CN108560250A - A kind of preparation method and applications of the flexible strain transducer based on conductive fiber - Google Patents
A kind of preparation method and applications of the flexible strain transducer based on conductive fiber Download PDFInfo
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- CN108560250A CN108560250A CN201810372234.7A CN201810372234A CN108560250A CN 108560250 A CN108560250 A CN 108560250A CN 201810372234 A CN201810372234 A CN 201810372234A CN 108560250 A CN108560250 A CN 108560250A
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M11/00—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising
- D06M11/83—Treating fibres, threads, yarns, fabrics or fibrous goods made from such materials, with inorganic substances or complexes thereof; Such treatment combined with mechanical treatment, e.g. mercerising with metals; with metal-generating compounds, e.g. metal carbonyls; Reduction of metal compounds on textiles
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/02—Detecting, measuring or recording pulse, heart rate, blood pressure or blood flow; Combined pulse/heart-rate/blood pressure determination; Evaluating a cardiovascular condition not otherwise provided for, e.g. using combinations of techniques provided for in this group with electrocardiography or electroauscultation; Heart catheters for measuring blood pressure
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- D—TEXTILES; PAPER
- D06—TREATMENT OF TEXTILES OR THE LIKE; LAUNDERING; FLEXIBLE MATERIALS NOT OTHERWISE PROVIDED FOR
- D06M—TREATMENT, NOT PROVIDED FOR ELSEWHERE IN CLASS D06, OF FIBRES, THREADS, YARNS, FABRICS, FEATHERS OR FIBROUS GOODS MADE FROM SUCH MATERIALS
- D06M15/00—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment
- D06M15/19—Treating fibres, threads, yarns, fabrics, or fibrous goods made from such materials, with macromolecular compounds; Such treatment combined with mechanical treatment with synthetic macromolecular compounds
- D06M15/21—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
- D06M15/244—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons
- D06M15/256—Macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds of halogenated hydrocarbons containing fluorine
Abstract
The preparation method and applications of the present invention provides a kind of flexible strain transducer based on conductive fiber, conductive fiber by as conductive layer metal nanometer line, constitute as the electric spinning polymer nano fibrous membrane of protective layer and the elastomeric yarn as resilient support；Electrostatic spinning technique is used to coat one layer of polymeric nanofibres film on elastomeric yarn surface first in preparation process, then metal nanometer line is deposited on by multiple dip-coating on its surface texture again.The prepared flexible strain transducer based on conductive fiber has ability such as stretching, bending, the distortion of quickly detection various deformation, and its sensitivity is still maintained at 90% or more after stretching cycle-index and reaching 10,000 times；It can realize the beat pulse to human body, vocal cord vibration and more complicated multidigit point while detect that there is great application potential in terms of the intelligent wearable device such as virtual reality, man-machine interface, health monitoring.
Description
Technical field：
The invention belongs to the preparing technical fields of flexible electronic device, more particularly to one kind being based on metal nanometer line and electrospinning
The conductive fiber of polymer nanofibre film and the preparation method and application of flexible extensible strain transducer.
Background technology：
With the development of science and technology, conventional electronics will be difficult to meet the various demands of the mankind, and certainty is towards soft
Property, micromation, the directions such as wearableization develop, to break through the application range of conventional electronics, promote information and people
It organically combines.Wherein, strain transducer as it is a kind of monitoring stretch, bending, distortion etc. deformation sensor, electronic skin,
There is wide application space in the fields such as Flexible Displays, health monitoring, man-machine interface.Currently used strain gauge transducer is main
Using inorganic material as response body, but due to inorganic material lacking toughness, not resistant to bending, high deformation will be such that sensor is easy
It is damaged and can not restore.Therefore, Development of Novel can bear to be particularly important compared with the sensor of large deformation.Wherein, linearly
The electronic device of structure can not only the excellent flexibility of retainer member, and meet with stresses occur moderate finite deformation when, moreover it is possible to
The integrality of retainer member and show stable electric property.
Strain main body of the conductive fiber as linear transducer is to realize high deformability and the every sensing capabilities of monitoring
Basis.In recent years, mainly there is following method for the preparation of conductive fiber：1, directly by conductive filling material (such as graphite
Alkene, carbon nanotube, metal nanoparticle etc.) dispersion acquisition composite conducting fiber is mixed with elastomer (such as rubber polymer),
This method is simple and effective, but needs the content for being accurately controlled conductive material, and loading is too small to cause electric conductivity poor,
Loading too conference causes system hardness to increase, and elasticity is deteriorated, and when deformation is easily broken.2, using elastomeric fiber conduct
Inner core layers, electrical-conductive nanometer material are adsorbed on elastomer surface as outer conductive layers, then carry out at hydrogen plasma again
Reason is heat-treated to improve the conductivity of composite fibre.The shortcomings that this method, can not be accurately controlled to the thickness of conductive coating
The electrically conductive particles of system, fiber surface are easy to fall off by the effects that friction, to influence the Long-Term Properties of device.3, directly to
Fill elastomeric polymer in three-dimensional porous micro-nano conductive network, this method to the integrity demands of three-dimensional conductive network compared with
The conductive fiber of height, acquisition is limited by conductive network mechanical property itself, and it is usually smaller can to bear strain.
In conclusion the application for the preparation method of High-elasticity conductive fiber and its in terms of strain transducer at present is all
There are certain problems, it is necessary to develop a kind of novel high conductivity, good mechanical performance conductive fiber, with further full
The needs of sufficient practical application.
Invention content：
The purpose of the present invention is to provide a kind of conductive fibers of the high conductivity to solve the above problems and high-mechanical property
Preparation method, the strain transducer based on this conductive fiber for stretch etc. strains have stablize and quickly detection energy
Power.The variation of itself electric property is shown as by perceiving extraneous faint deformation, and then applied to the arteries and veins of monitoring human body in real time
Fight bounce etc. health status.
For achieving the above object, the present invention provides a kind of elastomeric composite conducting fiber comprising as conduction
Layer metal nanometer line, as the electric spinning polymer nano fibrous membrane of protective layer and as the elastomeric yarn of resilient support, it is described
Elastomeric yarn include double-layer structure, the polyurethane yarn of the respectively internal rubber latex thread that can bear high deformation and external cross winding
Line layer, the electric spinning polymer nano fibrous membrane are coated on the surface of the elastomeric yarn, and the metal nanometer line is heavy
Product is on the surface of electric spinning polymer nano fibrous membrane.
The preparation method of conductive fiber provided by the invention based on metal nanometer line and electric spinning polymer nano fibrous membrane,
Its specific steps are：
First, elastomeric yarn is cleaned by ultrasonic in ethyl alcohol and deionized water, is then dried；
Secondly, the elastomeric yarn of pre-stretching is fixed on the collecting board of electrostatic spinning apparatus；
Then, polybenzazole precursor liquid solution is subjected to electrostatic spinning, a strata is coated on the elastomeric yarn surface of pre-stretching
Close object nano fibrous membrane；
Finally, the dispersion liquid dip-coating of metal nanometer line is made into gold in the electric spinning polymer nanofiber film surface of pre-stretching
Belong to nanowire deposition and be adsorbed on its surface texture, so repeatedly restore the deformation of elastomeric yarn after dip-coating, you can obtains high
The conductive fiber of electrical conductance and high-mechanical property.
Preferably, the outer yarn layer of the elastomeric yarn further includes but is not limited to polyolefin in addition to polyurethane elastomeric fiber
Class elastomer or polyesters elastomer or polyethers esters elastomer and its any of the above composite elastic fiber.
Preferably, the pre-stretching degree of the elastomeric yarn is depending on the type of elastomeric yarn, wherein for polyurethane
Class elastomeric yarn, prestretching extend to 2 times of former length.
Preferably, the polybenzazole precursor liquid solution is the polymer solution that can be used directly to electrostatic spinning, the polymerization
Object includes but not limited to Kynoar, poly- (vinylidene-trifluoro-ethylene), polystyrene, polyurethane, polyimides, poly- first
The copolymer etc. of base methyl acrylate, polyethylene terephthalate, polycaprolactone and the above polymer.
Preferably, during electrostatic spinning, used spinning voltage should regard the poly- of electrospinning with the parameters such as distance are received
Depending on conjunction species, wherein voltage range used by poly- (vinylidene-trifluoro-ethylene) polymer of electrospinning is 10~15,000
Volt, it is 10~20 centimetres to receive distance.
Preferably, during electrostatic spinning, the elastomeric yarn of pre-stretching should in axial direction slowly run, and ensure electrospinning
Uniform cladding of the nano fibrous membrane on its surface.
Preferably, the duration of the electrostatic spinning process is 3~5 minutes.
Preferably, the metal nanometer line includes but not limited to that nano silver wire, nanowires of gold, copper nano-wire and its alloy are received
Rice noodles, a concentration of 1~10 milligram every milliliter in alcohol solvent of nanowire dispersion.
Preferably, in the dip coating process of metal nanometer line, the amount for coating consumed nanowire dispersion is added dropwise every time
It is per cm for 0.01~0.05 milliliter.It could be soaked next time after needing equal solvent to volatilize completely after the completion of each dip coating process
It applies.
Preferably, the resistance for the conductive fiber that the dip-coating number of metal nanometer line obtains after 5~7 times can be less than 5 Europe
Nurse is per cm.
The present invention has the characteristics that compared with prior art and advantage：(1) elastomeric yarn of the present invention has
The higher ability for adapting to deformation, increases the detectable range of strain transducer.(2) polymer prepared by method of electrostatic spinning
Nano fibrous membrane has the function of protecting internal structure, while excellent absorption carrier can also be provided for metal nanometer line.(3)
Prestretching process can be such that the external crossed yarn layer of elastomeric yarn is separated from each other, to promote electro spinning nano fiber inside it
The deposition of body structure surface and absorption.After restoring deformation, be conducive to the formation of pleated structure on the surface of electro spinning nanometer fiber membrane,
This structure can protect metal nanometer line to be not easy to be destroyed when by external stress.Meanwhile prestretching process also helps gold
Belong to infiltration and absorption of the nano wire in electro spinning nanometer fiber membrane internal structure, to form more stable conductive network.(4) institute
The strain transducer based on the conductive fiber prepared has ability such as stretching, bending, the distortion of quickly detection various deformation, and
And its sensitivity is still maintained at 90% or more after stretching cycle-index and reaching 10,000 times.(5) prepared by based on the conduction
The strain transducer of fiber has the ability of monitoring human motion in real time, can realize the beat pulse to human body, vocal cord vibration
And more complicated multidigit point detects simultaneously, in terms of the intelligent wearable device such as virtual reality, man-machine interface, health monitoring
With great application potential.
Description of the drawings：
Fig. 1：The preparation flow schematic diagram and corresponding morphology characterization of conductive fiber.(a) elastomeric yarn structural schematic diagram and its
Surface SEM morphology characterizations.(b) structural schematic diagram and its surface SEM morphology characterizations after one layer of nano fibrous membrane of electrospinning.(c) it inhales
Structural schematic diagram after attached nano silver wire and its surface SEM morphology characterizations.
Fig. 2：The morphology characterization of prepared conductive fiber cross section.
Fig. 3：The nano silver wire conductive layer and pleated structure of prepared conductive fiber surfaces.
Fig. 4：Under different dropwise addition numbers, the distribution situation of conductive fiber surfaces nano silver wire.(a) it is added dropwise primary.(b) it drips
Add three times.(c) it is added dropwise five times.
Fig. 5：Under different dropwise addition numbers, the change curve of conductive fiber resistance value.
Fig. 6：The tensile test device of conductive fiber prepared by embodiment 3 and fine from the former long conduction stretched after 50%
Tie up pictorial diagram.
Fig. 7：The change curve of conductive fiber prepared by embodiment 3 from resistance value when former long stretching 100%.
Fig. 8：When conductive fiber level of stretch prepared by embodiment 3 is 0.5%, the cycle period change curve of resistance value.
Fig. 9：Conductive fiber prepared by embodiment 3 stretches the conservation rate test curve of cycle medium sensitivity at 10,000 times.
Figure 10：Conductive fiber prepared by embodiment 3 is placed in the curve for the beat pulse tested at wrist radial artery.
Specific implementation mode：
It is described in further detail by way of example and in conjunction with the accompanying drawings.Following embodiment is in order to further illustrate this
Invention, but should not be understood as limiting the scope of the invention.
By taking nano silver wire and poly- (vinylidene-trifluoro-ethylene) polymer as an example.
Embodiment 1：
A. the cleaning of elastomeric yarn：Shown in internal structure and surface topography such as Fig. 1 (a) of elastomeric yarn, one section 5 lis are intercepted
The long elastomeric yarn of rice, is cleaned by ultrasonic 20 minutes respectively in ethyl alcohol and deionized water, be then placed in baking oven 60 degrees Celsius it is straight
To complete drying.
B. the preparation of poly- (vinylidene-trifluoro-ethylene) nanofiber：First, by 1 gram poly- (vinylidene-trifluoro-ethylene)
Be dissolved in the mixed solution of 2 grams of N-N dimethylformamides and 2 grams of acetone, be stirred at room temperature 2 hours it is uniform to precursor solution
It is transparent.Then, 1 milliliter of precursor solution is taken to start electrostatic spinning in 5 milliliters of disposable plastic needle tubings.Spinning parameter is：Electricity
10 kilovolts of pressure receives 10 centimetres of distance.
C. the cladding of nano fibrous membrane：The elastomeric yarn that prestretching is extended to 2 times of length is placed on collecting board, and edge slowly
Axial rotation, it is one layer of nano fibrous membrane so that electro spinning nano fiber is constantly uniformly deposited on the surface of elastomeric yarn and is coated,
Sedimentation time is 3 minutes, shown in internal structure and surface topography such as Fig. 1 (b) after the completion of depositing.Then by the bullet of this pre-stretching
Property yarn is vertically fixed on iron stand.
D. the absorption of nano silver wire：Take 0.2 milliliter a concentration of 5 milligrams every milliliter of nano silver wire alcohol dispersion liquid from upper and
Lower dropwise addition is on the surface of electro spinning nanometer fiber membrane.With the volatilization of ethyl alcohol, gradually deposition is adsorbed on electrospun fiber membrane to nano silver wire
Surface texture on, as shown in Fig. 1 (c).After ethyl alcohol volatilization completely, removes elastomeric yarn and restore long to original, that is, complete to prepare
Process.
Embodiment 2：
Embodiment 1 is repeated, there is following difference：During d after ethyl alcohol volatilization completely, according to the silver nanoparticle of same concentrations
Line dispersion liquid and dripping quantity repeat d processes again, so totally 3 times, you can remove elastomeric yarn and restore long to original, complete to prepare
Process.
Embodiment 3：
Embodiment 1 is repeated, there is following difference：During d after ethyl alcohol volatilization completely, according to the silver nanoparticle of same concentrations
Line dispersion liquid and dripping quantity repeat d processes again, so totally 5 times, you can remove elastomeric yarn and restore long to original, complete to prepare
Process.
Embodiment 1-3 results：As shown in Fig. 2, can be clear by the cross-sectional morphology figure of the conductive fiber prepared by embodiment 3
Tell the structure of each layer in ground.Fig. 3 be conductive fiber surfaces absorption nano silver wire and restore be pre-stretched deformation after in electricity
The pleated structure that spinning nano fibre film surface is formed.As shown in Figure 4, as the increase of number is added dropwise in nano silver wire dispersion liquid,
The nano silver wire of electrospinning fibre film surface deposition absorption is more and more.As shown in Figure 5, its resistance value of the conductive fiber thus prepared
As the increase that number is added dropwise is gradually lowered, this is because the increase of nano silver wire quantity can cause the contact between nano wire
Point increases, and conductive channel is more, to improve electric conductivity.Wherein, its resistance value of the conductive fiber of the preparation of embodiment 1 is about
6.7kΩ·cm-1, its resistance value of the conductive fiber of the preparation of embodiment 2 is about 440 Ω cm-1, the conduction of the preparation of embodiment 3
Its resistance value of fiber is about 20 Ω cm-1。
Embodiment 4：
Tensile property is tested：Two fine copper wires are adhered to the both ends of conductive fiber prepared by embodiment 3 by aluminium glue band
It is assembled into strain transducer to draw device two end electrodes.The electric property of strain transducer passes through electrochemical workstation
(CHI 760e series) measures, and measurement voltage is 1V.Its electricity under different stretch strain is tested using the stretching device in Fig. 6
The change curve of performance and the stability under cyclic tension.Wherein, sensor is stretched to required length by initial length
Then degree restores to the process of initial length to be that a stretching recycles again.
4 result of embodiment：As shown in Figure 7, the maximum tension shape of the strain transducer becomes 100%, the variation of resistance value
Increase with the increase of stretcher strain.Under 0.5% faint stretcher strain, 1.5% or so, this is inspection for the variation of resistance value
The weak signal intensity of micrometer provides possibility；Under 100% larger stretcher strain, 450% or so, this can for the variation of resistance value
Realize the detection to the moving situation of human body.As shown in figure 8, response variation of the sensor under same faint stretcher strain is quick
And stablize, show the high sensitivity and cyclical stability of the strain transducer.In addition, as shown in figure 9, being stretched at 10,000 times
After cycle, the sensitivity of device is maintained to, 90% or more, it is steady in a long-term to illustrate that the strain-responsive of the sensor has
Ability, provide potential for the further practical application of sensor.
Embodiment 5：
Human pulse monitors：Strain transducer in embodiment 4 is placed at the radial artery on human body wrist, such as Figure 10 institutes
Show, which can show that the curve of the beat pulse of tested person, and the pulse that tested person can be calculated by curve is jumped
Dynamic number is 73 times per minute.It can thus be appreciated that the strain transducer can successfully monitor the bounce situation of human pulse, Jin Ershi
Now to the real-time monitoring of every physical condition of human body.
Claims (10)
1. a kind of preparation method of the flexible strain transducer based on conductive fiber, it is characterised in that the conductive fiber includes making
Metal nanometer line for conductive layer, the electric spinning polymer nano fibrous membrane as protective layer and the elastomeric yarn as resilient support
Line, the elastomeric yarn include double-layer structure, the respectively internal rubber latex thread that can bear high deformation and external cross winding
Polyurethane yarn layer, the electric spinning polymer nano fibrous membrane are coated on the surface of the elastomeric yarn, the metal
Nanowire deposition is on the surface of electric spinning polymer nano fibrous membrane.
2. a kind of preparation method of flexible strain transducer based on conductive fiber according to claim 1, feature exist
Include the following steps in the preparation method of the conductive fiber：
First, elastomeric yarn is cleaned by ultrasonic in ethyl alcohol and deionized water, is then dried；
Secondly, the elastomeric yarn of pre-stretching is fixed on the collecting board of electrostatic spinning apparatus；
Then, polybenzazole precursor liquid solution is subjected to electrostatic spinning, one layer of polymeric is coated on the elastomeric yarn surface of pre-stretching
Nano fibrous membrane；
Finally, metal is made to receive in the electric spinning polymer nanofiber film surface of pre-stretching the dispersion liquid dip-coating of metal nanometer line
Rice noodles are deposited and are adsorbed on its surface texture, so repeatedly restore the deformation of elastomeric yarn after dip-coating, you can obtain high conductance
The conductive fiber of property and high-mechanical property.
3. a kind of preparation method of flexible strain transducer based on conductive fiber according to claim 1 or 2, feature
It is that the outer yarn layer of the elastomeric yarn further includes but is not limited to polyolefins elastomer in addition to polyurethane elastomeric fiber
Or polyesters elastomer or polyethers esters elastomer and its any of the above composite elastic fiber.
4. a kind of preparation method of flexible strain transducer based on conductive fiber according to claim 2, feature exist
It is the polymer solution that can be used directly to electrostatic spinning in the polybenzazole precursor liquid solution, the polymer includes but unlimited
In Kynoar, poly- (vinylidene-trifluoro-ethylene), polystyrene, polyurethane, polyimides, polymethyl methacrylate,
The blend of polyethylene terephthalate, polycaprolactone and the above polymer.
5. according to a kind of preparation method of the flexible strain transducer based on conductive fiber of claim 1-4 any one of them,
It is characterized in that during electrostatic spinning, used spinning voltage should polymerize species with the parameters such as distance are received depending on electrospinning
Depending on class, wherein voltage range used by poly- (vinylidene-trifluoro-ethylene) polymer of electrospinning is 10~15 kilovolts, is received
Distance is 10~20 centimetres.
6. according to a kind of preparation method of the flexible strain transducer based on conductive fiber of claim 1-5 any one of them,
It is characterized in that during electrostatic spinning, the elastomeric yarn of pre-stretching should in axial direction slowly run, and ensure electrospinning polymerization
Uniform cladding of the object nano fibrous membrane on its surface；Preferably, the duration of the electrostatic spinning process is 3~5 minutes.
7. according to a kind of preparation method of the flexible strain transducer based on conductive fiber of claim 1-6 any one of them,
It is characterized in that metal nanometer line includes but not limited to nano silver wire, nanowires of gold, copper nano-wire and its alloy nano-wire, nanometer
A concentration of 1~10 milligram every milliliter in alcohol solvent of line dispersion liquid.
8. a kind of preparation method of flexible strain transducer based on conductive fiber according to claim 1 or 2, feature
It is in the dip coating process of metal nanometer line, it is 0.01~0.05 to be added dropwise coat the amount of consumed nanowire dispersion every time
Milliliter is per cm, and dip-coating next time could be carried out after needing equal solvent to volatilize completely after the completion of each dip coating process；Preferably, metal
The resistance for the conductive fiber that the dip-coating number of nano wire obtains after 5~7 times can be less than 5 Ohms per centimeters.
9. the flexible strain sensing utensil based on conductive fiber that a kind of preparation method by described in claim 1-8 is prepared
Such as stretching, bending, the distortion of the ability of standby quickly detection various deformation, and its is sensitive after stretching cycle-index and reaching 10,000 times
Degree is still maintained at 90% or more.
10. a kind of flexible strain transducer based on conductive fiber described in claim 9 shakes in beat pulse, the vocal cords of human body
The application that dynamic and more complicated multidigit point detects simultaneously, being included in the intelligence such as virtual reality, man-machine interface, health monitoring can
Application in terms of wearable device.
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