time, such as Fig. 4.As can be seen from the figure
By the bending after stress, electric current there occurs obvious change to flexible sensor, and peaking can be arrived in 0.03s.Implement above
Example is attained by similar effect.
Above-described embodiment is only preferrred embodiment of the present invention, and embodiments of the present invention are not arranged by above-mentioned implementation case
Limitation, every equivalents carried out on the basis of technical solution of the present invention and improvement should not be excluded of the invention
Outside protection domain.
Claims (3)
1. a kind of carbon nano-tube/poly aniline laminated film flexible force sensitive sensor, it is characterised in that include：
(1) carbon nano-tube/poly aniline laminated film；
(2) carbon nano-tube/poly aniline laminated film upper surface polydimethylsiloxane insulating protective layer；
(3) carbon nano-tube/poly aniline laminated film lower surface metal interdigital electrode flexible substrates；
The metal interdigital electrode be direct plating on a flexible substrate, the part and carbon nano-tube/poly aniline laminated film structure
Into the quick unit of power of flexible force sensitive sensor；
The composite that the carbon nano-tube/poly aniline laminated film is formed by polyaniline is evenly coated on CNT is made
Film；Described CNT is carboxylated SWCN or functionalized multi-wall carbonnanotubes.
2. the carbon nano-tube/poly aniline laminated film flexible force sensitive sensor according to claim 1, it is characterised in that
The flexible base material is polyimides.
3. the method for preparing carbon nano-tube/poly aniline laminated film flexible force sensitive sensor as claimed in claim 1 or 2, it is special
Levy and be, step is as follows：
1) metal interdigital electrode flexible substrates manufacture craft is used, carbon nano-tube/poly aniline laminated film lower surface metal is made
Interdigital electrode flexible substrates, the thickness is 75~150 μm of flexible substrates oxygen plasma treatment, design parameter：Vacuum
0.1Pa, is passed through oxygen, and 10~20sccm of oxygen flow makes operating pressure reach 20~120Pa, 60~100W of radio-frequency power, room
The lower treatment 5min of temperature；
2) the 100 μm of Ti-Au interdigital electrodes in interval are plated in flexible substrates using photoetching technique；Design parameter is as follows, uv-exposure
Parameter：110 DEG C of front baking 3min of AZ5214 glue, expose 1s, and 2min is dried after 120 DEG C, expose 20s, and develop 1min；Electron beam evaporation plating is joined
Number：Vacuum 5 × 10-6Mbar, metal electrode thickness is 50nm-200nm；
3) carbon nano tube dispersion liquid：20mg CNTs are taken, concentrated nitric acid and 27mL mass that 9mL mass fractions are 68% is dispersed in
During fraction is 98% concentrated sulfuric acid, 45~90min are stirred in 110 DEG C of oil baths, and CNT is washed till into neutrality, dried carbon nanometer
Pipe is made into 0.2mg/mL mixed liquors, and neopelex, neopelex SDBS mass are also included in mixed liquor
It is the 1% of mixed liquor quality, and in 300~1000W ultrasonic disperses 30~60 minutes；
4) 40mL concentration for 1mol/L HCl in add 60mg ammonium persulfates, add 300 μ L steps 3) prepare concentration be
0.2mg/mL CNT mixed liquors, ultrasound 5~30 minutes stirs 20min at 5 DEG C, is eventually adding 43 μ L aniline, control reaction
Temperature stirs 3~12h at 5 DEG C, that is, be made the composite of carbon nano-tube/poly aniline；
5) in step 2) in the metal interdigital electrode flexible substrates that prepare, composite in 4) is uniformly coated with spraying process, room
The lower drying of temperature；After solvent volatilizees completely, in interdigital flexible electrode 2) on form uniform carbon nano-tube/poly aniline composite
Film；The carbon nano-tube/poly aniline composite material film thickness control is at 100~200 μm；
6) in step 5) one layer of polydimethylsiloxane insulation of uniform coating on carbon nano-tube/poly aniline composite material film
Protective layer, resulting carbon nano-tube/poly aniline laminated film flexible force sensitive sensor.
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| CN110608825B (en) * | 2019-09-12 | 2021-08-20 | 复旦大学 | Flexible pressure sensor based on polyimide substrate microstructure and preparation method thereof |
| CN110608825A (en) * | 2019-09-12 | 2019-12-24 | 复旦大学 | Flexible pressure sensor based on polyimide substrate microstructure and preparation method thereof |
| CN111307204A (en) * | 2019-11-28 | 2020-06-19 | 杭州电子科技大学 | Flexible multifunctional sensor |
| CN111055554A (en) * | 2019-12-31 | 2020-04-24 | 苏州能斯达电子科技有限公司 | Novel flexible intelligent fabric sensor and manufacturing method thereof |
| CN114152359A (en) * | 2020-09-08 | 2022-03-08 | 哈尔滨理工大学 | Flexible temperature sensor and preparation method thereof |
| CN112697317A (en) * | 2020-12-15 | 2021-04-23 | 嘉兴学院 | Flexible pressure sensor with high sensitivity and wide range and preparation method thereof |
| WO2022236768A1 (en) * | 2021-05-08 | 2022-11-17 | 中国科学院深圳先进技术研究院 | Flexible temperature sensor based on composite material and preparation method therefor and application thereof |
| CN114088258A (en) * | 2021-11-18 | 2022-02-25 | 建木柔电(深圳)智能设备有限公司 | Flexible pressure sensor containing CNT (carbon nanotube) composite organic material and preparation method thereof |
| CN114354029A (en) * | 2022-01-10 | 2022-04-15 | 北京航空航天大学 | Preparation method of flexible carbon nanotube composite film, flexible sensor and preparation method |
| CN115507979A (en) * | 2022-08-24 | 2022-12-23 | 西南交通大学 | Flexible pressure sensor based on bionic gradient microstructure and preparation method thereof |
| CN117705896A (en) * | 2024-02-04 | 2024-03-15 | 西安电子科技大学 | Flexible NO 2 Preparation method of gas sensor and sensor |
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