CN111122021B - Flexible composite film and preparation method thereof, flexible pressure sensor and preparation method thereof - Google Patents
Flexible composite film and preparation method thereof, flexible pressure sensor and preparation method thereof Download PDFInfo
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- CN111122021B CN111122021B CN201911398996.5A CN201911398996A CN111122021B CN 111122021 B CN111122021 B CN 111122021B CN 201911398996 A CN201911398996 A CN 201911398996A CN 111122021 B CN111122021 B CN 111122021B
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- 239000002131 composite material Substances 0.000 title claims abstract description 101
- 238000002360 preparation method Methods 0.000 title claims abstract description 27
- 239000010410 layer Substances 0.000 claims abstract description 125
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- 239000002243 precursor Substances 0.000 claims abstract description 39
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 34
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 33
- 239000002245 particle Substances 0.000 claims abstract description 18
- 230000001678 irradiating effect Effects 0.000 claims abstract description 5
- 238000002955 isolation Methods 0.000 claims description 34
- -1 polyethylene terephthalate Polymers 0.000 claims description 26
- 239000004205 dimethyl polysiloxane Substances 0.000 claims description 24
- 229920000435 poly(dimethylsiloxane) Polymers 0.000 claims description 24
- 238000000034 method Methods 0.000 claims description 22
- 239000000725 suspension Substances 0.000 claims description 18
- 125000000524 functional group Chemical group 0.000 claims description 17
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims description 16
- JRPBQTZRNDNNOP-UHFFFAOYSA-N barium titanate Chemical compound [Ba+2].[Ba+2].[O-][Ti]([O-])([O-])[O-] JRPBQTZRNDNNOP-UHFFFAOYSA-N 0.000 claims description 13
- 229910002113 barium titanate Inorganic materials 0.000 claims description 13
- 238000004519 manufacturing process Methods 0.000 claims description 12
- 238000004528 spin coating Methods 0.000 claims description 12
- 239000004642 Polyimide Substances 0.000 claims description 8
- 229920001707 polybutylene terephthalate Polymers 0.000 claims description 8
- 229920000139 polyethylene terephthalate Polymers 0.000 claims description 8
- 239000005020 polyethylene terephthalate Substances 0.000 claims description 8
- 229920001721 polyimide Polymers 0.000 claims description 8
- 239000004743 Polypropylene Substances 0.000 claims description 6
- 229920001155 polypropylene Polymers 0.000 claims description 6
- 229920000468 styrene butadiene styrene block copolymer Polymers 0.000 claims description 6
- 239000011112 polyethylene naphthalate Substances 0.000 claims description 4
- 229920003225 polyurethane elastomer Polymers 0.000 claims description 4
- VEALVRVVWBQVSL-UHFFFAOYSA-N strontium titanate Chemical compound [Sr+2].[O-][Ti]([O-])=O VEALVRVVWBQVSL-UHFFFAOYSA-N 0.000 claims description 3
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 claims description 2
- 229920003207 poly(ethylene-2,6-naphthalate) Polymers 0.000 claims description 2
- 230000035945 sensitivity Effects 0.000 abstract description 9
- 239000010408 film Substances 0.000 abstract 6
- 239000010409 thin film Substances 0.000 abstract 1
- KFZMGEQAYNKOFK-UHFFFAOYSA-N Isopropanol Chemical compound CC(C)O KFZMGEQAYNKOFK-UHFFFAOYSA-N 0.000 description 12
- 230000000694 effects Effects 0.000 description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 8
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- 239000000243 solution Substances 0.000 description 7
- 238000009832 plasma treatment Methods 0.000 description 6
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 description 5
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- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000001035 drying Methods 0.000 description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 4
- 229960000583 acetic acid Drugs 0.000 description 4
- FPCJKVGGYOAWIZ-UHFFFAOYSA-N butan-1-ol;titanium Chemical compound [Ti].CCCCO.CCCCO.CCCCO.CCCCO FPCJKVGGYOAWIZ-UHFFFAOYSA-N 0.000 description 4
- 239000012362 glacial acetic acid Substances 0.000 description 4
- 229920000166 polytrimethylene carbonate Polymers 0.000 description 4
- 238000003756 stirring Methods 0.000 description 4
- ITHZDDVSAWDQPZ-UHFFFAOYSA-L barium acetate Chemical compound [Ba+2].CC([O-])=O.CC([O-])=O ITHZDDVSAWDQPZ-UHFFFAOYSA-L 0.000 description 3
- 238000001514 detection method Methods 0.000 description 3
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- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 2
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 description 2
- RTAQQCXQSZGOHL-UHFFFAOYSA-N Titanium Chemical compound [Ti] RTAQQCXQSZGOHL-UHFFFAOYSA-N 0.000 description 2
- 230000008859 change Effects 0.000 description 2
- 239000011248 coating agent Substances 0.000 description 2
- 238000000576 coating method Methods 0.000 description 2
- 229910052802 copper Inorganic materials 0.000 description 2
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- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
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- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
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- 238000006243 chemical reaction Methods 0.000 description 1
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- 239000007789 gas Substances 0.000 description 1
- PCHJSUWPFVWCPO-UHFFFAOYSA-N gold Chemical compound [Au] PCHJSUWPFVWCPO-UHFFFAOYSA-N 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 239000010931 gold Substances 0.000 description 1
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- 238000011065 in-situ storage Methods 0.000 description 1
- 239000012528 membrane Substances 0.000 description 1
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Classifications
-
- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/16—Measuring force or stress, in general using properties of piezoelectric devices
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Physics & Mathematics (AREA)
- General Physics & Mathematics (AREA)
- Nanotechnology (AREA)
- Composite Materials (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- Materials Engineering (AREA)
- Crystallography & Structural Chemistry (AREA)
- Laminated Bodies (AREA)
Abstract
The invention relates to a preparation method of a flexible composite film, which comprises the following steps: forming a precursor layer containing a ferroelectric material on a surface of a first flexible thin film; then irradiating the surface by adopting laser to form a composite structure on the surface, wherein the composite structure comprises a graphene microstructure and ferroelectric material particles embedded in the graphene microstructure and/or on the surface; and transferring at least part of the composite structure to one surface of the second flexible film to form a functional layer on one surface of the second flexible film, thereby obtaining the flexible composite film. The invention also provides the flexible composite film obtained by the preparation method, a flexible pressure sensor and the preparation method thereof. The flexible composite film has high sensitivity and good flexibility.
Description
Technical Field
The invention relates to the technical field of sensors, in particular to a flexible composite film and a preparation method thereof, a flexible pressure sensor and a preparation method thereof.
Background
At present, all intelligent wearable sensors are powered by various chemical energy batteries, and the sensors need to be replaced regularly, are high in recycling difficulty and can pollute the environment. Whereas a self-generating flexible pressure sensor is capable of converting mechanical energy of a living being into electrical energy to achieve near lifetime energy delivery to the flexible pressure sensor.
However, the traditional flexible sensor microstructure is prepared by adopting a microelectronic mechanical system processing technology, which relates to a series of complex processes such as corrosion, bonding, photoetching, oxidation, diffusion, sputtering and the like. And the sensitivity of the flexible sensing device is affected to a certain extent after the flexibility of the flexible sensing device is improved, so that the sensitivity of the pressure sensor is low.
Disclosure of Invention
Based on the above, it is necessary to provide a flexible composite film and a preparation method thereof, and a flexible pressure sensor and a preparation method thereof, wherein the preparation method has the advantages of simple process, low equipment dependence, excellent performance of the obtained flexible composite film, high sensitivity, high flexibility degree and the like of the flexible pressure sensor prepared based on the flexible film.
The invention provides a preparation method of a flexible composite film, which comprises the following steps:
providing a first flexible film and a suspension containing a ferroelectric material precursor, forming the suspension on one surface of the first flexible film to form a precursor layer on the surface;
irradiating the surface of the first flexible film with the precursor layer by adopting laser to form a graphene microstructure on the surface of the first flexible film, and converting the ferroelectric material precursor into ferroelectric material particles and embedding the ferroelectric material particles into the graphene microstructure and/or the graphene microstructure to obtain a composite structure;
and transferring at least part of the composite structure to one surface of a second flexible film to form a functional layer on one surface of the second flexible film, so as to obtain the flexible composite film.
In one embodiment, the conditions of the laser irradiation include: the laser wavelength is more than 355nm, the laser scanning speed is 100-3000 mm/s, and the laser single pulse energy range is 10-300 muJ.
In one embodiment, the surface of the first flexible film for carrying the suspension comprises at least one functional group of-OH, -COOH.
In one embodiment, the first flexible film is treated with ultraviolet radiation or with plasma to form at least one functional group of-OH, -COOH on the surface of the first flexible film.
In one embodiment, the first material of the first flexible film comprises at least one of polyimide, polyethylene terephthalate, polybutylene terephthalate; and/or the number of the groups of groups,
the second material of the second flexible film comprises at least one of polydimethylsiloxane, polyurethane elastomer, poly (trimethyl carbonate), polypropylene, polyethylene naphthalate, and styrene-butadiene-styrene block copolymer.
In one embodiment, the step of transferring the composite structure to the second flexible film comprises: and placing a solution containing the second material on the surface of the first flexible film with the composite structure, curing to obtain the second flexible film on the surface of the composite structure, and separating to enable the composite structure to be at least partially transferred to the second flexible film.
In one embodiment, the ferroelectric material precursor includes at least one of a strontium titanate precursor, a barium titanate precursor.
In one embodiment, the suspension is applied to the surface of the first flexible film by spin coating at a speed of 200rpm to 5000rpm for a period of 10s to 60s.
The invention also provides a flexible composite film which is prepared by the preparation method and comprises a second flexible film and a functional layer arranged on one surface of the second flexible film, wherein the functional layer comprises a graphene microstructure and ferroelectric material particles embedded in and/or on the graphene microstructure.
According to the preparation method of the flexible composite film, the graphene microstructure is formed on the surface of the first flexible film in situ through carbonization under the action of laser heat, the ferroelectric material precursor is decomposed into ferroelectric material particles, and under the action of the impact force of laser irradiation, the ferroelectric material particles are embedded on the surface of the graphene microstructure and enter the interior of the graphene microstructure to form the composite structure. And transferring at least part of the composite structure to the surface of the second flexible film to obtain the flexible composite film comprising the functional layer. Therefore, in the flexible composite film, the graphene microstructure and ferroelectric material particles in the functional layer can generate a synergistic effect, a percolation conductive network is established, and the capacity of storing charges is improved, so that the dielectric constant of the composite structure is greatly improved, the dielectric loss is reduced, and the output performance can be effectively improved.
Meanwhile, the preparation method overcomes the defects of the processing technology of the micro-electromechanical system and has the advantages of simple process, low cost, high flexibility degree and large-size preparation.
A method of making a flexible pressure sensor, comprising:
providing the flexible composite film obtained by the preparation method and a third flexible film;
paving an isolation layer on the flexible composite film, surrounding the functional layer, and enabling the height of the isolation layer to be larger than that of the functional layer;
attaching and bonding the third flexible film and the isolation layer to each other to obtain a flexible pressure sensor;
the surface of the flexible composite film far away from the functional layer is further provided with a first conductive layer, the surface of the third flexible film far away from the isolation layer is further provided with a second conductive layer, and the first conductive layer and the second conductive layer form a conductive loop.
In one embodiment, the surface of the flexible composite film for bearing the first conductive layer comprises at least one functional group of-OH and-COOH;
and/or the surface of the third flexible film for bearing the second conductive layer comprises at least one functional group of-OH and-COOH.
In one embodiment, the height of the isolation layer is 100-5000 μm, and the material of the isolation layer comprises at least one of polydimethylsiloxane, polyethylene terephthalate and polybutylene terephthalate.
A flexible pressure sensor made by the above-described method of making, comprising:
the first electrode layer comprises the flexible composite film, the first conductive layer and the isolation layer, the first conductive layer is arranged on the surface of the flexible composite film, which is away from the functional layer, the isolation layer is arranged around the functional layer, and the height of the isolation layer is larger than that of the functional layer;
the second electrode layer is arranged on the surface of the flexible composite film, which is provided with the isolating layer, and comprises the third flexible film and the second conductive layer, and the second conductive layer is arranged on the surface of the third flexible film, which is far away from the flexible composite film;
wherein the first electrode layer and the second electrode layer form a conductive loop.
The flexible pressure sensor device maintains excellent flexibility, biocompatibility and high electrical output performance. Meanwhile, the functional layer on the first electrode layer has higher roughness, and when the flexible pressure sensor manufactured by the functional layer applies tiny pressure outside, the change amount of the contact area between the functional layer and the upper polar plate can be increased, so that the functional layer has high sensitivity and has good effect on detecting tiny pressure.
Drawings
FIG. 1 is a flow chart of a process for preparing a flexible composite film according to an embodiment of the present invention;
FIG. 2 is a flow chart of a process for preparing a flexible composite film according to another embodiment of the present invention;
FIG. 3 is a flow chart of a process for manufacturing the flexible pressure sensor of the present invention;
fig. 4 is a graph showing the variation of the output voltage of the flexible pressure sensor according to embodiment 1 of the present invention.
In the figure: 1. a first electrode layer; 2. a second electrode layer; 10. a second flexible film; 11. a composite structure; 12. a functional layer; 13. an isolation layer; 14. a first conductive layer; 20. a third flexible film; 21. a second conductive layer; 30. a precursor layer; 40. a first flexible film; 110. a graphene microstructure; 111. particles of ferroelectric material.
Detailed Description
The flexible composite membrane, the preparation method and the self-generating flexible pressure sensor provided by the invention are further described below.
As shown in fig. 1 and 2, the preparation method of the flexible composite film provided by the invention comprises the following steps:
s1, providing a first flexible film 40 and a suspension containing ferroelectric material precursors, and forming the suspension on one surface of the first flexible film 40 to form a precursor layer 30 on the surface;
s2, irradiating the surface of the first flexible film 40 with the precursor layer 30 by adopting laser, so that a graphene microstructure 110 is formed on the surface of the first flexible film 40, and the ferroelectric material precursor is converted into ferroelectric material particles 111 and embedded in the interior and/or the surface of the graphene microstructure 110 to obtain a composite structure 11;
and S3, transferring at least part of the composite structure to one surface of the second flexible film 10 to form a functional layer 12 on one surface of the second flexible film 10, so as to obtain the flexible composite film.
In step S1, the material of the first flexible film 40 includes at least one of Polyimide (PI), polyethylene terephthalate (PET), and polybutylene terephthalate (PBT). More preferably, a Polyimide (PI) material having relatively excellent thermal stability is selected.
The ferroelectric material precursor comprises at least one of a strontium titanate precursor and a barium titanate precursor, and the barium titanate precursor is preferable. The barium titanate precursor suspension can be obtained by referring to the following steps:
dissolving butyl titanate and glacial acetic acid in isopropanol (the molar ratio of the butyl titanate to the isopropanol to the glacial acetic acid is 1:6:3), and uniformly stirring to obtain a mixed solution A;
weighing equimolar amount of barium acetate, dissolving in distilled water, and stirring to completely dissolve the barium acetate to obtain a solution B;
mixing the solution B with the mixed solution A, uniformly stirring, standing for 1-20 h, then vacuum drying at 100-200 ℃ for 1-10 h to obtain a preform, and washing the preform with ethanol for 1-3 times to obtain a barium titanate precursor;
and dispersing the barium titanate precursor with isopropanol to obtain a barium titanate precursor suspension with the concentration of 1-20%.
In addition, the method of disposing the suspension on the surface of the first flexible film 40 includes spin coating, knife coating, etc., and the present invention preferably employs a spin coating method to dispose the suspension on the surface of the first flexible film 40 at a spin coating speed of 200rpm to 5000rpm for 10s to 60s, and finally drying in an oven at 50 ℃ to 150 ℃ to obtain the precursor layer 30 on the surface. Thus, the automated production of the precursor layer 30 may be achieved by spin coating.
Meanwhile, by controlling the rotation speed of spin coating and the time of spin coating, the thickness of the precursor layer 30 can be controlled.
In order to allow a better spreading of the suspension on the surface of the first flexible film 40, the surface of the first flexible film 40 for carrying the suspension comprises at least one functional group of-OH, -COOH, so as to allow a better wettability, i.e. hydrophilicity, of the surface of the first flexible film 40.
Specifically, the first flexible film 40 may be irradiated with ultraviolet rays or treated with plasma, and the treated first flexible film 40 is dried at 60 to 120 ℃ so that at least one functional group of-OH, -COOH is formed on the surface of the first flexible film 40.
When ultraviolet irradiation is used, the wavelength of the ultraviolet light is less than 355nm, and when the wavelength is more than 355nm, the photon energy is smaller than the bond energy of the chemical bond of the material of the first flexible film 40, so that functional groups such as-OH, -COOH and the like cannot be generated. The irradiation time of the ultraviolet ray is preferably 0.5 to 72 hours because the surface of the first flexible film 40 has insufficient content of functional groups such as-OH, -COOH, etc. and insufficient wettability when the irradiation time is less than 0.5 hours, the content of functional groups such as-OH, -COOH, etc. of the surface of the first flexible film 40 gradually increases as the irradiation time is prolonged, and the content of functional groups hardly changes when the irradiation time is more than 72 hours.
When plasma treatment is adopted, the generated gas of the plasma comprises at least one of oxygen, hydrogen and nitrogen, and the time of the plasma treatment is 10 s-60 min.
In step S2, under the action of laser heat, chemical bonds such as C-O, C-H or c=o on the surface of the first flexible film 40 can be broken to generate CO 2 、H 2 O and the like volatilize into air to generate a graphene microstructure 110, and at the same time, the ferroelectric material precursor can be decomposed into ferroelectric material particles 111, and under the impact force of laser irradiation, the ferroelectric material particles 111 are embedded on the surface of the graphene microstructure 110 and enter the interior of the graphene microstructure 110 to form a composite structure 11. Therefore, in order to cause photothermal rather than photochemical effects on the surface, it is preferred that the laser wavelength be greater than 355nm.
It will be appreciated that, depending on the impact force of the laser irradiation, the ferroelectric material particles 111 may completely enter the graphene microstructure 110, or may be embedded on the surface of the graphene microstructure 110, or may be partially enter the graphene microstructure 110, or may be partially embedded on the surface of the graphene microstructure 110.
The laser single pulse energy is preferably in the range of 10 muj to 300 muj when laser irradiation, because when the single pulse energy is less than 10 muj, the photothermal effect is weak, and graphene and titanate are difficult to form; when the single pulse energy is more than 300 mu J, the thermal influence is increased, the surface of the film is melted and swelled, and the material is deformed, so that the subsequent use is influenced.
When the laser is irradiated, the laser scanning speed is preferably in the range of 100-3000 mm/s, because when the scanning speed is less than 100mm/s, the material is deformed under the accumulated heat action, and the use is influenced; when the scanning speed is greater than 3000mm/s, the laser spot overlap ratio is lower, and the quality of formed graphene and titanate is also poorer.
In step S3, the composite structure formed in the above step is at least partially transferred to the surface of the second flexible film 10 by means of transfer, and the functional layer 12 is formed on one surface of the second flexible film 10, and this transfer is preferably a transfer.
The material of the second flexible film 10 includes at least one of Polydimethylsiloxane (PDMS), polyurethane elastomer (TPU), poly (trimethylene carbonate) (PTMC), polypropylene (PP), polyethylene naphthalate (PEN), and styrene-butadiene-styrene block copolymer (SBS). Among them, the material of the second flexible film 10 is preferably PDMS in view of the best biocompatibility and thermal stability of PDMS.
The step of transferring the composite structure 11 to the second flexible film 10 comprises: the solution containing the above materials is placed on the surface of the first flexible film 40 with the composite structure 11, cured to obtain the second flexible film 10 on the surface of the composite structure 11, and separated to allow the composite structure 11 to be at least partially transferred to the second flexible film 10. In this transfer process, the bonding force of the composite structure 11 to the first flexible film 40 is weaker than the bonding force of the composite structure 11 to the second flexible film 10.
When the material of the second flexible film 10 is PDMS, the specific transfer method may be obtained by referring to the following steps:
mixing PDMS monomer and curing agent according to the weight ratio of 10: (0.9-1.1), pouring the PDMS mixture on the surface of the first flexible film 40 with the composite structure, curing for 0.25-24 hours at 25-150 ℃ to obtain a second flexible film 10, and separating the first flexible film 40 from the second flexible film 10, so that the composite structure 11 is at least partially transferred to the second flexible film 10.
Wherein, in the curing process, when the concentration of the curing agent is not changed by more than 10%, the curing time and the performance after curing of PDMS are hardly affected; when the concentration of the curing agent is reduced by more than 10%, the PDMS becomes soft, and the tensile property is reduced; when the curing agent concentration increases more than 10%, PDMS becomes hard and tensile properties are also reduced.
In the curing process, when the curing temperature is less than 25 ℃, the curing time is about 10 hours, the molding efficiency is affected, and the faster the curing speed is, the shorter the time is along with the increase of the curing temperature. When the curing temperature is higher than 150 ℃, the reaction is too fast, and small molecules generated in the curing process are not diffused out, so that a honeycomb structure is formed. Therefore, the curing time has close relation with the curing temperature, the effect of improving the curing temperature is the same as that of reducing the curing time, and the proper curing time is determined to be between 0.25 and 24 hours according to the curing temperature range.
Through the transfer printing step, the composite structure 11 on the first flexible film 40 can be partially or completely transferred to the second flexible film 10 to form the functional layer 12, as shown in fig. 1, where the composite structure 11 is completely transferred to the second flexible film 10 to form the functional layer 12, and in fig. 2, a part of the composite structure 11 is transferred to the second flexible film 10 to form the functional layer 12. In actual operation, the specific transfer is determined by the difference in bonding force between the composite structure 11 and the first and second flexible films 40 and 10, and the laser irradiation intensity.
The invention also provides a flexible composite film, which is obtained by the preparation method, and comprises a second flexible film 10 and a functional layer 12 arranged on one surface of the second flexible film 10, wherein the functional layer 12 comprises a graphene microstructure 110 and ferroelectric material particles 111 embedded in and/or on the graphene microstructure 110.
In the functional layer 12 in the flexible composite film, the ferroelectric material particles 111 and the graphene microstructure 110 can establish a percolation conductive network, so that the capacity of the functional layer 12 for storing charges is improved, the dielectric constant of the functional layer 12 is greatly improved, the dielectric loss is reduced, and the output performance of the functional layer can be effectively improved.
Meanwhile, the functional layer 12 obtained by laser irradiation has higher roughness, so that when the external micro pressure is applied to the flexible pressure sensor prepared by the functional layer 12, the change amount of the contact area between the flexible pressure sensor and the functional layer 12 can be increased, the sensitivity is high, and the flexible pressure sensor has a good effect on detecting the micro pressure.
As shown in fig. 3, the method for manufacturing the flexible pressure sensor provided by the invention comprises the following steps:
s4, providing the flexible composite film obtained by the preparation method and a third flexible film 20;
s5, paving an isolation layer 13 on the flexible composite film, surrounding the functional layer 12, and enabling the height of the isolation layer 13 to be larger than that of the functional layer 12;
and S6, attaching and bonding the third flexible film 20 and the isolation layer 13 to each other to obtain the flexible pressure sensor.
In step S4, the material of the third flexible film 20 includes at least one of Polydimethylsiloxane (PDMS), polyurethane elastomer (TPU), polytrimethylene carbonate (PTMC), polypropylene (PP), polyethylene naphthalate (PEN), and styrene-butadiene-styrene block copolymer (SBS), preferably PDMS.
In step S5, the isolation layer 13 surrounds the periphery of the functional layer 12 to improve the subsequent packaging effect, and the height of the isolation layer 13 is 100 μm-5000 μm and higher than the height of the functional layer 12, so as to ensure that the third flexible film 20 is not contacted with the functional layer 12 during packaging, and ensure the detection sensitivity.
The material of the spacer layer 13 is at least one of Polydimethylsiloxane (PDMS), polyethylene terephthalate (PET), polybutylene terephthalate (PBT), and preferably PDMS.
In step S6, after the third flexible film 20 and the isolation layer 13 are attached to each other, the third flexible film and the isolation layer are bonded by using a bonding material such as a 3M tape.
In addition, the surface of the flexible composite film far away from the functional layer 12 is further provided with a first conductive layer 14, the surface of the third flexible film 20 far away from the isolating layer 13 is further provided with a second conductive layer 21, and the first conductive layer 14 and the second conductive layer 21 form a conductive loop.
The first conductive layer 14 may be provided before or after the third flexible film 20 is laminated with the flexible composite film, and is preferably provided before. The method comprises the following steps: coating conductive pastes such as silver paste, copper paste and the like in a spin coating mode, a knife coating mode and the like, and drying to form a first conductive layer 14; alternatively, a metal conductive layer such as gold, silver, copper, or the like is sputtered to form the first conductive layer 14; alternatively, a conductive carbon material such as graphene, carbon nanotube, carbon black, or the like is provided to form the first conductive layer 14.
The second conductive layer 21 may be provided with reference to the method of the first conductive layer 14.
Also, in order to better spread the first conductive layer 14 on the surface of the flexible composite film, the flexible composite film may be irradiated with ultraviolet rays or treated with plasma to support the surface of the first conductive layer 14 so as to include at least one functional group of-OH, -COOH. In order to better spread the second conductive layer 21 on the surface of the third flexible film 20, ultraviolet irradiation or plasma treatment may be used to treat the surface of the third flexible film 20 for supporting the second conductive layer 21, so that it includes at least one functional group of-OH, -COOH.
The invention also provides a flexible pressure sensor, which is prepared by the preparation method, and comprises the following steps:
a first electrode layer 1, wherein the first electrode layer 1 comprises the flexible composite film, the first conductive layer 14 and the isolation layer 13, the first conductive layer 14 is laminated on the surface of the flexible composite film, which is away from the functional layer 12, the isolation layer 13 is arranged around the functional layer 12, and the height of the isolation layer 13 is greater than the height of the functional layer 12;
a second electrode layer 2, wherein the second electrode layer 2 is laminated on the surface of the flexible composite film with the isolating layer 13, the second electrode layer 2 comprises the third flexible film 20 and the second conductive layer 21, and the second conductive layer 21 is laminated on the surface of the third flexible film 20 far from the flexible composite film;
wherein the first electrode layer 1 and the second electrode layer 2 form a conductive loop.
The functional layer 12 in the flexible pressure sensor can supply power to the flexible pressure sensor, and has good and stable output effect. Meanwhile, the action principle of the flexible pressure sensor can be regarded as a piezoelectric principle, namely, due to the existence of the functional layer 12, the sensitivity of the flexible pressure sensor can be improved, and the flexible pressure sensor has a good detection effect on micro pressure.
In addition, the second flexible film 10 and the third flexible film 20 are completely packaged, so that the pressure sensor can ensure excellent flexibility, biocompatibility and higher electric output performance, and has good effect on detecting micro pressure.
Hereinafter, the flexible composite film, the preparation method and the self-generating flexible pressure sensor will be further described by the following specific examples.
Example 1
The preparation method of the flexible composite film comprises the following steps:
butyl titanate and glacial acetic acid are dissolved in isopropanol (the molar ratio of the butyl titanate to the isopropanol to the glacial acetic acid is 1:6:3), and the mixture is stirred uniformly to obtain a mixed solution A. An equimolar amount of barium acetate was weighed and dissolved in distilled water, and stirred to be completely dissolved, to obtain a solution B. Slowly adding the solution B into the solution A, stirring uniformly, standing for 1h, vacuum drying at 200 ℃ for 10h, washing the product with ethanol for 1 time to obtain a barium titanate precursor, and dispersing the precursor with isopropanol to obtain a barium titanate precursor suspension with the concentration of 20%;
selecting a film made of Polyimide (PI) and adopting O 2 And (3) carrying out plasma treatment for 1min to enable the surface to generate functional groups such as-OH, -COOH and the like. Then spin-coating barium titanate precursor suspension on the surface, and drying for 1h at 60 ℃ to obtain a barium titanate precursor layer;
irradiating the surface of a first flexible film with a barium titanate precursor layer by using laser, wherein the laser wavelength is 532nm, the single pulse energy is 50 mu J, and the scanning speed is 800mm/s so as to obtain a composite structure on the surface of the first flexible film, and the composite structure comprises a graphene microstructure and ferroelectric material particles embedded in and/or on the graphene microstructure;
commercially available PDMS monomer and curing agent were mixed according to a ratio of 10:1, uniformly mixing, removing bubbles in vacuum, pouring the PDMS mixture directly on the surface of the first flexible film with the composite structure, curing for 4 hours at 85 ℃ to obtain a second flexible film, and stripping the first flexible film directly from the second flexible film to form a functional layer on one surface of the second flexible film to obtain the flexible composite film.
And paving an isolation layer on the flexible composite film and surrounding the functional layer, wherein the thickness of the isolation layer is 100 mu m, and the isolation layer is made of PDMS.
O is adopted on the surface of the flexible composite film facing away from the functional layer 2 And carrying out plasma treatment, spin-coating conductive silver paste on the surface of the substrate, and then drying the substrate at 100 ℃ to obtain the first conductive layer. The flexible composite film, the isolation layer and the first conductive layer are integrally used as a first electrode layer.
Selecting a third flexible film made of PDMS, and adopting O to one surface of the third flexible film 2 And carrying out plasma treatment, spin-coating conductive silver paste on the surface, and drying at 100 ℃ to obtain a second conductive layer. The third flexible film and the second conductive layer are integrally formed as a second electrode layer.
And attaching the surface of the second electrode layer, which is away from the second conductive layer, to the isolation layer in the first electrode layer, cutting two thin wires, respectively placing the two thin wires on the surfaces of the first conductive layer and the second conductive layer, then coating a layer of conductive silver adhesive to fix the wires and form a conductive loop, and simultaneously packaging the first electrode layer and the second electrode layer by using packaging materials such as 3M adhesive tapes and the like to obtain the flexible pressure sensor.
The flexible pressure sensor of this example was subjected to conditions of 50℃and 80% humidity to detect the output voltage at 1kPa for various periods of time, as shown in FIG. 4, with a sensitivity of 20.83mV/Pa and a linear detection range of 4.12kPa.
The differences between examples 2 to 9 and example 1 are shown in Table 1.
TABLE 1
The differences between comparative examples 1 to 6 and example 1 are shown in Table 2.
TABLE 2
The technical features of the above-described embodiments may be arbitrarily combined, and all possible combinations of the technical features in the above-described embodiments are not described for brevity of description, however, as long as there is no contradiction between the combinations of the technical features, they should be considered as the scope of the description.
The above examples illustrate only a few embodiments of the invention, which are described in detail and are not to be construed as limiting the scope of the invention. It should be noted that it will be apparent to those skilled in the art that several variations and modifications can be made without departing from the spirit of the invention, which are all within the scope of the invention. Accordingly, the scope of protection of the present invention is to be determined by the appended claims.
Claims (13)
1. A method of making a flexible composite film comprising:
providing a first flexible film and a suspension containing a ferroelectric material precursor, forming the suspension on one surface of the first flexible film to form a precursor layer on the surface;
irradiating the surface of the first flexible film with the precursor layer by adopting laser so that a graphene microstructure is formed on the surface of the first flexible film, converting the ferroelectric material precursor into ferroelectric material particles and embedding the ferroelectric material particles into the graphene microstructure to obtain a composite structure, wherein the laser irradiation conditions comprise: the laser wavelength is more than 355nm, the laser scanning speed is 100 mm/s-3000 mm/s, and the laser single pulse energy range is 10 mu J-300 mu J;
and transferring at least part of the composite structure to one surface of a second flexible film to form a functional layer on one surface of the second flexible film, so as to obtain the flexible composite film.
2. The method for producing a flexible composite film according to claim 1, wherein the conditions of the laser irradiation include: the laser wavelength is 1064nm, the laser scanning speed is 800mm/s, and the laser single pulse energy range is 50 mu J.
3. The method of claim 1, wherein the surface of the first flexible film for supporting the suspension comprises at least one functional group of-OH, -COOH.
4. The method of producing a flexible composite film according to claim 3, wherein the first flexible film is treated with ultraviolet irradiation or with plasma so that at least one functional group of-OH, -COOH is formed on the surface of the first flexible film.
5. The method of producing a flexible composite film according to claim 1, wherein the first material of the first flexible film comprises at least one of polyimide, polyethylene terephthalate, polybutylene terephthalate; and/or the number of the groups of groups,
the second material of the second flexible film comprises at least one of polydimethylsiloxane, polyurethane elastomer, poly (trimethyl carbonate), polypropylene, polyethylene naphthalate, and styrene-butadiene-styrene block copolymer.
6. The method of preparing a flexible composite film according to claim 5, wherein transferring the composite structure to the second flexible film comprises: and placing a solution containing the second material on the surface of the first flexible film with the composite structure, curing to obtain the second flexible film on the surface of the composite structure, and separating to enable the composite structure to be at least partially transferred to the second flexible film.
7. The method of claim 1, wherein the ferroelectric material precursor comprises at least one of a strontium titanate precursor and a barium titanate precursor.
8. The method according to claim 1, wherein the suspension is coated on the surface of the first flexible film by spin coating at a speed of 200rpm to 5000rpm for 10s to 60s.
9. A flexible composite film, characterized in that the flexible composite film is prepared by the preparation method of any one of claims 1 to 8, the flexible composite film comprises a second flexible film and a functional layer arranged on one surface of the second flexible film, and the functional layer comprises a graphene microstructure and ferroelectric material particles embedded in and/or on the graphene microstructure.
10. A method of manufacturing a flexible pressure sensor, comprising:
providing the flexible composite film obtained by the preparation method according to any one of claims 1-8, and a third flexible film;
paving an isolation layer on the flexible composite film, surrounding the functional layer, and enabling the height of the isolation layer to be larger than that of the functional layer;
attaching and bonding the third flexible film and the isolation layer to each other to obtain a flexible pressure sensor;
the surface of the flexible composite film far away from the functional layer is further provided with a first conductive layer, the surface of the third flexible film far away from the isolation layer is further provided with a second conductive layer, and the first conductive layer and the second conductive layer form a conductive loop.
11. The method of claim 10, wherein the surface of the flexible composite film for supporting the first conductive layer comprises at least one functional group of-OH, -COOH;
and/or the surface of the third flexible film for bearing the second conductive layer comprises at least one functional group of-OH and-COOH.
12. The method for manufacturing a flexible pressure sensor according to claim 10, wherein the height of the isolation layer is 100 μm to 5000 μm, and the material of the isolation layer includes at least one of polydimethylsiloxane, polyethylene terephthalate, and polybutylene terephthalate.
13. A flexible pressure sensor, characterized in that it is manufactured by the manufacturing method according to any one of claims 10 to 12, comprising:
the first electrode layer comprises the flexible composite film, the first conductive layer and the isolation layer, the first conductive layer is arranged on the surface of the flexible composite film, which is away from the functional layer, the isolation layer is arranged around the functional layer, and the height of the isolation layer is larger than that of the functional layer;
the second electrode layer is arranged on the surface of the flexible composite film, which is provided with the isolating layer, and comprises the third flexible film and the second conductive layer, and the second conductive layer is arranged on the surface of the third flexible film, which is far away from the flexible composite film;
wherein the first electrode layer and the second electrode layer form a conductive loop.
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