CN109135567A - A kind of laminated film and preparation method for flexible electronic skin - Google Patents
A kind of laminated film and preparation method for flexible electronic skin Download PDFInfo
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Abstract
The invention belongs to the technical fields of electronic skin, provide a kind of laminated film and preparation method for flexible electronic skin.This method is as restoring graphene oxide film made from spin coating using hydroiodic acid, then fibroin is added dropwise on surface and air-dries film forming, laser ablation is recycled to produce the grating of periodic structure in film surface, surface is coated on after dimethyl silicone polymer is finally dissolved in dimethylformamide, the laminated film for flexible electronic skin is made in film-forming.It is compared with the traditional method, the laminated film of preparation of the invention, the mechanical property and tensile property of film are not only significantly improved by the addition of fibroin albumen, and dimethyl silicone polymer is deposited on laser ablation optical grating construction, improve the flexibility of the film, the electronic skin being prepared can be made flexible, tensile strength is high, is not easily broken, and can be widely used for electronic skin field.
Description
Technical field
The invention belongs to the technical fields of electronic skin, provide a kind of laminated film and system for flexible electronic skin
Preparation Method.
Background technique
Electronic skin also known as novel wearable flexible bionic touch sensor, are the electronic equipments being attached on " skin ", because
And habitually it is referred to as electronic skin.Compared to traditional rigid touch sensor, the more frivolous softness of electronic skin can quilt
It is processed into various shape, the body surface of human body either robot is attached to as clothes, it is made to have feeling and tactile.
Currently, electronic skin is mainly used in human body physiological parameter detection and robot flexibility touch sensor two is led greatly
Domain.By the way that electronic skin is installed to the corresponding key position of human body, to realize that human heart rate, blood pressure, muscle tone etc. are raw
Manage the detection of parameter.By the way that electronic skin is attached to robot finger, on arm, so that robot obtains the extraneous touching of impression
Touch the ability of power.The key of electronic skin is the research and development application of new material, have high-intensitive, highly sensitive composite material at
For first choice.
In recent years, graphene is widely used in electronic skin because of its excellent physicochemical properties, electronic transmission performance, existing
There is the method for commonly preparing three-dimensional grapheme material to have hydro-thermal method, sol-gal process and vapour deposition process etc., but these
The grapheme material that method obtains is graphically difficult, complex steps and yield during preparing flexible electronic skin material in the later period
It is low, cost of manufacture is high；Meanwhile base material multiselect used in the laminated film manufacturing method of existing flexible electronic skin is used
PDMS, PUA, PI etc., shortcoming are that these materials tensile property itself is not strong, therefore exists for improving graphene composite material
Performance in electronic skin becomes hot subject.
Certain effect has been achieved in terms of electronic skin technology, especially flexible electronic skin material both at home and abroad at present.
Wherein Zhang Ting et al. has invented a kind of Piezoresistive electronic skin and preparation method thereof (Chinese invention patent application number
201310396009.4), the invention Piezoresistive electronic skin uses carbon nano-tube film as conductive layer and has micro-nano pattern
The materials such as dimethyl silicone polymer, poly- polyethylene terephthalate, polyvinyl alcohol, polyvinyl formal, polyethylene be substrate,
So that substrate has many advantages, such as that high flexibility is flexible, and its operating voltage is low, small power consumption, and high sensitivity, response time are short.Separately
Outside, Li great Wei et al. has invented a kind of electronic skin based on native cellulose nanofiber and preparation method thereof (Chinese invention
Number of patent application 201711128891.9), carbon nanotube, graphene, silver nanowires etc. are led using suction filtration or Electrostatic Absorption method
Electric nano material is fixed on imparting tunica fibrosa conductive characteristic on bacteria cellulose (BC) nano fibrous membrane；It will be as the poly- of dielectric layer
Vinyl film is placed among the uniform conductive BC nano fibrous membrane of two panels thickness and constitutes miniature stretchable, compressible capacitor, i.e.,
The electronic skin based on native cellulose nanofiber is made.
As it can be seen that electronic skin film in the prior art, including graphene film flexible electrode, there are unbearable larger
Stress stretches the problems such as threshold range is low, it is not strong to stretch performance, flexible bad and returns, so how to pass through the method for simple low cost
The problem of obtaining the laminated film of flexible electronic skin becomes this field urgent need to resolve.
Summary of the invention
It in response to this, can be significant it is proposed that a kind of laminated film and preparation method for flexible electronic skin
The mechanical property and tensile property of graphene composite film are improved, so that the electronic skin being prepared is flexible, tensile strength
Height is not easily broken.
To achieve the above object, specific technical solution of the present invention is as follows:
A kind of preparation method of the laminated film for flexible electronic skin, by the way that graphene oxide film made from spin coating is sharp
It is restored with hydroiodic acid, fibroin then is added dropwise on surface and air-dries film forming, laser ablation is recycled to produce period knot in film surface
The grating of structure is coated on surface after dimethyl silicone polymer is finally dissolved in dimethylformamide, and film-forming is made for soft
The laminated film of property electronic skin.Specific step is as follows for preparation:
(1) it adds graphene oxide into deionized water, graphene oxide dispersion is made in ultrasonic disperse, then pretreated
Silicon chip surface carries out spin-coating film, and graphene oxide film is made, and then sprays hydroiodic acid and carries out reduction reaction, graphene is made
Film；
(2) silk fibroin water solution that mass concentration is 6 ~ 10% is prepared, the graphene film made from step (1) is then added dropwise
Surface air-dries film forming, then removes from silicon chip surface, and graphene/silk-fibroin flexible conductive film is made；
(3) graphene made from step (2)/silk-fibroin flexible conductive film is subjected to laser ablation, is etched in film surface
There is graphene/silk-fibroin flexible conductive film of optical grating construction on grating with periodic structure, obtained surface；
(4) dimethyl silicone polymer is added in dimethylformamide, ultrasonic disperse is uniform, is then coated with and is made in step (3)
Flexible conductive film surface, the laminated film for flexible electronic skin is made in film-forming.
Preferably, the revolving speed of step (1) described spin-coating film is 600 ~ 800r/min, and spin-coating time is 1 ~ 2h.
Preferably, step (1) silicon wafer is one of monocrystalline silicon piece, polysilicon chip, and silicon wafer thickness is 200 ~ 400 μ
m。
Preferably, the temperature of step (1) described reduction reaction is 100 ~ 120 DEG C, and the reaction time is 50 ~ 70min.
Preferably, the parts by weight of step (1) each raw material are, 10 ~ 15 parts by weight of graphene oxide, deionized water 73 ~
82 parts by weight, 8 ~ 12 parts by weight of hydroiodic acid.
Preferably, the temperature of step (2) the air-dried film forming be 35 ~ 45 DEG C, relative humidity be 30 ~ 35%, wind speed be 0.5 ~
1m/s, film formation time are 8 ~ 12h.
Preferably, the 320 ~ 400nm of optical maser wavelength, 40 ~ 80kHz of laser repetition rate of step (3) described laser ablation.
Preferably, the parts by weight of step (4) each raw material are 20 ~ 40 parts by weight of dimethyl silicone polymer, dimethyl methyl
60 ~ 80 parts by weight of amide.
The innovation of the invention consists in that: it is carved using laser etching techniques on graphene/silk-fibroin flexible conductive film surface
Optical grating construction out is lost, so that the polydimethyl siloxane content being deposited on dramatically increases.The chemical shape of dimethyl silicone polymer
State dimethicone, transparency is high, and there is heat resistance, cold resistance, viscosity to vary with temperature, and small, waterproofness, surface tension are small, have
There is thermal conductivity, it is non-toxic and tasteless, there is physiological inertia, good chemical stability, electrical insulating property and weatherability, hydrophobicity are good, and
With very high anti-shear ability, there is excellent physical characteristic；In the present invention, its special construction (main chain Si-O is utilized
Key, helically type), significantly increase the flexibility of membrane material.In addition, fibroin albumen itself has good mechanical performance and physics and chemistry
Matter, such as good flexibility and tensile strength, breathable moisture permeability, slow release, and good biocompatibility, the present invention pass through
There is excellent mechanical property adding membrane material obtained.
The present invention also provides the laminated films for flexible electronic skin that a kind of above-mentioned preparation method is prepared.It should
Laminated film is to prepare graphene oxide film in silicon chip surface using the method for spin coating, is then reduced into graphene through hydroiodic acid
Film, and then fibroin albumen is added dropwise on graphene film surface, it is removed after air-drying film forming from silicon chip surface, is prepared for a kind of graphite
Alkene/silk-fibroin flexible conductive film；Laser etching techniques are recycled to go out in graphene/silk-fibroin flexible conductive film surface etch
Grating with periodic structure；Dimethyl silicone polymer solution is dissolved in dimethylformamide organic solvents again, is coated
There is upper graphene/silk-fibroin flexible conductive film of optical grating construction on surface；Final curing film forming is made.
The present invention provides a kind of laminated films and preparation method for flexible electronic skin, compared with prior art,
Its feature protruded and excellent effect are:
1. laminated film prepared by the present invention can make the electronic skin being prepared flexible, tensile strength is high, is not easily broken,
It can be widely used for electronic skin field.
2. preparation method of the invention, by adding fibroin albumen in the film, significantly improve film mechanical property and
Tensile property.
3. preparation method of the invention is carved using laser etching techniques on graphene/silk-fibroin flexible conductive film surface
Optical grating construction out is lost, so that the polydimethyl siloxane content being deposited on dramatically increases, significantly improves the flexibility of film.
Specific embodiment
In the following, the present invention will be further described in detail by way of specific embodiments, but this should not be interpreted as to the present invention
Range be only limitted to example below.Without departing from the idea of the above method of the present invention, according to ordinary skill
The various replacements or change that knowledge and customary means are made, should be included in the scope of the present invention.
Embodiment 1
13kg graphene oxide is added in 78kg deionized water, graphene oxide dispersion is made in ultrasonic disperse, then pre-
The monocrystalline silicon sheet surface that the average thickness of processing is 320 μm carries out spin-coating film, revolving speed 710r/min, and spin-coating time is
Graphene oxide film is made in 1.5h, then sprays 9kg hydroiodic acid, and the reduction reaction of 60min, system are carried out at 112 DEG C of temperature
Obtain graphene film；Then the silk fibroin water solution that compound concentration is 7% is added dropwise on graphene film surface, air-dries film forming,
The temperature for air-drying film forming is 42 DEG C, relative humidity 33%, wind speed 0.7m/s, film formation time 11h, then from silicon chip surface
Graphene/silk-fibroin flexible conductive film is made in removing；Film is subjected to laser ablation, optical maser wavelength 370nm, laser repeats
Frequency 50kHz etches the grating with periodic structure in film surface, and there is graphene/silk egg of optical grating construction on obtained surface
White flexible conductive film；Finally 28kg dimethyl silicone polymer is added in 72kg dimethylformamide, ultrasonic disperse is uniform, so
It is coated on flexible conductive film surface afterwards, the laminated film for flexible electronic skin is made in film-forming.
Test method:
(1) flexibility is tested in pendulum impact test: film produced by the present invention being cut into the sample of 100mm × 100mm, much
In 10, tested using the computer-controlled anti-pendulum percussion instrument of the FIT-01 of Labthink blue streak, punch diameter 12.7mm,
Fixture inner ring diameter 89mm, capacity counterweight are 3J, and test result simultaneously calculates average value；
(2) tensile strength and elongation at break test: it is 15mm, length 150mm that film produced by the present invention, which is cut into width,
Sample, no less than 10, LYNZ-W film instron is pleased using water chestnut and is tested, test speed 500mm/
Min, measures the tensile strength of material, and XLW-500N PC elongation at break tester measures the elongation at break of film.
The data obtained is as shown in table 1.
Embodiment 2
10kg graphene oxide is added in 82kg deionized water, graphene oxide dispersion is made in ultrasonic disperse, then pre-
The polysilicon chip surface progress spin-coating film that the average thickness of processing is 200 μm, revolving speed 600r/min, spin-coating time 2h,
Graphene oxide film is made, then sprays 8kg hydroiodic acid, the reduction reaction of 70min is carried out at 100 DEG C of temperature, stone is made
Black alkene film；Then the silk fibroin water solution that compound concentration is 6% is added dropwise on graphene film surface, air-dries film forming, air-dries
The temperature of film forming is 35 DEG C, relative humidity 30%, then wind speed 0.5m/s, film formation time 12h are removed from silicon chip surface,
Graphene/silk-fibroin flexible conductive film is made；Film is subjected to laser ablation, optical maser wavelength 320nm, laser repetition rate
80kHz etches the grating with periodic structure in film surface, and obtained surface has graphene/silk-fibroin of optical grating construction soft
Property conductive film；Finally 20kg dimethyl silicone polymer is added in 80kg dimethylformamide, ultrasonic disperse is uniform, then applies
It is overlying on flexible conductive film surface, the laminated film for flexible electronic skin is made in film-forming.
Test method and embodiment 1 are consistent, and the data obtained is as shown in table 1.
Embodiment 3
11kg graphene oxide is added in 80kg deionized water, graphene oxide dispersion is made in ultrasonic disperse, then pre-
The monocrystalline silicon sheet surface that the average thickness of processing is 50 μm carries out spin-coating film, revolving speed 650r/min, spin-coating time 2h, system
At graphene oxide film, 9kg hydroiodic acid is then sprayed, the reduction reaction of 65min is carried out at 105 DEG C of temperature, graphite is made
Alkene film；Then the silk fibroin water solution that compound concentration is 6 ~ 10% is added dropwise on graphene film surface, air-dries film forming, air-dries
The temperature of film forming is 36 DEG C, relative humidity 32%, then wind speed 0.6m/s, film formation time 11h are removed from silicon chip surface,
Graphene/silk-fibroin flexible conductive film is made；Film is subjected to laser ablation, optical maser wavelength 340nm, laser repetition rate
70kHz etches the grating with periodic structure in film surface, and obtained surface has graphene/silk-fibroin of optical grating construction soft
Property conductive film；Finally 25kg dimethyl silicone polymer is added in 74kg dimethylformamide, ultrasonic disperse is uniform, then applies
It is overlying on flexible conductive film surface, the laminated film for flexible electronic skin is made in film-forming.
Test method and embodiment 1 are consistent, and the data obtained is as shown in table 1.
Embodiment 4
15kg graphene oxide is added in 73kg deionized water, graphene oxide dispersion is made in ultrasonic disperse, then pre-
The polysilicon chip surface progress spin-coating film that the average thickness of processing is 400 μm, revolving speed 800r/min, spin-coating time 1h,
Graphene oxide film is made, then sprays 12kg hydroiodic acid, the reduction reaction of 50min is carried out at 120 DEG C of temperature, stone is made
Black alkene film；Then the silk fibroin water solution that compound concentration is 10% is added dropwise on graphene film surface, air-dries film forming, air-dries
The temperature of film forming is 45 DEG C, relative humidity 35%, and then wind speed 1m/s, film formation time 8h are removed from silicon chip surface, system
Obtain graphene/silk-fibroin flexible conductive film；Film is subjected to laser ablation, optical maser wavelength 400nm, laser repetition rate
40kHz etches the grating with periodic structure in film surface, and obtained surface has graphene/silk-fibroin of optical grating construction soft
Property conductive film；Finally 40kg dimethyl silicone polymer is added in 60kg dimethylformamide, ultrasonic disperse is uniform, then applies
It is overlying on flexible conductive film surface, the laminated film for flexible electronic skin is made in film-forming.
Test method and embodiment 1 are consistent, and the data obtained is as shown in table 1.
Embodiment 5
14kg graphene oxide is added in 75kg deionized water, graphene oxide dispersion is made in ultrasonic disperse, then pre-
The monocrystalline silicon sheet surface progress spin-coating film that the average thickness of processing is 350 μm, revolving speed 750r/min, spin-coating time 1h,
Graphene oxide film is made, then sprays 11kg hydroiodic acid, the reduction reaction of 55min is carried out at 115 DEG C of temperature, stone is made
Black alkene film；Then the silk fibroin water solution that compound concentration is 9% is added dropwise on graphene film surface, air-dries film forming, air-dries
The temperature of film forming is 42 DEG C, relative humidity 34%, then wind speed 0.9m/s, film formation time 9h are removed from silicon chip surface,
Graphene/silk-fibroin flexible conductive film is made；Film is subjected to laser ablation, optical maser wavelength 380nm, laser repetition rate
50kHz etches the grating with periodic structure in film surface, and obtained surface has graphene/silk-fibroin of optical grating construction soft
Property conductive film；Finally 35kg dimethyl silicone polymer is added in 65kg dimethylformamide, ultrasonic disperse is uniform, then applies
It is overlying on flexible conductive film surface, the laminated film for flexible electronic skin is made in film-forming.
Test method and embodiment 1 are consistent, and the data obtained is as shown in table 1.
Embodiment 6
12kg graphene oxide is added in 78kg deionized water, graphene oxide dispersion is made in ultrasonic disperse, then pre-
The polysilicon chip surface that the average thickness of processing is 300 μm carries out spin-coating film, revolving speed 700r/min, and spin-coating time is
Graphene oxide film is made in 1.5h, then sprays 10kg hydroiodic acid, and the reduction reaction of 60min is carried out at 110 DEG C of temperature,
Graphene film is made；The silk fibroin water solution that compound concentration is 8%, is then added dropwise on graphene film surface, air-dries into
Film, the temperature for air-drying film forming is 40 DEG C, relative humidity 32%, wind speed 0.8m/s, film formation time 10h, then from silicon wafer table
Face removing, is made graphene/silk-fibroin flexible conductive film；Film is subjected to laser ablation, optical maser wavelength 60nm, laser repeats
Frequency 60kHz etches the grating with periodic structure in film surface, and there is graphene/silk egg of optical grating construction on obtained surface
White flexible conductive film；Finally 30kg dimethyl silicone polymer is added in 70kg dimethylformamide, ultrasonic disperse is uniform, so
It is coated on flexible conductive film surface afterwards, the laminated film for flexible electronic skin is made in film-forming.
Test method and embodiment 1 are consistent, and the data obtained is as shown in table 1.
Comparative example 1
In laminated film preparation process, it is not added with fibroin albumen, other preparation conditions and embodiment 6 are consistent.
Comparative example 2
In laminated film preparation process, uncoated dimethyl silicone polymer, other preparation conditions and embodiment 6 are consistent.
Test method and embodiment 1 are consistent, and the data obtained is as shown in table 1.
Table 1:
| Performance indicator | Impact strength (J/m) | Tensile strength (MPa) | Elongation at break (%) |
| Embodiment 1 | 25.2 | 34.2 | 657.2 |
| Embodiment 2 | 26.4 | 36.4 | 660.3 |
| Embodiment 3 | 25.6 | 35.6 | 658.8 |
| Embodiment 4 | 25.4 | 35.8 | 659.4 |
| Embodiment 5 | 25.7 | 35.4 | 658.3 |
| Embodiment 6 | 26.1 | 36.1 | 642.3 |
| Comparative example 1 | 22.8 | 20.2 | 421.1 |
| Comparative example 2 | 14.8 | 25.2 | 488.8 |
Claims (9)
1. a kind of preparation method of the laminated film for flexible electronic skin, which is characterized in that as by oxygen made from spin coating
Graphite alkene film is restored using hydroiodic acid, and fibroin then is added dropwise on surface and air-dries film forming, recycles laser ablation in film
The grating of periodic structure is produced on surface, and finally dimethyl silicone polymer is dissolved in after dimethylformamide and is coated on surface, solidification
Film forming, is made the laminated film for flexible electronic skin.Specific step is as follows for preparation:
(1) it adds graphene oxide into deionized water, graphene oxide dispersion is made in ultrasonic disperse, then pretreated
Silicon chip surface carries out spin-coating film, and graphene oxide film is made, and then sprays hydroiodic acid and carries out reduction reaction, graphene is made
Film；
(2) silk fibroin water solution that mass concentration is 6 ~ 10% is prepared, the graphene film made from step (1) is then added dropwise
Surface air-dries film forming, then removes from silicon chip surface, and graphene/silk-fibroin flexible conductive film is made；
(3) graphene made from step (2)/silk-fibroin flexible conductive film is subjected to laser ablation, is etched in film surface
There is graphene/silk-fibroin flexible conductive film of optical grating construction on grating with periodic structure, obtained surface；
(4) dimethyl silicone polymer is added in dimethylformamide, ultrasonic disperse is uniform, is then coated with and is made in step (3)
Flexible conductive film surface, the laminated film for flexible electronic skin is made in film-forming.
2. a kind of preparation method of the laminated film for flexible electronic skin according to claim 1, it is characterised in that: step
Suddenly the revolving speed of (1) described spin-coating film is 600 ~ 800r/min, and spin-coating time is 1 ~ 2h.
3. a kind of preparation method of the laminated film for flexible electronic skin according to claim 1, it is characterised in that: step
Suddenly (1) described silicon wafer is one of monocrystalline silicon piece, polysilicon chip, and silicon wafer thickness is 200 ~ 400 μm.
4. a kind of preparation method of the laminated film for flexible electronic skin according to claim 1, it is characterised in that: step
Suddenly the temperature of (1) described reduction reaction is 100 ~ 120 DEG C, and the reaction time is 50 ~ 70min.
5. a kind of preparation method of the laminated film for flexible electronic skin according to claim 1, it is characterised in that: step
Suddenly the parts by weight of (1) described each raw material are, 10 ~ 15 parts by weight of graphene oxide, 73 ~ 82 parts by weight of deionized water, hydroiodic acid 8 ~
12 parts by weight.
6. a kind of preparation method of the laminated film for flexible electronic skin according to claim 1, it is characterised in that: step
Suddenly the temperature of (2) described air-dried film forming be 35 ~ 45 DEG C, relative humidity be 30 ~ 35%, wind speed be 0.5 ~ 1m/s, film formation time be 8 ~
12h。
7. a kind of preparation method of the laminated film for flexible electronic skin according to claim 1, it is characterised in that: step
Suddenly 320 ~ the 400nm of optical maser wavelength of (3) described laser ablation, 40 ~ 80kHz of laser repetition rate.
8. a kind of preparation method of the laminated film for flexible electronic skin according to claim 1, it is characterised in that: step
Suddenly the parts by weight of (4) described each raw material are 20 ~ 40 parts by weight of dimethyl silicone polymer, 60 ~ 80 parts by weight of dimethylformamide.
9. the laminated film for flexible electronic skin that any one of claim 1 ~ 8 preparation method is prepared.
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| CN110057476A (en) * | 2019-05-28 | 2019-07-26 | 中国科学院上海高等研究院 | A kind of multi signal response flexible electronic skin and preparation method thereof |
| CN110779639A (en) * | 2019-11-19 | 2020-02-11 | 重庆交通大学 | Manipulator sliding sensation sensor based on fiber bragg grating |
| CN111110222A (en) * | 2019-12-26 | 2020-05-08 | 中国科学院上海微***与信息技术研究所 | Biological protein flexible skin patch type electrode and preparation method thereof |
| CN112216807A (en) * | 2020-09-29 | 2021-01-12 | 吉林大学 | Method for preparing highly-ordered flexible silver nanowire electrode by utilizing capillary force and application |
| CN113308881A (en) * | 2021-07-15 | 2021-08-27 | 华东师范大学 | Waterproof breathable electronic skin and preparation method thereof |
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2018
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|---|---|---|---|---|
| CN110057476A (en) * | 2019-05-28 | 2019-07-26 | 中国科学院上海高等研究院 | A kind of multi signal response flexible electronic skin and preparation method thereof |
| CN110779639A (en) * | 2019-11-19 | 2020-02-11 | 重庆交通大学 | Manipulator sliding sensation sensor based on fiber bragg grating |
| CN111110222A (en) * | 2019-12-26 | 2020-05-08 | 中国科学院上海微***与信息技术研究所 | Biological protein flexible skin patch type electrode and preparation method thereof |
| CN112216807A (en) * | 2020-09-29 | 2021-01-12 | 吉林大学 | Method for preparing highly-ordered flexible silver nanowire electrode by utilizing capillary force and application |
| CN113358240A (en) * | 2021-06-04 | 2021-09-07 | 燕山大学 | DUS-FBG-based large-area flexible intelligent skin temperature and pressure sensor |
| CN113358240B (en) * | 2021-06-04 | 2024-04-26 | 燕山大学 | Temperature and pressure sensor of large-area flexible intelligent skin based on DUS-FBG |
| CN113308881A (en) * | 2021-07-15 | 2021-08-27 | 华东师范大学 | Waterproof breathable electronic skin and preparation method thereof |
| CN113670484A (en) * | 2021-08-18 | 2021-11-19 | 吉林大学重庆研究院 | Flexible pressure sensor with complementary spiral structure, preparation method and application thereof |
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Application publication date: 20190104 |