CN106519939B - A kind of self-repair type conductive sensor high molecular material based on shape memory - Google Patents
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Abstract
The present invention relates to shape memory macromolecule composite material and conductive material fields, and in particular to a kind of conductive material with conductive network structure such as metal nanometer line, nanometer powder, carbon nanotube, graphene, carbon dust and a kind of self-repair type conductive sensor high molecular material based on shape memory being prepared with self-repair material, shape-memory material such as polyurethane.
Description
Technical field
The present invention relates to shape memory macromolecule composite material and conductive material fields, and in particular to one kind is remembered based on shape
Application of the self-repair type conductive sensor high molecular material and the material recalled in terms of conductive sensor, such as smart phone are convenient
The intellectual materials application such as sensor flexible of formula.
Background introduction
Material plays an important role for the production and life of the mankind.The development of science and technology has pushed mankind society
Meeting is constantly progressive, and at the same time, requirement of the people for material is higher and higher, and therefore, various new materials come into being, intelligence
Energy material is wherein important one kind, is with a wide range of applications.As the Typical Representative of new material, intellectual material is opened
Mankind's design and the new era using material are created.So-called intellectual material itself can perceive the generation of the external environment locating for it
Variation, and a kind of material of corresponding instantaneous active reaction is made to the variation.It is simply that have self diagnosis, from
A series of a kind of material of specific functions such as my adaptation, self-regeneration.Common intellectual material has automatically cleaning and self-repair material,
Magnetostriction materials, piezoelectric material, marmem and shape-memory polymer etc.
Earliest shape-memory polymer (Shape Memory Polymer, abbreviation SMP) is the coalification of France in the world
(CDF-Chimie) company's polynorbornene succeeded in developing in 1984, Japan have synthesized the poly- ammonia of shape memory in 1988,
There are also crosslinked polyethylene, ethylene-vinyl acetate copolymer, polycaprolactone, poly- fluoroolefins and trans--for its shape-memory polymer
1,4- polyisoprene etc..Compared with other shapes memory polymer, shape memory polyurethane (SMPU) has weatherability strong, anti-
Pinking is good, repeats the features such as deformation effects are good, light refraction and moisture vapor permeability are excellent, in engineering construction, clothes, health care
And the application potential of daily life etc. is huge.Shape-memory polymer (Shape Memory Polymer) refers to one
Kind has original shape, is deformed after fixing under the effect of certain external condition, can by the outside stimulus such as heat, electricity, magnetic, light
Reply the polymer of its original shapes.Representative document has: Hayashi S etc. passes through the heating power credit to SMPU and general SMP
(TMA) comparison is analysed, it is found that it is different from general SMP, the ratio between coefficient of expansion reachable 5~10 above and below shape memory temperature SMPU.
It can be with preparation temperature sensor using this property.Such as can be used for manufacturing the attachment device of fire-alarm, when connection is first made
Shape, then post forming be disconnect when shape；When fire occurs, connector resiles automatically and keeps circuit disconnected
It opens, alarm is just started to work.
Self-repair material is a kind of new material that self-regeneration is able to carry out in object damage.This material is infused
Enter into high molecular polymer, when object scratches, the material of injection can be released under multiple stimulation to impaired object
Surface is automatically repaired.Conventional selfreparing mechanism includes microcapsule method, and representative document has: University of Illinois
White is applied to microcapsules selfreparing matrix in epoxide resin material, he is coated on renovation agent dicyclopentadiene (DCPD)
In urea-formaldehyde resin microcapsule, and catalyst is dispersed in epoxy resin-base material, when basis material damages, is caused micro-
Capsule ruptures, and renovation agent is released to the plane of disruption, meets with catalyst and polymerization reaction occurs, to repair the plane of disruption；Again
Such as reacted using the Diels-Alder of thermal reversion, representative document has: Chen etc. prepared it is a kind of have review one's lessons by oneself reactivation
The highly cross-linked polymer composites of power, this composite material is under conditions of 120 DEG C of heating, crosslinking point off therein
It opens, but crosslinking points are after the cooling period, and can re-close and to form new chemical bond, thus repair crack face.Shape memory from
Reparation is the P.T in the U.S. in 2011
What Mather was proposed, over nearly 5 years, the selfreparing based on shape memory obtains huge development, it is considered to be the
Three generations's self-healing system.
It is deepened continuously research based on the self-repair function of shape memory, however, also less high with the sensing of compliant conductive
Molecule combines.Data in terms of wearable electronic, flexible sensing device.As recent, Beijing University of Chemical Technology Sun Xiaoming
Professor, associate professor Wan Pengbo and Nanyang Technological University Chen Xiaodong professor, Shenzhen University professor Zhang Han etc. cooperate, in institute's structure
On the basis of the series of tasks such as flexible, transparent, the selfreparing thin film sensor built, look back to comprehensive system in recent years based on half
The flexibility of the materials such as conductor nano material, carbon material, Conductive polymers building, transparent gas sensor；System summary is promoted
The strategy of the flexible, transparency, sensing capabilities, the assembling mode of control, material including sensing material pattern, the uniform of film sink
Product, selection and optimization of substrate etc.；Existing flexible, clear sensor deficiency is proposed, such as volatile organic gas specificity
Quickly detection is difficult, practical application when sensitive to environmental change, portable wearable property and signal radio transmission performance it is not good enough etc.；And it opens up
It has hoped flexibility, the further developing direction of clear sensor towards wearable device, for example has further realized and improve and is a variety of
Gas detects simultaneously, the Multifunctional centralized of the environmental stability that senses, portable wearable device becomes second nature, the micromation and biography of sensor
Signal is felt to wireless transmission integrations of equipment such as Ipad, mobile phone, Watch class etc..This will be following flexible, transparent, wearable
The development of gas sensor provides new Research Thinking and theoretical foundation.
Flexible material referred to herein, while containing the selfreparing intelligent attributes and electrical-conductive nanometer high score of shape memory
The strain of son relies on (strain-dependent) performance, and final obtain has novel multifunctional sensing macromolecule.
Summary of the invention
In view of the deficiencies of the prior art, it is an object of the present invention to provide a kind of, and the self-repair type conduction based on shape memory passes
Feel high molecular material and preparation method thereof.
Specific method of the present invention are as follows:
A kind of self-repair type conductive sensor high molecular material based on shape memory, the raw material including following mass percent
It is prepared:
1. conductive material, dosage 0.5%-1.5%.
2. self-repair material, dosage 35%-45%.
3. shape-memory material, dosage 53.5%-64.5%.
The preparation method of the above-mentioned self-repair type conductive sensor high molecular material based on shape memory, includes the following steps:
1. conductive material is dissolved in solvent A, simultaneously ultrasound a period of time is stirred.By its drop coating on matrix, dry
It is put into after to conductive film or drying in Muffle furnace and obtains conductive film for 24 hours at 200 DEG C.
2. self-repair material is dissolved in solvent B.Heating stirring and ultrasound a period of time, keep solution uniform.
3. shape-memory material is dissolved in solvent C.Heating stirring and ultrasound a period of time, keep solution uniform.
4. self-repair material solution and shape-memory material solution are blended in different proportions and ultrasound is uniform.Drop coating or
It is spin-coated on the conductive film of above-mentioned steps 1.It places and is first heated at 70-80 DEG C in a vacuum drying oven a period of time again, it is rear to take out
Vacuum obtains composite membrane, i.e. the self-repair type conductive sensor high molecular material based on shape memory for 24 hours.
The conductive material is silver nanowires, carbon nanotube, graphene oxide, nano-Ag particles etc., solvent A used
Including but not limited to ethyl alcohol, water etc.；The self-repair material is pla-pcl (PCL).
And shape-memory material includes but is not limited to elastic epoxy macromolecule, shape memory polyurethane (SMPU) or elasticity
Siloxanes macromolecule, used solvent B and C is n,N-dimethylacetamide, n,N dimethylformamide, tetrahydrofuran etc..
Described matrix is polytetrafluoroethylene (PTFE), glass slide etc..Above-mentioned self-repair material solution and shape-memory material solution
Mixed proportion is 2-8:10.
The conductive flexible multifunctional material damage rehabilitation method of above-mentioned selfreparing: 60-100 DEG C of range of material or electricity are kept
Triggering, the modes such as near-infrared can repair after 1-20min.
Compared with prior art, the method have the advantages that:
The present invention is prepared for a kind of self-repair type conductive sensor high molecular material based on shape memory, preparation method compared with
To be simple, obtained composite material has conductive and certain self-healing properties on the basis of shape-memory properties, this
Kind is conductive and the utilization of application and the growth of service life and increase in terms of sensing in terms of intellectual material is greatly improved in selfreparing.
Special appearance increases mechanical property simultaneously.
Detailed description of the invention
Fig. 1 composite material prepares schematic diagram
Fig. 2 conductive layer/SMPU/PCL composite material surface texture
Wherein (a) is the surface of composite material, (b) is the section of composite material
Fig. 3 conductive layer/SMPU/PCL composite material self-healing properties
Wherein (a) is the composite material that the composite material (b) scratched is selfreparing
Specific embodiment
In order to make technological means of the invention, creation characteristic is reached purpose and is readily apparent from effect, below by specific
The present invention is further described in detail for embodiment.It is necessary to note that embodiment once is protection scope of the present invention.
Embodiment 1
1. silver nanowires 0.8-1.2mg is dissolved in ethanol solution, simultaneously ultrasound 10-20s is stirred.By its drop coating in matrix
On.And it dries and obtains conductive film.
2. it is 100mg/ml that self-repair material PCL, which is dissolved in DMAC N,N' dimethyl acetamide (DMAC) and is configured to concentration,.Add
Thermal agitation and ultrasound a period of time, keep solution uniform.
3. shape memory polyurethane SMPU is dissolved in N, it is 100mg/ that concentration is configured in N dimethyl acetamide (DMAC)
ml.Heating stirring and ultrasound a period of time, keep solution uniform.
4. simultaneously ultrasound is blended with PCL:SMPU=6:10 ratio in self-repair material solution and shape memory polyurethane solution
Uniformly.Drop coating is on the conductive film of above-mentioned steps 1.Place and first at 80 DEG C heat 2-3h in a vacuum drying oven, after vacuumize
Composite membrane, i.e. the self-repair type conductive sensor high molecular material based on shape memory are obtained for 24 hours.
Obtained composite membrane repair time and temperature are 10-20min and 60-100 degree.Conductive structure repairing effect exists
40%-80%.
Embodiment 2
1. the carbon nanotube of 10-20mg is dissolved in ethanol solution, simultaneously ultrasound 10-20s is stirred.By its drop coating in matrix
On.And it dries and obtains conductive film.
2. it is 100mg/ml that self-repair material PCL, which is dissolved in DMAC N,N' dimethyl acetamide (DMAC) and is configured to concentration,.Add
Thermal agitation and ultrasound a period of time, keep solution uniform.
3. shape memory polyurethane SMPU is dissolved in N, it is 100mg/ that concentration is configured in N dimethyl acetamide (DMAC)
ml.Heating stirring and ultrasound a period of time, keep solution uniform.
4. by self-repair material solution and shape memory polyurethane solution to be blended and surpass with PCL:SMPU=6:10 ratio
Sound is uniform.Drop coating is on the conductive film of above-mentioned steps 1.It places and first heats 2-3h at 80 DEG C in a vacuum drying oven, it is rear to take out very
Sky obtains composite membrane for 24 hours, the self-repair type conductive sensor high molecular material based on shape memory.
Obtained composite membrane repair time and temperature are 10-20min and 60-100 degree.Conductive structure repairing effect exists
40%-80%.
Embodiment 3
1. being as (0:10,1:9,2:8,3:7) makes gross mass in varing proportions by graphene oxide and carbon nanotube
10mg is dissolved in ethanol solution, stirs simultaneously ultrasound 10-20s.By its drop coating on matrix.And it dries.After be put into Muffle furnace
Conductive film is obtained for 24 hours at 200 DEG C.
2. it is 100mg/ml that self-repair material PCL, which is dissolved in DMAC N,N' dimethyl acetamide (DMAC) and is configured to concentration,.Add
Thermal agitation and ultrasound a period of time, keep solution uniform.
3. shape memory polyurethane SMPU is dissolved in N, it is 100mg/ that concentration is configured in N dimethyl acetamide (DMAC)
ml.Heating stirring and ultrasound a period of time, keep solution uniform.
4. simultaneously ultrasound is blended with PCL:SMPU=6:10 ratio in self-repair material solution and shape memory polyurethane solution
Uniformly.Drop coating is on the conductive film of above-mentioned steps 1.Place and first at 80 DEG C heat 2-3h in a vacuum drying oven, after vacuumize
For 24 hours, composite membrane, i.e. the self-repair type conductive sensor high molecular material based on shape memory are obtained.
The repair time of its composite membrane and temperature are 10-20min and 60-100 degree.Conductive structure repairing effect is in 40%-
80%.
Embodiment 4
1. graphene oxide 8-20mg is dissolved in ethanol solution, stir and is centrifuged 10min revolving speed after ultrasound 30min
10000 turns, remove upper layer impurity.Afterwards by its drop coating on matrix such as (polytetrafluoroethylene (PTFE), glass slide etc.).And it dries.After be put into
Conductive film is obtained for 24 hours at 200 DEG C in Muffle furnace.
2. it is 100mg/ml that self-repair material PCL, which is dissolved in DMAC N,N' dimethyl acetamide (DMAC) and is configured to concentration,.Add
Thermal agitation and ultrasound a period of time, keep solution uniform.
3. shape memory polyurethane SMPU is dissolved in N, it is 100mg/ that concentration is configured in N dimethyl acetamide (DMAC)
ml.Heating stirring and ultrasound a period of time, keep solution uniform.
4. by self-repair material solution and shape memory polyurethane solution in different proportions with PCL:SMPU=6:10 ratio
Example is blended and ultrasound is uniform.Drop coating is on the conductive film of above-mentioned steps 1.It places and first heats 2- at 80 DEG C in a vacuum drying oven
3h, after vacuumize for 24 hours, obtain composite membrane, i.e. the self-repair type conductive sensor high molecular material based on shape memory.
The repair time of its composite membrane and temperature are 10-20min and 60-100 degree.Conductive structure repairing effect is in 40%-
80%.
Embodiment 5
1. nano-Ag particles 0.8-2mg is dissolved in ethanol solution, simultaneously ultrasound 10-20s is stirred.By its drop coating in matrix
On.And it dries.
2. it is 100mg/ml that self-repair material PCL, which is dissolved in DMAC N,N' dimethyl acetamide (DMAC) and is configured to concentration,.Add
Thermal agitation and ultrasound a period of time, keep solution uniform.
3. shape memory polyurethane SMPU is dissolved in N, it is 100mg/ that concentration is configured in N dimethyl acetamide (DMAC)
ml.Heating stirring and ultrasound a period of time, keep solution uniform.
4. being blended self-repair material solution and shape memory polyurethane solution in different proportions with PCL:SMPU=6:
10 ratios are simultaneously ultrasonic uniform.Drop coating is on the conductive film of above-mentioned steps 1.It places and first heats 2- at 80 DEG C in a vacuum drying oven
3h, after vacuumize for 24 hours, obtain composite membrane, i.e. the self-repair type conductive sensor high molecular material based on shape memory.
The repair time of its composite membrane and temperature are 10-20min and 60-100 degree.Conductive structure repairing effect is in 60%-
80%.
Embodiment 6
1. nano-silver thread and carbon nanotube are dissolved in ethanol solution with 1:9, the two dosage summation is 10mg, and stirring is simultaneously
Ultrasonic 10-20s.By its drop coating on matrix.And it dries.
2. it is 100mg/ml that self-repair material PCL, which is dissolved in DMAC N,N' dimethyl acetamide (DMAC) and is configured to concentration,.Add
Thermal agitation and ultrasound a period of time, keep solution uniform.
3. shape memory polyurethane SMPU is dissolved in N, it is 100mg/ that concentration is configured in N dimethyl acetamide (DMAC)
ml.Heating stirring and ultrasound a period of time, keep solution uniform.
4. being blended self-repair material solution and shape memory polyurethane solution in different proportions with PCL:SMPU=6:
10 ratios are simultaneously ultrasonic uniform.Drop coating is on the conductive film of above-mentioned steps 1.It places and first heats 2- at 80 DEG C in a vacuum drying oven
3h, after vacuumize for 24 hours, obtain composite membrane, i.e. the self-repair type conductive sensor high molecular material based on shape memory.
The repair time of its composite membrane and temperature are 10-20min and 60-100 degree.Conductive structure repairing effect is in 40%-
80%.
Claims (3)
1. a kind of self-repair type conductive sensor high molecular material based on shape memory, by the original of following components and mass percent
Material is prepared:
Conductive material, dosage 0.5%-1.5%,
Self-repair material, dosage 35%-45%,
Shape-memory material, dosage 53.5%-64.5%,
The above-mentioned self-repair type conductive sensor high molecular material based on shape memory, includes the following steps:
Conductive material is dissolved in solvent A, simultaneously ultrasound a period of time is stirred, by its drop coating on matrix, and dries and is led
It is put into Muffle furnace after electrolemma or drying and obtains conductive film for 24 hours at 200 DEG C；
Self-repair material is dissolved in solvent B, heating stirring and ultrasound a period of time, keeps solution uniform；
Shape-memory material is dissolved in solvent C, heating stirring and ultrasound a period of time, keeps solution uniform；
By self-repair material solution and shape-memory material solution be blended in certain proportion and ultrasound uniformly, drop coating or be spin-coated on
On conductive film；
Place and first heat a period of time at 70-80 DEG C in a vacuum drying oven, after vacuumize and obtain composite membrane for 24 hours, that is, be based on
The self-repair type conductive sensor high molecular material of shape memory；
The solvent A includes second alcohol and water；
The solvent B and solvent C are DMAC N,N' dimethyl acetamide, N, any one in N-dimethylformamide and tetrahydrofuran；
Conductive material is any one in silver nanowires, carbon nanotube, graphene oxide and nano-Ag particles；
The self-repair material is pla-pcl；
The shape-memory material is the siloxanes high score of elastic epoxy macromolecule, shape memory polyurethane (SMPU) or elasticity
Any one in son.
2. a kind of self-repair type conductive sensor high molecular material based on shape memory as described in claim 1, feature exist
In the mixed proportion of self-repair material solution and shape-memory material solution is (2-8): 10.
3. a kind of self-repair type conductive sensor high molecular material based on shape memory as described in claim 1, feature exist
In damage rehabilitation method is that heating material to 60-100 DEG C, electricity triggering or near infrared light is handled；After 1-20min
It can repair.
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