CN118189798B - Flexible strain sensor based on heterogeneous modulus matching and preparation method thereof - Google Patents
Flexible strain sensor based on heterogeneous modulus matching and preparation method thereof Download PDFInfo
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- G—PHYSICS
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- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
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- 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 flexible strain sensor based on heterogeneous modulus matching and a preparation method thereof. The invention has simple processing technology, low technology cost, good processing consistency, convenient large-scale manufacture and good application prospect.
Description
Technical Field
The invention relates to the field of flexible strain sensor preparation, in particular to a flexible strain sensor based on heterogeneous modulus matching and a preparation method thereof.
Background
With the development of modern technology and the rapid rise of artificial intelligence, flexible electronics have received a great deal of attention. The flexible strain sensor is used as an important component of flexible electronics, has wide application prospect in the fields of motion monitoring, man-machine interaction, electronic skin, soft robots, medical rehabilitation and the like, and can realize motion tracking, expression recognition, sign language translation, pulse breath detection of a human body and the like. The main categories of strain sensors are resistive, capacitive and piezoelectric. The capacitive strain sensor has high sensitivity, but has poor response performance to strain due to structural limitation, and the piezoelectric strain sensor has high response speed, but has high piezoelectric performance requirement on materials, and is not suitable for measuring static signals. In contrast, the resistive strain sensor has the advantages of simple structure, wide sensing range, easy manufacture and the like, and is a hot spot for research in recent years. Unless otherwise specified, the strain sensors described below are all resistive.
Sensitivity (GF) and stretchability (working range) are two of the most critical parameters for evaluating high performance flexible strain sensors. Ideally, the flexible strain sensor should have high sensitivity and greater stretchability (npj Flexible Electronics, 2018, 2 (1): 1-10). However, high sensitivity (GF > 100) and large stretchability (stretch ratio > 50%) are difficult to achieve simultaneously (adv. Funct. Mater. 2019, 29, 1807882) because: high sensitivity requires that the sensor undergo a sharp change in resistance at small strains, while high stretchability requires that the sensor remain in a conductive path at large strains. Thus, optimization of sensitivity and stretchability has been a major challenge for high performance flexible strain sensors (ACS appl. Mate. Interfaces 2022, 14, 36611-36621).
At present, there are two main optimization strategies for the high sensitivity and large stretchability of the resistive flexible film strain sensor:
one is to mix nanomaterials with different types/sizes/properties. Yang et al (adv. Funct. Mater. 2019, 29, 1807882) etched Ti 3C2Tx MXene through HF and TMAH (tetramethylammonium hydroxide), respectively, to adjust its microscopic morphology, constructed a hybrid network structure consisting of Ti 3C2Tx MXene nanoparticles and nanoplatelets, and prepared strain sensors achieved high sensitivity (GF > 178.4) and a wide working range (53%). However, the method has complex etching process and high operation requirement, and is not convenient for mass production. Shi et al (adv. Funct. Mater. 2018, 28, 1800850) propose a layered conductive network structure comprising a zero-dimensional (0D) C 60, one-dimensional (1D) Ag nanowires (AgNWs), and two-dimensional (2D) Graphene Oxide (GO), wherein C 60 provides lubricity, agNWs provides excellent conductivity, GO provides a layered structure, and the obtained flexible strain sensor has high sensitivity and wide operating range. However, the method requires a complex material dispersing process, and the screen printing equipment has the advantages of more parameters, complicated adjustment and high processing cost. Han et al (npj Flexible Electronics, 2018, 2 (1): 1-10) propose the fabrication of nanowire-microfluidic hybrid strain sensors by doping metal nanowires (AgNWs, cuNWs) or Carbon Nanotubes (CNTs) and a conductive organic solution poly (3, 4-ethylenedioxythiophene): polystyrene sulfonate (PEDOT: PSS), which have both high sensitivity and high stretchability, and when nanowires are detached or disconnected from each other under large strains, the conductive solution provides an electroosmotic flow path, thus enabling a wide range of sensing. However, the consistency of the process is poor, and the conductive solution is added into the micro-channel through the injector, so that the sensor packaging is challenged.
And secondly, the combination of different crack structures. Wang et al (Small 2023, 19, 2304033) create a non-uniform surface by treating PDMS substrates with ultraviolet-ozone (UVO) under a mask. Sparse penetrating cracks with large crack depth are formed on the PDMS substrate after being treated by UVO for a long time, and dense microcrack networks with small depths are generated on the PDMS substrate after being treated by UVO for a short time. The penetrating large crack penetrates the AgNW/MXene composite film during stretching to obtain high sensitivity, the dense micro crack maintains a conductive percolation path under large strain to provide a wide sensing range, and the sensor exhibits high sensitivity (gf≡244) and a wide linear range (60%). However, the method has the disadvantages of complex substrate surface treatment process, poor process consistency and poor sensor cycle durability due to the fact that the substrate is required to be pre-stretched to form cracks.
In summary, the conventional method for realizing the combination of high sensitivity and high stretchability of the resistive flexible film strain sensor has a plurality of disadvantages. If a preparation method which is simple in process, low in cost and convenient for large-scale manufacturing can be provided, the integration of conductive materials with various performances on the same stretchable flexible substrate is realized, and each conductive material can exert the respective performances to the greatest extent, the preparation method has great significance for manufacturing the flexible strain sensor with high sensitivity and large stretchability.
Disclosure of Invention
Based on the problems of the prior art, the invention aims to provide a preparation method of a flexible strain sensor based on heterogeneous modulus matching.
The invention provides an idea of integrating a plurality of conductive materials through a heterogeneous modulus substrate for the first time, and specifically comprises the following steps: strain sensors made of 1D materials such as Ag nanowires, for example, typically exhibit greater stretchability and lower sensitivity because 1D materials with high aspect ratios can maintain good interconnectivity and exhibit insignificant resistance changes over a large strain range. In contrast, strain sensors based on 2D materials (e.g., graphene, MXene, etc.) generally exhibit higher sensitivity and less stretchability, probably due to the strong interactions between adjacent sheets of 2D material that prevent effective sliding between sheets, allowing the 2D material to quickly break apart and sever the conductive pathways during stretching (adv. Function. Mater. 2019, 29, 1807882). The application of the two to the flexible strain sensor often cannot enable the sensor to have high sensitivity and high stretchability. If multiple conductive materials of different conductive characteristics could be integrated simultaneously on the same flexible substrate, it would be of great significance to manufacture flexible strain sensors of high sensitivity and large stretchability. According to the material mechanics, the surface strain distribution of a homogeneous modulus substrate is uniform during stretching, and if conductive materials with different conductive properties are integrated on the homogeneous modulus substrate, the performance of the strain sensor will still be limited by the conductive material with small stretchability. While also based on material mechanics, the surface strain distribution of a heterogeneous modulus substrate is non-uniform during stretching, with regions of lower modulus having greater stretch. Therefore, if a flexible substrate with heterogeneous modulus can be designed, the conductive material with small stretchability is arranged in the area with larger Young's modulus of the substrate, and the conductive material with large stretchability is arranged in the area with smaller Young's modulus of the substrate, so that the respective performances of various conductive materials can be exerted to the greatest extent, and the perfect combination of high sensitivity and large stretchability of the flexible strain sensor is realized.
Based on the technical principle, the invention provides a flexible strain sensor based on heterogeneous modulus matching, which is characterized in that: a flexible substrate comprising a heterogeneous modulus, the flexible substrate being divided into n regions according to young's modulus from small to large or from large to small: the 1 st Young modulus region, the 2 nd Young modulus region, … … th Young modulus region and the n Young modulus region, the 1 st Young modulus region is positioned in the middle of the flexible substrate, and the 2 nd Young modulus region, the … … th Young modulus region and the n Young modulus region are symmetrically arranged from the 1 st Young modulus region to two sides in sequence.
The flexible substrate is provided with n conductive material films which are sequentially divided from small to large according to the stretchability, the n conductive material films are distributed in n areas of the flexible substrate in a one-to-one correspondence mode according to the stretchability, the conductive material film with the largest stretchability is arranged in the area with the smallest Young modulus, the conductive material film with the smallest stretchability is arranged in the area with the largest Young modulus, and the like.
There are two specific configuration methods, as shown in fig. 1:
When the flexible substrate is divided into n regions according to young's modulus from small to large: the young's modulus gradually increases from the 1 st young's modulus region to the n-th young's modulus region. The 1 st Young's modulus region is positioned in the middle of the flexible substrate, symmetrically arranged as the 2 nd Young's modulus region on two sides of the flexible substrate, and then sequentially and symmetrically arranged as the 3 rd Young's modulus region, … … th Young's modulus region and the n's modulus region. The flexible substrate exhibits a symmetrical structure in which Young's modulus gradually increases from the middle to both sides. At this time, the 1 st young's modulus region matches the conductive material film having the largest stretchability, the 2 nd young's modulus region matches the conductive material film having the largest stretchability, … … nd young's modulus matches the conductive material film having the smallest stretchability.
When the flexible substrate is divided into n regions from large to small according to young's modulus: the Young's modulus gradually decreases from the 1 st Young's modulus region to the n's modulus region. The 1 st Young's modulus region is positioned in the middle of the flexible substrate, symmetrically arranged as the 2 nd Young's modulus region on two sides of the flexible substrate, and then sequentially and symmetrically arranged as the 3 rd Young's modulus region, … … th Young's modulus region and the n's modulus region. The flexible substrate exhibits a symmetrical structure in which Young's modulus gradually decreases from the middle to both sides. At this time, the 1 st young's modulus region matches the conductive material film having the smallest stretchability, the 2 nd young's modulus region matches the conductive material film having the 2 nd smallest stretchability, … … th young's modulus matches the conductive material film having the largest stretchability.
The stretchability of the conductive material film refers to the ability of the conductive material film to maintain a conductive path in a stretched state, and the quantization parameter is the maximum stretchability of the conductive material film to maintain an effective conductive path, the greater the maximum stretchability, the better the stretchability of the conductive material film. The testing method is to deposit the conductive material on a certain flexible substrate (such as PDMS, ecoflex, etc.) through a certain process (such as spraying, dripping, dry transfer, etc.), to manufacture the flexible strain sensor, and test the maximum elongation rate.
Therefore, in the structure of the flexible strain sensor, the conductive material with small stretchability is essentially arranged in the area with larger Young modulus of the substrate, and the conductive material with large stretchability is arranged in the area with smaller Young modulus of the substrate, so that the respective performances of the conductive materials can be exerted to the greatest extent, and the perfect combination of high sensitivity and large stretchability of the flexible strain sensor is realized.
Further, n is a positive integer greater than or equal to 2.
The invention also provides a preparation method of the flexible strain sensor based on heterogeneous modulus matching, which comprises the following steps: the patterning integration of n conductive material films with different stretchability is realized by using a mask deposition method, a flexible substrate with heterogeneous modulus is prepared by using the chemical property of a photoinitiator and an ultraviolet light mask gradient exposure method, and then the conductive material films are combined with the flexible substrate with heterogeneous modulus according to region matching by using a dry transfer method, so that the high-performance flexible strain sensor with high sensitivity and large stretchability is prepared. The invention has simple preparation process, low requirement on processing conditions, convenient mass production and good application prospect.
Further, the preparation method comprises the following steps:
(1) Preparing a dispersion liquid of n conductive materials with different stretchability;
(2) Designing n mask patterns by using plane drawing software;
(3) Processing patterns on the polymer plate by utilizing a laser cutting mode according to the mask patterns designed in the step (2) to obtain n masks;
(4) Sequentially depositing n conductive materials obtained in the step (1) on the same receiving substrate through n masks obtained in the step (3), and forming an integrated film formed by combining the n conductive materials;
(5) Adding an organic solution of a photoinitiator into a flexible polymer prepolymer, pouring the mixture into a mold, and exposing different areas of the mixture to ultraviolet light for different times through a mask to enable the different areas to have different Young modulus, so as to obtain a flexible substrate with heterogeneous modulus;
(6) Heating the flexible substrate with the heterogeneous modulus obtained in the step (5) to obtain a pre-cured flexible substrate with the heterogeneous modulus;
(7) Cutting an integrated film formed by combining n conductive materials obtained in the step (4) into a shape matched with a flexible substrate, transferring the integrated film to the pre-cured flexible substrate with heterogeneous modulus obtained in the step (6), and enabling all areas of the integrated film to be attached to all areas of the flexible substrate in a one-to-one correspondence manner to obtain the flexible substrate with heterogeneous modulus and a conductive layer;
(8) And (3) heating and curing the flexible substrate with the heterogeneous modulus of the conductive layer obtained in the step (7), and removing the receiving substrate to obtain the flexible strain sensor with the Young modulus of the flexible substrate matched with the stretchability of the conductive material.
Further, the conductive material in the step (1) is one or more of Ag nanowires (Ag NWs), cu nanowires (Cu NWs), au nanowires (Au NWs), silver nanoparticles (AgNPs), carbon Black (CB), carbon Nanotubes (CNT), graphene Oxide (GO), reduced graphene oxide (rGO), MXene, liquid metal, and Au.
Further, the power of the laser cutting in the step (3) is set to 80-130W, the speed is set to 15-25mm/s, and the thickness of the polymer plate is 2-4mm.
Further, the deposition method in the step (4) is one or more of spraying, dripping, suction filtration and sputtering.
Further, the photoinitiator in the step (5) is benzophenone, and the flexible polymer is a silicone rubber material. Preferably, the silicone rubber material is PDMS or Ecoflex, or the like.
Further, the ultraviolet light exposure time in the step (5) is 0-15min.
Further, the heating in the step (6) is to make the flexible substrate in an adhesive semi-cured state. Preferably, the heating temperature is 60-80deg.C, and the heating time is 10-45min.
Further, the transferring method in the step (7) is pressing, so that the two are tightly combined.
Further, the heating temperature of the heating curing in the step (8) is 60-80 ℃ and the heating time is 8-12h.
Further, the method of removing the receiving substrate in step (8) is to peel or dissolve the receiving substrate.
According to the preparation method of the flexible strain sensor based on heterogeneous modulus matching, the prepared conductive materials are selected from a plurality of materials with gradient change of stretchability, and then matching deposition is carried out according to the method that the conductive materials with small stretchability are arranged in the area with larger Young modulus of the substrate and the conductive materials with large stretchability are arranged in the area with smaller Young modulus of the substrate. To ensure that the conductive material deposition areas are conducted mutually, a certain area (such as 0.5 mm) is deposited at the boundary of the front conductive material and the rear conductive material in an overlapping way when the materials are deposited sequentially. In the deposition process, the receiving substrate is selected to be non-reactive with the dispersion solvent to ensure complete removal of the receiving substrate after transfer to the flexible substrate. In the preparation of the flexible substrate with heterogeneous modulus, benzophenone reacts with hydrogenated silicon groups in the flexible polymer under the irradiation condition of ultraviolet light, so that the reaction quantity of a main agent of the flexible polymer and a curing agent is reduced, and the Young modulus of the area is reduced. And controlling the ultraviolet light exposure time of different areas of the flexible substrate by using a mask, so as to form the heterogeneous modulus substrate with the Young modulus gradient change. For example, the Young's modulus of PDMS (ratio of main agent to curing agent is 10:3) is 2.4MPa, the PDMS (10:3) prepolymer containing benzophenone is exposed to ultraviolet light for different time, and then the Young's modulus is measured and calculated through a stretching experiment, and the result shows that after the PDMS is exposed to ultraviolet light for 5min, the Young's modulus of PDMS is reduced to 2MPa, and after the PDMS is exposed to ultraviolet light for 10min, the Young's modulus of PDMS is reduced to 1.3MPa. Compared with a method of directly splicing materials with multiple moduli, the method reduces the interface effect at the contact surface, reduces stress concentration, and provides a foundation for the large stretchability of the flexible substrate. Meanwhile, it should be noted that the dimensions of each exposure area of the substrate and the dimensions of each deposition area of the characteristic conductive material are in one-to-one correspondence, which is the key of matching the flexible substrate with the characteristic conductive material.
According to the invention, the prepared flexible strain sensor is clamped on a universal tensile testing machine for a tensile test, the tensile speed is set to be 5mm/min, and a universal meter is used for connecting the strain sensor, so that resistance data in the tensile process are acquired in real time. Experimental results show that the sensitivity coefficient GF of the flexible strain sensor can reach 246, the maximum tensile rate can reach 89%, and the comprehensive performance of the sensor is superior to that of a sensor prepared by respectively and independently depositing each conductive material on a heterogeneous modulus substrate.
Compared with the prior art, the invention has the beneficial effects that:
1. The matching strategy of the heterogeneous modulus substrate and the characteristic conductive materials is firstly provided, so that each conductive material can exert the respective performance advantages to the greatest extent, and a new design method is provided for preparing the flexible strain sensor with high sensitivity and large stretching range.
2. The flexible strain sensor based on heterogeneous modulus matching, which is prepared by the invention, has the advantages of simple processing technology, low processing cost, good processing consistency, convenience for large-scale manufacturing and good application prospect.
3. The flexible strain sensor based on heterogeneous modulus matching prepared by the invention has higher sensitivity and larger stretching range (the flexible strain sensor gf=246, the maximum stretching ratio is 89% as provided in the example).
Drawings
FIG. 1 is a schematic diagram of matching a flexible substrate of heterogeneous modulus with a film of conductive material of different stretchability.
Fig. 2 is a plan view of a mask pattern in embodiment 1.
FIG. 3 is a diagram of a mask process in example 1.
Fig. 4 is a schematic diagram of a multi-conductive material-bonded conductive film AACAM formed by suction filtration of AgNWs, agNWs/CNT, agNWs/MXene in example 1.
FIG. 5 is a schematic view of the PDMS zonal exposure in example 1.
Fig. 6 is a schematic diagram of a flexible strain sensor with a heterogeneous modulus PDMS substrate bonded to a multi-conductive material AACAM in example 1.
Fig. 7 is a physical view of AACAM flexible strain sensor in example 1.
Fig. 8 is a sensitivity curve of AACAM flexible strain sensor in example 1.
Fig. 9 is a sensitivity profile of the AgNWs flexible strain sensor of comparative example 1.
Fig. 10 is a sensitivity profile of the AgNWs/CNT flexible strain sensor of comparative example 2.
FIG. 11 is a plot of the sensitivity of the AgNWS/MXene flexible strain sensor of comparative example 3.
FIG. 12 is a plot of the sensitivity of AACAM flexible strain sensors made from a homogeneous modulus substrate (PDMS 10:3) in comparative example 4.
The sensitivity curve in fig. 8-12 is the relative resistance change/initial resistance (Δr/R 0) versus elongation epsilon, the sensitivity coefficient gf= (Δr/R 0）/ε=((R-R0 )/R0)/epsilon, where R 0 is the initial resistance of the sensor, epsilon is the elongation, and R is the resistance when the elongation of the sensor should be epsilon. Epsilon= (l-l 0）/l0, wherein l is the length of the sensor after stretching, l 0 is the initial length of the sensor, piecewise linear fitting is performed on the sensitivity curve, and as shown by the dotted line in the figure, the sensitivity coefficient GF is the slope of the corresponding fit line.
Detailed Description
The following description of the technical solutions in the embodiments of the present invention will be clear and complete, and it is obvious that the described embodiments are only some embodiments of the present invention, but not all embodiments. All other embodiments, which can be made by those skilled in the art based on the embodiments of the invention without making any inventive effort, are intended to be within the scope of the invention.
Example 1
(1) Three dispersions of different conductive materials were prepared, respectively: an ethanol dispersion of AgNWs at a volume of 10mL at 0.2 mg/mL; an ethanol dispersion with a total concentration of 0.3mg/mL and a volume of 10mL and a AgNWs/CNT mass ratio of 5:1; ethanol dispersion with a total concentration of 0.3mg/mL and a volume of 10mL and a AgNWS/MXene mass ratio of 5:1.
(2) Using the flat drawing software, 3 mask patterns were designed as shown in fig. 2.
(3) And (3) cutting the acrylic plate with the thickness of 2mm by using a carbon dioxide laser according to the mask pattern designed in the step (2) to obtain 3 masks, as shown in fig. 3.
(4) And (3) sequentially carrying out suction filtration on the three conductive material dispersion liquids obtained in the step (1) on the same polytetrafluoroethylene filter membrane through the 3 masks obtained in the step (3) to form an integrated film (called AACAM film for short, agNWS+AgNWS/CNT+AgNWS/MXene) formed by combining the 3 conductive material films, as shown in fig. 4.
(5) Preparing a dimethylbenzene solution with the mass fraction of 40% of benzophenone, adding the solution into PDMS (10:3) prepolymer with the mass fraction of 6%, pouring the solution into a 50mm multiplied by 30mm rectangular polytetrafluoroethylene mould, exposing an area with the middle of 6mm multiplied by 30mm to light for 5min by ultraviolet light, and exposing an area with the middle of 20mm multiplied by 30mm to light for 5min to obtain a heterogeneous modulus PDMS substrate, as shown in figure 5.
(6) And (3) heating the heterogeneous modulus PDMS substrate obtained in the step (5) at 65 ℃ for 29min to obtain the pre-cured heterogeneous modulus PDMS substrate.
(7) Cutting the AACAM conductive film obtained in the step (4) into a rectangle with the length of 0.5mm multiplied by 44mm, transferring the AACAM conductive film to the pre-cured heterogeneous modulus PDMS substrate obtained in the step (6), and attaching each area of the integrated film to each area of the flexible substrate in a one-to-one correspondence manner to obtain the heterogeneous modulus PDMS substrate with the AACAM conductive layer as shown in figure 6.
(8) Heating the PDMS substrate with AACAM conductive layer obtained in the step (7) at 65deg.C for 10h, and stripping polytetrafluoroethylene filter membrane to obtain the material shown in figure 7. Then, copper wires are bonded at two ends by using conductive silver paste to prepare AACAM flexible strain sensors, the flexible strain sensors are clamped on a universal tensile testing machine and stretched at a speed of 5mm/min, meanwhile, the copper wires are connected with a universal meter, real-time resistance values are recorded, and a sensitivity curve diagram is shown in FIG. 8.
In example 1, when the prepared heterogeneous modulus PDMS substrate was divided into 3 regions according to young's modulus from small to large, the exposure time of the 1 st young's modulus region located in the middle was 10min, and its young's modulus was 1.3MPa; the exposure time of the 2 nd Young's modulus regions at the two sides of the 1 st Young's modulus region is 5min, and the Young's modulus is 2MPa; the 3 rd Young's modulus region at the outermost side was not exposed, and the Young's modulus was 2.4MPa. Thus, the prepared heterogeneous modulus PDMS substrate exhibits a symmetrical structure in which young's modulus gradually increases from the middle to both sides.
In example 1, agNWs had a large aspect ratio, high conductivity, and maintained good interconnectivity over a large tensile range. CNT is also a 1D structural material, but its aspect ratio is relatively small, conductivity is poor, and secondary clusters are very likely to occur, so AgNWs and CNT-doped strain sensors are less stretchable than pure AgNWs strain sensors. MXene is a 2D structural material with good electrical conductivity and rapidly breaks apart and cuts off conductive paths during stretching. Therefore, the strain sensor doped with AgNWs and MXene can greatly improve the sensitivity of the sensor compared with the strain sensor doped with pure AgNWs, and meanwhile, the stretchability is sacrificed. AgNWS, agNWS/CNT (5:1) and AgNWS/MXene (5:1) are respectively deposited on a PDMS (10:3) substrate through vacuum suction filtration and dry transfer processes to prepare corresponding strain sensors, and the maximum stretching rates of the strain sensors are tested to be 100%, 77% and 47% in sequence. In combination with the above, agNWs/CNT (5:1), and AgNWs/MXene (5:1) were used as matching materials for the small, medium, and large modulus substrate regions, respectively.
Comparative example 1
The use of AgNWs as a conductive layer contrasts the advantages of matching and combining heterogeneous moduli with a multi-conductive material, as follows:
(1) An ethanol dispersion of AgNWs was prepared at a concentration of 1mg/mL and a volume of 10 mL.
(2) And (3) filtering the ethanol dispersion liquid of AgNWs obtained in the step (1) on a polytetrafluoroethylene filter membrane to form an AgNWs conductive film.
(3) Preparing a dimethylbenzene solution with the mass fraction of 40% of benzophenone, adding the solution into PDMS (10:3) prepolymer with the mass fraction of 6%, pouring the solution into a 50mm multiplied by 30mm rectangular polytetrafluoroethylene mould, exposing an area with the middle of 6mm multiplied by 30mm to light for 5min by utilizing ultraviolet light, and exposing an area with the middle of 20mm multiplied by 30mm to light for 5min to obtain the heterogeneous modulus PDMS substrate.
(4) And (3) heating the heterogeneous modulus PDMS substrate obtained in the step (3) at 65 ℃ for 29min to obtain the pre-cured heterogeneous modulus PDMS substrate.
(5) Cutting the AgNWs conductive film obtained in the step (2) into a rectangle with the length of 0.5mm multiplied by 44mm, and transferring the rectangle onto the pre-cured heterogeneous modulus PDMS substrate obtained in the step (4) by a dry method to obtain the heterogeneous modulus PDMS substrate with the AgNWs conductive layer.
(6) Heating the heterogeneous modulus PDMS substrate with the AgNWs conducting layer obtained in the step (5) for 10 hours at 65 ℃, peeling off the polytetrafluoroethylene filter membrane, and then bonding copper wires at two ends by using conductive silver paste to obtain the flexible strain sensor with the heterogeneous modulus PDMS substrate combined with AgNWs. Then the sample was clamped on a universal tensile tester and stretched at a rate of 5mm/min, and simultaneously copper wires were connected to a multimeter, and the actual resistance was recorded as a sensitivity profile, as shown in FIG. 9.
Comparative example 2
The AgNWs/CNT was used as a conductive layer to compare the advantages of matching and combining heterogeneous moduli with a multi-conductive material as follows:
(1) An ethanol dispersion was prepared at a concentration of 1mg/mL and a volume of 10mL, with a AgNWs/CNT mass ratio of 5:1.
(2) And (3) filtering the ethanol dispersion of AgNWS/CNT obtained in the step (1) on a polytetrafluoroethylene filter membrane to form an AgNWS/CNT conductive film.
(3) Preparing a dimethylbenzene solution with the mass fraction of 40% of benzophenone, adding the solution into PDMS (10:3) prepolymer with the mass fraction of 6%, pouring the solution into a 50mm multiplied by 30mm rectangular polytetrafluoroethylene mould, exposing an area with the middle of 6mm multiplied by 30mm to light for 5min by utilizing ultraviolet light, and exposing an area with the middle of 20mm multiplied by 30mm to light for 5min to obtain the heterogeneous modulus PDMS substrate.
(4) And (3) heating the heterogeneous modulus PDMS substrate obtained in the step (3) at 65 ℃ for 29min to obtain the pre-cured heterogeneous modulus PDMS substrate.
(5) Cutting the AgNWS/CNT conductive film obtained in the step (2) into a rectangle with the length of 0.5mm multiplied by 44mm, and transferring the rectangle onto the pre-cured non-uniform modulus PDMS substrate obtained in the step (4) by a dry method to obtain the non-uniform modulus PDMS substrate with the AgNWS/CNT conductive layer.
(6) Heating the heterogeneous modulus PDMS substrate with the AgNWS/CNT conductive layer obtained in the step (5) for 10 hours at 65 ℃, peeling off the polytetrafluoroethylene filter membrane, and then bonding copper wires at two ends by using conductive silver paste to obtain the flexible strain sensor with the heterogeneous modulus PDMS substrate combined with the AgNWS/CNT. Then the sample was clamped on a universal tensile tester and stretched at a rate of 5mm/min, and simultaneously copper wires were connected to a multimeter, and the actual resistance was recorded as a sensitivity profile, as shown in FIG. 10.
Comparative example 3
The use of AgNWs/MXene as the conductive layer contrasts the advantages of a multi-conductive material combined with a heterogeneous modulus match as follows:
(1) An ethanol dispersion was prepared at a concentration of 1mg/mL and a volume of 10mL, with a AgNWS/MXene mass ratio of 5:1.
(2) And (3) filtering the ethanol dispersion liquid of AgNWS/MXene obtained in the step (1) on a polytetrafluoroethylene filter membrane to form the AgNWS/MXene conductive film.
(3) Preparing a dimethylbenzene solution with the mass fraction of 40% of benzophenone, adding the solution into PDMS (10:3) prepolymer with the mass fraction of 6%, pouring the solution into a 50mm multiplied by 30mm rectangular polytetrafluoroethylene mould, exposing an area with the middle of 6mm multiplied by 30mm to light for 5min by utilizing ultraviolet light, and exposing an area with the middle of 20mm multiplied by 30mm to light for 5min to obtain the heterogeneous modulus PDMS substrate.
(4) And (3) heating the heterogeneous modulus PDMS substrate obtained in the step (3) at 65 ℃ for 29min to obtain the pre-cured heterogeneous modulus PDMS substrate.
(5) Cutting the AgNWS/MXene conductive film obtained in the step (2) into a rectangle with the length of 0.5mm multiplied by 44mm, and transferring the rectangle onto the pre-cured heterogeneous modulus PDMS substrate obtained in the step (4) by a dry method to obtain the heterogeneous modulus PDMS substrate with the AgNWS/MXene conductive layer.
(6) Heating the heterogeneous modulus PDMS substrate with the AgNWS/MXene conductive layer obtained in the step (5) for 10 hours at 65 ℃, peeling off the polytetrafluoroethylene filter membrane, and then bonding copper wires at two ends by using conductive silver paste to obtain the flexible strain sensor with the heterogeneous modulus PDMS substrate combined with the AgNWS/MXene. Then the sample was clamped on a universal tensile tester and stretched at a rate of 5mm/min, and simultaneously copper wires were connected to a multimeter, and the actual resistance was recorded as a sensitivity profile, as shown in FIG. 11.
Comparative example 4
A homogeneous modulus substrate (PDMS 10: 3) was used to compare the advantages of a multi-conductive material combined with a heterogeneous modulus match, as follows:
PDMS (10:3) prepolymer was poured into a 50mm by 30mm rectangular polytetrafluoroethylene mold and heated at 65℃for 29min to obtain a pre-cured homogeneous modulus substrate.
The AACAM conductive film obtained in step (4) of example 1 was cut into a rectangle of 0.5mm×44mm and then transferred onto a homogeneous modulus substrate to obtain a homogeneous modulus substrate with AACAM conductive layer.
Heating the homogeneous modulus substrate with AACAM conductive layers obtained in the step (2) for 4 hours at 65 ℃, peeling off a polytetrafluoroethylene filter membrane, bonding copper wires at two ends by using conductive silver paste to prepare a flexible strain sensor, clamping the flexible strain sensor on a universal tensile testing machine, stretching at a speed of 5mm/min, simultaneously connecting the copper wires with a universal meter, recording the actual resistance value thereof, and making a sensitivity curve chart, as shown in figure 12.
In fig. 9, the AgNWs flexible strain sensor has a maximum sensitivity gf=93 and a maximum elongation of 109%, which indicates that the sensor has good stretchability but has a low sensitivity; the maximum sensitivity gf=111, up to 72% maximum elongation of the AgNWs/CNT flexible strain sensor in fig. 10, illustrates that both its stretchability and sensitivity are at a moderate level; the maximum sensitivity gf=1284 and the maximum elongation of the AgNWs/MXene flexible strain sensor in fig. 11 is up to 47%, which indicates that the flexible strain sensor has higher sensitivity but poorer stretchability; in fig. 8, the maximum sensitivity gf=246 and the maximum elongation of the AACAM flexible strain sensor reach 89%, which indicates that the AACAM flexible strain sensor based on the heterogeneous modulus matching has both high sensitivity and high elongation on the heterogeneous modulus substrate compared to the flexible strain sensor made of a single conductive material.
The flexible strain sensor AACAM made from a homogeneous modulus substrate (PDMS 10: 3) in fig. 12 had a maximum sensitivity of 97 and a maximum elongation of 71%. By contrast, the AACAM flexible strain sensor based on heterogeneous modulus matching has significantly improved performance in both sensitivity and tensile range compared with the homogeneous modulus AACAM flexible strain sensor.
The above embodiments are merely exemplary embodiments of the present invention and are not intended to limit the present invention, but any modifications, equivalents, improvements and modifications falling within the spirit and principles of the invention should be included in the scope of the present invention.
Claims (9)
1. Flexible strain sensor based on heterogeneous modulus matches, its characterized in that: a flexible substrate comprising a heterogeneous modulus, the flexible substrate being divided into n regions according to young's modulus from small to large or from large to small: the 1 st Young modulus region, the 2 nd Young modulus region, … … th Young modulus region and the n Young modulus region, wherein the 1 st Young modulus region is positioned in the middle of the flexible substrate, and the 1 st Young modulus region, the … … nd Young modulus region and the n Young modulus region are symmetrically arranged from the 1 st Young modulus region to two sides in sequence;
The flexible substrate is provided with n conductive material films which are sequentially divided from small to large according to the stretchability, the n conductive material films are distributed in n areas of the flexible substrate in a one-to-one correspondence mode according to the stretchability, the conductive material film with the largest stretchability is arranged in the area with the smallest Young modulus, the conductive material film with the smallest stretchability is arranged in the area with the largest Young modulus, and the like.
2. A method of manufacturing a heterogeneous modulus matching based flexible strain sensor as claimed in claim 1, wherein: the patterning integration of n conductive material films with different stretchability is realized by using a mask deposition method, a flexible substrate with heterogeneous modulus is prepared by using the chemical property of a photoinitiator and an ultraviolet light mask gradient exposure method, and then the conductive material films are combined with the flexible substrate with heterogeneous modulus according to region matching by using a dry transfer method, so that the flexible strain sensor based on the heterogeneous modulus matching is prepared.
3. The method of manufacturing according to claim 2, comprising the steps of:
(1) Preparing a dispersion liquid of n conductive materials with different stretchability;
(2) Designing n mask patterns by using plane drawing software;
(3) Processing patterns on the polymer plate by utilizing a laser cutting mode according to the mask patterns designed in the step (2) to obtain n masks;
(4) Sequentially depositing n conductive materials obtained in the step (1) on the same receiving substrate through n masks obtained in the step (3), and forming an integrated film formed by combining the n conductive materials;
(5) Adding an organic solution of a photoinitiator into a flexible polymer prepolymer, pouring the mixture into a mold, and exposing different areas of the mixture to ultraviolet light for different times through a mask to enable the different areas to have different Young modulus, so as to obtain a flexible substrate with heterogeneous modulus;
(6) Heating the flexible substrate with the heterogeneous modulus obtained in the step (5) to obtain a pre-cured flexible substrate with the heterogeneous modulus;
(7) Cutting an integrated film formed by combining n conductive materials obtained in the step (4) into a shape matched with a flexible substrate, transferring the integrated film to the pre-cured flexible substrate with heterogeneous modulus obtained in the step (6), and enabling all areas of the integrated film to be attached to all areas of the flexible substrate in a one-to-one correspondence manner to obtain the flexible substrate with heterogeneous modulus of the conductive layer;
(8) And (3) heating and curing the flexible substrate with the heterogeneous modulus of the conductive layer obtained in the step (7), and removing the receiving substrate to obtain the flexible strain sensor with the Young modulus of the flexible substrate matched with the stretchability of the conductive material.
4. A method of preparation according to claim 3, characterized in that: the conductive material in the step (1) is one or more of Ag nanowires, cu nanowires, au nanowires, ag nanoparticles, carbon black, carbon nanotubes, graphene oxide, reduced graphene oxide, MXene, liquid metal and Au.
5. A method of preparation according to claim 3, characterized in that: the power of the laser cutting in the step (3) is set to 80-130W, the speed is set to 15-25mm/s, and the thickness of the polymer plate is 2-4mm.
6. A method of preparation according to claim 3, characterized in that: the photoinitiator in the step (5) is diphenyl ketone, and the flexible polymer is a silicone rubber material.
7. A method of preparation according to claim 3, characterized in that: the ultraviolet exposure time in the step (5) is 0-15min.
8. A method of preparation according to claim 3, characterized in that: the heating in the step (6) is to enable the flexible substrate to be in an adhesive semi-cured state.
9. A method of preparation according to claim 3, characterized in that: the heating temperature of the heating curing in the step (8) is 60-80 ℃ and the heating time is 8-12h.
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