CN117245934B - Flexible stretching sensor based on microelectronic printing and preparation method thereof - Google Patents
Flexible stretching sensor based on microelectronic printing and preparation method thereof Download PDFInfo
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- 238000007639 printing Methods 0.000 title claims abstract description 46
- 238000004377 microelectronic Methods 0.000 title claims abstract description 35
- 238000002360 preparation method Methods 0.000 title claims abstract description 26
- 239000000017 hydrogel Substances 0.000 claims abstract description 24
- 239000000758 substrate Substances 0.000 claims abstract description 15
- 238000005516 engineering process Methods 0.000 claims abstract description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000011889 copper foil Substances 0.000 claims abstract description 5
- 238000010257 thawing Methods 0.000 claims abstract description 5
- 230000008014 freezing Effects 0.000 claims abstract description 4
- 238000007710 freezing Methods 0.000 claims abstract description 4
- 239000004372 Polyvinyl alcohol Substances 0.000 claims description 24
- 229920002451 polyvinyl alcohol Polymers 0.000 claims description 24
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 20
- 238000000034 method Methods 0.000 claims description 16
- IAZDPXIOMUYVGZ-UHFFFAOYSA-N Dimethylsulphoxide Chemical compound CS(C)=O IAZDPXIOMUYVGZ-UHFFFAOYSA-N 0.000 claims description 14
- 229910021538 borax Inorganic materials 0.000 claims description 9
- 235000010339 sodium tetraborate Nutrition 0.000 claims description 9
- 229920001609 Poly(3,4-ethylenedioxythiophene) Polymers 0.000 claims description 8
- UQGFMSUEHSUPRD-UHFFFAOYSA-N disodium;3,7-dioxido-2,4,6,8,9-pentaoxa-1,3,5,7-tetraborabicyclo[3.3.1]nonane Chemical compound [Na+].[Na+].O1B([O-])OB2OB([O-])OB1O2 UQGFMSUEHSUPRD-UHFFFAOYSA-N 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 8
- 239000004328 sodium tetraborate Substances 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 6
- 229910021641 deionized water Inorganic materials 0.000 claims description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 6
- 238000010438 heat treatment Methods 0.000 claims description 3
- 238000002156 mixing Methods 0.000 claims description 3
- 238000003756 stirring Methods 0.000 claims description 3
- 230000035945 sensitivity Effects 0.000 abstract description 29
- 230000008859 change Effects 0.000 abstract description 6
- 238000012544 monitoring process Methods 0.000 abstract description 4
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- 230000003993 interaction Effects 0.000 abstract description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 6
- 229920000144 PEDOT:PSS Polymers 0.000 description 6
- 238000004140 cleaning Methods 0.000 description 6
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- 238000000576 coating method Methods 0.000 description 6
- 238000010586 diagram Methods 0.000 description 6
- 239000011521 glass Substances 0.000 description 6
- 235000011187 glycerol Nutrition 0.000 description 5
- 229920001467 poly(styrenesulfonates) Polymers 0.000 description 5
- 239000000243 solution Substances 0.000 description 5
- 230000008901 benefit Effects 0.000 description 4
- 229920001940 conductive polymer Polymers 0.000 description 4
- 230000008569 process Effects 0.000 description 4
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- 239000007864 aqueous solution Substances 0.000 description 3
- 238000001035 drying Methods 0.000 description 3
- 239000000499 gel Substances 0.000 description 3
- 230000000877 morphologic effect Effects 0.000 description 3
- 229920000172 poly(styrenesulfonic acid) Polymers 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- 238000004132 cross linking Methods 0.000 description 2
- 238000011161 development Methods 0.000 description 2
- 230000000694 effects Effects 0.000 description 2
- 239000000463 material Substances 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 238000009864 tensile test Methods 0.000 description 2
- 238000012360 testing method Methods 0.000 description 2
- GKWLILHTTGWKLQ-UHFFFAOYSA-N 2,3-dihydrothieno[3,4-b][1,4]dioxine Chemical compound O1CCOC2=CSC=C21 GKWLILHTTGWKLQ-UHFFFAOYSA-N 0.000 description 1
- 206010016807 Fluid retention Diseases 0.000 description 1
- 239000004695 Polyether sulfone Substances 0.000 description 1
- XUIMIQQOPSSXEZ-UHFFFAOYSA-N Silicon Chemical compound [Si] XUIMIQQOPSSXEZ-UHFFFAOYSA-N 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 238000006136 alcoholysis reaction Methods 0.000 description 1
- 238000005452 bending Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
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- 239000004020 conductor Substances 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 229910052802 copper Inorganic materials 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 229910010272 inorganic material Inorganic materials 0.000 description 1
- 239000011147 inorganic material Substances 0.000 description 1
- 150000002500 ions Chemical class 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 238000010329 laser etching Methods 0.000 description 1
- 238000001000 micrograph Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 238000007254 oxidation reaction Methods 0.000 description 1
- 229920006393 polyether sulfone Polymers 0.000 description 1
- 239000002861 polymer material Substances 0.000 description 1
- 238000006116 polymerization reaction Methods 0.000 description 1
- 229960002796 polystyrene sulfonate Drugs 0.000 description 1
- 239000011970 polystyrene sulfonate Substances 0.000 description 1
- 230000002035 prolonged effect Effects 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 230000004044 response Effects 0.000 description 1
- 229910052710 silicon Inorganic materials 0.000 description 1
- 239000010703 silicon Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002195 synergetic effect Effects 0.000 description 1
- -1 tetrahydroxyborate ions Chemical class 0.000 description 1
- 238000010023 transfer printing Methods 0.000 description 1
- BSVBQGMMJUBVOD-UHFFFAOYSA-N trisodium borate Chemical compound [Na+].[Na+].[Na+].[O-]B([O-])[O-] BSVBQGMMJUBVOD-UHFFFAOYSA-N 0.000 description 1
Classifications
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J3/00—Processes of treating or compounding macromolecular substances
- C08J3/02—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques
- C08J3/03—Making solutions, dispersions, lattices or gels by other methods than by solution, emulsion or suspension polymerisation techniques in aqueous media
- C08J3/075—Macromolecular gels
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
- B29C64/10—Processes of additive manufacturing
- B29C64/106—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material
- B29C64/112—Processes of additive manufacturing using only liquids or viscous materials, e.g. depositing a continuous bead of viscous material using individual droplets, e.g. from jetting heads
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
- B29C64/30—Auxiliary operations or equipment
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
- B29C64/30—Auxiliary operations or equipment
- B29C64/35—Cleaning
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C64/00—Additive manufacturing, i.e. manufacturing of three-dimensional [3D] objects by additive deposition, additive agglomeration or additive layering, e.g. by 3D printing, stereolithography or selective laser sintering
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- B29C64/379—Handling of additively manufactured objects, e.g. using robots
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
- B29C—SHAPING OR JOINING OF PLASTICS; SHAPING OF MATERIAL IN A PLASTIC STATE, NOT OTHERWISE PROVIDED FOR; AFTER-TREATMENT OF THE SHAPED PRODUCTS, e.g. REPAIRING
- B29C65/00—Joining or sealing of preformed parts, e.g. welding of plastics materials; Apparatus therefor
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B29C66/00—General aspects of processes or apparatus for joining preformed parts
- B29C66/70—General aspects of processes or apparatus for joining preformed parts characterised by the composition, physical properties or the structure of the material of the parts to be joined; Joining with non-plastics material
- B29C66/74—Joining plastics material to non-plastics material
- B29C66/742—Joining plastics material to non-plastics material to metals or their alloys
- B29C66/7428—Transition metals or their alloys
- B29C66/74281—Copper or alloys of copper
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B29—WORKING OF PLASTICS; WORKING OF SUBSTANCES IN A PLASTIC STATE IN GENERAL
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- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
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- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y40/00—Auxiliary operations or equipment, e.g. for material handling
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- B33Y—ADDITIVE MANUFACTURING, i.e. MANUFACTURING OF THREE-DIMENSIONAL [3-D] OBJECTS BY ADDITIVE DEPOSITION, ADDITIVE AGGLOMERATION OR ADDITIVE LAYERING, e.g. BY 3-D PRINTING, STEREOLITHOGRAPHY OR SELECTIVE LASER SINTERING
- B33Y70/00—Materials specially adapted for additive manufacturing
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
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- C08J5/18—Manufacture of films or sheets
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B7/00—Measuring arrangements characterised by the use of electric or magnetic techniques
- G01B7/16—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge
- G01B7/18—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge using change in resistance
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08J—WORKING-UP; GENERAL PROCESSES OF COMPOUNDING; AFTER-TREATMENT NOT COVERED BY SUBCLASSES C08B, C08C, C08F, C08G or C08H
- C08J2325/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2325/18—Homopolymers or copolymers of aromatic monomers containing elements other than carbon and hydrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2329/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2329/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2329/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2425/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an aromatic carbocyclic ring; Derivatives of such polymers
- C08J2425/18—Homopolymers or copolymers of aromatic monomers containing elements other than carbon and hydrogen
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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- C08J2429/00—Characterised by the use of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by an alcohol, ether, aldehydo, ketonic, acetal, or ketal radical; Hydrolysed polymers of esters of unsaturated alcohols with saturated carboxylic acids; Derivatives of such polymer
- C08J2429/02—Homopolymers or copolymers of unsaturated alcohols
- C08J2429/04—Polyvinyl alcohol; Partially hydrolysed homopolymers or copolymers of esters of unsaturated alcohols with saturated carboxylic acids
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- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
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- C08K3/38—Boron-containing compounds
- C08K2003/387—Borates
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- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
The invention discloses a flexible stretching sensor based on microelectronic printing and a preparation method thereof, and belongs to the technical field of flexible sensing equipment. Firstly preparing special ink, constructing a sensing layer film with a surface microstructure on a substrate by using a microelectronic printing technology, repeatedly freezing and thawing to obtain a hydrogel film, and fixing copper foils at two ends of the film to obtain the flexible stretching sensor with the ridge microstructure on a single surface. The whole preparation process is simple, and has high repeatability; when the extending direction of the ridge structure on the film is vertical to the stretching direction of the device and the distance between the adjacent ridge structures is 3 mm, the sensitivity of the sensing layer film can reach 5.3, the elongation of the flexible stretching sensor prepared based on the sensing layer film reaches 328.06%, the flexible stretching sensor stretches for 200 times under 100% strain, the resistance change rate is not obviously reduced, and the flexible stretching device with higher sensitivity and stability has good application prospect in the fields of human health monitoring, man-machine interaction and the like.
Description
Technical Field
The invention belongs to the technical field of flexible sensing equipment, and particularly relates to a flexible stretching sensor based on microelectronic printing and a preparation method thereof.
Background
The flexible stretching sensor has the characteristics of high flexibility, strong sensitivity and the like, and can convert vital sign signals and various mechanical signals into electric signals, so that the flexible stretching sensor can be used for simulating a human body sensing structure, and has wide application prospects in the fields of health monitoring, flexible robots, wearable electronic equipment, human-computer interaction, electronic skin and the like. Compared with the traditional rigid silicon-based sensor, the flexible stretching sensor can better capture mechanical signals on a curved surface and maintain stability in the bending/stretching process. Therefore, flexible stretch sensors with fast response, high repeatability and high stretchability are becoming a direction of future development.
Hydrogels are a representative flexible sensor due to their good mechanical, biological and electrical conductivity. Common pure polyvinyl alcohol (PVA) hydrogels are paid attention to because of good biocompatibility and self-healing property, but the problems of poor mechanical properties, low conductivity and the like limit the further development of the gels, and in order to improve the mechanical and electrical conductivity of gel materials, a scheme of adding conductive fillers into the PVA hydrogels is reported successively. Among them, conductive polymer hydrogels have attracted much attention because they can provide both electron conductivity and ion conductivity, and have the advantages of low young's modulus, good flexibility, stability, good biocompatibility, and the like.
Compared with the hydrogel prepared by using the inorganic material, the conductive polymer has the advantage of difficult oxidization, and the flexible sensor prepared by using the hydrogel based on the conductive polymer material has good tensile property, obviously prolonged service life and higher stability, and can meet the requirement of close fitting of a human body and the surface of flexible equipment.
Jiang Mengyue in the master paper entitled "preparation of PVA/MXene/PEDOT: PSS hydrogel and its use in Flexible Strain Sensors" it is noted that: the P/M/P (PVA/MXene/PEDOT: PSS) hydrogel with excellent mechanical properties and high conductivity can be prepared by introducing MXene conductive material and poly 3, 4-ethylenedioxythiophene/polystyrene sulfonate (PEDOT: PSS) with high conductivity and stability into PVA gel, the mechanical properties and conductivity of the hydrogel can be changed by regulating the MXene content and the PEDOT: PSS content, the maximum tensile strength of the obtained P/M/P hydrogel is 93.57 kPa, and the conductivity is 0.2109S M -1 . The P/M/P hydrogel has self-healing property based on the dynamic crosslinking between PVA and tetrahydroxyborate ions in the system and the hydrogen bonding action between PVA, MXene and PEDOT: PSS. Meanwhile, the P/M/P hydrogel also has biocompatibility and degradability. Under the synergistic effect of the performances, the P/M/P hydrogel has a wider strain range (0-763%) when used as a flexible strain sensor, and can be used for monitoring human body movement. However, the sensor material disclosed in this document has drawbacks, particularly in that: although the tensile strength of the sensor is obviously improved, the sensor still has difficulty in meeting the application requirements of special fields, has lower sensitivity (GF=2.31), and is used for sensing signalsThere is still a large room for improvement in terms of awareness.
One of the effective ways to improve the sensitivity of the flexible tensile sensor is to construct a microstructure on the sensing layer, so that the flexible sensor can generate larger deformation under a smaller pressure condition, the construction of the micro-nano structure usually adopts a template transfer printing method, a template with uniform structure is usually obtained by adopting a laser etching method, and the method has the defects of complex procedure and longer time consumption, has high preparation cost and limits the large-scale production of the flexible tensile sensor; the cost of the method is obviously reduced by using the plant surface as a mould for manufacturing the microstructure, but the method has low repeatability and poor controllability and is not suitable for mass production.
Disclosure of Invention
The invention aims to provide a flexible stretching sensor based on microelectronic printing and a preparation method thereof, wherein after specific ink is prepared, a flexible stretching sensing layer is formed on the surface of a substrate by using a microelectronic printing technology, and a ridged microstructure is constructed, so that the sensitivity of the sensing layer can be obviously improved, and a sensing device prepared based on the flexible stretching sensor has ultrahigh toughness and stability.
The technical scheme of the invention is as follows: a preparation method of a flexible tension sensor based on microelectronic printing comprises the following steps:
1. preparation of ink
1) Dissolving polyvinyl alcohol (124 type) in deionized water under heating;
2) Adding dimethyl sulfoxide, PEDOT, PSS and glycerol into the polyvinyl alcohol solution, and stirring and uniformly mixing;
3) Dropwise adding a sodium tetraborate solution into the solution obtained in the step 2) to obtain ink;
2. preparation of sensing layer film based on microelectronic printing technology
1) Pretreating a substrate;
2) Preparing a sensing layer film with a ridged microstructure on the surface on a substrate by using the ink prepared in the first step on a microelectronic printing equipment platform;
3. preparation of the sensor
1) Repeatedly freezing and thawing the sensing layer film prepared in the second step to obtain a hydrogel film;
2) And fixing copper foils at two ends of the hydrogel film to prepare the flexible stretching sensor.
In the first step, the mass ratio of polyvinyl alcohol to PEDOT to PSS to glycerol to dimethyl sulfoxide is 4-6:15-18:30-34:3-4; the mass ratio of the polyvinyl alcohol to the sodium tetraborate is 30:1-1.5.
Dimethyl sulfoxide is added in the preparation of the ink because the conductivity of poly (3, 4-ethylenedioxythiophene) -poly (styrenesulfonic acid) can be effectively improved by stripping the poly (styrenesulfonic acid). And the addition of glycerol is beneficial to improving the water retention of the hydrogel and effectively prolonging the service life of the flexible stretching sensor.
The application makes targeted study on the dosage of different components in the ink to obtain a final value, and finds out in the experimental process: the high content of the polyvinyl alcohol can influence the conductivity of the film, and the blending of the polyvinyl alcohol solution with proper concentration can not excessively reduce the conductivity of the film, and can also enable the viscosity of the ink to be suitable for the microelectronic printing process. Too high or too low concentration of the aqueous solution of sodium tetraborate can affect the crosslinking performance of the polyvinyl alcohol, and too high concentration of the aqueous solution of sodium tetraborate can greatly increase the viscosity of the ink and affect the printing effect.
Further, in the second step, a 27G needle with the inner diameter of 0.21-mm is used in microelectronic printing, the printing speed is 5-7 mm/s, and the air pump pressure is 100-200 kPa.
Further, in the second step, the extending direction of the ridge structure on the obtained sensing layer film is parallel or perpendicular to the stretching direction of the device, and preferably, the extending direction of the ridge structure is perpendicular to the stretching direction of the device.
Further, when the extending direction of the ridge microstructures on the sensing layer film is perpendicular to the stretching direction, the interval between adjacent ridge microstructures is 2-4 mm, preferably 3-mm.
In the third step, when the hydrogel film is prepared, the sensing layer film prepared in the second step is frozen for 8-12 hours at the temperature of minus 10 ℃ to minus 18 ℃, then thawed for 3-5 hours at room temperature, and the freezing and thawing are repeated for 3 times.
The flexible stretching sensor prepared by the method has higher sensitivity and cycle stability, and the sensitivity reaches 3.1 when the extending direction of the ridge structure on the sensing layer film is parallel to the stretching direction of the device and the interval between the adjacent ridge structures is 2 mm; when the extending direction of the ridge structure on the sensing layer film is perpendicular to the stretching direction of the device and the interval between the adjacent ridge structures is 3 mm, the sensitivity of the sensing layer film reaches 5.3, compared with the traditional conductive polymer hydrogel, the sensitivity is obviously improved, the elongation f of the flexible stretching sensor prepared based on the sensing layer film with the extending direction of the ridge structure perpendicular to the stretching direction of the device is 328.06%, the flexible stretching sensor is stretched for 200 cycles under 100% strain, and the resistance change rate is not obviously reduced.
Compared with the prior art, the invention has the following advantages:
1. the printing ink is prepared from the main raw materials of polyvinyl alcohol, dimethyl sulfoxide, PEDOT (polyether sulfone), PSS (sodium borate), glycerol and sodium tetraborate, has the advantages of simple preparation method, mild condition and controllable viscosity, and is suitable for a microelectronic printing technology;
2. the application prepares the sensing layer film by using the microelectronic printing technology, can perform personalized pattern design, can construct microstructures with different shapes on the sensing layer, has simple preparation process, high precision, strong controllability and high repeatability;
3. the sensing layer film with the ridged microstructure on the surface is prepared by utilizing special ink and a microelectronic printing technology, when the extending direction of the ridged structure on the film is vertical to the stretching direction of a device and the distance between adjacent ridged structures is 3 mm, the sensitivity of the sensing layer film can reach 5.3, the elongation of the flexible stretching sensor prepared based on the sensitivity reaches 328.06 percent, the flexible stretching sensor is stretched for 200 times under 100 percent strain, and the resistance change rate is not obviously reduced;
4. the flexible stretching sensor prepared by the method disclosed by the application has ultrahigh toughness and stability, and has huge application potential in the fields of health monitoring, electronic skin, human-computer interaction and the like.
Drawings
FIG. 1 is a flow chart of the fabrication of a microelectronic print-based flexible stretch sensor disclosed herein;
FIG. 2 is a schematic structural diagram of the sensing layer film with surface microstructure prepared in examples 1, 2 and 3, wherein the arrow in the drawing indicates the stretching direction of the device, and the panel a is a schematic structural diagram of the sensing layer film with ridge microstructure parallel to the stretching direction of the device prepared in example 1; panel b is a schematic structural diagram of the sensing layer film with the ridge microstructure perpendicular to the stretching direction of the device, which is prepared in example 2; c, drawing is a schematic structural diagram of the sensing layer film with hemispherical microstructure on the surface, which is prepared in example 3;
FIG. 3 is a sensitivity factor fitting curve of the sensing layer film with ridged microstructure prepared in example 1;
FIG. 4 is a sensitivity factor fitting curve of the sensing layer film with ridged microstructure prepared in example 2;
FIG. 5 is a sensitivity factor fitting curve of the sensing layer film with hemispherical microstructure prepared in example 3;
FIG. 6 is a graph showing the resistance change of the flexible tensile sensor according to the application example after 200 tensile cycles under 100% strain;
FIG. 7 is a schematic diagram of a scanning electron microscope of a sensing layer film with a ridged microstructure prepared in example 2.
Detailed Description
The following description of the present invention is provided with reference to the accompanying drawings, but is not limited to the following description, and any modifications or equivalent substitutions of the present invention should be included in the scope of the present invention without departing from the spirit and scope of the present invention.
The polyvinyl alcohol used in the application is produced by national pharmaceutical group chemical reagent limited company (124 type; alcoholysis degree 98-99%, average polymerization degree 2400-2500); PEDOT PSS is manufactured by He Lishi Heraeus (Clevelos PH 1000).
Example 1 preparation of Flexible tensile sensor based on microelectronic printing
Step one, preparation of ink
1) 600 mg polyvinyl alcohol was added to 5 mL deionized water and stirred at 95 ℃ with heating for 1 h until the polyvinyl alcohol was completely dissolved.
2) To the polyvinyl alcohol solution, 0.3. 0.3 mL dimethyl sulfoxide (0.33. 0.33 g), 1.5. 1.5 mL aqueous poly (3, 4-ethylenedioxythiophene) -poly (styrenesulfonic acid) dispersion (PEDOT: PSS,1.5 g,1.3 wt%) and 2.5. 2.5 mL glycerin (3.225 g) were sequentially added, and stirring was continued to be uniform.
3) To the mixture obtained in step 2) was added dropwise an aqueous solution of sodium tetraborate (0.02. 0.02 g) of 0.5. 0.5 mL.
The viscosity of the mixture prepared in the above step was measured to be 1.75 Pa.s using a BROOKFIELD viscometer.
Step two, preparing a sensing layer film with a ridged microstructure on the surface
1) Pretreatment of a substrate: and cleaning the glass substrate sequentially by deionized water, acetone and absolute ethyl alcohol, carrying out ultrasonic treatment, and drying at 60 ℃ for 2 h for later use after cleaning.
2) Microelectronic printing: fixing the pretreated glass substrate on a microelectronic printing equipment platform (model: IMAGE MASTER PC Smart), placing the ink prepared in the first step into a needle cylinder, printing by using a 27G needle with an inner diameter of 0.21 mm, printing at a speed of 7 mm/s and an air pump pressure of 100 kPa, coating according to a pattern drawn by AutoCAD software, and preparing a sensing layer film with a ridged microstructure on the surface, wherein the film has a length of 45 mm and a width of 15 mm, the extending direction of the raised ridged structure on the film is parallel to the stretching direction, the cross section of a single ridged strip is semicircular, the radius of the ridged strip is 0.15 mm, and the interval between adjacent ridged strips is 2 mm.
3) And printing a sensing layer film with no bulge on the surface of the film and a sensing layer film with a ridge microstructure with the extending direction parallel to the stretching direction of the device on the surface and the spacing between adjacent ridge strips of 1 mm and 1.5 mm respectively.
The sensitivity of the different morphological sense layer films was tested and the results are shown in fig. 3: the slope of the fitted curve represents the sensitivity of the sensing layer film, and the sensitivity of the film is improved to a certain extent along with the introduction of the microstructure of the sensing layer, and when the film is provided with the ridge microstructure parallel to the stretching direction and the interval between the adjacent ridge strips is 2 mm, the sensitivity gf=3.1 of the sensing layer film reaches the highest.
Example 2 preparation of Flexible tensile sensor based on microelectronic printing
Step one, the ink preparation process was the same as in example 1.
And step two, preparing a sensing layer film with a ridged microstructure on the surface.
1) Pretreatment of a substrate: and cleaning the glass substrate sequentially by deionized water, acetone and absolute ethyl alcohol, carrying out ultrasonic treatment, and drying at 60 ℃ for 2 h for later use after cleaning.
2) Microelectronic printing: fixing the pretreated glass substrate on a microelectronic printing equipment platform (model: IMAGE MASTER PC Smart), placing the ink prepared in the first step into a needle cylinder, printing by using a 27G needle head with an inner diameter of 0.21 mm, printing at a speed of 7 mm/s, air pump pressure of 100 kPa, coating according to a pattern drawn by AutoCAD software, and preparing a sensing layer film with a ridged microstructure on the surface, wherein the film has a length of 45 mm and a width of 15 mm, the extending direction of a raised ridged strip on the film is perpendicular to the stretching direction, the cross section of a single ridged strip is semicircular, the distance between adjacent ridged strips is 2 mm, and the radius of the ridged strip is 0.15 mm as shown in a small diagram of FIG. 2; FIG. 7 is a scanning electron microscope image of the prepared sensing layer film.
3) And printing a sensing layer film with no bulge on the surface of the film and a sensing layer film with a ridge microstructure with the extending direction perpendicular to the stretching direction of the device on the surface and with the spacing between adjacent ridge strips of 3 mm, 4 mm and 5 mm respectively.
The sensitivity of the different morphological sense layer films was tested and the results are shown in fig. 4: the slope of the fitted curve represents the sensitivity of the sensing layer film, the sensitivity of the film is improved to a certain extent along with the introduction of the microstructure of the sensing layer, the sensitivity of the sensing layer shows a trend of increasing and then decreasing along with the increase of the distance between microstructures, and when the film is provided with a ridge microstructure vertical to the stretching direction of the device and the distance between adjacent ridge strips is 3 mm, the sensitivity gf=5.3 of the sensing layer film is obviously improved compared with the sensing layer film prepared in the embodiment 1, which indicates that the effect is better when the ridge microstructure on the sensing layer film is vertical to the stretching direction.
Example 3 preparation of Flexible tensile sensor based on microelectronic printing
Step one, the ink preparation process was the same as in example 1.
And step two, preparing a sensing layer film with a hemispherical microstructure on the surface.
1) Pretreatment of a substrate: and cleaning the glass substrate sequentially by deionized water, acetone and absolute ethyl alcohol, carrying out ultrasonic treatment, and drying at 60 ℃ for 2 h for later use after cleaning.
2) Microelectronic printing: fixing the pretreated glass substrate on a microelectronic printing equipment platform (model: IMAGE MASTER PC Smart), placing the ink prepared in the first step into a needle cylinder, printing by using a 27G needle head with an inner diameter of 0.21 mm, printing at a speed of 7 mm/s and an air pump pressure of 100 kPa, coating according to a pattern drawn by AutoCAD software, and preparing a sensing layer film with a hemispherical microstructure on the surface, wherein the film has a length of 45 mm, a width of 15 mm, a residence time of 2.0s for coating a single hemisphere, and a spacing between adjacent hemispherical protrusions of 3 mm, as shown in a small graph of c in FIG. 2.
3) The same conditions were used to print out a film with hemispherical microstructures on the surface and the coating residence times of the hemispherical microstructures were 1.5 s, 1.0 s and 0.5 s, respectively, i.e., to print out a sensing layer film with hemispherical microstructures of different radii.
The sensitivity of the different morphological sense layer films was tested and the results are shown in fig. 5: the slope of the fitted curve represents the sensitivity of the sensing layer film, and the sensitivity of the film is improved to a certain extent along with the introduction of the microstructure of the sensing layer, and when the film is provided with a hemispherical microstructure and the coating residence time of the microstructure is 1.5 s, the sensitivity gf=3.7 of the sensing layer film reaches the highest.
Application example, preparation of Flexible tensile sensor
1) The film with the highest sensitivity and the ridge structure prepared in example 2 was frozen at-18 ℃ for 8 h, then thawed at room temperature for 3 h, and the freeze thawing was repeated 3 times to obtain a hydrogel film with the ridge structure on the surface.
2) Copper foil with the thickness of 0.1 and mm is fixed at two ends of the hydrogel film by using a copper tape, and the flexible stretching sensor is assembled.
The maximum strain at break Δl=98.42 mm of the resulting flexible tensile sensor was tested, and the tensile test electrode spacing l=0.03 m. The initial resistance was 6.12M Ω, the maximum bearing force F was 2.75N, the calculated conductivity ρ was 0.94S/cm, the tensile strength σ was 5.24 Mpa, and the elongation f=Δl/l×100% = 328.06%.
Testing the sensor performance by a universal tester: the two ends of the flexible tensile sensor are respectively clamped at the two ends of the universal testing machine, the tensile direction is vertical to the extending direction of the ridged microstructure, the copper foil is connected to the electrochemical workstation, the prepared flexible tensile sensor is subjected to 200 tensile tests in a 100% strain state, the experimental result is shown in fig. 6, and the resistance change rate of the sensor is reduced in the first 20 cycles without obvious attenuation. The rate of change of resistance remained stable over 200 cycles. After the experiment, the surface of the film has no obvious cracks, which indicates that the prepared flexible stretching sensor has good stability and reliability.
The foregoing description is only illustrative of the present invention and is not intended to limit the scope of the invention, and all equivalent structures or equivalent processes or direct or indirect application in other related arts are included in the scope of the present invention.
Claims (7)
1. The preparation method of the flexible tension sensor based on microelectronic printing is characterized by comprising the following steps of:
1. preparation of ink
1) Dissolving polyvinyl alcohol in deionized water under heating;
2) Adding dimethyl sulfoxide, PEDOT, PSS and glycerol into the polyvinyl alcohol solution, and stirring and uniformly mixing;
3) Dropwise adding a sodium tetraborate solution into the solution obtained in the step 2);
2. preparation of sensing layer film based on microelectronic printing technology
1) Pretreating a substrate;
2) Preparing a sensing layer film with a ridged microstructure on the surface on a substrate by using the ink prepared in the first step on a microelectronic printing equipment platform;
3. preparation of the sensor
1) Repeatedly freezing and thawing the sensing layer film prepared in the second step to obtain a hydrogel film;
2) Fixing copper foil at two ends of the hydrogel film to prepare a flexible stretching sensor;
in the first step, the mass ratio of polyvinyl alcohol to PEDOT to PSS to glycerol to dimethyl sulfoxide is 4-6:15-18:30-34:3-4; the mass ratio of the polyvinyl alcohol to the sodium tetraborate is 30:1-1.5.
2. The method for manufacturing the flexible tension sensor based on microelectronic printing as claimed in claim 1, wherein in the second step, a 27G needle with an inner diameter of 0.21-mm is used in microelectronic printing, the printing speed is 5-7 mm/s, and the air pump pressure is 100-200 kPa.
3. The method for manufacturing a flexible tensile sensor based on microelectronic printing as claimed in claim 1, wherein in the second step, the extending direction of the ridge microstructure on the obtained sensing layer film is perpendicular to the device tensile direction.
4. A method of manufacturing a flexible tensile sensor based on microelectronic printing according to claim 3, wherein the spacing between adjacent ridge structures on the sensing layer film is 2-4 mm.
5. The method of manufacturing a flexible tensile sensor based on microelectronic printing according to claim 4, wherein the spacing between adjacent ridge structures on the sensing layer film is 3 mm.
6. The method for preparing the flexible tensile sensor based on microelectronic printing as claimed in claim 1, wherein in the third step, when the hydrogel film is prepared, the sensing layer film prepared in the second step is frozen for 8-12 hours at the temperature of minus 10 ℃ to minus 18 ℃, then thawed for 3-5 hours at room temperature, and repeatedly frozen and thawed for 3 times.
7. A flexible stretch sensor, characterized in that it is manufactured on the basis of a method for manufacturing a flexible stretch sensor based on microelectronic printing according to any of claims 1-6.
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