CN114046913A - Flexible graphene pressure sensor and preparation method thereof - Google Patents
Flexible graphene pressure sensor and preparation method thereof Download PDFInfo
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- CN114046913A CN114046913A CN202111363584.5A CN202111363584A CN114046913A CN 114046913 A CN114046913 A CN 114046913A CN 202111363584 A CN202111363584 A CN 202111363584A CN 114046913 A CN114046913 A CN 114046913A
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Classifications
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/20—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress
- G01L1/22—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress using resistance strain gauges
- G01L1/2287—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress using resistance strain gauges constructional details of the strain gauges
- G01L1/2293—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress using resistance strain gauges constructional details of the strain gauges of the semi-conductor type
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- General Physics & Mathematics (AREA)
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Abstract
The invention relates to a flexible graphene pressure sensor and a preparation method thereof, belonging to the technical field of sensors, wherein the sensor comprises a flexible substrate, a microstructure bottom layer, an electrode, a graphene film and a flexible packaging layer; the preparation method comprises the steps of preparing a graphene film, manufacturing a flexible substrate, performing reverse mold operation on the flexible substrate, manufacturing a cylinder array, and finally combining to prepare the flexible graphene pressure sensor. The sensor designed by the invention has the characteristics of good flexibility, simple preparation method, low cost and high sensitivity, and can be applied to flexible electronic equipment.
Description
Technical Field
The invention relates to a flexible graphene pressure sensor and a preparation method thereof, and belongs to the technical field of sensors.
Background
At present, the intelligent sensor technology develops in three trends: firstly, the application of new materials, the important basis of the sensor technology is sensitive materials such as low-dimensional nano materials and the like, and the development and utilization of the materials enable the sensor to be more easily subjected to low cost, miniaturization, integration, multiple functionalization and high performance; the adoption of a new process, along with the continuous development of a micro-nano technology, a three-dimensional technology and the like, enables more novel sensors to be manufactured, and has great promotion effect on the future industrialization and commercialization of the novel sensors; thirdly, the design of novel sensor, various novel structures are designed, very big improvement each item performance of sensor. At present, the novel sensor mainly has the characteristics of flexibility, transparency, multifunction, miniaturization, high performance and the like, and needs to be continuously innovated in various aspects such as a new principle, a new material, a new technology and the like.
Since the discovery of graphene, a great deal of research around this innovative nanomaterial has been carried out by academia, including mechanical, electrical, optical, thermal, etc. properties of graphene and graphene-based nanodevices, and the research shows that graphene has incomparable excellent properties with other semiconductor materials, its young modulus is about 1 TPa, maximum tensile strain can reach 20%, and its carrier migration rate at room temperature is up to 15000cm2V · s, can be widely applied to NEMS.
The flexible electronic device has huge application potential in the fields of human motion perception, personalized health monitoring, electronic skin, flexible robots and the like, wherein the flexible stress-strain sensor can be well attached to a curved surface in a proper shape due to sufficient mechanical flexibility, can generate good signal response to deformation, and is the leading direction of current research.
Disclosure of Invention
The invention aims to provide a flexible graphene pressure sensor and a preparation method thereof, wherein the sensor has the characteristics of good flexibility, short response time, simple preparation method and high sensitivity, and can be applied to flexible electronic equipment.
In order to achieve the purpose, the invention adopts the technical scheme that:
a flexible graphene pressure sensor comprises a flexible substrate, a microstructure bottom layer, electrodes, a graphene film and a flexible packaging layer; the flexible packaging layer and the flexible substrate are arranged in parallel, a graphene film is attached to the lower surface of the flexible packaging layer, and two electrodes which are not in contact with each other are arranged on the lower surface of the graphene film; the upper surface of the flexible substrate is provided with a microstructure bottom layer, and the microstructure bottom layer is in contact with the electrodes.
The technical scheme of the invention is further improved as follows: the flexible substrate is prepared from polydimethylsiloxane, and the thickness of the flexible substrate is 0.4-0.6 mm.
The technical scheme of the invention is further improved as follows: the bottom layer of the microstructure is a cylinder array and is manufactured on the flexible substrate in a reverse mould mode; the thickness of cylinder array is 0.3 ~ 0.5mm, and the cylinder specification is radius 0.25mm, and the wheel base is 0.8 mm.
The technical scheme of the invention is further improved as follows: the electrode is a strip-shaped conductive silver coating, and the thickness of the strip-shaped conductive silver coating is 0.08-0.12 mm.
The technical scheme of the invention is further improved as follows: the graphene film is a double-layer graphene film prepared by a CVD method.
The technical scheme of the invention is further improved as follows: the flexible packaging layer is prepared from polydimethylsiloxane, and the thickness of the flexible packaging layer is 0.1-0.2 mm.
A preparation method of a flexible graphene pressure sensor comprises the following steps:
1) pretreating the copper foil;
2) preparing a graphene film by using a CVD (chemical vapor deposition) method;
3) preparing a graphene protective layer material, and uniformly covering the graphene protective layer material on the graphene film;
4) preparing a corrosive liquid, and corroding the copper substrate to obtain a graphene/protective layer composite structure;
5) manufacturing a flexible substrate;
6) performing reverse mould operation on the flexible substrate to manufacture a microstructure bottom layer of the cylinder array, and coating electrodes on the microstructure bottom layer;
7) and preparing the flexible graphene pressure sensor in a combined manner.
The technical scheme of the invention is further improved as follows: the graphene film prepared in the step 2) is a double-layer graphene film.
Due to the adoption of the technical scheme, the invention has the following technical effects:
the sensor designed by the invention has the characteristics of good flexibility, simple preparation method, low cost and high sensitivity, and can be applied to flexible electronic equipment.
The flexible graphene pressure sensor prepared by the invention has high sensitivity, stability and linearity, and PDMS is used as the substrate and the packaging layer, so that the sensor has good flexibility and transparency, can be tightly attached to the surface of a measured object, can be used for detecting micro mechanical force such as bending force and torsion force, can also be used for detecting micro pressure caused by voice vibration, mechanical vibration and the like, and can also be used for detecting human physiological signals such as pulse, respiration, heartbeat and the like.
According to the invention, the cylindrical microstructure is prepared on the substrate by adopting a reverse mold process, so that a deformation space can be provided as much as possible on the basis of providing support for the graphene film, and the electronic performance of the sensor is improved.
Drawings
Fig. 1 is a schematic view of the overall structure of a flexible graphene pressure sensor according to the present invention;
fig. 2 is a top view of the overall structure of the flexible graphene pressure sensor according to the present invention;
fig. 3 is a dynamic response curve of the flexible graphene pressure sensor according to the present invention;
fig. 4 is a loading response curve of the flexible graphene pressure sensor of the present invention;
fig. 5 is a measured radial artery waveform of the flexible graphene pressure sensor of the present invention;
the flexible packaging structure comprises a flexible substrate 1, a flexible substrate 2, a microstructure bottom layer 3, an electrode 4, a graphene film 5 and a flexible packaging layer.
Detailed Description
The invention is described in further detail below with reference to the following figures and specific embodiments:
a flexible graphene pressure sensor comprises a flexible substrate 1, a microstructure bottom layer 2, electrodes 3, a graphene film 4 and a flexible packaging layer 5. The flexible substrate 1 is prepared from polydimethylsiloxane, and the thickness of the flexible substrate is 0.4-0.6 mm; the microstructure bottom layer 2 is a cylinder array, and is manufactured on the flexible substrate 1 in a reverse mould mode, the thickness of the cylinder array is 0.3-0.5 mm, the specification of a cylinder is 0.25mm in radius, and the axle center distance is 0.8 mm; the electrode 3 is a strip-shaped conductive silver coating with the thickness of 0.08-0.12 mm; the graphene film 4 is a double-layer graphene film prepared by a CVD method; the flexible packaging layer 5 is made of polydimethylsiloxane, and the thickness of the flexible packaging layer is 0.1-0.2 mm.
As shown in fig. 1 and 2, the flexible encapsulation layer 5 and the flexible substrate 1 are arranged in parallel, a graphene film 4 is conformally attached to the lower surface of the flexible encapsulation layer 5, and two electrodes 3 which are not in contact with each other are arranged on the lower surface of the graphene film 4; the upper surface of the flexible substrate 1 is provided with a microstructure bottom layer 2, and the microstructure bottom layer 2 is in contact with the electrode 3.
A preparation method of a flexible graphene pressure sensor comprises the following steps:
1) pretreatment of copper foil
Cutting a copper foil with the thickness of 1cm multiplied by 1cm, putting the copper foil into a mixed cleaning solution of acetone and hydrochloric acid with the volume ratio of 1:20, putting the copper foil into an ultrasonic cleaning machine, cleaning the copper foil for 15 minutes by using ultrasonic waves, taking the copper foil out, cleaning the copper foil for 2-3 times by using absolute ethyl alcohol, cleaning the copper foil for 3-5 times by using deionized water, and quickly drying the copper foil by using a nitrogen gun to prevent a copper substrate from being oxidized.
2) And preparing the graphene film by using a CVD method
And (2) growing two-dimensional graphene by taking methane as a carbon source and copper foil as a substrate at 1050 ℃ under normal pressure to obtain the graphene/copper foil/graphene composite structure film.
3) Preparing a graphene protective layer material, and uniformly covering the graphene protective layer material on the graphene film
Polydimethylsiloxane (PDMS) was used as a graphene protective layer, and the thickness of the graphene was measured in terms of bulk (SYLGUARD-184A), curing agent (SYLGUARD-184B) = 10: 1 and left for half an hour to remove air bubbles from the gel.
4) Preparing corrosive liquid, corroding a copper substrate to obtain the graphene/protective layer composite structure
Placing the graphene/copper foil/graphene prepared in the step 2) on a spin coater, taking a proper amount of PDMS solution by using a disposable dropper, dripping the PDMS solution in the center of the graphene, dividing the spin coater into two operation stages of high speed and low speed, firstly operating at the low speed of 1000r/min for 10 seconds, then switching to the high speed of 2000r/min for 30 seconds, uniformly and completely spin-coating PDMS on the surface of the graphene to obtain PDMS/graphene/copper foil/graphene, and placing the PDMS in a vacuum drying box to be heated and cured; placing PDMS/graphene/copper foil/graphene in corrosive liquid, and heating in water bath during corrosion; and finally, taking out the graphene composite structure, washing the graphene composite structure for 3-5 times by using deionized water, and removing impurity ions adsorbed by the graphene film, wherein the graphene composite structure is PDMS/graphene.
5) Preparing the flexible substrate
The flexible substrate is prepared from PDMS, the PET film is used as the substrate, the PET film is placed on a spin coater, a proper amount of PDMS solution is dripped in the center of the PET film through a disposable dropper, the spin coater only runs at a low rotating speed in the spin coating process, the PDMS solution is uniformly spin-coated on the surface of the PET, and then the PET solution is placed in a drying oven for heating and curing.
6) Performing reverse mould operation on the flexible substrate to manufacture a microstructure bottom layer of the cylinder array, and coating a conductive layer on the microstructure bottom layer
And 5) during PDMS liquid-solid conversion, performing reverse mould operation by using a mould to prepare a cylindrical microstructure bottom layer, pressing, continuing heating and curing, removing the PET film after curing and forming, and coating an electrode on the microstructure bottom layer.
7) Combined preparation of flexible graphene pressure sensor
And (3) transferring the PDMS/graphene obtained in the step (4) onto the flexible substrate/microstructure bottom layer/electrode obtained in the step (6), drying, and finally packaging to obtain the flexible graphene pressure sensor.
Fig. 3 is a dynamic response curve of the flexible graphene pressure sensor prepared by the invention, and it can be seen from the graph that the response time of the sensor under each stress is consistent, the detection lower limit is low, and the linearity is good.
Fig. 4 is a stress loading response curve of the flexible graphene pressure sensor prepared by the present invention, after the flexible graphene pressure sensor is applied with pressure, the sensor cannot respond to the applied pressure immediately, there is a time difference from the time point of the applied pressure to the time point when the sensor responds, and it can be seen from the graph that the response time is about 36ms, which indicates that the sensor responds quickly.
Fig. 5 shows the waveform of the radial artery actually measured by the flexible graphene pressure sensor of the invention, and it can be seen from the figure that the sensor can clearly represent the waveform of the artery, and can be applied to the detection of physiological signals of human bodies and the like.
In summary, the invention discloses a flexible graphene pressure sensor structure and a preparation method thereof, the flexible graphene pressure sensor structure comprises a polydimethylsiloxane substrate, a cylinder array is processed on the polydimethylsiloxane substrate through a reverse mold process, two conductive silver coating tapes are attached to the cylinder array as conductive layers so as to lead out electrodes, a graphene film is used as a sensitive material to cover the cylinder array and leads of a pair of electrodes, when the pressure difference between the inside and the outside of the graphene sensitive film on the array changes, the graphene film deforms to generate strain, the resistance value of the graphene film changes, and the resistance value change is converted into voltage change through an external circuit, so that the subsequent utilization and analysis are facilitated, and the pressure detection is completed.
Although the present invention has been described in detail with reference to the above embodiments, those skilled in the art can make modifications and equivalents to the specific embodiments of the present invention, and any modifications and equivalents without departing from the spirit and scope of the present invention are intended to be included in the scope of the present invention. As a result of the observation: like reference numbers and letters refer to like items in the following figures, and thus, once an item is defined in one figure, it need not be further defined and explained in subsequent figures.
Claims (8)
1. A flexible graphene pressure sensor is characterized in that: the graphene film is characterized by comprising a flexible substrate (1), a microstructure bottom layer (2), an electrode (3), a graphene film (4) and a flexible packaging layer (5); the flexible packaging layer (5) and the flexible substrate (1) are arranged in parallel, a graphene film (4) is attached to the lower surface of the flexible packaging layer (5), and two electrodes (3) which are not in contact with each other are arranged on the lower surface of the graphene film (4); the upper surface of the flexible substrate (1) is provided with a microstructure bottom layer (2), and the microstructure bottom layer (2) is in contact with the electrode (3).
2. The flexible graphene pressure sensor according to claim 1, wherein: the flexible substrate (1) is prepared from polydimethylsiloxane, and the thickness of the flexible substrate is 0.4-0.6 mm.
3. The flexible graphene pressure sensor according to claim 1, wherein: the microstructure bottom layer (2) is a cylinder array and is manufactured on the flexible substrate (1) in a reverse mould mode; the thickness of cylinder array is 0.3 ~ 0.5mm, and the cylinder specification is radius 0.25mm, and the wheel base is 0.8 mm.
4. The flexible graphene pressure sensor according to claim 1, wherein: the electrode (3) is a strip-shaped conductive silver coating, and the thickness of the strip-shaped conductive silver coating is 0.08-0.12 mm.
5. The flexible graphene pressure sensor according to claim 1, wherein: the graphene film (4) is a double-layer graphene film prepared by a CVD method.
6. The flexible graphene pressure sensor according to claim 1, wherein: the flexible packaging layer (5) is made of polydimethylsiloxane, and the thickness of the flexible packaging layer is 0.1-0.2 mm.
7. The method for preparing the flexible graphene pressure sensor according to any one of claims 1 to 6, comprising the following steps:
1) pretreating the copper foil;
2) preparing a graphene film by using a CVD (chemical vapor deposition) method;
3) preparing a graphene protective layer material, and uniformly covering the graphene protective layer material on the graphene film;
4) preparing a corrosive liquid, and corroding the copper substrate to obtain a graphene/protective layer composite structure;
5) manufacturing a flexible substrate;
6) performing reverse mould operation on the flexible substrate to manufacture a microstructure bottom layer of the cylinder array, and coating electrodes on the microstructure bottom layer;
7) and preparing the flexible graphene pressure sensor in a combined manner.
8. The method for preparing a flexible graphene pressure sensor according to claim 7, wherein the method comprises the following steps: the graphene film prepared in the step 2) is a double-layer graphene film.
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| CN115060406A (en) * | 2022-06-08 | 2022-09-16 | 北京工道风行智能技术有限公司 | Flexible ionization type three-dimensional force sensor and preparation method thereof |
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| 路鹏: "基于表面微结构的柔性传感器", 《中国优秀博硕士学位论文全文数据库(硕士)信息科技辑》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115060406A (en) * | 2022-06-08 | 2022-09-16 | 北京工道风行智能技术有限公司 | Flexible ionization type three-dimensional force sensor and preparation method thereof |
| CN115060406B (en) * | 2022-06-08 | 2023-11-21 | 北京工道风行智能技术有限公司 | Flexible off-electricity type three-dimensional force sensor and preparation method thereof |
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