CN108485234A - A kind of self-healing sensing polymer composite and preparation method thereof based on orderly conductive network structure - Google Patents
A kind of self-healing sensing polymer composite and preparation method thereof based on orderly conductive network structure Download PDFInfo
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- CN108485234A CN108485234A CN201810163772.5A CN201810163772A CN108485234A CN 108485234 A CN108485234 A CN 108485234A CN 201810163772 A CN201810163772 A CN 201810163772A CN 108485234 A CN108485234 A CN 108485234A
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J5/00—Manufacture of articles or shaped materials containing macromolecular substances
- C08J5/18—Manufacture of films or sheets
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2367/00—Characterised by the use of polyesters obtained by reactions forming a carboxylic ester link in the main chain; Derivatives of such polymers
- C08J2367/04—Polyesters derived from hydroxy carboxylic acids, e.g. lactones
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2375/00—Characterised by the use of polyureas or polyurethanes; Derivatives of such polymers
- C08J2375/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/001—Conductive additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K2201/00—Specific properties of additives
- C08K2201/011—Nanostructured additives
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K7/00—Use of ingredients characterised by shape
- C08K7/02—Fibres or whiskers
- C08K7/04—Fibres or whiskers inorganic
- C08K7/06—Elements
Abstract
The invention discloses a kind of, and the self-healing based on orderly conductive network structure senses polymer composite and preparation method thereof, is that nano silver wire is carried out ordered arrangement using the method for interface self assembly, constructs orderly nano silver wire conductive film；Then self-healing polycaprolactone and shape memory polyurethane blending are uniformly obtained into macromolecule mixed liquor, macromolecule is mixed into drop-coated by the way of stratiform mixing or is spun to orderly nano silver wire conductive film surface；Heat treatment is carried out again and removes organic solvent, and final stripping obtains the sensing polymer composite of the self-healing based on orderly conductive network structure.The preparation method of the present invention is simple, the good conductivity of self-healing obtained sensing polymer composite, compared with unordered silver nanowire composite material, the resistance variations response time faster, resistance change rate bigger, while there is conductive and self-healing effect.
Description
Technical field
The present invention relates to sensing material field, more particularly to a kind of self-healing sensing based on orderly conductive network structure is high
Molecular composite material and preparation method thereof.
Background technology
Material plays an important roll the production and life of the mankind, while new material also advances scientific progress.Closely
Nian Lai, various excellent special type function materials emerge one after another, wherein especially prominent is flexible electronic device.Due to conditional electronic
The fragility of device, it is of high cost the shortcomings of, flexible electronic device has the performance of flexible, ductility and low cost, causes full generation
The extensive concern on boundary is simultaneously rapidly developed.
Silver nano material has unique optics, mechanics and catalytic performance, especially nano silver wire as 1-dimention nano material
Material, has the characteristics that high conductivity and thermal conductivity, large specific surface area and transparency are high, shows the amount of general nano-sized materials
Sub- effect is widely used in medical domain, Industrial Catalysis and optical field, in optics such as surface-enhanced Raman, strong UV absorptions
Aspect is using more.In addition, in the flexible electronic devices such as wearable electronic, ultracapacitor field, nano silver wire is also normal
As conductive material, if Guangdong University of Technology professor Luo Hongsheng is compound layer by layer by nano silver wire and shape memory high molecule progress,
Constructed it is a kind of based on shape memory response electro photoluminescence nano silver wire polymer composite (referring to H.Luo, Z.Li, G.Yi,
et al.,Electro-responsive silver nanowire-shape memory polymer composites,
Mater.Lett.134(2014)172-175)。
In addition, the nano silver wire of unique properties is carried out after being orderly orientated, its superior performance can be greatly played.As king builds
The superfine ordered structure using the nano silver wire after being orientated realizes surface Raman enhancement (referring to Wang, J.C.；Luo,H.S.；
Zhang,M.H.；Zu,X.H.；Li,Z.W.；Yi,G.B.Aligned Chemically Etched Silver Nanowire
Monolayer as Surface-Enhanced Raman Scattering Substrates Nanoscale Res Lett
2017,12.) and orderly nano silver wire is used for optical characterisation and application aspect by Chu et al..
However, when nano silver wire is introduced on high molecular material, although electric conductivity is good, there are resistance variations
The problems such as low, not sensitive enough, in terms of practical sensing can not being applied to.Therefore, it is necessary to design new conductive network, including replaces and receive
Rice conductive material designs its structure；But at present seldom studies have reported that the ordered arrangement structure of nano silver wire is applied to soft
On property senser element.
Invention content
It is an object of the invention to overcome disadvantage existing in the prior art, provide a kind of based on orderly conductive network structure
Self-healing sense polymer composite, compared with mixed and disorderly unordered nano silver wire polymer composite, spirit can be improved
Sensitivity and mechanical property, while promoting its resistance change rate.
Another object of the present invention is to provide the preparation methods that a kind of above-mentioned self-healing senses polymer composite.
The purpose of the invention is achieved by the following technical solution：
A kind of preparation method of the self-healing sensing polymer composite based on orderly conductive network structure, is to use boundary
Nano silver wire is carried out ordered arrangement by the method for face self assembly, constructs orderly nano silver wire conductive film；Then self-healing is gathered oneself
Lactone and shape memory polyurethane blending uniformly obtain macromolecule mixed liquor, by macromolecule mixed liquor by the way of stratiform mixing
Drop coating is spun to orderly nano silver wire conductive film surface；Heat treatment is carried out again and removes organic solvent, and final stripping obtains base
Polymer composite is sensed in the self-healing of orderly conductive network structure.Specifically include following step：
(1) aqueous solution of a concentration of (0.5~15) mg/ml nano silver wires is added drop-wise to chloroform soln surface, waits for silver
After nano thread ordered orientation, nano silver wire is taken out with sheet glass, natural drying or heating, drying, obtaining weight density is
0.04-1.2mg/cm2Orderly nano silver wire conductive film；
(2) it is (0~60) by mass ratio:The polycaprolactone and shape memory polyurethane of (40~100) are dissolved in organic respectively
In solvent, carries out heating stirring and obtain macromolecule mixed liquor, temperature is 60~70 DEG C, and the time is 0.5~1h；Then spin coating is used
Or the mode of drop coating, macromolecule mixed liquor is uniformly spread on the orderly nano silver wire conductive film, is dried prior to 60~70 DEG C
Heating 12 in case~for 24 hours, then vacuum drying 12 in 50~60 DEG C of vacuum drying chambers~for 24 hours is placed it in, organic solvent is removed, most
It is peeled off from sheet glass afterwards and the self-healing sensing polymer composite based on orderly conductive network structure is made.
In step (2), the organic solvent is N, N dimethyl acetamide, n,N dimethylformamide, dimethyl trident maple
Or one kind in tetrahydrofuran.
A kind of self-healing sensing polymer composite based on orderly conductive network structure, is prepared using the above method
It obtains.
The self-healing based on orderly conductive network structure senses polymer composite, by orderly nano silver wire and height
Molecule base material is constituted, and integral composite is layer structure, and polymer-based bottom material is by self-healing polycaprolactone, macromolecule
Elastomer is constructed, and has the ability of strain sensing and thermostimulation sensing.The orderly conductive network structure refers to passing through interface
The method of self assembly is orientated linear nano silver wire, forms the orderly conductive network structure of align uniaxial；The self-healing
In the case that conjunction refers to material by certain outer damage (such as scuffing), the means of material warms are made by heating etc., it can be from
Healing impainnent position is sent out, its internal structure is made to be repaired；The sensing refers to a degree of to material progress differently- oriented directivity
It stretches, material can rely on natural resiliency rebound or heat and reply, which can generate conductive network certain influence, this variation
Result be changed into electric signal, that is, change material itself internal resistance value.
The polycaprolactone refers to that melting transition temperature is 60 DEG C, and molecular weight is the thermoplastic polymer of 10000-80000.
The macromolecular elastomer refers to that molecular weight is 10000-1000000 and flexible shape memory polyurethane.
In the polymer-based bottom material, the mass fraction of polycaprolactone is 0~60%, the quality point of macromolecular elastomer
Number is 40~100%.
The present invention has the following advantages that compared with prior art and effect：
(1) preparation method is simple, the good conductivity of self-healing sensing polymer composite obtained, with unordered silver nanoparticle
Line composite material is compared, the resistance variations response time faster, resistance change rate bigger.
(2) self-healing of the invention sensing polymer composite has simultaneously on the basis of having shape recovery function
There is conductive and self-healing effect.
(3) present invention is successfully realized on the nano silver wire appendix to high molecular material that will be orderly orientated, and is expected to be applied to
Flexible wearable electronic equipment.
Description of the drawings
Fig. 1 is the preparation flow schematic diagram of the present invention
Fig. 2 is 300 times of scanning electron microscope (SEM) photographs of ordered structure silver wire.
Fig. 3 is 500 times of scanning electron microscope (SEM) photographs of ordered structure silver wire.
Fig. 4 is the curent change that composite material scratches heating healing.
Fig. 5 is the heated current variation under composite material different stretch ratio.
Fig. 6 is that LED light is lit schematic diagram in composite material access direct current.
Specific implementation mode
Further detailed description is done to the present invention with reference to embodiment, embodiments of the present invention are not limited thereto.
Embodiment 1
(1) aqueous solution of 10mg/ml nano silver wires is added dropwise into chloroform soln dropwise at glass wall, waits for Yin Na
After the completion of rice noodles are orientated, orderly nano silver wire is taken out with 10 × 25mm sheet glass, the Ordered Silver that quality is 1.56mg is obtained and receives
Rice noodles conductive film, detailed process are as shown in Figure 1.
(2) it will be dissolved in N respectively, the polycaprolactone and polyurethane of N dimethyl acetamide mix, the total matter of macromolecule mixed liquor
Amount is 30mg, and wherein polycaprolactone accounts for 30%, stirs 0.5h, then drop coating or is spun to above-mentioned orderly nano silver wire conductive film
On, heating 12 hours in 70 DEG C of baking ovens are first put into, vacuum drying 12 hours in vacuum drying chamber are placed into, obtain being based on orderly leading
The self-healing of electric network structure senses polymer composite.Morphology observation is carried out to material with scanning electron microscope, such as Fig. 2,3 institutes
Show, the nano silver wire for imbedding polymer-based bottom material has directionality, and orientation is substantially parallel with draw direction, in each to different
Property, be conducive to the sensitivity for improving self-healing sensing polymer composite.
(3) it is 25mm*5mm*0.05mm self-healing sensing polymer composite to be cut out a block length * wide * thickness
Sample.1V voltages are passed through toward material, it is 0.384A to measure its electric conductivity；Tensile deformation 10%, 6.18 times of resistance variations, heating
Restore completely；It heats and repairs after sample is scratched, healing time and temperature are 10min and 80 DEG C, and electric conductivity restores
46.7%, as shown in Figure 4.10%, 15%, 20% stretching is carried out to material, heating restores 95%-100%, such as Fig. 5 institutes
Show.As shown in fig. 6, material is accessed in direct current, it can lightening LED lamp (5V12W).
Embodiment 2
(1) aqueous solution of 10mg/ml nano silver wires is added dropwise into chloroform soln dropwise at glass wall, waits for Yin Na
After the completion of rice noodles are orientated, orderly nano silver wire is taken out with 10 × 25mm sheet glass, the Ordered Silver that quality is 0.64mg is obtained and receives
Rice noodles conductive film.
(2) it will be dissolved in N respectively, the polycaprolactone and polyurethane of N dimethyl acetamide mix, the total matter of macromolecule mixture
Amount is 30mg, and wherein polycaprolactone accounts for 30%, stirs 0.5h, then drop coating or is spun to above-mentioned orderly nano silver wire conductive film
On, heating 12 hours in 70 DEG C of baking ovens are first put into, vacuum drying 12 hours in vacuum drying chamber are placed into, obtain being based on orderly leading
The self-healing of electric network structure senses polymer composite.
(3) it is 25mm*5mm*0.05mm self-healing sensing polymer composite to be cut out a block length * wide * thickness
Sample.1V voltages are passed through toward material, it is 0.0823A to measure its electric conductivity；Tensile deformation 10%, 162.85 times of resistance variations,
Heating restores completely；It heats and repairs after sample is scratched, healing time and temperature are 10min and 80 DEG C, and electric conductivity is extensive
Multiple 45.1%.
Embodiment 3
(1) aqueous solution of 10mg/ml nano silver wires is added dropwise into chloroform soln dropwise at glass wall, waits for Yin Na
After the completion of rice noodles are orientated, orderly nano silver wire is taken out with 10 × 25mm sheet glass, the Ordered Silver that quality is 2.37mg is obtained and receives
Rice noodles conductive film.
(2) it will be dissolved in N respectively, the polycaprolactone and polyurethane of N dimethyl acetamide mix, the total matter of macromolecule mixture
Amount is 30mg, and wherein polycaprolactone accounts for 30%, stirs 0.5h, then drop coating or is spun to above-mentioned orderly nano silver wire conductive film
On, heating 12 hours in 70 DEG C of baking ovens are first put into, vacuum drying 12 hours in vacuum drying chamber are placed into, obtain being based on orderly leading
The self-healing of electric network structure senses polymer composite.
(3) it is 25mm*5mm*0.05mm self-healing sensing polymer composite to be cut out a block length * wide * thickness
Sample.1V voltages are passed through toward material, it is 0.391A to measure its electric conductivity；Tensile deformation 10%, 3.10 times of resistance variations, heating
Restore completely；It heats and repairs after sample is scratched, healing time and temperature are 10min and 80 DEG C, and electric conductivity restores
36.6%.
Claims (8)
1. a kind of preparation method of the self-healing sensing polymer composite based on orderly conductive network structure, feature exist
In：It is that nano silver wire is carried out by ordered arrangement using the method for interface self assembly, constructs orderly nano silver wire conductive film；Then will
Self-healing polycaprolactone and shape memory polyurethane blending uniformly obtain macromolecule mixed liquor, will be high by the way of stratiform mixing
Molecular mixing drop-coated is spun to orderly nano silver wire conductive film surface；Heat treatment is carried out again and removes organic solvent, finally
Stripping obtains the sensing polymer composite of the self-healing based on orderly conductive network structure.
2. the preparation of the self-healing sensing polymer composite according to claim 1 based on orderly conductive network structure
Method, it is characterised in that include the following steps：
(1) aqueous solution of a concentration of (0.5~15) mg/ml nano silver wires is added drop-wise to chloroform soln surface, waits for silver nanoparticle
Line orderly be orientated after, nano silver wire is taken out with sheet glass, natural drying or heating, drying, obtain weight density be 0.04~
1.2mg/cm2Orderly nano silver wire conductive film；
(2) it is (0~60) by mass ratio:The polycaprolactone and shape memory polyurethane of (40~100) are dissolved in organic solvent respectively
In, it carries out heating stirring and obtains macromolecule mixed liquor, temperature is 60~70 DEG C, and the time is 0.5~1h；Then spin coating or drop are used
The mode of painting uniformly spreads over macromolecule mixed liquor on the orderly nano silver wire conductive film, in prior to 60~70 DEG C baking ovens
Heating 12~for 24 hours, then place it in 50~60 DEG C of vacuum drying chambers vacuum drying 12~for 24 hours, removes organic solvent, finally from
It is peeled off on sheet glass and the self-healing sensing polymer composite based on orderly conductive network structure is made.
3. the preparation of the self-healing sensing polymer composite according to claim 2 based on orderly conductive network structure
Method, it is characterised in that：In step (2), the organic solvent is N, N dimethyl acetamide, n,N dimethylformamide, two
One kind in methyl trident maple or tetrahydrofuran.
4. a kind of self-healing based on orderly conductive network structure senses polymer composite, it is characterised in that：It is using power
Profit requires any one of 1~3 method to be prepared.
5. the self-healing according to claim 4 based on orderly conductive network structure senses polymer composite, special
Sign is：It is made of orderly nano silver wire and polymer-based bottom material, integral composite is layer structure, polymer-based ground
Material is constructed by self-healing polycaprolactone, macromolecular elastomer, has the ability of strain sensing and thermostimulation sensing.
6. the self-healing according to claim 5 based on orderly conductive network structure senses polymer composite, special
Sign is：The polycaprolactone refers to the thermoplastic polymer that melting transition temperature is 60 DEG C, molecular weight is 10000-80000.
7. the self-healing according to claim 5 based on orderly conductive network structure senses polymer composite, special
Sign is：The macromolecular elastomer refers to that molecular weight is 10000-1000000 and flexible shape memory polyurethane.
8. the self-healing according to claim 4 based on orderly conductive network structure senses polymer composite, special
Sign is：In the polymer-based bottom material, the mass fraction of polycaprolactone is 0~60%, the quality point of macromolecular elastomer
Number is 40~100%.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109337102A (en) * | 2018-09-06 | 2019-02-15 | 中国人民解放军陆军工程大学 | Self-adaptive electromagnetic pluse shielding method for manufacturing thin film, obtained film and application |
| CN113823440A (en) * | 2021-11-22 | 2021-12-21 | 明鑫(深圳)技术研究有限公司 | Preparation method and application of self-healing polyurethane stretchable electrode |
| CN113861662A (en) * | 2021-09-30 | 2021-12-31 | 南昌航空大学 | Self-repairing polyurethane heat-conducting composite material and preparation method thereof |
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| CN106519939A (en) * | 2016-09-29 | 2017-03-22 | 广东工业大学 | Self-repairing type conductive sensing high polymer material based on shape memory |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109337102A (en) * | 2018-09-06 | 2019-02-15 | 中国人民解放军陆军工程大学 | Self-adaptive electromagnetic pluse shielding method for manufacturing thin film, obtained film and application |
| CN109337102B (en) * | 2018-09-06 | 2021-03-30 | 中国人民解放军陆军工程大学 | Preparation method of self-adaptive electromagnetic pulse shielding film, prepared film and application |
| CN113861662A (en) * | 2021-09-30 | 2021-12-31 | 南昌航空大学 | Self-repairing polyurethane heat-conducting composite material and preparation method thereof |
| CN113823440A (en) * | 2021-11-22 | 2021-12-21 | 明鑫(深圳)技术研究有限公司 | Preparation method and application of self-healing polyurethane stretchable electrode |
| CN113823440B (en) * | 2021-11-22 | 2022-02-22 | 明鑫(深圳)技术研究有限公司 | Preparation method and application of self-healing polyurethane stretchable electrode |
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Application publication date: 20180904 |