CN108877996A - The method for preparing the flexible electronic device of highly conductive, selfreparing and tensility - Google Patents
The method for preparing the flexible electronic device of highly conductive, selfreparing and tensility Download PDFInfo
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- CN108877996A CN108877996A CN201810717363.5A CN201810717363A CN108877996A CN 108877996 A CN108877996 A CN 108877996A CN 201810717363 A CN201810717363 A CN 201810717363A CN 108877996 A CN108877996 A CN 108877996A
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- tensility
- selfreparing
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B5/00—Non-insulated conductors or conductive bodies characterised by their form
- H01B5/14—Non-insulated conductors or conductive bodies characterised by their form comprising conductive layers or films on insulating-supports
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01B—CABLES; CONDUCTORS; INSULATORS; SELECTION OF MATERIALS FOR THEIR CONDUCTIVE, INSULATING OR DIELECTRIC PROPERTIES
- H01B13/00—Apparatus or processes specially adapted for manufacturing conductors or cables
- H01B13/0026—Apparatus for manufacturing conducting or semi-conducting layers, e.g. deposition of metal
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Abstract
The present invention relates to a kind of methods of flexible electronic device for preparing highly conductive, selfreparing and tensility, belong to conductive elastomeric material field.Method includes：Using acrylic amides such as acrylic acid -2- methoxy acrylate and n-isopropyl acrylamide as monomer, the elastomeric material for having self-repairability, high stretch, surface tackiness high using the method preparation of bulk polymerization is used as elastomeric substrate；Substrate is done with the graphene oxide dispersion that Hummers method is prepared, graphene oxide membrane is prepared using the method for room temperature self assembly, then the oxidation graphene film with high conductivity is reduced by hydrogen iodide.After tensile elasticity body substrate to certain length, oxidation graphene film is affixed directly in elastomeric substrate, preparation can be used for the conductive material of flexible sensing.Duplicature conductive elastomeric material of the invention has tensility, high conductivity, room temperature self-repairability and sensitivities.The method of the present invention is simple to operation and is easy to scale use, is conducive to promote.
Description
Technical field
The present invention relates to a kind of methods of flexible electronic device for preparing highly conductive, selfreparing and tensility, belong to and lead
Electric elastomeric material field.
Background technique
Self-repairability and tensility are property required for next-generation wearable electronic, and as conductive elastomer
The most basic component part of material.Due to elastomeric material to the self-healing properties of conductive elastomeric material and tensile property at
Function exploitation plays a key effect, and is currently in the study frontier in conductive elastomeric material field.Early stage prepare conductive, selfreparing and
The main method of the flexible electronic device of tensility is to mix conductive materials (such as graphene, carbon nanotube, conducting polymer)
Enter into the elastomeric material with self-repairability, the two carries out compound conductive, self-repairability and the draftability of preparing
Material is used to prepare flexible electronic device.But the material conductivity that this method is prepared is not high, and preparation complexity cannot expire
The many practical application requests of foot.In addition there are preparation have draftability and self-repairability elastomer thin film material, with deposition or
Conductive material (such as silver nanowires metal material) is attached in selfreparing elastomeric substrate by the method for coating.But this method
Condition requires strictly, and draftability is limited, and durability is poor, limits the possibility of its large-scale production.And it is polymerize with self-repairability
Object material prepares the double membrane structure of ripple struction as base material, in the method that its surface assigns one layer conductive film, energy
It is enough that provide, one kind simply preparing highly conductive, selfreparing draftability and the flexible electronic device of high stretch provides possibility.
Summary of the invention
The purpose of the present invention is there is the deficiency in self-repairability and tensility conductive material method for existing preparation,
A kind of method of flexible electronic device for simply preparing highly conductive, selfreparing and tensility is provided, this method has with surface
The esters of acrylic acid self-repairability polymer material of viscosity is substrate, and by it, one layer of surface mount highly conductive in a stretched state
Oxidation graphene film is as conductive layer, so that the conduction material with highly conductive, selfreparing and tensility be prepared
Material.
The purpose of the present invention is what is be achieved through the following technical solutions.
A method of the flexible electronic device of highly conductive, selfreparing and tensility being prepared, specific step is as follows：
Step 1: preparation graphene oxide solution, graphene oxide solution concentration is 3-10mg/ml, adjusts pH value and is adjusted to
10；Graphene oxide solution is placed in culture dish.Configured solution is prepared into oxidation stone in the method for room temperature self assembly
Black alkene film.Graphene oxide film passes through hydrogen iodide solution reduction at room temperature and obtains highly conductive, surfacing oxygen reduction
The thin film of graphite；
Step 2: acrylic acid -2- methoxy acrylate (MEA), amides olefinic monomer and initiator are uniformly mixed, then
It is circulated into polytetrafluoroethylene (PTFE) board mold, surface is prepared by the method heating initiation of bulk polymerization and has sticking review one's lessons by oneself
The acrylic polymer elastomeric material of multiple high stretch.The amides olefinic monomer includes：N- isopropyl acrylamide
Amine (NIPAM) or N- methoxy -2- methyl -2- acrylamide (MMP) or hydroxymethyl acrylamide (HAM) or N, N- diformazan
Base acrylamide (DMAA)；
Step 3: after the polymer elastomer material that step 2 is prepared stretches, then the reduction that step 1 is obtained
The thin film tiling of graphite oxide obtains the flexible electrical with highly conductive, selfreparing and tensility to after above, discharging stress
Sub- device.
5-30 μm of reduction-oxidation graphite thin film thickness described in step 1.
More's ratio of acrylic acid -2- methoxy acrylate described in step 2 and amides olefinic monomer is 9:1~7:It is any in 3
Value.
Initiator described in step 2 is benzoyl peroxide, benzoyl peroxide or methyl ethyl ketone peroxide；It is described
Initiator content is any in acrylic acid -2- methoxy acrylate (MEA) and the 0.5%-1.2% of amides olefinic monomer gross mass
Value.
Reaction temperature in the method for bulk polymerization described in step 2 is 60 DEG C, polymerization time 6-24 hours.
Polymer elastomer material described in step 2 with a thickness of 0.5-2mm.
The application of the flexible electronic device with highly conductive, selfreparing and tensility is conductor material, sensor
Part or flexible electronic skin.
Beneficial effect
1) mechanical performance that the elastomeric material being prepared has had adapts to various forms of mechanical strain behaviors；
The adhesiveness having had can be combined with conductive film；Have excellent self-healing properties, can resistant to mechanical damage, improve use the longevity
Life.
2) the thin film of reduction-oxidation graphite restored by the method for room temperature self assembly and physics is as conductive layer, energy
It is enough to be combined well with elastomeric substrate, and electric conductivity height, surfacing, durability are good.
3) the ripple struction bilayer membrane material of the redox graphene film based on monolith, which has, resists conductive fault rupture
Performance.
4) the method for the present invention is simple to operation and is easy to scale use, is conducive to promote.
Detailed description of the invention
Fig. 1 is embodiment 1 with acrylic acid -2- methoxy acrylate (MEA) and n-isopropyl acrylamide (NIPAM) for monomer
After the elastomer base material pre-stretching respectively 100%, 200% and 300% being prepared, with the graphene with a thickness of 20 μm
The comparative example scanning electron microscope diagram (SEM) for the conducting bilayer membrane material that film preparation obtains；
Fig. 2 is that the conducting bilayer membrane material elongation strain prepared in the embodiment of the present application 1 is 100%, 200% and 300%
Comparative example cyclic tension figure；,
Fig. 3 is the conducting bilayer under 100%, 200% and 300% stretch rate of comparative example prepared in present application example 1
The relative change rate of electric conductivity under the elongation strain of film；
Fig. 4 is the stretching resistance cyclical stability figure of the conducting bilayer membrane material prepared in the embodiment of the present application 1；
Fig. 5 is the scanning electron microscope diagram before and after the conducting bilayer membrane material selfreparing prepared in the embodiment of the present application 1
With electrically conductive drawn linearity curve after selfreparing；
Fig. 6 is the sensing curve graph of the conducting bilayer membrane material response digital flexion prepared in the embodiment of the present application 1.
Specific embodiment
In order to make the foregoing objectives, features and advantages of the present invention clearer and more comprehensible, with reference to the accompanying drawing with specific reality
Applying mode, the present invention will be further described in detail.
Embodiment 1
Step 1: the graphene oxide solution of configuration 7mg/ml, adjusts PH=10 and stirs evenly, pour into room in culture dish
Temperature dries into graphene oxide membrane, the dilute film of graphite oxide is immersed in the HI solution that content is 46% after restoring 12h, clear with ethyl alcohol
It washes 5 times and obtains the thin film of reduction-oxidation graphite；
Step 2: the monomer ratio of configuration acrylic acid -2- methoxy acrylate (MEA) and n-isopropyl acrylamide (NIPAM)
It is 7:The benzoyl peroxide of MEA and NIPAM gross mass 0.7% is added as initiator, after magnetic agitation is uniform in 3 solution
It is injected into the mold that polyfluortetraethylene plate is made into, 12 hours of polymerization obtain a kind of esters of acrylic acid bullet under conditions of 60 DEG C
Elastomer material (is named as M7N3)；It prepares one big elastomeric material of three materials or preparation and is cut into four small materials
Material is used for the use of step 3.
Step 3: by the above-mentioned elastomer M being prepared7N3It is stretched to 50%, 100%, 200% and 300%, will be restored
The thin film of graphite oxide is laid in pressing decurl above (if needing stronger knot in graphene film and elastomeric substrate
The conjunction is suitably pasted with binder), final conducting bilayer membrane material is obtained after discharging stress.
Detection and data description are carried out to substance
1), 50%, 100%, 200% is respectively provided with to what embodiment (embodiment 1) was prepared with scanning electron microscope
It is tested with the surface texture of the duplicature elastomer of 300% elongation strain.As shown in Figure 1：With initial elasticity body material
The trend increased to concentration is presented in the increase of elongation strain, the ripple struction on surface.
2) electronics universal material testing, is used as a comparison case to the conducting bilayer membrane material for the different stretch ratio being prepared
Machine carries out cyclic tension test, tensile speed 5mm/min.As shown in Figure 2：With the increase of stretching ratio, material have compared with
Small stretching hysteresis loop, illustrate conducting bilayer membrane material have stable stretching cyclicity, it is sustainable carry out using.
3), to the comparative example being prepared with digital four-point probe test its during stretching electric conductivity with
The opposite variation of elongation strain.As shown in Figure 3：100%, 200% and 300% conducting bilayer membrane material of preparation was stretching
Electric conductivity variation is relatively stable in journey, but the changes in material rate of different stretch ratio is also different, as the increase of draw ratio is presented
The trend of increase.
4) it, is tested in the electricity of drawing process with digital four-point probe to the conducting bilayer membrane material being prepared
Resistive, variation of the test material in original state and 20 cyclic process resistance being stretched under 300% state.Such as Fig. 4 institute
Show：In 20 stretching cyclic processes, for resistance in original state and stretching 300%, the changing value of resistance is more stable, explanation
Conducting bilayer membrane material has stable stretching electric conductivity.
5) after, cutting off the conducting bilayer membrane material being prepared with blade, incision is reapposed together, and room temperature is put
After setting 2h, surface texture at anteroposterior incision is repaired with scanning electron microscope test material, and test and repair post-tensioning process
Electric conductivity variation.As shown in Figure 5：Conductive layer links together well after reparation, and conductive elastomeric material stretches after repair
Still there is good electric conductivity when to 120%.
6) the double-deck membrane material being prepared, is prepared into simple sensing flexible electronic device, is fixed on finger, benefit
With electrochemical workstation measure digital flexion during, electric current with the time change curve.As shown in Figure 6:In bend cycles
Curent change is stablized in the process, illustrates that the material can be applied to flexible electronic skin, sensing material and artificial software driver
Equal fields.
Embodiment 2
Step 1: the graphene oxide solution of configuration 6mg/ml, adjusts PH=10 and stirs evenly, pour into room in culture dish
Temperature dries into graphene oxide membrane, the dilute film of graphite oxide is immersed in the HI solution that content is 46% after restoring 12h, clear with ethyl alcohol
It washes 5 times and obtains the thin film of reduction-oxidation graphite；
Step 2: the monomer ratio of configuration acrylic acid -2- methoxy acrylate (MEA) and n-isopropyl acrylamide (NIPAM)
It is 8:The benzoyl peroxide of MEA and NIPAM gross mass 0.7% is added as initiator, after magnetic agitation is uniform in 2 solution
It is injected into the mold that polyfluortetraethylene plate is made into, 12 hours of polymerization obtain a kind of esters of acrylic acid bullet under conditions of 60 DEG C
Property film material (is named as M8N2, film thickness 1mm).
Step 3: by the above-mentioned elastomer M being prepared8N2200% is stretched, the thin film of reduction-oxidation graphite is laid in
Press above decurl (if needed in graphene film and elastomeric substrate the stronger combination moment suitably use binder into
Row is pasted), final conducting bilayer membrane material is obtained after discharging stress.
Embodiment 3
Step 1: the graphene oxide solution of configuration 6mg/ml, adjusts PH=10 and stirs evenly, pour into room in culture dish
Temperature dries into graphene oxide membrane, the dilute film of graphite oxide is immersed in the HI solution that content is 46% after restoring 12h, clear with ethyl alcohol
It washes 5 times and obtains the thin film of reduction-oxidation graphite；
Step 2: the monomer ratio of configuration acrylic acid -2- methoxy acrylate (MEA) and n-isopropyl acrylamide (NIPAM)
It is 9:The benzoyl peroxide of MEA and NIPAM gross mass 0.7% is added as initiator, after magnetic agitation is uniform in 1 solution
It is injected into the mold that polyfluortetraethylene plate is made into, 12 hours of polymerization obtain a kind of esters of acrylic acid bullet under conditions of 60 DEG C
Property film material (is named as M9N1, film thickness 1mm).
Step 3: by the above-mentioned elastomer M being prepared9N1Long 200% is stretched, the thin film of reduction-oxidation graphite is tiled
Decurl is pressed above (if needing the stronger combination moment suitably to use binder in graphene film and elastomeric substrate
Pasted), final conducting bilayer membrane material is obtained after discharging stress.
Embodiment 4
Step 1: the graphene oxide solution of configuration 7mg/ml, adjusts PH=10 and stirs evenly, pour into room in culture dish
Temperature dries into graphene oxide membrane, the dilute film of graphite oxide is immersed in the HI solution that content is 46% after restoring 12h, clear with ethyl alcohol
It washes 5 times and obtains the thin film of reduction-oxidation graphite；
Step 2: configuration acrylic acid -2- methoxy acrylate (MEA) and N- methoxy -2- methyl -2- acrylamide
(MMP) monomer ratio is 7:The benzoyl peroxide of MEA and MMP gross mass 0.7% is added as initiator, magnetic force in 3 solution
It is injected into the mold that polyfluortetraethylene plate is made into after mixing evenly, 12 hours of polymerization obtain one kind third under conditions of 80 DEG C
Olefin(e) acid esters elastomer thin film material (is named as M7P3, film thickness 1mm).
Step 3: by the above-mentioned elastomer M being prepared7N3200% is stretched, the thin film of reduction-oxidation graphite is laid in
Press above decurl (if needed in graphene film and elastomeric substrate the stronger combination moment suitably use binder into
Row is pasted), final conducting bilayer membrane material is obtained after discharging stress.
Embodiment 5
Step 1: the graphene oxide solution of configuration 7mg/ml, adjusts PH=10 and stirs evenly, pour into room in culture dish
Temperature dries into graphene oxide membrane, the dilute film of graphite oxide is immersed in the HI solution that content is 46% after restoring 12h, clear with ethyl alcohol
It washes 5 times and obtains the thin film of reduction-oxidation graphite；
Step 2: the monomer ratio of configuration acrylic acid -2- methoxy acrylate (MEA) and hydroxymethyl acrylamide (HAM) are 7:3
Solution, the benzoyl peroxide of MEA and HAM gross mass 0.7% is added as initiator, is injected into after magnetic agitation is uniform poly-
In the mold that tetrafluoroethene plate is made into, 12 hours of polymerization obtain a kind of acrylic ester elastomer film under conditions of 70 DEG C
Material (is named as M7H3, film thickness 1mm).
Step 3: by the above-mentioned elastomer M being prepared7N3100% is stretched, the thin film of reduction-oxidation graphite is laid in
Press above decurl (if needed in graphene film and elastomeric substrate the stronger combination moment suitably use binder into
Row is pasted), final conducting bilayer membrane material is obtained after discharging stress.
The ratio of MEA and NIPAM is from 9 in this application:1 to 7:When 3, the elongation strain of elastomeric material can gradually drop
It is low, but its stress and self-repairability gradually increase, and the stickiness of surface of elastomer is in the trend of enhancing.In monomer molar quality
Than being 7:The elastomeric material self-repairability aggregated into when 3 is most strong, and 90% or more can be repaired in 2h.
In this application, the thickness of elastomeric substrate can be controlled on demand, but when elastomeric substrate thickness is excessively high
The duplicature marginal position of preparation can be tilted to centre, the too thin realization that will affect self-healing properties.Film is chosen in embodiment
Thickness is that the elastomer of 1mm is studied.
In this application, the thickness of the dilute film of reduction-oxidation graphite is controlled according to graphene oxide film thickness, graphite oxide
Alkene film thickness general control is too thick to be difficult to prepare at 10~40 μm, and too thin film influences the performance of reduction caudacoria.Exist as a result,
Range of the film thickness monitoring for the redox graphene film prepared in embodiment at 5-30 μm.
In this application, elastomeric substrate tensile elongation can exist according to practical application during preparing conducting bilayer film
It is chosen in the stretchable range of strain of elastomer polymer.But the too long service life for influencing its own of tensile elongation,
Easy damaged.The elongation strain for only choosing 50%, 100%, 200%, 300% in embodiment 1 is used as research.
In order to enable those skilled in the art to better understand the present invention, illustrate in the application below by way of specific embodiment
The method that simple preparation has the flexible electronic device of high conductivity, self-repairability and tensility.Material in these examples
Amount is substantially all by taking laboratory level as an example, certainly in actual production, the inventory value range of each reactant can with than
The amplification of example, be not described in detail this one by one.
There are many variable in this application, graphene concentration discussed above, film thickness, reaction temperature, reaction time, difference
To last result is invented, there are big influences for the conditions such as monomer, different monomers ratio, for example, different graphene concentration preparations
There is the material adhesion difference different, different monomers are prepared in obtained flexible electronic device electric conductivity.But due to writing
Content is limited, is not being compared description one by one in embodiment below, only (is stretched with the influence factor that can macroscopically observe
Than) discussed as a comparison case.
Have above to a kind of simple and quick preparation based on highly conductive redox graphene film provided by the present invention
Self-repairability, draftability the method for flexible electronic device be described in detail, specific case used herein is to this hair
Bright embodiment is expounded, and the above embodiments are only used to help understand, and method and core of the invention is thought
Think；At the same time, for those skilled in the art, according to the thought of the present invention, in specific embodiment and application range
There will be changes, in conclusion the contents of this specification are not to be construed as limiting the invention.
Claims (7)
1. a kind of method for the flexible electronic device for preparing highly conductive, selfreparing and tensility, it is characterised in that：Specific steps
It is as follows：
Step 1: preparation graphene oxide solution, graphene oxide solution concentration is 3-10mg/ml, and adjusting pH value is 10；By oxygen
Graphite alkene solution is placed in culture dish；It is thin that configured solution is prepared into graphene oxide in the method for room temperature self assembly
Film；Graphene oxide film passes through hydrogen iodide solution reduction at room temperature and obtains highly conductive and surfacing reduction-oxidation graphite
Thin film；
Step 2: acrylic acid -2- methoxy acrylate is uniformly mixed with amides olefinic monomer and initiator, then it is circulated into poly-
In tetrafluoroethene board mold, is caused by the method heating of bulk polymerization and the sticking selfreparing of surface tool and Gao La is prepared
The acrylic polymer elastomeric material of stretching property；Acrylic acid -2- the methoxy acrylate rubs with amides olefinic monomer
You are than being 9:1~7:3；The initiator content is acrylic acid -2- methoxy acrylate and amides olefinic monomer gross mass
0.5%-1.2%；
Step 3: after the polymer elastomer material that step 2 is prepared stretches, then the reduction-oxidation that step 1 is obtained
The thin film tiling of graphite obtains the flexible electronic device with highly conductive, selfreparing and tensility to after above, discharging stress
Part.
2. a kind of method for the flexible electronic device for preparing highly conductive, selfreparing and tensility as described in claim 1,
It is characterized in that：5-30 μm of reduction-oxidation graphite dilute film thickness described in step 1.
3. a kind of method for the flexible electronic device for preparing highly conductive, selfreparing and tensility as described in claim 1,
It is characterized in that：Amides olefinic monomer described in step 2 includes：N-isopropyl acrylamide or N- methoxy -2- methyl -
2- acrylamide or hydroxymethyl acrylamide or N, N- dimethacrylamide.
4. a kind of method for the flexible electronic device for preparing highly conductive, selfreparing and tensility as described in claim 1,
It is characterized in that：Initiator described in step 2 is benzoyl peroxide, benzoyl peroxide or methyl ethyl ketone peroxide.
5. a kind of method for the flexible electronic device for preparing highly conductive, selfreparing and tensility as described in claim 1,
It is characterized in that：Polymer elastomer material described in step 2 with a thickness of 0.5-2mm.
6. a kind of method for the flexible electronic device for preparing highly conductive, selfreparing and tensility as described in claim 1,
It is characterized in that：Reaction temperature in the method for bulk polymerization described in step 2 is 60 DEG C, polymerization time 6-24 hours.
7. a kind of method for the flexible electronic device for preparing highly conductive, selfreparing and tensility as described in claim 1,
It is characterized in that：The application of the flexible electronic device with highly conductive, selfreparing and tensility is conductor material, sensor
Part or flexible electronic skin.
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