CN108053946B - A kind of preparation method of stretchable, low resistance variation conductive fiber - Google Patents
A kind of preparation method of stretchable, low resistance variation conductive fiber Download PDFInfo
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- CN108053946B CN108053946B CN201711236658.2A CN201711236658A CN108053946B CN 108053946 B CN108053946 B CN 108053946B CN 201711236658 A CN201711236658 A CN 201711236658A CN 108053946 B CN108053946 B CN 108053946B
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- H01B13/008—Apparatus or processes specially adapted for manufacturing conductors or cables for manufacturing extensible conductors or cables
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- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/06—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the coating material
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- C23C14/20—Metallic material, boron or silicon on organic substrates
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- C—CHEMISTRY; METALLURGY
- C23—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; CHEMICAL SURFACE TREATMENT; DIFFUSION TREATMENT OF METALLIC MATERIAL; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL; INHIBITING CORROSION OF METALLIC MATERIAL OR INCRUSTATION IN GENERAL
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- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
- C23C14/22—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material characterised by the process of coating
- C23C14/24—Vacuum evaporation
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- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F1/00—General methods for the manufacture of artificial filaments or the like
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F6/00—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof
- D01F6/88—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds
- D01F6/94—Monocomponent artificial filaments or the like of synthetic polymers; Manufacture thereof from mixtures of polycondensation products as major constituent with other polymers or low-molecular-weight compounds of other polycondensation products
Abstract
The preparation method of stretchable, low resistance variation the conductive fiber of one kind disclosed by the invention is the following steps are included: dimethyl silicone polymer is added drop-wise on the water surface, heat treatment, then go out polydimethylsiloxanefilm film from the sur-face peeling of water, to prepare polydimethylsiloxanefilm film；With metal evaporation instrument in the polydimethylsiloxanefilm film deposited metal film, as conductive layer；There is the polydimethylsiloxanefilm film of metal film to be laid on substrate load, is rolled up and is prepared into the conductive fiber.Conductive fiber has the characteristics that stretchable, low resistance variation, and preparation method is simple, preparation condition is mild, has far reaching significance to further exploitation, the popularization of flexible electrode and flexible electronic.
Description
Technical field
The present invention relates to fields prepared by the fields such as flexible electronic, sensing more particularly to stretchable electrode and conductor, specifically
It is related to a kind of preparation method of stretchable, low resistance variation conductive fiber.
Background technique
In recent years, stretchable device causes the extensive concern of people.Stretchable device is that flexible device further develops
Trend, and have very big market.It is wearable device that stretchable device is oriented in human-computer interaction, intelligent health monitoring, soft
Property robot, energy storage field wilderness demand under have development at full speed.These devices change people for medical treatment and
The cognition and behavior of health field, while bionic machine man-based development is also promoted, even more open up flexible energy storage
The market of equipment.
A large amount of flexible sensor currently, germinating in flexible electronic field, such as pliable pressure sensor, flexible drawing
Force snesor etc., while also having expedited the emergence of the equipment such as flexible super capacitor, flexible battery.In these devices, stretchable electrode
A vital role is played in electronic component wherein.Such as in flexible super capacitor and flexible battery
In, stretchable electrode is used to collected current；In flexible sensor, stretchable electrode be used to docile in human skin surface or
Organization internal collects physiological signal etc..
Why will we make electrode stretchable in practical applications? such as when we with implant electrode measure heart or
When the electric signal of other organs of person, heart is moved in beating heart, so the surface of heart can be continued for the generation of deformation.
This when, we can be good at docile in heart surface by desired electrode, must just assign the tensility of electrode.If electric
Pole is rigid, then will cause to damage to heart and histoorgan.
In this case, the electric conductivity that electrode can also be kept when electrode has deformation is that we need to go to solve
The problem of.When stretchable electrode is transformed into non-conductive by conduction when being stretched, this point stretched is the catastrophe point of electrode.Mesh
Before for, in the stretchable electrode using flexible resilient as substrate to prepare, the maximum drawing for stretching mutation and being up to 13 times
Elongation.Wherein common flexible substrates have the macromolecular elastomers such as dimethyl silicone polymer (PDMS), common conductive material
There are metal, carbon material and some conducting polymers such as polypyrrole etc..However, conductive material is usually rigid material, for example, it is golden
Maximum tensile strength there was only 5 percent.So conductive material is prepared into bending or spring in some strategies
Shape, be then supported in flexible substrates realize it is stretchable.But the flexible extensible electrode of this method preparation can only be from device
The both ends of part are gone to stretch, and conductive material is substantially or rigid material.If electrode micro-meter scale local pressure or some
The conductive material of unit stress, electrode will be damaged.
In face of these problems, by the strategy of network micro-structure and micro-cracked structure can the stress of stretching by crackle come
The problem of discharging, thus can solve electrode local pressure.But in practical applications, metal film generates fine fisssure when stretching
Line will cause the substantially increase of resistance, can have an impact to electrode collecting signal.
Summary of the invention
The purpose of the present invention is to provide the purpose of the present invention is to provide a kind of stretchable, low resistance variation conduction is fine
The preparation method of dimension, solves one or more of the above-mentioned prior art problem.Present invention incorporates macromolecular elastomers certainly
The characteristics of characteristic of body and characteristic of electrical-conductive nanometer film, self encapsulation layer by layer having using fiber spiral shape structure itself,
Devise a kind of method for preparing stretchable conductive fiber of simple process.
The english abbreviation of dimethyl silicone polymer in the present invention is PDMS, and PDMS monomer is from Sigma-Aldrich
The purchase of (Shanghai) trade Co., Ltd.
The present invention a kind of preparation method of stretchable, low resistance variation conductive fiber is provided the following steps are included:
S1, dimethyl silicone polymer is added drop-wise on the water surface, heats, then goes out poly dimethyl from the sur-face peeling of water
Siloxane film, to prepare polydimethylsiloxanefilm film；
S2, with metal evaporation instrument in the polydimethylsiloxanefilm film deposited metal film, as conductive layer；
S3, there is the polydimethylsiloxanefilm film of metal film to be laid on substrate load, be rolled up described in being prepared into
Conductive fiber.
The draftability of the conductive fiber of this method preparation is equal to the property of dimethyl silicone polymer, can stretch 100%
More than.
In some embodiments, the temperature heated in step S1 is 60 DEG C, time 2h.
In some embodiments, the polydimethylsiloxanefilm film that step S1 is obtained with a thickness of 10~20 μm.
Preferably, polydimethylsiloxanefilm film with a thickness of 10 μm.
In some embodiments, the metal film being deposited in step S2 is golden film.
In some embodiments, the metal film being deposited in step S2 with a thickness of 40~120nm.
Preferred metal film with a thickness of 60nm.
In some embodiments, the method being deposited in step S2 is to be vapor deposition raw material with metallic particles, vacuum is deposited
Degree is 2.0 × 10-6Torr, evaporation rate arePallet rotation speed is 30rpm.
In some embodiments, the substrate in step S3 is one of silicon wafer, sapphire sheet, polymer plastic piece.
Wherein, polymer plastic piece includes PTFE plastic sheet, POM plastic piece or PE plastic sheet.
Preferably, substrate is silicon wafer.
In some embodiments, dimethyl silicone polymer preparation method the following steps are included:
A1, dimethyl silicone polymer monomer and crosslinking agent are mixed with mass ratio 10:1, and are stirred；
A2, it will be uniformly mixed dimethyl silicone polymer in the step A1 and is placed in vacuum desiccator and removes bubble removing, temperature
Degree is room temperature, and the pumpdown time is 30min or so.
In some embodiments, conductive fiber diameter is 350~800 μm.
Preferably, conductive fiber diameter is 400 μm.
Wherein, the conductive fiber for diameter at 400 μm or so, resistance are about 50 Ohms per centimeters.The conduction is fine
It ties up when stretching 50% tensile elongation, resistance increases 50% or so；When fiber is stretched to 100%, resistance increases 3 times of left sides
It is right.Illustrate, after which is stretched, resistance variations are low.
In some embodiments, the coiling method in step S3 is that the PDMS film that upper metal film is deposited is laid in
It seals on adhesive plaster, it is then that PDMS film cut growth is rectangular, it is started to curl up by a side of PDMS film, with the side of helix-coil
PDMS film is rolled into the stretchable electrode of threadiness by formula, and golden film is crimped onto the internal layer of PDMS film, achievees the effect that encapsulation, and
Liquid metal, connection line are coated at the both ends of fiber electrode.
Wherein, liquid metal is eutectic gallium-indium liquid metal, from Sigma-Aldrich (Shanghai) trade Co., Ltd
Purchase.
The utility model has the advantages that
1, the embodiment of the present invention is can to overcome tradition using the stretchable electrode of metal micro-nano network structure preparation
Stretchable electrode is in local pressure, the problem of being easily destroyed；
2, fiber spiral structure is utilized in the embodiment of the present invention, has the effect of encapsulating layer by layer, can effectively inhibit
Gold nanometer film generates the extension of micro-crack when stretching, so as to keep satisfactory electrical conductivity；
3, the stretchable fiber electrode of the embodiment of the present invention is encapsulated in metal conducting layer inside macromolecule membrane, effectively
Protection metal conducting layer, keep the stability in use and high reusability of the fiber；
4, stretchable, low resistance variation the conductive fiber of the embodiment of the present invention preparation, preparation method is simple, prepares item
Part is mild, has far reaching significance to further exploitation, the popularization of flexible electrode and flexible electronic.
Detailed description of the invention
Fig. 1 is the pictorial diagram of conductive fiber in an embodiment of the present invention；
Fig. 2 be an embodiment of the present invention in conductive fiber be stretched 50% when golden film micro-crack microscope figure；
The microscope figure of the conductive fiber of Fig. 3 different-diameter；
The polydimethylsiloxanefilm film of Fig. 4 normal load golden film and conductive fiber be stretched 50% when resistance variations
Comparison diagram；
The load of Fig. 5 comparative example preparation has the pictorial diagram of the polydimethylsiloxanefilm film of golden film；
In Fig. 6 comparative example the polydimethylsiloxanefilm film of normal load golden film be stretched 50% when golden film fine fisssure
The microscope figure of line.
Specific embodiment
With reference to the accompanying drawings of the specification, the present invention is described in more detail.
Embodiment 1:
A kind of preparation method of the conductive fiber of stretchable, low resistance variation the following steps are included:
The preparation of α 1, PDMS film: being mixed PDMS monomer and crosslinking agent with the mass ratio of 10:1 first, stirring
5min, uniformly mixed PDMS are placed on bubble removing in vacuum desiccator, then pour into the culture dish that diameter is 18cm suitable
Deionized water is measured, few drops of surfaces in deionized water are added dropwise in the PDMS in addition to bubble, culture dish is finally placed 60 DEG C of baking ovens,
After 2h, PDMS film can be stripped out from the water surface, by adjusting the amount that PDMS is added dropwise, the thin of different-thickness can be prepared
Film.By the way that the PDMS of 25 μ L is added dropwise, the film thickness of preparation is probably at 10 μm.
The preparation of α 2, conductive layer: PDMS film after water surface removing, 60 DEG C of baking oven drying 30min are placed to remove
Deionized water on the surface PDMS is then placed on the pallet of hot evaporation instrument.The condition of hot evaporation are as follows: with gold particle be steam
Raw material are plated, vapor deposition vacuum degree is 2.0 × 10-6Torr, and evaporation rate isPallet rotation speed is 30rpm,
Evaporation time is 1333s, and golden film is deposited with a thickness of 40nm.
The preparation of α 3, conductive fiber: the PDMS film that upper golden film is deposited is laid on silicon wafer, then PDMS film is cut
It is cut into rectangle, is started to curl up by a side of PDMS film, PDMS film, which is rolled into threadiness, in a manner of helix-coil to draw
Electrode is stretched, and golden film is crimped onto the internal layer of PDMS film, achievees the effect that encapsulation, as shown in Figure 1, and at the both ends of fiber electrode
Coat liquid metal, connection line.We are using the film curling having a size of 4cm*1cm wide, as shown in Figure 3a, finally, obtaining
Conductive fiber diameter be 382.03 μm, length 4cm.
Embodiment 2:
A kind of preparation method of the conductive fiber of stretchable, low resistance variation the following steps are included:
The preparation of β 1, PDMS film: being mixed PDMS monomer and crosslinking agent with the mass ratio of 10:1 first, stirring
5min, uniformly mixed PDMS are placed on bubble removing in vacuum desiccator, then pour into the culture dish that diameter is 18cm suitable
Deionized water is measured, few drops of surfaces in deionized water are added dropwise in the PDMS in addition to bubble, culture dish is finally placed 60 DEG C of baking ovens,
After 2h, PDMS film can be stripped out from the water surface, by adjusting be added dropwise PDMS amount, available different-thickness it is thin
Film.By the way that the PDMS of 32.5 μ L is added dropwise, the film thickness of preparation is about 13 μm.
The preparation of β 2, conductive layer: PDMS film after water surface removing, 60 DEG C of baking oven drying 30min are placed to remove
Deionized water on the surface PDMS is then placed on the pallet of hot evaporation instrument.The condition of hot evaporation are as follows: with gold particle be steam
Raw material are plated, vapor deposition vacuum degree is 2.0 × 10-6Torr, and evaporation rate isPallet rotation speed is 30rpm,
Evaporation time is 1667s, and golden film is deposited with a thickness of 50nm.
The preparation of β 3, conductive fiber: the PDMS film that upper golden film is deposited is laid in POM plastic on piece, then PDMS
Film cut growth is rectangular, is started to curl up by a side of PDMS film, PDMS film is rolled into fiber in a manner of helix-coil
The stretchable electrode of shape, and golden film is crimped onto the internal layer of PDMS film, achieve the effect that encapsulation, and coat at the both ends of fiber electrode
Liquid metal, connection line.We are using the film curling having a size of 4cm*2cm wide, as shown in Figure 3b, finally, what is obtained leads
Electric fibre diameter is 576.01 μm, length 4cm.
Embodiment 3:
A kind of preparation method of the conductive fiber of stretchable, low resistance variation the following steps are included:
The preparation of γ 1, PDMS film: PDMS monomer and crosslinking agent are mixed with the mass ratio of 10:1 first, stirred
5min is mixed, uniformly mixed PDMS is placed on bubble removing in vacuum desiccator, then pours into the culture dish that diameter is 18cm
PDMS in addition to bubble is added dropwise few drops of surfaces in deionized water, culture dish is finally placed 60 DEG C of bakings by appropriate amount of deionized water
Case after 2h, can be stripped out PDMS film from the water surface, by adjusting the amount that PDMS is added dropwise, available different-thickness
Film.By the way that the PDMS of 37.5 μ L is added dropwise, the film thickness of preparation is about 15 μm.
The preparation of γ 2, conductive layer: PDMS film after water surface removing, 60 DEG C of baking oven drying 30min are placed to remove
Deionized water on the surface PDMS is then placed on the pallet of hot evaporation instrument.The condition of hot evaporation are as follows: with gold particle be steam
Raw material are plated, vapor deposition vacuum degree is 2.0 × 10-6Torr, and evaporation rate isPallet rotation speed is 30rpm,
Evaporation time is 2000s, and golden film is deposited with a thickness of 60nm.
The preparation of γ 3, conductive fiber: being laid in the PDMS film that upper golden film is deposited on PTFE plastic sheet, then
PDMS film cut growth is rectangular, is started to curl up by a side of PDMS film, PDMS film is rolled into a manner of helix-coil
The stretchable electrode of threadiness, and golden film is crimped onto the internal layer of PDMS film, achieve the effect that encapsulation, and at the both ends of fiber electrode
Coat liquid metal, connection line.We are using the film curling having a size of 4cm*3cm wide, as shown in Figure 3c, finally, obtaining
Conductive fiber diameter be 643.09 μm, length 4cm.
Embodiment 4:
A kind of preparation method of the conductive fiber of stretchable, low resistance variation the following steps are included:
The preparation of θ 1, PDMS film: being mixed PDMS monomer and crosslinking agent with the mass ratio of 10:1 first, stirring
5min, uniformly mixed PDMS are placed on bubble removing in vacuum desiccator, then pour into the culture dish that diameter is 18cm suitable
Deionized water is measured, few drops of surfaces in deionized water are added dropwise in the PDMS in addition to bubble, culture dish is finally placed 60 DEG C of baking ovens,
After 2h, PDMS film can be stripped out from the water surface, by adjusting be added dropwise PDMS amount, available different-thickness it is thin
Film.By the way that the PDMS of 50 μ L is added dropwise, the film thickness of preparation is about 20 μm.
The preparation of θ 2, conductive layer: PDMS film after water surface removing, 60 DEG C of baking oven drying 30min are placed to remove
Deionized water on the surface PDMS is then placed on the pallet of hot evaporation instrument.The condition of hot evaporation are as follows: with gold particle be steam
Raw material are plated, vapor deposition vacuum degree is 2.0 × 10-6Torr, and evaporation rate isPallet rotation speed is 30rpm,
Evaporation time is 4000s, and golden film is deposited with a thickness of 120nm.
The preparation of θ 3, conductive fiber: being laid in the PDMS film that upper golden film is deposited in sapphire sheet, then that PDMS is thin
Film cut growth is rectangular, is started to curl up by a side of PDMS film, PDMS film is rolled into threadiness in a manner of helix-coil
Stretchable electrode, and golden film is crimped onto the internal layer of PDMS film, achieve the effect that encapsulation, and apply upper liquid at the both ends of fiber electrode
State metal, connection line.We are using the film curling having a size of 4cm*4cm wide, as shown in Figure 3d, finally, obtained conduction
Fibre diameter is 784.66 μm, length 4cm.
Comparative example 1:
Take the load prepared in 1 step of embodiment to have the polydimethylsiloxanefilm film of golden film, be cut into long 2 centimetres,
Wide 1 centimetre of sample, sample are as shown in Figure 5.
Performance test: by microscopic after the sample of embodiment 1 and comparative example 1 is stretched 50%, and its electricity is tested
Resistive.
As shown in Fig. 2, the conductive fiber of embodiment 1 be stretched 50% when golden film micro-crack microscope figure, from figure
In it is found that the micro-crack size on conductive fiber is smaller, be able to maintain more conductive paths.
As shown in fig. 6, the polydimethylsiloxanefilm film of comparative example 1 be stretched 50% when golden film micro-crack microscope
Figure, it can be seen that polydimethylsiloxanefilm film be stretched after on micro-crack size be significantly greater than case of the present invention in lead
Electric fiber be stretched after micro-crack, it is larger so as to cause resistance variations.
As shown in figure 4, the normal load polydimethylsiloxanefilm film of golden film and the conduction of embodiment 1 in comparative example 1
Fiber be stretched 50% when resistance variations comparison diagram, it can be seen that illustrate the embodiment of the present invention conductive fiber stretch after
Resistance variations have apparent reduction relative to the polydimethylsiloxanefilm film resistance variations that are stretched.
The conductive fiber of the embodiment of the present application has the characteristics that stretchable, low resistance variation, and preparation method is simple, system
Standby mild condition has far reaching significance to further exploitation, the popularization of flexible electrode and flexible electronic.
The above statement is only preferred embodiment of the invention, it is noted that those skilled in the art, not
Under the premise of being detached from the invention design, various modifications and improvements can be made, these also should be regarded as protection of the invention
Within the scope of.
Claims (9)
1. a kind of preparation method of stretchable, low resistance variation conductive fiber, which comprises the following steps:
S1, dimethyl silicone polymer is added drop-wise on the water surface, heats, then goes out polydimethylsiloxanes from the sur-face peeling of water
Alkane film, to prepare polydimethylsiloxanefilm film；
S2, with metal evaporation instrument in the polydimethylsiloxanefilm film deposited metal film, as conductive layer；
S3, the polydimethylsiloxanefilm film of metal film is laid on substrate load, by polydimethylsiloxanefilm film
One side starts to curl up, and polydimethylsiloxanefilm film is rolled into threadiness in a manner of helix-coil, and metal film is crimped
Polydimethylsiloxanefilm film internal layer to get arrive the conductive fiber.
2. one kind according to claim 1 is stretchable, the preparation method of the conductive fiber of low resistance variation, feature exists
In the temperature heated in the step S1 is 60 DEG C, time 2h.
3. one kind according to claim 1 is stretchable, the preparation method of the conductive fiber of low resistance variation, feature exists
In, the polydimethylsiloxanefilm film that the step S1 is obtained with a thickness of 10~20 μm.
4. one kind according to claim 1 is stretchable, the preparation method of the conductive fiber of low resistance variation, feature exists
In the metal film being deposited in the step S2 is golden film.
5. one kind according to claim 1 is stretchable, the preparation method of the conductive fiber of low resistance variation, feature exists
In, the metal film being deposited in the step S2 with a thickness of 40~120nm.
6. one kind according to claim 1 is stretchable, the preparation method of the conductive fiber of low resistance variation, feature exists
In it is vapor deposition raw material with metallic particles that the method being deposited in the step S2, which is, and vapor deposition vacuum degree is 2.0 × 10-6Torr,
Evaporation rate isPallet rotation speed is 30rpm.
7. one kind according to claim 1 is stretchable, the preparation method of the conductive fiber of low resistance variation, feature exists
In the substrate in the step S3 is one of silicon wafer, sapphire sheet, polymer plastic piece.
8. one kind according to claim 1 is stretchable, the preparation method of the conductive fiber of low resistance variation, feature exists
In, the dimethyl silicone polymer preparation method the following steps are included:
A1, dimethyl silicone polymer monomer and crosslinking agent are mixed with mass ratio 10:1, and are stirred；
A2, it will be uniformly mixed dimethyl silicone polymer in the step A1 and is placed in vacuum desiccator and removes bubble removing, temperature is
Room temperature, pumpdown time 30min.
9. one kind according to claim 1 is stretchable, the preparation method of the conductive fiber of low resistance variation, feature exists
In the conductive fiber diameter is 350~800 μm.
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| CN110284210B (en) * | 2019-06-17 | 2022-04-05 | 深圳第三代半导体研究院 | Flexible stretchable fiber with internal microstructure and preparation method and application thereof |
| CN113061285B (en) * | 2021-02-26 | 2021-10-22 | 中国科学院深圳先进技术研究院 | Preparation method of ultrathin porous stretchable film electrode |
| CN114360809A (en) * | 2021-12-01 | 2022-04-15 | 中国科学院深圳先进技术研究院 | Preparation method of ultrathin stretchable film electrode |
| CN114672896B (en) * | 2022-03-16 | 2023-02-14 | 华中科技大学 | Preparation method of polydimethylsiloxane fiber and polydimethylsiloxane fiber |
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| CN107034679A (en) * | 2017-05-17 | 2017-08-11 | 东华大学 | A kind of self-driven human action based on sheath core structural friction generator catches sensor and preparation method thereof |
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