CN113720255A - Amorphous carbon-based flexible sensor based on crack fold structure and preparation method thereof - Google Patents
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- G—PHYSICS
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- 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
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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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- C23C14/00—Coating by vacuum evaporation, by sputtering or by ion implantation of the coating forming material
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- C—CHEMISTRY; METALLURGY
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- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
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- C23C14/3435—Applying energy to the substrate during sputtering
- C23C14/345—Applying energy to the substrate during sputtering using substrate bias
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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
- C23C—COATING METALLIC MATERIAL; COATING MATERIAL WITH METALLIC MATERIAL; SURFACE TREATMENT OF METALLIC MATERIAL BY DIFFUSION INTO THE SURFACE, BY CHEMICAL CONVERSION OR SUBSTITUTION; COATING BY VACUUM EVAPORATION, BY SPUTTERING, BY ION IMPLANTATION OR BY CHEMICAL VAPOUR DEPOSITION, IN GENERAL
- 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
- C23C14/34—Sputtering
- C23C14/35—Sputtering by application of a magnetic field, e.g. magnetron sputtering
Abstract
The invention discloses an amorphous carbon-based flexible sensor based on a crack fold structure, which comprises: the flexible substrate comprises a flexible substrate, an amorphous carbon film and conductive electrodes, wherein the amorphous carbon film is deposited on the surface of the flexible substrate, the conductive electrodes are located at two ends of the amorphous carbon film, and the amorphous carbon film is of a crack and fold structure. The amorphous carbon-based flexible sensor has higher sensitivity in a larger stretching measurement range. The invention also provides a preparation method of the amorphous carbon-based flexible sensor based on the crack wrinkle structure, which comprises the steps of pre-stretching the flexible substrate to deposit the surface of the amorphous carbon film, releasing the pre-stretched flexible substrate, and enabling the rebounded amorphous carbon film on the surface of the pre-stretched flexible substrate to have the crack wrinkle structure so as to obtain the amorphous carbon-based flexible sensor based on the crack wrinkle structure. The method is simple and efficient in preparation and easy for large-scale production.
Description
Technical Field
The invention belongs to the technical field of sensor manufacturing, and particularly relates to an amorphous carbon-based flexible sensor based on a crack fold structure and a preparation method thereof.
Background
With the development of electronic science and technology and the continuous improvement of the living standard of people, flexible wearable electronic equipment attracts more and more attention. Compared with traditional electronic equipment, the flexible wearable electronic equipment has higher flexibility and can meet the requirements of people on various deformation of the equipment. For example, the method can be applied to various aspects of daily life, such as a flexible touch display screen, electronic skin, a wearable computer, a flexible robot, a flexible pressure monitoring insole pedometer and the like.
Currently, highly flexible, stretchable wearable sensors have received considerable attention due to the potential applications of artificial robot skin, advanced prosthetics, and continuous health monitoring. In particular, flexible strain sensors can provide electrical feedback in response to external forces (including pulsatile blood flow, respiration, and human touch/motion), can be used for continuous health monitoring, and thus provide real and real-time medical solutions. These applications require that the device must make conformal contact with a curved surface and be electrically stable under large deformation conditions, and therefore require the design of stretchable electrodes with electrically stable properties.
To develop a stretchable electrode, in addition to using an intrinsically stretchable conductive polymer as a conductive matrix, one also develops a stretchable electrode using structural design, including folds, waves, meshes, serpentines, cuts, cracks, and the like. These structures enable high stretchability of hard metal-based electrodes, and applications in stretchable and soft body electronics. Among them, the fold structure is one of the most commonly used design structures, and can give the wearable device high stretchability, high mechanical stability and comfort between human-computer interaction.
At present, the wrinkle structure is mainly formed by compounding a conductive material and a pre-stretched or pre-stressed substrate, and the conductive material is deformed out of plane or in plane after the elastic substrate is pre-stretched or pre-stressed and released. The substrate shrinks by heat-induced (heating or cooling) polymer shrinkage, solvent expansion and de-expansion or directly by mechanical pre-stretching and release. The thermal induction method generally deposits a conductive layer on the surface of a shape memory material (PS, PVP, etc.), and causes the substrate layer to shrink by heating or cooling, thereby promoting the conductive layer to form a corrugated structure. The solvent swelling/de-swelling method is to soak a thermosetting elastic matrix (e.g., PDMS) in a solvent (chloroform), the elastic matrix becomes bulky, and at this time, a conductive layer is deposited on the surface of the elastic matrix, and the solvent in the swollen thermosetting elastic matrix shrinks when volatilizing, thereby obtaining a conductive layer with a wrinkled structure. The heat-induced shrinkage and the solvent expansion can both obtain uniformly shrunk fold structures, but the problems of limited polymer shrinkage rate, limited stretchability of the composite electrode, material waste and even environmental pollution exist.
The mechanical pre-stretching method is widely applied, and is characterized in that an elastic substrate is pre-stretched in a single-shaft or double-shaft system, then the elastic substrate is compounded with a conductive material, and after the pre-stretched elastic substrate is released, the stretchable electrode with a folded structure is obtained. The pre-stretching method has the advantages of simplicity, easiness in operation and controllable substrate shrinkage rate, but a uniformly contracted wrinkle structure cannot be obtained, and cracks and delamination are easy to occur between the elastic substrate and the conductive layer. In addition, the stretchable electronic device prepared by the uniaxial or biaxial stretching process generally has directionality, resulting in orientation of electrical stability, and the external force applied to the stretchable electronic material in practical applications is random, so that the electrical reliability of multi-angle stretching cannot be guaranteed.
In conclusion, due to the limitations of material and structural design, the existing flexible sensor is difficult to have both high sensitivity (GF >100) and large tensile measurement range (epsilon > 50%), and meanwhile, the preparation of the novel flexible sensor relates to a complex process for transferring sensitive materials and is difficult to meet the wide requirements of flexible sensing, so that the development of the novel flexible sensor is urgently needed.
Disclosure of Invention
The invention provides an amorphous carbon-based flexible sensor based on a crack fold structure, which has high sensitivity in a large stretching measurement range, and also provides a preparation method of the sensor.
An amorphous carbon-based flexible sensor based on a crack pleat structure, comprising: the flexible substrate comprises a flexible substrate, an amorphous carbon film and conductive electrodes, wherein the amorphous carbon film is deposited on the surface of the flexible substrate, the conductive electrodes are located at two ends of the amorphous carbon film, and the amorphous carbon film is of a crack and fold structure.
The crack density in the crack fold structure is that 10-30 cracks exist in the range of 200 multiplied by 200 mu m, the crack direction is mostly parallel to the stretching direction, and the fold structure is perpendicular to the stretching direction and is rectangular, trapezoidal or triangular. Based on the crack fold structure, the device has high sensitivity, can still recover the original structure after being subjected to larger strain, and simultaneously has better repeatability because the resistance is recovered to the initial value.
The amorphous carbon film is formed of sp of carbon2And sp3The mixed materials have high piezoresistive sensitivity, corrosion resistance and scratch resistance, and can realize signal sensing under working conditions of human sweat, scratch and the like. In addition, the amorphous carbon can be directly deposited on the flexible substrate to realize flexible sensing. At the same time, due to high stress: (>10GPa) and high brittleness, when amorphous carbon is directly deposited on a flexible substrate, the amorphous carbon film has cracks and folds due to overlarge mechanical property difference, large-range deformation detection is obtained based on the mechanical flexibility of the flexible substrate, and large resistance change response is made to small external force change based on the amorphous carbon cracks, so that high sensitivity (GF) is prepared>100) And a large tensile measurement range (>50) A flexible strain sensor.
The flexible substrate material comprises any one of Polydimethylsiloxane (PDMS), polyvinylidene fluoride (PVDF), polyethylene terephthalate (PET), polypropylene (PP), Polyimide (PI), polymethyl methacrylate (PMMA), Natural Rubber (NR), styrene-butadiene rubber (SBR), epoxy resin or thermoplastic elastomer (TPU, SBCS and POE). Further, the flexible substrate material is Polydimethylsiloxane (PDMS).
The invention also provides a preparation method of the amorphous carbon-based flexible sensor based on the crack wrinkle structure, which comprises the following steps:
the method comprises the steps of pre-stretching a flexible substrate, placing the pre-stretched flexible substrate in a vacuum cavity, continuously introducing Ar gas, rotating the pre-stretched flexible substrate, starting a solid carbon source target by adopting a magnetron sputtering technology, depositing an amorphous carbon film on the surface of the pre-stretched flexible substrate, pasting and curing conductive metal to two ends of the amorphous carbon film, and releasing the pre-stretched flexible substrate, so that the rebounded amorphous carbon film on the surface of the pre-stretched flexible substrate has a crack wrinkle structure, and the amorphous carbon-based flexible sensor based on the crack wrinkle structure is obtained.
Further, the solid carbon source target is a graphite target. Gaseous carbon sources such as methane, acetylene, etc. are not used because hydrogen-containing carbon sources increase the resistance of the deposited carbon film and are uncontrollable.
The elongation of the pre-stretched flexible substrate is 10% -100%. After the pre-stretching elongation is too long and the substrate is hardened after etching, the substrate cannot rebound effectively; the pre-stretching length is too short, and the wrinkle effect is not obvious.
The flow rate of the Ar gas is 40-100 sccm.
The specific steps of rotationally prestretching the flexible substrate are as follows: rotating forwards at 10-50rpm for 10-80min, and then rotating backwards for 10-80 min.
The amorphous carbon film with proper thickness is produced at proper rotating speed and deposition time, and the forward rotation and reverse rotation time are kept consistent, so that the carbon film can be uniformly deposited.
Before the solid carbon source is started, the rotary pre-stretched flexible substrate is etched.
Further, the etching process comprises: the pulse bias is 350-450V, the vacuum degree of the chamber is 1.6 × 10-5-2.5×10-5And Torr, and the etching time is 10-60 min. Based on the surface cleanliness degree, the flexible substrate is etched in proper etching time, so that the surface of the flexible substrate is hardened, and the strength of the surface of the flexible substrate is enhancedAnd subsequent amorphous carbon film.
Further, after the rotating pre-stretched flexible substrate is etched, the bias power supply is turned off before the solid carbon source target is turned on, and the graphite target is self-cleaned, wherein the self-cleaning process comprises the following steps: the direct current power is 2-3kW, the pressure in the vacuum cavity is 2-4mTorr, and the cleaning time is 5-20 min.
The sputtering process of the solid carbon source target comprises the following steps: the DC sputtering power is 1.6-4.2kW, the deposition time is 20-160min, the bias voltage is 200-.
The curing time is 15-120min, and the curing temperature is 30-150 ℃. The curing is carried out at a proper temperature, so that the curing speed is accelerated, but the temperature is not proper to be too high, otherwise, the PDMS matrix is influenced to a certain extent.
The design idea of the invention is as follows: researching the sensing mechanism of the prepared amorphous carbon-based flexible strain sensor based on the crack wrinkle structure to obtain the following results: for surface-deposited strain sensors, the crack propagation mechanism may be its primary sensing mechanism because cracks propagate very easily in the brittle conductive layer during stretching. In the critical strain range, the conductivity of the sensor is primarily dependent on the extent of crack propagation, and after removal of the applied strain, the cracks created by the sensitive material reclose, returning the sensor resistance to substantially its original state. Therefore, reversible generation/closure of cracks is a prerequisite for a strain sensor with high sensitivity and good reproducibility. Furthermore, there may be a possibility of receiving conductive sp distributed in the amorphous carbon film2The influence of the cluster can change the sp of the film by regulating the carbon source type, the substrate pulse bias, the sputtering power, the deposition time and the like2And sp3The content, the cluster size and the distribution, thereby regulating and controlling the GF value of the element; and the thickness of the film can be changed, so that the initial resistance value of the element can be regulated and controlled. Therefore, by regulating and controlling the process parameters in the preparation method, the flexible strain sensor with high GF value and large stretching range can be obtained as required, and the flexible strain sensor with strong combination, long service life, high sensitivity and large stretching range can be realizedA rapid preparation technology. In summary, the invention uses the amorphous carbon film based on the crack wrinkle structure as the sensitive material, the amorphous carbon film is directly deposited on the surface of the prestretched flexible substrate, and the metal electrode is arranged on the surface of the amorphous carbon film to form the flexible strain sensor.
Compared with the prior art, the invention has the beneficial effects that:
(1) in the prior art, the flexible strain sensor has the advantages of low sensitivity, high preparation cost, complex preparation process and short service life. The method for presetting the microcrack fold structure on the amorphous carbon film layer is adopted, so that the sensor has the advantages of simple structure, convenience in testing, high sensitivity, good fatigue resistance and the like in specific use.
(2) The amorphous carbon-based flexible strain sensor based on the crack wrinkle structure has an ultra-high GF value and a large stretching range, wherein the GF value is 100-1000, and the maximum elongation can reach more than 50%; moreover, the GF value and the initial resistance value can be further regulated and controlled by changing the process parameters.
(3) Compared with the graphene and carbon nanotube equal-resistance material, the amorphous carbon film is simple and convenient to prepare, low in production cost, easy to process, capable of large-area in-situ deposition and free of manual transfer, and therefore has obvious process advantages.
(4) The amorphous carbon-based flexible strain sensor based on the crack wrinkle structure provided by the invention takes the amorphous carbon film as the functional layer, has excellent performances similar to those of diamond, such as friction resistance, chemical inertness and the like, and also has excellent electrical characteristics, so that the prepared product is low in price and high in cost performance.
(5) The flexible strain sensor with the microcrack fold structure provided by the invention can monitor the strain change in real time through the change of resistance, and the excellent performance has wide application prospects in the fields of electronic skin, human health monitoring devices and the like.
Drawings
FIG. 1 is a schematic flow chart of an embodiment of an amorphous carbon-based flexible strain sensor based on a crack-wrinkle structure;
FIG. 2 is a structural schematic picture of an amorphous carbon-based flexible strain sensor based on a crack-wrinkle structure;
FIG. 3 is a picture of the microstructure and the three-dimensional structure of the amorphous carbon-based flexible strain sensor based on the crack wrinkle structure, which is prepared in example 1;
fig. 4 is a graph of the relationship between the resistivity and the sensitivity coefficient of the amorphous carbon-based flexible strain sensor based on the crack wrinkle structure in the loading stage, which is prepared in example 1, and the change with strain;
fig. 5 is a voltage trend chart of 1500 times of cyclic loading and unloading of the crack wrinkle structure-based amorphous carbon-based flexible strain sensor prepared in example 1 at a constant current source of 1 nA.
FIG. 6 is a picture of the microstructure and the three-dimensional structure of the amorphous carbon-based flexible strain sensor based on the crack wrinkle structure, which is prepared in example 5;
fig. 7 is a graph of the relationship between the resistivity and the sensitivity coefficient of the amorphous carbon-based flexible strain sensor based on the crack wrinkle structure in the loading stage, which is prepared in example 5, and the change with strain;
fig. 8 is a voltage trend chart of 1500 times of cyclic loading and unloading of the crack wrinkle structure-based amorphous carbon-based flexible strain sensor prepared in example 5 at a constant current source of 10 nA.
Detailed Description
The invention will be described in further detail below with reference to the embodiments of the drawing, which are intended to facilitate the understanding of the invention and are not intended to limit the invention in any way.
As shown in fig. 1, the flexible substrate is fixed, stretched, amorphous carbon is deposited on the stretched flexible substrate, and finally the flexible substrate is rebounded to obtain the crack wrinkle structure-based amorphous carbon-based flexible strain sensor
Example 1:
in this embodiment, as shown in fig. 2, the flexible strain sensor is composed of a PDMS substrate, an amorphous carbon film with a preset crack wrinkle structure, and a conductive silver paste electrode, where the amorphous carbon film with the preset crack wrinkle structure is located on the surface of the PDMS substrate, and the metal electrode is located at two ends of the amorphous carbon film with the preset crack wrinkle structure, that is, the silver paste electrode is located at two ends of the surface of the amorphous carbon film.
The preparation method of the flexible strain sensor comprises the following steps:
(1) the PDMS substrate was pre-stretched with a self-made stretching device at 10% elongation and tested to have a tensile strength of 4MPa, a tear strength of 7kN/m and an elongation at break of 100%. Reserving 2 regions of 50mm × 10mm to-be-deposited electrodes on the surface, covering the rest regions with a mask plate, fixing the mask plate on a substrate support rotating in a vacuum cavity, and pre-vacuumizing to 2.5 × 10mm-5Torr；
(2) In order to obtain higher bonding strength, Ar gas is introduced into the coating cavity, and the flow rate of the Ar gas is 100 sccm; etching the PDMS substrate for 20min under the conditions that the bias voltage of the pulse substrate is-400V and the working pressure is 1.1 Pa;
(3) turning off the bias power supply, turning on the direct current power supply, and carrying out self-cleaning on the target material for 10min under the conditions that the direct current power is 2.1kW and the cavity pressure is 3.3 mTorr;
(4) introducing Ar gas into the chamber, wherein the flow rate of the Ar gas is 65 sccm; and simultaneously turning on a bias voltage and a direct current power supply, and sputtering the graphite target under the conditions that the working pressure is 0.3Pa, the bias voltage of the pulse substrate is-200V and the direct current power is 2.1 kW. The deposition time is generally 20min, and the film thickness is controlled at 110-130 nm. In the deposition process, the substrate rotates forwards for 10min at the speed of 10rpm and then rotates backwards for 10min so as to improve the uniformity of the film;
(5) connecting a platinum wire to two ends of the surface of the amorphous carbon film by using conductive silver paste, and curing for 20 minutes at 120 ℃;
(6) the rebounded amorphous carbon film on the surface of the pre-stretched flexible substrate has a crack wrinkle structure so as to obtain an amorphous carbon-based flexible sensor based on the crack wrinkle structure, the surface appearance of the obtained amorphous carbon-based flexible sensor is as shown in fig. 3, 10-15 cracks are distributed in the visual field range of 200 x 200 μm, and the shape of the block wrinkle structure is approximately rectangular or trapezoidal. The crack direction is mostly parallel to the stretching direction, and the fold structure is perpendicular to the stretching direction.
The prepared amorphous carbon-based flexible strain sensor is subjected to sensing performance test, namely the sensor is stretched, the resistance change of the sensor is observed, as shown in fig. 4, the resistivity is in an ascending trend along with the increase of the strain degree and has good linearity, and the sensitivity of the sensor reaches the highest when the stretching rate is in a range of 20-30%. Applying tensile deformation to the sensing element by a micro-stress applying and testing system through a micro-stress device; the four-point method is adopted to test the I-V curve of the sensor at room temperature through a nano-volt meter and a current source, and as shown in FIG. 5, when the constant current source is 1nA, the trend of the voltage curve shows good reproducibility along with the increase of the number of times of loading and unloading of the circulation, which indicates that the prepared sensor has excellent dynamic circulation stability. Calculating the resistance value R of the linear contact region by using ohm's law to obtain the relation of the resistance change rate along with the change of strain, and then passing through the following formula:
(R0initial resistance value, R is the resistance value of the film after stretching, and epsilon is the corresponding tensile strain) has a maximum GF value of about 155.
Example 2:
in this embodiment, the structure of the flexible strain sensor is exactly the same as in embodiment 1.
In this embodiment, the preparation method of the flexible strain sensor is substantially the same as that in embodiment 1, except that the tensile strength of the PDMS substrate selected in step (1) is 3.5MPa, the tear strength is 15kN/m, and the elongation at break is 350%.
And (3) carrying out sensing performance test on the prepared amorphous carbon-based flexible strain sensor, namely stretching the sensor and observing the resistance change of the sensor. Applying tensile deformation to the sensing element by a micro-stress applying and testing system through a micro-stress device; the method comprises the following steps of testing an I-V curve of the sensor at room temperature by a four-point method through a nano-volt meter and a current source, calculating the resistance R of a linear contact region by using ohm's law, obtaining the relation of the resistance change rate along with the change of strain, and then obtaining the following formula:
(R0initial resistance, R is the resistance of the film after stretching, and epsilon is the corresponding tensile strain), with a maximum GF value of about 105.
Example 3:
in this embodiment, the structure of the flexible strain sensor is exactly the same as in embodiment 1.
In this example, the flexible strain sensor was prepared in substantially the same manner as in example 1, except that the PDMS substrate was pre-stretched at an elongation of 20% in step (1).
And (3) carrying out sensing performance test on the prepared amorphous carbon-based flexible strain sensor, namely stretching the sensor and observing the resistance change of the sensor. Applying tensile deformation to the sensing element by a micro-stress applying and testing system through a micro-stress device; the method comprises the following steps of testing an I-V curve of the sensor at room temperature by a four-point method through a nano-volt meter and a current source, calculating the resistance R of a linear contact region by using ohm's law, obtaining the relation of the resistance change rate along with the change of strain, and then obtaining the following formula:
(R0initial resistance value, R is the film resistance value after stretching, and epsilon is the corresponding tensile strain), the maximum GF value is about 278.
Example 4:
in this embodiment, the structure of the flexible strain sensor is exactly the same as in embodiment 1.
In this example, the method of manufacturing the flexible strain sensor is substantially the same as that in example 1, except that the thin film deposition time in step (5) is 160 min.
And (3) carrying out sensing performance test on the prepared amorphous carbon-based flexible strain sensor, namely stretching the sensor and observing the resistance change of the sensor. Applying tensile deformation to the sensing element by a micro-stress applying and testing system through a micro-stress device; the method comprises the following steps of testing an I-V curve of the sensor at room temperature by a four-point method through a nano-volt meter and a current source, calculating the resistance R of a linear contact region by using ohm's law, obtaining the relation of the resistance change rate along with the change of strain, and then obtaining the following formula:
(R0initial resistance, R is the resistance of the film after stretching, and e is the corresponding tensile strain), and its maximum GF value is about 746.
Example 5:
in this embodiment, the flexible strain sensor is composed of a PDMS substrate, an amorphous carbon film with a preset crack wrinkle structure, and conductive silver colloid electrodes, where the amorphous carbon film with the preset crack wrinkle structure is located on the surface of the PDMS substrate, and the silver colloid electrodes are located at two ends of the surface of the amorphous carbon film with the preset crack wrinkle structure.
The preparation method of the flexible strain sensor comprises the following steps:
(1) the two ends of the PDMS substrate are fixed with self-made stretching devices, a cylinder with the diameter of 10mm is inserted in the middle of the PDMS substrate to bend the PDMS substrate, and the test shows that the tensile strength of the PDMS substrate is 4MPa, the tear strength is 7kN/m, and the elongation at break is 100%. Reserving 2 regions of 50mm × 10mm to-be-deposited electrodes on the surface, covering the rest regions with a mask plate, fixing the mask plate on a substrate support rotating in a vacuum cavity, and pre-vacuumizing to 1.6 × 10-5Pa。
(2) In order to obtain higher bonding strength, Ar gas is introduced into the coating cavity, and the flow rate of the Ar gas is 40 sccm; and etching the PDMS substrate for 60min under the conditions that the bias voltage of the pulse substrate is-350V and the working pressure is 1.5 Pa.
(3) And (3) closing the bias power supply, opening the direct current power supply, and carrying out self-cleaning on the target material for 20min under the conditions that the direct current power is 3kW and the cavity pressure is 2.4 mTorr.
(4) Introducing Ar gas into the chamber, wherein the flow rate of the Ar gas is 80 sccm; and simultaneously turning on a bias voltage and a direct current power supply, and sputtering the graphite target under the conditions that the working pressure is 0.5Pa, the bias voltage of the pulse substrate is-320V and the direct current power is 2.8 kW. The deposition time is generally 10min, and the film thickness is controlled to be about 110-130 nm. In the deposition process, the substrate rotates forwards for 50min at the speed of 30rpm and then rotates backwards for 50min so as to improve the uniformity of the film;
(5) connecting a platinum wire to two ends of the surface of the amorphous carbon film by using conductive silver paste, and curing for 120 minutes at 30 ℃;
(6) the rebounded amorphous carbon film on the surface of the pre-stretched flexible substrate has a crack wrinkle structure so as to obtain an amorphous carbon-based flexible sensor based on the crack wrinkle structure, the physical diagram is shown in fig. 6 so as to obtain the surface appearance of the amorphous carbon-based flexible sensor, 20-30 cracks are distributed in the visual field range of 200 x 200 mu m, and the shape of the block wrinkle structure is approximately a rectangular big block and a triangular small block. The crack direction is mostly parallel to the stretching direction, and the fold structure is perpendicular to the stretching direction. The sensing performance of the prepared amorphous carbon-based flexible strain sensor is tested, namely the sensor is stretched, the resistance change of the sensor is observed, as shown in fig. 7, the relative resistance change shows an ascending trend along with the increase of the strain degree and has good linearity, and the sensitivity of the sensor reaches the highest when the stretching rate is in a range of 20-30%. Applying tensile deformation to the sensing element by a micro-stress applying and testing system through a micro-stress device; the four-point method is adopted to test the I-V curve of the sensor at room temperature through a nano-volt meter and a current source, and as shown in FIG. 8, when the constant current source is 10nA, the trend of the voltage curve shows good reproducibility along with the increase of the number of times of loading and unloading of the circulation, which indicates that the prepared sensor has excellent dynamic circulation stability. Calculating the resistance value R of the linear contact region by using ohm's law to obtain the relation of the resistance change rate along with the change of strain, and then passing through the following formula:
(R0is an initial resistance value, R is a resistance value of the film after stretching, and ε is a value corresponding toTensile strain of (f) having a maximum GF value of about 567;
the embodiments described above are intended to illustrate the technical solutions of the present invention in detail, and it should be understood that the above-mentioned embodiments are only specific embodiments of the present invention, and are not intended to limit the present invention, and any modifications and improvements made within the scope of the principles of the present invention should be included in the protection scope of the present invention.
Claims (10)
1. An amorphous carbon-based flexible sensor based on a crack pleat structure, comprising: the flexible substrate comprises a flexible substrate, an amorphous carbon film and conductive electrodes, wherein the amorphous carbon film is deposited on the surface of the flexible substrate, the conductive electrodes are located at two ends of the amorphous carbon film, and the amorphous carbon film is of a crack and fold structure.
2. An amorphous carbon based flexible sensor based on a crack pleat structure as claimed in claim 1, characterized in that the density of cracks in the crack pleat structure is 10-30 stripes/200 x 200 μm, and the pleat structure is rectangular, trapezoidal or triangular.
3. An amorphous carbon-based flexible sensor based on a crack pleat structure as claimed in claim 1, wherein the flexible substrate material comprises any one of polydimethylsiloxane, polyvinylidene fluoride, polyethylene terephthalate, polypropylene, polyimide, polymethyl methacrylate, natural rubber, styrene-butadiene rubber, epoxy resin or thermoplastic elastomer.
4. A method of manufacturing an amorphous carbon based flexible sensor based on a crack pleat structure according to any of the claims 1-3, comprising:
pre-stretching a flexible substrate, placing the pre-stretched flexible substrate in a vacuum cavity, continuously introducing Ar gas, rotating the pre-stretched flexible substrate, starting a solid carbon source target by adopting a magnetron sputtering technology, depositing an amorphous carbon film on the surface of the pre-stretched flexible substrate, pasting and curing conductive metal to two ends of an amorphous carbon film, and releasing the pre-stretched flexible substrate to obtain the amorphous carbon-based flexible sensor based on the crack fold structure.
5. The method for preparing an amorphous carbon-based flexible sensor based on a crack pleat structure as claimed in claim 4, wherein the elongation of the pre-stretched flexible substrate is 10% -100%.
6. The method for preparing an amorphous carbon-based flexible sensor based on a crack pleat structure as claimed in claim 4, wherein the gas flow rate of Ar gas is 40-100 sccm.
7. The method for preparing the amorphous carbon-based flexible sensor based on the crack pleat structure as claimed in claim 4, wherein the specific steps of pre-stretching the flexible substrate by rotation are as follows: rotating forwards at 10-50rpm for 10-80min, and then rotating backwards for 10-80 min.
8. The method for preparing an amorphous carbon-based flexible sensor based on a crack pleat structure as claimed in claim 4, wherein the rotating pre-stretched flexible substrate is etched before the solid carbon source is started.
9. The method for preparing the amorphous carbon-based flexible sensor based on the crack wrinkle structure as claimed in claim 8, wherein the etching process is as follows: the pulse bias is 350-450V, the vacuum degree of the chamber is 1.6 × 10-5-3×10-5And Torr, and the etching time is 10-60 min.
10. The method for preparing an amorphous carbon-based flexible sensor based on a crack wrinkle structure as claimed in claim 4, wherein the sputtering process of the solid carbon source target material is as follows: the sputtering power is 1.6-4.2kW, the deposition time is 20-160min, the bias voltage is 200-350V, and the pressure in the vacuum chamber is 2-4 mTorr.
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