CN106840483B - 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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- CN106840483B CN106840483B CN201710205510.6A CN201710205510A CN106840483B CN 106840483 B CN106840483 B CN 106840483B CN 201710205510 A CN201710205510 A CN 201710205510A CN 106840483 B CN106840483 B CN 106840483B
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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 sensors and preparation method thereof.Comprising: dimethyl silicone polymer (PDMS) insulating protective layer and metal interdigital electrode flexible substrates of carbon nano-tube/poly aniline laminated film upper and lower surfaces；Insulating protective layer is attached to carbon nano-tube/poly aniline laminated film upper surface；Interdigital electrode flexible substrates are located at carbon nano-tube/poly aniline laminated film or less；Interdigital electrode flexible substrates and carbon nano-tube/poly aniline laminated film constitute the quick unit of flexible force sensitive sensor power.Carbon nano-tube/poly aniline laminated film has the characteristics that good flexibility, reproducible, performance stabilization and long service life in the flexible force sensitive sensor.
Description
Technical field
The invention belongs to nanotechnology and field of sensing technologies, in particular to a kind of carbon nano-tube/poly aniline laminated film
Flexible force sensitive sensor and preparation method.
Background technique
Flexible sensor is and wide because with excellent bendability and unrestricted with testee face shaping
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
Material is cheap, synthesis is simple, environment temperature is good, high temperature resistant and good conductivity and the advantages that physical and chemical performance,
Extensive research and application by researcher.Carbon nanotube has also been opened up because of its superior mechanics, electricity and chemical property
Open globalization research.Application of the composite material of research and development carbon nanotube and polyaniline on force-sensing sensor, design one
The sensor of significant change can occur with the variation of stress degree for kind of polyaniline and the composite material of carbon nanotube its resistance,
With good significance of scientific research and application prospect.Existing flexible force sensitive sensor utilizes carbon nanotube/non-conductive polymer (two
Methylsiloxane or Styrene-Butadiene-Styrene Block Copolymer) it is used as force-sensitive material (application number
201010260505.3), such composite material is mainly to be transmitted using carbon nanotube conducting as signal, unavoidably be will appear
The problems such as conduction is delayed, stability is poor, these disadvantages limit the quick conductive material of non-conductive polymer power in high-performance flexible power
Application on dependent sensor.
Summary of the invention
In view of the above-mentioned problems, the present invention is in order to avoid carbon nanotube/non-conductive polymer (dimethyl siloxane or benzene second
Alkene-butadiene-styrene block copolymer) deficiency present in force-sensing sensor, it provides a kind of based on carbon nano-tube/poly aniline
Laminated film flexible force sensitive sensor and preparation method, with flexibility, good, reproducible, performance is stablized special with long service life etc.
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 comprising:
(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 electrode be direct plating on a flexible substrate, the part and carbon nano-tube/poly aniline THIN COMPOSITE
The quick unit of power of film composition flexible force sensitive sensor；It is characterized by:
The carbon nano-tube/poly aniline laminated film is that polyaniline is evenly coated in carbon nanotube, the composite wood of formation
Film made of expecting；
The flexible base material is polyimides (PI).
The carbon nano-tube/poly aniline laminated film flexible force sensitive sensor, which is characterized in that the carbon nanotube
For carboxylated single-walled carbon nanotube or functionalized multi-wall carbonnanotubes.
Carbon nano-tube/poly aniline laminated film flexible force sensitive sensor preparation method provided by the invention, its step are 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, it is described with a thickness of 75~150 μm of flexible polyimide (PI) substrate oxygen plasma treatments,
Design parameter: vacuum degree 0.1Pa is passed through oxygen, and 10~20sccm of oxygen flow makes operating pressure reach 20~120Pa, radio frequency
60~100W of power, handles 5min at room temperature；
2) design such as Fig. 2 interdigital electrode plates the 100 μm of metallic tines in interval in polyimides (PI) substrate using photoetching technique
Refer to electrode.Design parameter is as follows, uv-exposure parameter: 110 DEG C of front baking 3min of AZ5214 glue, exposes 1s, dries 2min after 120 DEG C,
20s is exposed, develop 1min；Electron beam evaporation plating parameter: vacuum degree 5 × 10-6Mbar, Ti, Au thickness are respectively 10nm, 100nm；
3) carbon nano tube dispersion liquid: taking 20mg carbon nanotube, is dispersed in concentrated nitric acid and 27mL that 9mL mass fraction is 68%
In the concentrated sulfuric acid that mass fraction is 98%, 45~90min is stirred in 110 DEG C of oil baths, carbon nanotube is washed till neutrality, the carbon after drying
Nanotube is made into 0.2mg/mL mixed liquor, 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 disperse；
4) 60mg ammonium persulfate (APS) is added in the HCl that 40mL concentration is 1mol/L, adds 300 μ L steps 3) system
Standby concentration is 0.2mg/mL carbon nanotube mixed liquor, and ultrasound 5~30 minutes in 5 DEG C of stirring 20min, is eventually adding 43 μ L benzene
Amine controls reaction temperature at 5 DEG C, stirs 3~12h, that is, the composite material of carbon nano-tube/poly aniline is made；
5) in the interdigital flexible substrates of step 2) preparation, composite material in 4) is uniformly coated with spray coating method, at room temperature
It is dry；After solvent volatilizees completely, in interdigital flexible electrode 2) on to form uniform carbon nano-tube/poly aniline composite material thin
Film；The carbon nano-tube/poly aniline composite material film controls 100~200 μm of thickness；
6) a strata dimethyl siloxane is uniformly coated on step 5) carbon nano-tube/poly aniline composite material film
(PDMS) insulating protective layer, acquired carbon nano-tube/poly aniline laminated film flexible force sensitive sensor.
The operation principle of the present invention is that: 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 when being transmitted on carbon nano-tube/poly aniline film, contact condition between carbon nano-tube/poly aniline composite material and
Gap changes therewith, and composite material resistance is caused to change；Size by measuring interdigital electrode both ends resistance can reflect
The size of pressure out.
Electrode is made of metal interdigital electrode in the present invention, and the soft of standard can be used with the insulating protective layer of attachment thereon
Property circuit-board processes production.
Carbon nano-tube/poly aniline composite material is prepared using in-situ polymerization in the present invention.Carboxylic can be selected in carbon nanotube
Base single-walled carbon nanotube or functionalized multi-wall carbonnanotubes, the raw material of synthesized polyaniline are aniline.Carbon nano-tube/poly aniline is multiple
The principle of conjunction is to guarantee that carbon nanotube is uniformly dispersed in synthetic system.
The preparation process of carbon nano-tube/poly aniline composite membrane are as follows: take 20mg carbon nanotube, be dispersed in 9mL mass point
In the concentrated sulfuric acid that the concentrated nitric acid and 27mL mass fraction that number is 68% are 98%, 45min are stirred in 110 DEG C of oil baths, by carbon nanotube
It is washed till neutrality, the carbon nanotube after drying is made into 0.2mg/mL mixed liquor, is added in mixed liquor also comprising dodecyl benzene sulfonic acid
Sodium, neopelex SDBS mass are the 1% of mixed liquor solution quality, and in 300~1000W ultrasonic disperse 30~60
Minute；60mg ammonium persulfate (APS) is added in the HCl that 40mL concentration is 1mol/L, adds the dense of 300 μ L steps 3) preparation
Degree is 0.2mg/mL carbon nanotube mixed liquor, and ultrasound 5~30 minutes in 5 DEG C of stirring 20min, is eventually adding 43 μ L aniline, is controlled
Reaction temperature stirs 3~12h, that is, the composite material of polyaniline and carbon nanotube is made at 5 DEG C.With spray coating method by composite material
It is coated uniformly in interdigital flexible substrates, dries at room temperature；After solvent volatilizees completely, the shape on the interdigital flexible electrode of Ti-Au
At uniform carbon nano-tube/poly aniline composite material film.
A strata dimethyl silica is uniformly coated on above-mentioned manufactured carbon nano-tube/poly aniline composite material film surface
Alkane (PDMS) insulating protective layer, acquired carbon nano-tube/poly aniline laminated film flexible force sensitive sensor.
The excellent effect of the present invention is that: in conductive material, polyaniline has that raw material is cheap, synthesis is simple, environment temperature
The advantages that good, high temperature resistant of property and good conductivity and physical and chemical performance；Carbon nanotube have superior mechanics, electricity and
Chemical property；Carbon nanotube is prepared using in-situ polymerization and the composite material of polyaniline its resistance can be with the variation of stress degree
And significant change occurs；The composite material of carbon nanotube and polyaniline has good flexility；Carbon nano-tube/poly aniline is multiple
Mutual distance between condensation material can change with material strain, and carbon nano-tube/poly aniline composite material will not be made because of pressure
With and damage, thus force-sensitive property shows significant stability；By repeated ultrasonic decentralized processing, carbon nanotube is in entire body
It is uniformly dispersed in system, it is compound good with polyaniline.
It is passed through 2V constant voltage during the test, after the resistance stabilization of force-sensing sensor, among flexible sensor
Position fast application pressure makes its bending, then removes pressure, and after so that it is restored to the original state, it is several quickly to repeat the above movement again
Period, while the curent change on monitoring computer draw the change curve of electric current and time, such as Fig. 4.As can be seen from the figure
Flexible sensor passes through the bending after stress, and electric current has occurred apparent variation, can arrive reach to peak value in 0.03s.
Detailed description of the invention
Fig. 1 flexible force sensitive sensor diagrammatic cross-section, 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 diagram.
Fig. 3 sensing material scanning electron microscope (SEM) photograph
The quick response curve of Fig. 4 power
Fig. 5 bend test influences sensitivities
Specific embodiment
It is described further by way of example and in conjunction with the accompanying drawings.
Embodiment 1:
1) Ti-Au metal interdigital electrode flexible substrates manufacture craft is used, is made under carbon nano-tube/poly aniline laminated film
The Ti-Au metal interdigital electrode flexible substrates of surface 50nm thickness, it is described with a thickness of 75 μm of flexible polyimide (PI) substrate oxygen
Corona treatment, design parameter: vacuum degree 0.1Pa is passed through oxygen, and oxygen flow 10sccm makes operating pressure reach 20Pa,
Radio-frequency power 60W, handles 5min at room temperature；
2) design such as Fig. 2 interdigital electrode plates the 100 μm of metallic tines in interval in polyimides (PI) substrate using photoetching technique
Refer to electrode.Design parameter is as follows, uv-exposure parameter: 110 DEG C of front baking 3min of AZ5214 glue, exposes 1s, dries 2min after 120 DEG C,
20s is exposed, develop 1min；Electron beam evaporation plating parameter: vacuum degree 5 × 10-6Mbar, Ti, Au thickness are respectively 10nm, 100nm；
3) carbon nano tube dispersion liquid: taking 20mg carbon nanotube, is dispersed in concentrated nitric acid and 27mL that 9mL mass fraction is 65%
In the concentrated sulfuric acid that mass fraction is 98%, 45min is stirred in 110 DEG C of oil baths, carbon nanotube is washed till neutrality, the carbon nanometer after drying
Pipe is made into 0.2mg/mL mixed liquor, is added in mixed liquor also comprising neopelex, neopelex SDBS
Quality was the 1% of mixed liquor solution quality, and at 300W ultrasonic disperse 30 minutes；
4) 60mg ammonium persulfate (APS) is added in the HCl that 40mL concentration is 1mol/L, adds 300 μ L steps 3) system
Standby concentration is 0.2mg/mL carbon nanotube mixed liquor, and ultrasound 10 minutes in 5 DEG C of stirring 20min, is eventually adding 43 μ L aniline,
Reaction temperature is controlled at 5 DEG C, 8h is stirred, that is, the composite material of polyaniline and carbon nanotube is made；
5) in the metal interdigital electrode flexible substrates of step 2) preparation, composite material in 4) is uniformly applied with spray coating method
It covers, dries at room temperature；After solvent volatilizees completely, in interdigital flexible electrode 2) on to form uniform carbon nano-tube/poly aniline multiple
Condensation material film；The carbon nano-tube/poly aniline composite material film controls 150 μm of thickness；
6) a strata dimethyl siloxane is uniformly coated on step 5) carbon nano-tube/poly aniline composite material film
(PDMS) insulating protective layer, acquired carbon nano-tube/poly aniline laminated film flexible force sensitive sensor.
Embodiment 2:
1) Al metal interdigital electrode flexible substrates manufacture craft is used, carbon nano-tube/poly aniline laminated film following table is made
The Al metal interdigital electrode flexible substrates of face 200nm thickness, it is described with a thickness of 75 μm of flexible polyimide (PI) substrate oxygen etc. from
Daughter processing, design parameter: vacuum degree 0.1Pa is passed through oxygen, and oxygen flow 10sccm makes operating pressure reach 20Pa, radio frequency
Power 60W, handles 5min at room temperature；
2) design such as Fig. 2 interdigital electrode plates the 100 μm of metallic tines in interval in polyimides (PI) substrate using photoetching technique
Refer to electrode.Design parameter is as follows, uv-exposure parameter: 110 DEG C of front baking 3min of AZ5214 glue, exposes 1s, dries 2min after 120 DEG C,
20s is exposed, develop 1min；Electron beam evaporation plating parameter: vacuum degree 5 × 10-6Mbar, Ti, Au thickness are respectively 10nm, 100nm；
3) carbon nano tube dispersion liquid: taking 20mg carbon nanotube, is dispersed in concentrated nitric acid and 27mL that 9mL mass fraction is 65%
In the concentrated sulfuric acid that mass fraction is 98%, 45min is stirred in 110 DEG C of oil baths, carbon nanotube is washed till neutrality, the carbon nanometer after drying
Pipe is made into 0.2mg/mL mixed liquor, is added in mixed liquor also comprising neopelex, neopelex SDBS
Quality was the 1% of mixed liquor solution quality, and at 300W ultrasonic disperse 30 minutes；
4) 60mg ammonium persulfate (APS) is added in the HCl that 40mL concentration is 1mol/L, adds 300 μ L steps 3) system
Standby concentration is 0.2mg/mL carbon nanotube mixed liquor, and ultrasound 10 minutes in 5 DEG C of stirring 20min, is eventually adding 43 μ L aniline,
Reaction temperature is controlled at 5 DEG C, 8h is stirred, that is, the composite material of polyaniline and carbon nanotube is made；
5) in the metal interdigital electrode flexible substrates of step 2) preparation, composite material in 4) is uniformly applied with spray coating method
It covers, dries at room temperature；After solvent volatilizees completely, in interdigital flexible electrode 2) on to form uniform carbon nano-tube/poly aniline multiple
Condensation material film；The carbon nano-tube/poly aniline composite material film controls 150 μm of thickness；
6) a strata dimethyl siloxane is uniformly coated on step 5) carbon nano-tube/poly aniline composite material film
(PDMS) insulating protective layer, acquired carbon nano-tube/poly aniline laminated film flexible force sensitive sensor.
It is passed through 2V constant voltage during the test, after the resistance stabilization of force-sensing sensor, among flexible sensor
Position fast application pressure makes its bending, then removes pressure, and after so that it is restored to the original state, it is several quickly to repeat the above movement again
Period, while the curent change on monitoring computer draw the change curve of electric current and time, such as Fig. 4.As can be seen from the figure
Flexible sensor passes through the bending after stress, and electric current has occurred apparent variation, can arrive reach to peak value in 0.03s.It is above to implement
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 by above-mentioned implementation case column
Limitation, all equivalents and improvement carried out based on the technical solution of the present invention should not exclude of the invention
Except protection scope.
Claims (1)
1. a kind of preparation side of carbon nano-tube/poly aniline laminated film flexible force sensitive sensor
Method, the sensor includes:
(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, metal interdigital electrode flexible substrates and carbon nano-tube/poly
The quick unit of power of aniline laminated film composition flexible force sensitive sensor；
The carbon nano-tube/poly aniline laminated film is evenly coated at the composite material formed in carbon nanotube by polyaniline and is made
Film；The carbon nanotube is carboxylated single-walled carbon nanotube or functionalized multi-wall carbonnanotubes；
It is characterized in that, steps are 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, with a thickness of 75~150 μm of flexible substrates oxygen plasma treatments, design parameter: vacuum degree
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
Temperature is lower to handle 5min；
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, 2min are dried after 120 DEG C, expose 20s, and develop 1min；Electron beam evaporation plating ginseng
Number: vacuum degree 5 × 10-6Mbar, metal electrode is with a thickness of 50nm-200nm；
3) carbon nano tube dispersion liquid: taking 20mg carbon nanotube, is dispersed in concentrated nitric acid and 27mL mass that 9mL mass fraction is 68%
In the concentrated sulfuric acid that score is 98%, 45~90min is stirred in 110 DEG C of oil baths, carbon nanotube is washed till neutrality, the carbon nanometer after drying
Pipe is made into 0.2mg/mL mixed liquor, also includes neopelex, neopelex SDBS mass in mixed liquor
It is the 1% of mixed liquor quality, and at 300~1000W ultrasonic disperse 30~60 minutes；
4) 60mg ammonium persulfate is added in the HCl that 40mL concentration is 1mol/L, the concentration for adding the preparation of 300 μ L steps 3) is
0.2mg/mL carbon nanotube mixed liquor, ultrasound 5~30 minutes are eventually adding 43 μ L aniline, control reaction in 5 DEG C of stirring 20min
Temperature stirs 3~12h, that is, the composite material of carbon nano-tube/poly aniline is made at 5 DEG C；
5) in the metal interdigital electrode flexible substrates of step 2) preparation, composite material in step 4) is uniformly applied with spray coating method
It covers, dries at room temperature；After solvent volatilizees completely, uniform carbon nano-tube/poly is formed in metal interdigital electrode flexible substrates
Aniline composite material film；The carbon nano-tube/poly aniline composite material film thickness control is at 100~200 μm；
6) one layer of polydimethylsiloxane insulation is uniformly coated on step 5) carbon nano-tube/poly aniline composite material film
Protective layer obtains carbon nano-tube/poly aniline laminated film flexible force sensitive sensor.
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| 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 |
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