CN109520411A - Graphene flexibility strain transducer based on pre-stretching and preparation method thereof - Google Patents
Graphene flexibility strain transducer based on pre-stretching and preparation method thereof Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B7/00—Measuring arrangements characterised by the use of electric or magnetic techniques
- G01B7/16—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge
- G01B7/18—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge using change in resistance
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Abstract
The invention discloses a kind of graphene flexibility strain transducer and preparation method thereof based on pre-stretching.Graphene flexibility strain transducer based on pre-stretching includes the substrate after release, and the substrate after release is equipped with graphene sensitive layer, and the junction of the substrate behind graphene sensitive layer both ends and release is equipped with conductive silver glue, and conductive silver glue upper surface is equipped with electrode.The preparation method of graphene flexibility strain transducer based on pre-stretching is pre-stretched substrate before shifting graphene film, the transfer of graphene film is completed by dry type transfer method, and then prepare the graphene flexibility strain transducer based on pre-stretching.The sensor that the present invention makes realizes the measurement of large strain by pre-stretching, has stabilization well and repeatability, by dry type transfer method, improves and be fabricated to power, simplify preparation method, realizes high-volume and make.
Description
Technical field
The invention belongs to flexible electronic technical fields, strain and pass more particularly to a kind of graphene flexibility based on pre-stretching
Sensor and preparation method thereof.
Background technique
With bioielectronics, biomethanics, engineering in medicine, new material technology, sensor technology and robot technology etc.
The development and fusion of emerging cross discipline and direction, flexible strain transducer have obtained vast researcher, doctor and engineering
The attention and research of teacher, traditional strain transducer are mainly based upon metal and semiconductor material, with certain sensitivity,
But the disadvantage is that material is hard, tensility is poor, is less than < 5%, this disadvantage limits the application range of traditional strain transducer.
Compared with traditional strain transducer, flexible strain transducer overcomes the disadvantage that material is hard, tensility is poor, has soft
The advantages that property, biggish tensility (> 10%) and higher sensitivity.In flexible strain transducer, sensitive material is to determine
The key of strain transducer performance, the flexible common sensitive material of strain transducer existing at present includes: nanoparticle, nanometer
Line, carbon nanotube, graphene etc..Due to graphene conductivity with higher, outstanding flexible and higher Young's modulus, base
In the flexible strain transducer of graphene, there are many relevant researchs of flexible strain transducer based on graphene at present.Shen
Please number: 201610813162.6, denomination of invention: the preparation method of the double-deck oxidation graphene film flexibility strain transducer,
Publication date is on 2 22nd, 2017, and disclosing the sensor is that redox graphene is attached to flexible material substrate
(PDMS) it is prepared on, the measurement of large strain may be implemented, but the preparation method of its graphene is oxidation-reduction method, sensed
The sensitivity of device is lower.
Application number: 201710086475.0, denomination of invention: a kind of laser prepares different graphene pattern strain transducers
Method, publication date are on July 7th, 2017, and disclosing the sensor is by wet type transfer method by chemical vapour deposition technique (CVD)
The graphene of preparation is transferred to flexible substrate (PDMS) and is prepared, and the flexible strain transducer of this method preparation has biggish
Strain measurement range (10%) and higher strain sensitivity；But that there are graphenes is easy for the graphene prepared by wet type transfer method
The disadvantages of breakage, transfer success rate low, complicated for operation.
Application number: 201610256877.6, denomination of invention: graphene meets the system of nano-Au films flexibility strain transducer
Preparation Method and its strain transducer, publication date are on July 20th, 2016, disclose the sensor and are changed gold by wet type transfer method
Property graphene be transferred on PDMS substrate and be prepared, sensor sensitivity with higher, but since graphene single layer is special
Property, sensor effective strain are limited in scope (< 5%), less reproducible problem.
In conclusion the reported flexible strain transducer based on graphene has the following disadvantages: (1) by oxidation also
The graphene flexibility strain transducer sensitivity of former method preparation is lower；(2) the graphene flexibility prepared by wet type transfer method is answered
Become sensor and haves the shortcomings that cracky in transfer process, transfer success rate are low, complicated for operation；(3) single-layer graphene structure can
Draftability is lower, less reproducible problem.
Summary of the invention
The purpose of the present invention is to provide a kind of graphene flexibility strain transducer based on pre-stretching, solves existing skill
The lower problem of the graphene flexibility strain transducer sensitivity prepared in art by oxidation-reduction method.
The preparation side of another object of the present invention is to provide a kind of graphene flexibility strain transducer based on pre-stretching
Method, solving the graphene flexibility strain transducer for preparing in the prior art by wet type transfer method, there are fragile in transfer process
Damage, the problem that transfer success rate is low, complicated for operation and single-layer graphene structure tensility is lower, less reproducible.
The technical scheme adopted by the invention is that after the graphene flexibility strain transducer based on pre-stretching, including release
Substrate, substrate after release is equipped with graphene sensitive layer, the junction of the substrate behind graphene sensitive layer both ends and release
Equipped with conductive silver glue, conductive silver glue upper surface is equipped with electrode.
Further, the substrate thickness after the release is 3mm.
Further, the graphene sensitive layer with a thickness of 3.2nm, graphene sensitive layer is pleated structure.
Further, the conductive silver glue with a thickness of 0.5mm.
Another technical solution adopted in the present invention is that the preparation of the graphene flexibility strain transducer based on pre-stretching
Method specifically follows the steps below:
Step 1: it is thin that graphene is grown on copper sheet by chemical vapor deposition with deionized water, washes of absolute alcohol copper sheet
Film；
Substrate is prepared by spin-coating method, the substrate after substrate is pre-stretched is pre-stretched by mechanical clamp, after pre-stretching
The macromolecule polymeric material of one layer of semi-solid preparation of drop coating on substrate；
Step 2: the copper sheet of the attachment graphene film of step 1 is fitted on the macromolecule polymeric material of semi-solid preparation, pass through
Graphene film is connected by the macromolecule polymeric material of semi-solid preparation with the substrate after pre-stretching；
Step 3: etching copper sheet after the macromolecule polymeric material of semi-solid preparation is fully cured；
Step 4: the substrate after release pre-stretching, substrate and graphene sensitive layer after being released；
Step 5: the intersection of the substrate behind graphene sensitive layer two sides and release coats conductive silver glue, electrode and conductive silver
The center of glue connects, and then the graphene flexibility strain transducer based on pre-stretching is prepared.
Further, in the step 1 copper sheet with a thickness of 0.1mm.
Further, the substrate with a thickness of 2mm；
The material of the substrate is dimethyl silicone polymer；
The macromolecule polymeric material of the semi-solid preparation of drop coating with a thickness of 1mm.
Further, the macromolecule polymeric material of the step 2 semi-solid preparation is dimethyl silicone polymer, is by prepolymer
Vinyl methyl polysiloxanes and crosslinking agent hydrogen containing siloxane form, by hydrosilylation in 60-80 DEG C of crosslinking curing
2-3 hours, the dimethyl silicone polymer that curing ratio is 10:1 is made.
The invention has the advantages that the sensor that the present invention makes realizes the measurement of large strain by pre-stretching,
With good stable and repeatability, by graphene dry type transfer method, improves and be fabricated to power height, simplify preparation side
Method realizes high-volume and makes.The graphene film that sensor of the invention uses CVD method to prepare, spirit with higher
Sensitivity；The tensility and stability of graphene film are increased by the method for pre-stretching；It is improved by dry type transfer method
The success rate of transfer simplifies manufacture craft, and graphene flexibility strain transducer produced by the present invention, which has, realizes Gao Ling
The advantages of sensitivity, big strain, high stability.
Detailed description of the invention
In order to more clearly explain the embodiment of the invention or the technical proposal in the existing technology, to embodiment or will show below
There is attached drawing needed in technical description to be briefly described, it should be apparent that, the accompanying drawings in the following description is only this
Some embodiments of invention for those of ordinary skill in the art without creative efforts, can be with
It obtains other drawings based on these drawings.
Fig. 1 is preparation process flow schematic diagram of the invention.
Fig. 2 is sensor of the invention structural schematic diagram.
Fig. 3 is sensor of the invention cross-sectional structure schematic diagram.
Fig. 4 is electrode structure schematic diagram of the invention.
In figure, 1. copper sheets, 2. graphene films, 3. substrates, the substrate after 4. pre-stretchings, the high molecular polymerization of 5. semi-solid preparations
Material, the substrate after 6. releases, 7. graphene sensitive layers, 8. conductive silver glues, 9. electrodes.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Thinking of the invention is: graphene is one kind by sp2The netted two-dimensional material being formed by connecting of hydbridized carbon atoms, has
Excellent mechanics, electricity, optics, chemistry and magnetic performance.By graphene and flexible polymer it is compound can prepare to provide be based on
The big strain transducer of flexibility of graphene.When subjected to tension, graphene reticular structure can be broken this sensor, be caused
The variation of sensor resistance, the present invention realize the measurement to strain according to this principle.
Graphene flexibility strain transducer based on pre-stretching, as shown in Fig. 2, including the substrate 6 after release, after release
Substrate 6 is equipped with graphene sensitive layer 7, and the junction of the substrate 6 behind 7 both ends of graphene sensitive layer and release is equipped with conductive silver glue
8,8 upper surface of conductive silver glue is equipped with electrode 9.
Substrate 6 after release with a thickness of 3mm, graphene sensitive layer 7 with a thickness of 3.2nm.
Conductive silver glue 8 with a thickness of 0.5mm.
The preparation method of graphene flexibility strain transducer based on pre-stretching, as shown in Figure 1, specifically according to the following steps
It carries out:
Step 1: growing stone on copper sheet 1 by CVD, that is, chemical vapor deposition with deionized water, washes of absolute alcohol copper sheet 1
Black alkene film 2；
Substrate 3 is prepared by spin-coating method, the substrate 4 after substrate 3 is pre-stretched is pre-stretched by mechanical clamp, after pre-stretching
Substrate 4 on one layer of semi-solid preparation of drop coating macromolecule polymeric material 5；
Step 2: the copper sheet 1 of the attachment graphene film 2 of step 1 is fitted on the macromolecule polymeric material 5 of semi-solid preparation, lead to
Graphene film 2 is connected by more than half cured macromolecule polymeric materials 5 with the substrate 4 after pre-stretching；
Step 3: etching copper sheet 1 after the macromolecule polymeric material 5 of semi-solid preparation is fully cured；
Step 4: the substrate 4 after release pre-stretching, substrate 6 and graphene sensitive layer 7 after being released；
Step 5: the intersection of the substrate 6 behind 7 two sides of graphene sensitive layer and release coats conductive silver glue 8, such as Fig. 3-4 institute
Show, electrode 9 is connect with the center of conductive silver glue 8, and then the graphene flexibility strain sensing based on pre-stretching is prepared
Device, as shown in Figure 2.
In step 1, copper sheet 1 with a thickness of 0.1mm, the molten carbon rate of copper sheet 1 is low, the layer of the graphene grown on copper sheet 1
Number is easy to control, and the number of plies of graphene film 2 is 10 layers, every layer with a thickness of 0.32nm, the number of plies of graphene film 2 ensure that can
Draftability and sensitivity.
Substrate 3 with a thickness of 2mm, the intensity that has been able to maintain under tensional state；3 thickness of substrate, which is less than 2mm, will lead to biography
Sensor intensity is poor, and being thicker than 2mm will affect the flexibility of sensor；Material used in substrate 3 is dimethyl silicone polymer, that is, PDMS,
It is since PDMS has good tensility and flexibility using PDMS；The shape of substrate 3 be rectangle, shapes and sizes according to
Depending on actual demand.
The macromolecule polymeric material 5 of the semi-solid preparation of drop coating with a thickness of 1mm, it is real which can pass through spin coating, mask plate
Existing, simple process, stabilization, cost is relatively low.
In step 2, the macromolecule polymeric material 5 of semi-solid preparation is PDMS, and PDMS is by the poly- silicon oxygen of prepolymer ethylene ylmethyl
Alkane and crosslinking agent hydrogen containing siloxane form, by hydrosilylation 60-80 DEG C crosslinking curing 2-3 hour, be made and solidify
The cross-linking effect having had than the PDMS for 10:1；Time, the too short cross-linking effect that will lead to was poor, and overlong time is to final effect
Influence unobvious, and waste of resource；Temperature is too low, and to will lead to prepared film strength poor, and temperature is excessively high, and to will lead to material soft
Property is poor.
In step 4, the substrate 4 after being pre-stretched is discharged, being will be with 4 slave of substrate after the pre-stretching of graphene film 2
Tool fixture is removed, and original length is restored, and should limit rate of release in the process, release force is excessive to cause graphene film 2 broken
Damage；
Graphene sensitive layer 7 is located on the substrate 6 after release, and graphene sensitive layer 7 is transferred to release by dry type transfer method
Substrate 6 afterwards, dry type transfer method are that graphene sensitive layer 7 is adhered to the macromolecule polymeric material 5 of semi-solid preparation as " glue "
On the substrate 4 of pre-stretching, the transfer of graphene sensitive layer 7 is completed after solidification；Semi-solid preparation macromolecule polymer material 5 with
After copper sheet 1 with graphene film 2 is bonded, the macromolecule polymer material 5 of semi-solid preparation is heated, due to the macromolecule of semi-solid preparation
The cross-linking reaction of polymer material 5 can make graphene film 2 be connected with the substrate 4 after pre-stretching；Do not use substrate prestretching
Stretch, lead to prepared graphene film 2 easy fracture under larger pulled out condition, the tensility and stability of sensor compared with
Difference；
For substrate 6 after release with a thickness of 3mm, the substrate 6 after the release of 3mm thickness guarantees that sensor has tensility, is greater than 3mm
The flexibility that will affect sensor, the thickness less than 3mm will affect the stabilized soil pavement of sensor；6 shape of substrate after release
Be square, size is, shapes and sizes according to actual needs depending on；
Graphene sensitive layer 7 with a thickness of 3.2nm, the graphene sensitive layer 7 of 3.2nm guarantees the sensitivity of sensor；Graphene
The shape of sensitive layer 7 is rectangle, is in buckle condition, and size is, shapes and sizes according to actual needs depending on.
In step 6, conductive silver glue 8 with a thickness of 0.5mm, can guarantee the sufficiently conductive of electrode 9 and graphene, it is conductive
Elargol 8 is blocked up so that contact resistance is increased, and influence sensor performance, and conductive silver glue 8, which is less than 0.5mm, will affect sensor stabilization
Property.
Graphene sensitive layer 7 is transferred on the substrate 6 after release by dry type transfer method, is reduced broken in transfer process
Damage improves transfer success rate, is not have flexibility on copper sheet 1, be prepared by graphene prepared by chemical vapour deposition technique
Sensor needs to shift graphene film 2.The fold of graphene sensitive layer 7 is realized by the substrate 4 after release pre-stretching
, the measurement range that can increase sensor is done so, stability is improved, at the initial stage for stretching graphene sensitive layer 7, fold knot
The stress and strain of draw direction can be turned the stress and strain for being decomposed into stretched vertically direction by structure, and this stress and strain is concentrated
In the peaks and troughs of fold graphene sensitive layer 7, therefore, at the initial stage of stretching, graphene sensitive layer 7 is deposited due to fold
, deformation is smaller, so be subject to breakage it is smaller.With the increase of strain, larger breakage occurs for graphene sensitive layer 7, reaches
Its limit of stretch, therefore pleated structure improves measurement range and stability.
This characteristic of resistance variations after the present invention is stretched using graphene is strained by the graphene flexibility of pre-stretching preparation
Sensor can be measured less than or equal to its own 20% strain, due to the high conductivity of graphene film 2, cause to sense utensil
There is higher sensitivity；Due to the preparation process using pre-stretching, sensor has good stability and repeatability, and its
Cracky, transfer success rate be not high, easy to operate for graphene in preparation process.
Each embodiment in this specification is all made of relevant mode and describes, same and similar portion between each embodiment
Dividing may refer to each other, and each embodiment focuses on the differences from other embodiments.Especially for system reality
For applying example, since it is substantially similar to the method embodiment, so being described relatively simple, related place is referring to embodiment of the method
Part explanation.
The foregoing is merely illustrative of the preferred embodiments of the present invention, is not intended to limit the scope of the present invention.It is all
Any modification, equivalent replacement, improvement and so within the spirit and principles in the present invention, are all contained in protection scope of the present invention
It is interior.
Claims (8)
1. the graphene flexibility strain transducer based on pre-stretching, which is characterized in that including the substrate (6) after release, after release
Substrate (6) be equipped with graphene sensitive layer (7), graphene sensitive layer (7) both ends are set with the junction of substrate (6) after discharging
Have conductive silver glue (8), conductive silver glue (8) upper surface is equipped with electrode (9).
2. the graphene flexibility strain transducer according to claim 1 based on pre-stretching, which is characterized in that the release
Substrate (6) afterwards is with a thickness of 3mm.
3. the graphene flexibility strain transducer according to claim 1 based on pre-stretching, which is characterized in that the graphite
Alkene sensitive layer (7) with a thickness of 3.2nm, graphene sensitive layer (7) is pleated structure.
4. the graphene flexibility strain transducer according to claim 1 based on pre-stretching, which is characterized in that the conduction
Elargol (8) with a thickness of 0.5mm.
5. the preparation method of the graphene flexibility strain transducer based on pre-stretching as described in claim 1-4 any one,
It is characterized in that, specifically following the steps below:
Step 1: growing graphite on copper sheet (1) by chemical vapor deposition with deionized water, washes of absolute alcohol copper sheet (1)
Alkene film (2)；
Substrate (3) are prepared by spin-coating method, the substrate (4) after being pre-stretched by mechanical clamp pre-stretching substrate (3), pre-
The macromolecule polymeric material (5) of one layer of semi-solid preparation of drop coating on substrate (4) after stretching；
Step 2: the copper sheet (1) of the attachment graphene film (2) of step 1 to be fitted in the macromolecule polymeric material of semi-solid preparation
(5) on, graphene film (2) is connected with the substrate (4) after pre-stretching by the macromolecule polymeric material (5) of semi-solid preparation；
Step 3: etching copper sheet (1) after the macromolecule polymeric material (5) of semi-solid preparation is fully cured；
Step 4: the substrate (4) after release pre-stretching, substrate (6) and graphene sensitive layer (7) after being released；
Step 5: the intersection of the substrate (6) behind graphene sensitive layer (7) two sides and release coats conductive silver glue (8), electrode
(9) it is connect with the center of conductive silver glue (8), and then the graphene flexibility strain transducer based on pre-stretching is prepared.
6. the preparation method of the graphene flexibility strain transducer according to claim 5 based on pre-stretching, feature exist
In copper sheet (1) with a thickness of 0.1mm in the step 1.
7. the preparation method of the graphene flexibility strain transducer according to claim 5 based on pre-stretching, feature exist
In, the substrate (3) with a thickness of 2mm；
The material of the substrate (3) is dimethyl silicone polymer；
The macromolecule polymeric material (5) of the semi-solid preparation of drop coating with a thickness of 1mm.
8. the preparation method of the graphene flexibility strain transducer according to claim 5 based on pre-stretching, feature exist
In the macromolecule polymeric material (5) of the step 2 semi-solid preparation, which is dimethyl silicone polymer, to be gathered by prepolymer ethylene ylmethyl
Siloxanes and crosslinking agent hydrogen containing siloxane form, by hydrosilylation 60-80 DEG C crosslinking curing 2-3 hour, it is obtained
Curing ratio is the dimethyl silicone polymer of 10:1.
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| CN110455445B (en) * | 2019-07-19 | 2021-12-14 | 南京邮电大学 | Flexible stress sensor and preparation method thereof |
| CN111141423B (en) * | 2020-01-17 | 2022-04-01 | 闽江学院 | Stress sensor capable of simultaneously regulating sensitivity and ductility and preparation method thereof |
| CN111141423A (en) * | 2020-01-17 | 2020-05-12 | 闽江学院 | Stress sensor capable of simultaneously regulating sensitivity and ductility and preparation method thereof |
| CN112097967A (en) * | 2020-09-15 | 2020-12-18 | 闽江学院 | Self-energy-supply-based flexible extensible mechanical sensing system and preparation method thereof |
| CN113720255A (en) * | 2021-08-30 | 2021-11-30 | 中国科学院宁波材料技术与工程研究所 | Amorphous carbon-based flexible sensor based on crack fold structure and preparation method thereof |
| CN113834418A (en) * | 2021-09-06 | 2021-12-24 | 电子科技大学 | Flexible strain sensor with adjustable Poisson ratio |
| CN113834418B (en) * | 2021-09-06 | 2023-04-18 | 电子科技大学 | Flexible strain sensor with adjustable Poisson ratio |
| CN113865475A (en) * | 2021-09-23 | 2021-12-31 | 浙江大学 | Preparation method and application of bionic self-adaptive winding wearable sensor for monitoring diameter micro-change of plant stem |
| CN114061433A (en) * | 2021-09-24 | 2022-02-18 | 华中科技大学 | Breathable wearable strain sensor and preparation method and application thereof |
| CN114354035A (en) * | 2022-01-04 | 2022-04-15 | 深圳市溢鑫科技研发有限公司 | Flexible intelligent stress-strain sensor electrode and manufacturing method thereof |
| CN114858319A (en) * | 2022-04-26 | 2022-08-05 | 中国科学院上海微系统与信息技术研究所 | Preparation method of tension sensor and tension sensor |
| CN114993187A (en) * | 2022-05-25 | 2022-09-02 | 浙江大学 | Sensor based on combination of optical fiber macrobending loss and fiber-based system geometric buckling deformation and manufacturing method and application thereof |
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