CN110415889A - A kind of preparation method of the selfreparing electrode material based on supermolecule dual network structure - Google Patents
A kind of preparation method of the selfreparing electrode material based on supermolecule dual network structure Download PDFInfo
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- C08J2383/00—Characterised by the use of macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon with or without sulfur, nitrogen, oxygen, or carbon only; Derivatives of such polymers
- C08J2383/04—Polysiloxanes
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Abstract
The present invention relates to a kind of selfreparing electrode materials, and in particular to a kind of preparation method of the selfreparing electrode material based on supermolecule dual network structure.In the present invention, the synthetic method benefit of preparation selfreparing electrode material is simple and efficient, material has biocompatibility, not only with the engineering properties and the rheological equationm of state of selfreparing, energy band moving conductive network selfreparing simultaneously, and this process does not have any restrictions, does not need environmental stimuli, can carry out at any temperature.This method can targetedly be applied so that material property is controllable to make it have by changing the proportion of two kinds of networks.Self-repair material made from this method can restore completely self-repair material made from electric property this method in 25 minutes at normal temperature and be provided simultaneously with from adhesion, convenient for body electrode's material with the compound preparation fitting skin of conductive material.
Description
Technical field
The present invention relates to a kind of polydimethylsiloxaneelastomer elastomer base selfreparing electrode materials, and in particular to one kind is based on super
The preparation method of the selfreparing electrode material of molecule dual network structure.
Background technique
In recent years, flexible device is because it has the characteristics such as flexible, frivolous, biomedicine, energy storage and switching device,
It studies extensively in the fields such as wearable device, medical energy converter, portable equipment.But existing flexible device material tensility
Energy, electric property are poor, and the failure of flexible electronic device is much originated from mechanical damage, on the one hand seriously limit the longevity of device
Life, on the other hand leads to more and more electronic wastes.In order to solve problem above, self-repair material is applied to flexibility because having
The potentiality of stretchable electronic device, and the self-healing property of human skin can be simulated and seem most important.It is current from
Repair materials have two major classes, and one kind is external self-repair material, need to be previously implanted selfreparing medium, however the addition one of medium
Aspect is possible to hinder conductive path that electric conductivity is declined, on the other hand to the position of healing have a specified property and it is nonrandom more
It closes, and the cycle-index of selfreparing is limited；Another kind of is internal self-repair material, utilizes covalent bond recoverable in system
(such as disulfide bond) or dynamic interaction (such as hydrogen bond) complete selfreparing, but not can guarantee it after polymeric matrix selfreparing
Still has tensility, the selfreparing of nanostructure is the key that guarantee conductive network selfreparing in polymeric matrix.Therefore into
One step, which researchs and develops one kind, has very good mechanical properties, while having the electrode material of self-healing properties is current urgent need to resolve
Problem.
Summary of the invention
It is an object of the invention to overcome the shortcomings of existing selfreparing electrode material, provide a kind of based on supermolecule dual network
The preparation method of the selfreparing electrode material of structure.
The preparation method of a kind of selfreparing electrode material based on supermolecule dual network structure proposed by the present invention, with other
Selfreparing electrode material preparation method is compared to its advantage: synthetic method is simple and efficient and material has biocompatibility, electrode
Material not only has excellent selfreparing engineering properties and the rheological equationm of state, while matrix network selfreparing energy band moving conductive network is certainly
It repairs, and this process does not have any restrictions, does not need environmental stimuli, can carry out at any temperature.
A kind of preparation method of selfreparing electrode material based on supermolecule dual network structure proposed by the present invention is specific to walk
It is rapid as follows:
(1) it weighs 1-10 mg boric acid and the hydroxy-end capped dimethyl silicone polymer of 1 ~ 10 g is added in reaction flask, sufficiently stir
It mixes, is completely dispersed boric acid, obtain mebor；
(2) it weighs 0.1-1g crosslinking agent and 1 ~ 10 g commercialization silica gel is added in reaction flask, be sufficiently stirred, divide crosslinking agent completely
It dissipates, obtains commercial silica-gel mixture；
(3) in the case where being kept stirring, the commercial silica-gel mixture that step (2) obtains is added dropwise to step (1) and is obtained
Mebor in, in 115-125 DEG C of reaction 6-24h in vacuum drying oven, reaction flask is cooled to room temperature after reaction,
Colorless and transparent solid is obtained, is elastomer；
(4) silicic acid anhydride is carried out to substrate, i.e., by 1H, 1H, 2H, 2H-perfluoro capryl trichlorosilane, which is dissolved in n-hexane, matches
At the solution of 2-5mol/mL, substrate is impregnated into wherein 1h, it is dry after taking out, it is then placed at 150 DEG C 1 hour dry；
(5) conductive network solution is evenly coated in step (4) treated in substrate, formed several microns of film, be placed on vacuum
It is dry in baking oven, obtain the conductive film of nanometer grade thickness；
(6) elastomer that step (4) obtains is covered on the conductive film that step (5) obtains, conductive film is made to be covered on bullet
Property body lower surface, then peel, just be covered with the conducing composite material of conductive network to surface, or by conductive network with it is elastic
After body is sufficiently mixed, solidification obtains isotropic conducing composite material, and the conducing composite material is to review one's lessons by oneself overlying electrode material
Material.
In the present invention, reaction flask described in step (1) and step (2) is 10 ~ 100 mL.
In the present invention, dimethyl silicone polymer molecular weight described in step (1) is 7.7 kg/mol-117 kg/mol.
In the present invention, substrate described in step (4) is to appoint in the various materials for possessing flat surface such as silicon wafer or glass plate
It is a kind of.
In the present invention, conductive network solution described in step (5) is metallic particles, metal wire, sheet metal, carbon nanomaterial
It is any in (including carbon black, carbon nanotube, graphene, redox graphene) or conducting ceramic material etc..
The present invention has the advantages that compared with existing preparation selfreparing electrode material method
1, the preparation method of a kind of selfreparing electrode material based on supermolecule dual network structure proposed by the present invention.Synthetic method
It is simple and efficient, material has biocompatibility, and not only with the engineering properties and the rheological equationm of state of selfreparing, while matrix network is certainly
The network selfreparing of energy band moving conductive is repaired, and this process does not have any restrictions, does not need environmental stimuli, it can be in any temperature
Degree is lower to carry out.
2, this method can be by the proportion of two kinds of network structures of change, so that material property is controllable, to make it have
Targetedly apply.
3, self-repair material made from this method can restore completely electric property in 25 minutes at normal temperature
4, self-repair material made from this method is provided simultaneously with from adhesion, convenient for being bonded skin with the compound preparation of conductive material
Body electrode's material.
Detailed description of the invention
Fig. 1 is the schematic network structure for preparing poly- borosilicate alkane/dimethyl silicone polymer composite material.
Fig. 2 is PDMS, the infrared spectrum of PBS, PDMS/PBS.
Fig. 3 is the photo for the Self-repair Composites that the preparation of example 1 is applied in experiment.
Fig. 4 is that the conductive material used in embodiment 1 is prepared into the stretchable antenna of selfreparing, and resonance frequency is answered with stretching
The variation and its selfreparing effect of change.
Fig. 5 is the human body electrocardio figure that conductive material obtained in embodiment 1 is measured.
Specific embodiment
Above scheme is described further below in conjunction with specific embodiment.It should be understood that these embodiments are for illustrating
The present invention and be not limited to limit the scope of the invention.Implementation condition used in the examples can be done according to the condition of specific producer
Further adjustment, the implementation condition being not specified is usually the condition in routine experiment.
Below with reference to embodiment, the present invention will be described in detail, it should be understood that citing described herein is only used to explain this
Invention, is not intended to limit the present invention.
Embodiment 1
(1) boric acid and hydroxy-end capped dimethyl silicone polymer are weighed, is added in reaction flask with the mass ratio of 1:1, is sufficiently stirred
It mixes, is completely dispersed boric acid, obtain mebor；
(2) crosslinking agent and 2g commercialization silica gel for weighing 0.2g commercialization silica gel are added in reaction flask, are sufficiently stirred, are made crosslinking agent
It is completely dispersed, obtains commercial silica-gel mixture；
(3) in the case where being kept stirring, the commercial silica-gel mixture that step (2) obtains is added dropwise to 10 wt% ratios
It is after reaction, reaction flask is cooling in 120 DEG C of 24 h of reaction in vacuum drying oven in the mebor that step (1) obtains
To room temperature, colorless and transparent solid, as elastomer are obtained；
(4) silicic acid anhydride is carried out to substrate, i.e., by 1H, 1H, 2H, 2H-perfluoro capryl trichlorosilane, which is dissolved in n-hexane, matches
At the solution of 2-5mol/mL, substrate is impregnated into wherein 1 h, it is dry after taking out, it is then placed at 150 DEG C and toasts 1 hour.
(5) conductive network solution is evenly coated in step (4) treated in substrate, formed several microns of film and be placed on very
It is dry in empty baking oven, obtain the conductive film of nanometer grade thickness；The elastomer that step (3) obtains is covered on nanoscale conduction
On film, so that conductive film is covered on elastomer lower surface, then peel, so that it may obtain to surface and be covered with leading for conductive network
Composite；Or will be compound with the progress of 1 to 3 weight ratio with conductive silver sheet material by elastomer, obtain conducing composite material.
Embodiment 2: same as Example 1, dimethyl silicone polymer molecular weight described in step (1) is 85 kg/mol.
Embodiment 3: the stoichiometric ratio of boric acid described in step (1) and dimethyl silicone polymer is 1.
Embodiment 4: crosslinking agent described in step (2) is 0.1 with commercial silica gel quality ratio.
Embodiment 5: commercial silica gel is 70 wt% in silica-gel mixture weight percent in step (3).
Embodiment 6: it is same as Example 1, but commercial silica gel in silica-gel mixture weight percent is 90 in step (3)
wt%。
Embodiment 7: it is same as Example 1, but the conductive one-dimensional material such as conductive network solution carbon nanotube in step (4)
Material.
Embodiment 8: it is same as Example 1, but conductive material is changed to the conductive fillers such as graphene in step (5).
Fig. 1 is the reaction schematic diagram for preparing poly- borosilicate alkane/dimethyl silicone polymer composite material.Fig. 2 is PDMS, PBS,
The infrared spectrum of PDMS/PBS.As can be seen from the figure the reaction of two networks is mutually indepedent, does not influence mutually.Fig. 3 is to implement
The photo of Self-repair Composites prepared by example 1, therefrom it can be seen that the different degrees of diffusion of material agglutination dyestuff, and
Light microscopic lower cut gradually heals.Fig. 4 is that the conductive material used in embodiment 1 is prepared into the stretchable antenna of selfreparing, resonance
Frequency with elongation strain variation and its selfreparing effect.As can be seen from the figure conductive antenna is excellent, excludes signal interference
It is very capable, can accurate response go out strain variation and lead to the change of resonance frequency, and still have function after material fracture
Property.Fig. 5 is the human body electrocardio figure that conductive material obtained in embodiment 5 is measured.It can be seen that can by electrode prepared by the present invention
To obtain stable electrocardiosignal, the peak of feature electrocardiogram is high-visible, and still has functionality after material fracture.
The above embodiments merely illustrate the technical concept and features of the present invention, and its object is to allow person skilled in the art
It is to can understand the content of the present invention and implement it accordingly, it is not intended to limit the scope of the present invention.It is all according to the present invention
The equivalent transformation or modification that Spirit Essence is done, should be covered by the protection scope of the present invention.
Claims (5)
1. a kind of preparation method of the selfreparing electrode material based on supermolecule dual network structure, it is characterised in that specific steps are such as
Under:
(1) it weighs 1-10 mg boric acid and the hydroxy-end capped dimethyl silicone polymer of 1 ~ 10 g is added in reaction flask, sufficiently stir
It mixes, is completely dispersed boric acid, obtain mebor；
(2) it weighs 0.1-1g crosslinking agent and 1 ~ 10 g commercialization silica gel is added in reaction flask, be sufficiently stirred, divide crosslinking agent completely
It dissipates, obtains commercial silica-gel mixture；
(3) in the case where being kept stirring, the commercial silica-gel mixture that step (2) obtains is added dropwise to step (1) and is obtained
Mebor in, in 115-125 DEG C of reaction 6-24h in vacuum drying oven, reaction flask is cooled to room temperature after reaction,
Colorless and transparent solid is obtained, is elastomer；
(4) silicic acid anhydride is carried out to substrate, i.e., by 1H, 1H, 2H, 2H-perfluoro capryl trichlorosilane, which is dissolved in n-hexane, matches
At the solution of 2-5mol/mL, substrate is impregnated into wherein 1h, it is dry after taking out, it is then placed at 150 DEG C 1 hour dry；
(5) conductive network solution is evenly coated in step (4) treated in substrate, formed several microns of film, be placed on vacuum
It is dry in baking oven, obtain the conductive film of nanometer grade thickness；
(6) elastomer that step (4) obtains is covered on the conductive film that step (5) obtains, conductive film is made to be covered on bullet
Property body lower surface, then peel, just be covered with the conducing composite material of conductive network to surface, or by conductive network with it is elastic
After body is sufficiently mixed, solidification obtains isotropic conducing composite material, and the conducing composite material is to review one's lessons by oneself overlying electrode material
Material.
2. preparation method according to claim 1, it is characterised in that reaction flask described in step (1) and step (2) be 10 ~
100 mL。
3. preparation method according to claim 1, it is characterised in that dimethyl silicone polymer molecular weight described in step (1)
For 7.7 kg/mol-117 kg/mol.
4. preparation method according to claim 1, it is characterised in that substrate described in step (4) is in silicon wafer or glass plate
It is any.
5. preparation method according to claim 1, it is characterised in that conductive network solution described in step (5) is metal
It is any in grain, metal wire, sheet metal, carbon nanomaterial or conducting ceramic material.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113462281A (en) * | 2021-06-22 | 2021-10-01 | 复旦大学 | Method for enhancing adhesion of silicon rubber material |
| CN113462315A (en) * | 2021-06-22 | 2021-10-01 | 复旦大学 | Method for enhancing adhesion of silicon-based flexible conductive adhesive material |
| CN114141428A (en) * | 2021-11-12 | 2022-03-04 | 复旦大学 | Preparation method of ultrafast self-repairing, high-viscosity and deformable silicon rubber electrode material |
| CN115321829A (en) * | 2022-02-22 | 2022-11-11 | 江苏铁锚玻璃股份有限公司 | Fluoride-free and self-repairable super-hydrophobic glass and preparation method thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN113462281A (en) * | 2021-06-22 | 2021-10-01 | 复旦大学 | Method for enhancing adhesion of silicon rubber material |
| CN113462315A (en) * | 2021-06-22 | 2021-10-01 | 复旦大学 | Method for enhancing adhesion of silicon-based flexible conductive adhesive material |
| CN114141428A (en) * | 2021-11-12 | 2022-03-04 | 复旦大学 | Preparation method of ultrafast self-repairing, high-viscosity and deformable silicon rubber electrode material |
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| CN115321829A (en) * | 2022-02-22 | 2022-11-11 | 江苏铁锚玻璃股份有限公司 | Fluoride-free and self-repairable super-hydrophobic glass and preparation method thereof |
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