CN115479705A - Printable transparent stress sensor and preparation method thereof - Google Patents
Printable transparent stress sensor and preparation method thereof Download PDFInfo
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- CN115479705A CN115479705A CN202211000536.4A CN202211000536A CN115479705A CN 115479705 A CN115479705 A CN 115479705A CN 202211000536 A CN202211000536 A CN 202211000536A CN 115479705 A CN115479705 A CN 115479705A
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Images
Classifications
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- G01L1/00—Measuring force or stress, in general
- G01L1/18—Measuring force or stress, in general using properties of piezo-resistive materials, i.e. materials of which the ohmic resistance varies according to changes in magnitude or direction of force applied to the material
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M1/00—Inking and printing with a printer's forme
- B41M1/26—Printing on other surfaces than ordinary paper
- B41M1/34—Printing on other surfaces than ordinary paper on glass or ceramic surfaces
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B41—PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
- B41M—PRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
- B41M5/00—Duplicating or marking methods; Sheet materials for use therein
- B41M5/0041—Digital printing on surfaces other than ordinary paper
- B41M5/007—Digital printing on surfaces other than ordinary paper on glass, ceramic, tiles, concrete, stones, etc.
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D1/00—Coating compositions, e.g. paints, varnishes or lacquers, based on inorganic substances
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D175/00—Coating compositions based on polyureas or polyurethanes; Coating compositions based on derivatives of such polymers
- C09D175/04—Polyurethanes
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D183/00—Coating compositions based on macromolecular compounds obtained by reactions forming in the main chain of the macromolecule a linkage containing silicon, with or without sulfur, nitrogen, oxygen, or carbon only; Coating compositions based on derivatives of such polymers
- C09D183/04—Polysiloxanes
-
- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09D—COATING COMPOSITIONS, e.g. PAINTS, VARNISHES OR LACQUERS; FILLING PASTES; CHEMICAL PAINT OR INK REMOVERS; INKS; CORRECTING FLUIDS; WOODSTAINS; PASTES OR SOLIDS FOR COLOURING OR PRINTING; USE OF MATERIALS THEREFOR
- C09D5/00—Coating compositions, e.g. paints, varnishes or lacquers, characterised by their physical nature or the effects produced; Filling pastes
- C09D5/24—Electrically-conducting paints
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2201/00—Properties
- C08L2201/04—Antistatic
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- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
- C08L2205/00—Polymer mixtures characterised by other features
- C08L2205/02—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group
- C08L2205/025—Polymer mixtures characterised by other features containing two or more polymers of the same C08L -group containing two or more polymers of the same hierarchy C08L, and differing only in parameters such as density, comonomer content, molecular weight, structure
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Life Sciences & Earth Sciences (AREA)
- Materials Engineering (AREA)
- Wood Science & Technology (AREA)
- Organic Chemistry (AREA)
- Ceramic Engineering (AREA)
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Abstract
The invention discloses a printable transparent stress sensor and a preparation method thereof. The conductive nano material is prepared into a transparent film by a printing method and is transferred and embedded in the elastomer with the modulus gradient structure. The conductive nano material provides a transparent conductive network, so that high light transmittance and low square resistance are ensured; the relative sliding of the conductive nano materials enables the device to have higher sensitivity; the elastic body and the embedding structure with the modulus gradient structure can relieve stress concentration of the conductive nano material in the stretching process, the working range of the sensor is improved, the obtained transparent stress sensor has the characteristics of large working range, high sensitivity, high light transmittance, high surface flatness, excellent stretching stability and the like, and has huge application prospects in the fields of flexible touch screens, electronic skins, human-computer interaction, bionic robots and the like.
Description
Technical Field
The invention belongs to the technical field of flexible transparent stress sensors, relates to the technical field of flexible transparent conductive materials and printed electronic products, and particularly relates to a mechanical sensor with high light transmittance, high sensitivity and large working range and a preparation method thereof. The method is mainly used for screen fingerprint unlocking of the flexible touch screen and human motion information monitoring. Has great application prospect in the fields of human-computer interaction, electronic skin, bionic robot, and the like.
Background
With the popularization of flexible electronic devices, flexible transparent stress sensors have attracted extensive attention of people. For example, in the field of flexible touch screens, the screen unlocking function of Huashi flexible screen mobile phone Mate Xs is realized by adopting a flexible transparent stress sensor behind a screen backboard. In the field of flexible transparent wearable devices, "stealth" and "non-feel" characteristics can increase wearer comfort and aesthetics, an important feature of future flexible sensors. Therefore, the development of flexible transparent stress sensors is of great significance.
However, the search of flexible transparent stress sensors by researchers to date is still not ideal for high sensitivity, large tensile range, and high transparency. The working range is too small to meet the requirements of practical application, the sensitivity is too low to detect micro deformation, and the transparency is low to obviously reduce the light transmittance of the device.
Chinese patent publication No. CN 111678623A discloses an ultra-long-life self-repairing stress sensor based on a printable nanocomposite and a preparation method thereof. The method is characterized in that a one-dimensional metal nanowire, a two-dimensional inorganic nanosheet, a polymer material containing host-guest interaction, a corresponding high-boiling-point solvent and the like are compounded to prepare nanocomposite colloidal ink with rheological characteristics, and the stress sensor with in-situ self-repairing capability and long cycle service life is prepared by a screen printing method. In the working process of the sensor, the contained host-guest polymer material can repair the defects generated inside in real time and in situ, and the service life of the material is greatly prolonged. Meanwhile, the device has the characteristics of working strain range of more than 50%, sensitivity gauge factor of more than 100, strong self-repairing capability and strong sweat anti-interference capability. Has great application prospect in the fields of intelligent wearable devices and the like.
Chinese patent publication No. CN211376213U discloses a touch sensor based on a transparent conductive film. The touch sensor can only bend, limiting the application of the device to wearable electronics.
Chinese patent publication No. CN111895902A discloses a transparent flexible strain sensor based on a carbon nanofiber membrane. The transparent flexible strain sensor takes polyurethane as a substrate and an ultrathin carbon nanofiber membrane as a conductor. The working range of the transparent flexible strain sensor is more than 70%, the sensitivity can reach 846.7 at most, but the light transmittance is only 50%, so that the application of the sensor on a transparent device is limited.
Non-patent document 1 (ACS applied materials)&interfaces, 2019, 11: 40232-40242) describes a transparent stress sensor prepared by spraying silver nanowires onto a polyethylene terephthalate/polysilicylmethylsiloxane substrate, the sensitivity of the transparent stress sensor being up to 250; when the square resistance is 38.5 omega-sq -1 The light transmittance was 77.4%. But the transparent stress transferThe working range of the sensor is only 13%, and the application of the device in the wearable field is limited.
Non-patent document 2 (ACS applied materials & interfaces, 2017, 9: 26279-26285) describes a composite strain sensor prepared from solution-processed carbon nanotubes and polydimethylsiloxane, which has a light transmittance of 92% and a working range of 50%. However, the sensitivity of the strain sensor is only 2.6 at the maximum, which limits the application of the device in the wearable field.
Stress sensors with high sensitivity, large operating range and high light transmittance have not been reported.
Disclosure of Invention
In order to solve the defects of the prior art, the invention aims to: a transparent printable stress sensor is provided, wherein a transparent conductive film made of nano conductive materials is embedded in an elastomer substrate with modulus gradient, so that a flexible transparent sensor with an embedded structure is manufactured.
Yet another object of the present invention is to: a method of making the printable transparent stress sensor described above is provided.
The purpose of the invention is realized by the following scheme: the printable transparent stress sensor comprises a conductive layer and an elastic substrate, wherein the conductive layer is a transparent conductive layer formed by conductive nano materials; the elastic substrate is two or more than two transparent elastic layers with modulus gradient structures, and the transparent conductive layer is embedded in the elastic substrate and connected with the highest modulus layer.
Based on the scheme, when the square resistance is less than 50 omega-sq -1 When the transmittance is higher than 80%.
Wherein the elastomeric substrate refers to: styrenic block copolymer-type thermoplastic elastomer: SBS, SEBS, SIS; a polyurethane; a silicone elastomer: polydimethylsiloxane; one or more of polyethylene terephthalate, poly 4-methylpentene, polyvinyl alcohol, polyamide thermoplastic elastomer, ethylene-vinyl acetate copolymer, polyacrylate and polyolefin thermoplastic elastomer.
Further, the modulus of the base material with the modulus gradient gradually decreases from one side close to the conductive nanometer material to the other side.
Furthermore, the elastic substrate is two or more layers of polyurethane elastomers with different moduli, and the modulus of the substrate material with the modulus gradient gradually decreases from one side close to the conductive layer to the other side.
The nano conductive material is as follows:
zero-dimensional metal nanoparticles, one of gold, silver, copper, iron, chromium, nickel, aluminum, tungsten, platinum, gallium, indium, gallium-indium alloy and gallium-indium-tin alloy metal nanoparticles, with the particle size of 1-1000 nm; and/or the presence of a gas in the atmosphere,
one-dimensional metal nanowires, wherein the metal nanowires are one of gold, silver, copper, iron, nickel, platinum, palladium and aluminum, the diameter of the metal nanowires is 1-300 nm, and the length of the metal nanowires is 2-100 microns; and/or the presence of a gas in the atmosphere,
graphene, two-dimensional transition metal carbide or nitride (MXene) which is a two-dimensional structure similar to graphene and has a chemical general formula of M n+1 X n T z N = 1, 2, 3, wherein M is an early transition metal element, X is carbon or nitrogen, T is a surface-linked-F, -OH reactive functional group, including Ti 2 C、Ti 3 C 2 、Ti 3 CN、V 2 C、Nb 2 C、TiNbC、Nb 4 C 3 、Ta 4 C 3 、(Ti 0.5 Nb 0.5 ) 2 C or (V) 0.5 Cr 0.5 ) 3 C 2 To (3) is provided.
In the invention, the transparent conductive network is provided by the conductive nano material, so that higher light transmittance and lower square resistance are ensured; the relative sliding or deformation of the conductive nano material enables the device to have higher sensitivity; the embedded structure and the elastic body substrate with modulus gradient can relieve the stress concentration of the conductive nano material in the stretching process, improve the working range of the sensor, and the obtained transparent stress sensor has a large working range (>100%), high sensitivity: (>100 High light transmittance (square resistance less than 50 Ω · sq) -1 When the temperature of the water is higher than the set temperature,light transmittance of more than 80 percent) and high surface flatness (R) sq <10 nm) and excellent tensile stability (service life more than 1000 times at strain greater than 30%), etc.
The sensing mechanism of the transparent stress sensor is as follows: in the stretching process, the resistance is obviously increased due to poor contact, slippage or cracks among the conductive nano materials, and the sensitivity of the transparent sensor is improved.
The elastic substrate with the modulus gradient can obviously reduce the stress borne by the conductive material in the stretching process, reduce the resistance change and obviously enlarge the working range of the device.
The invention also provides a preparation method of the printable transparent stress sensor, which comprises the following steps:
(1) Mixing the conductive nano material with a solvent, uniformly dispersing the conductive nano material by ultrasonic oscillation, and preparing a transparent conductive film on a glass substrate by a printing method;
(2) Mixing two or more elastomer materials with larger modulus difference and approximate elongation at break according to different proportions to obtain elastomer solutions or precursor solutions with different moduli as elastomer base materials;
(3) Spreading the elastomer solution or precursor solution obtained in the step (2) on the surface of the conductive film in sequence from high modulus to low modulus, heating to evaporate the solvent or curing to form an elastic matrix with modulus gradient, wherein the elastic matrix is embedded with the transparent conductive film;
(4) And (4) tearing the elastic matrix embedded with the transparent conductive film from the glass substrate in the step (3) to obtain the transparent stress sensor.
In the elastomer with the modulus gradient structure, as the thickness of the transparent conductive film increases, the light transmittance of the transparent stress sensor is reduced correspondingly.
The preparation method is simple, has no harmful substances in the whole process, and can be used for mass production in a screen printing mode.
In the step (1), the printing method of the conductive film is as follows: screen printing, ink jet printing, blade coating, stencil printing, gravure printing, relief printing, offset printing, spin coating, dip coating, meyer rod coating, spray coating, slot coating, microcontact printing, direct writing printing.
The invention also provides an application of the printable transparent stress sensor, which is used for screen fingerprint unlocking of a flexible touch screen and transparent wearable equipment or used for detecting human motion signals, including pulse beat type micro-deformation signals and finger or knee bending type large-strain signals.
The sensor of the invention prepares the conductive nano material into a transparent conductive film by a printing method, and the transparent conductive film is transferred and embedded into an elastomer with a modulus gradient structure. The transparent stress sensor has good performance: the sensitivity is more than 100; the working range is more than 100 percent; under the strain of more than 30%, the service life exceeds 1000 times; has good light transmittance and square resistance, and when the square resistance is less than 50 omega-sq -1 When the transmittance is higher than 80%.
Drawings
FIG. 1 is a schematic structural diagram of a transparent stress sensor (defined as embodiment three, similar to the structure);
FIG. 2 is a working curve of the transparent stress sensor of embodiment 1;
FIG. 3 the useful life of the transparent stress sensor of example 1;
FIG. 4 light transmittance of the transparent stress sensor of example 1;
FIG. 5 is a diagram of the pulse detected by the prepared sensor;
FIG. 6 is a photograph of a prepared sensor for detecting knee joint flexion;
wherein the figure numbers indicate:
1-transparent conductive layer;
2-a high modulus elastomeric substrate layer; 3-medium modulus elastomeric substrate layer; 4-low modulus elastomeric substrate layer.
Detailed Description
Example 1
A printable transparent stress sensor comprising a conductive layer and an elastic substrate, characterized in that: the conducting layer is a transparent conducting layer made of conducting nano materials; the elastic substrate is a multilayer elastic layer with a modulus gradient structure, the transparent conducting layer is embedded in the elastic substrate and connected with the highest modulus layer, in the embodiment, the silver nanowire is used as the conducting nanomaterial, the elastic substrate is a film composed of polyurethane 6210 and polyurethane 6290 in different mixing ratios, and the preparation method comprises the following steps:
(1) Preparing a transparent conductive layer: selecting silver nanowires as a conductive nano material, dissolving the silver nanowires in ethanol, dispersing the silver nanowires uniformly by ultrasonic oscillation to obtain silver nanowire/ethanol dispersion liquid with the concentration of 2 mg/mL, weighing 100 muL of the silver nanowire/ethanol dispersion liquid, spin-coating the silver nanowire/ethanol dispersion liquid on a glass sheet by a printing method, wherein the rotating speed is 800 rpm, the spin-coating time is 15 s, heating is carried out at 60 ℃ for 1 min, and repeating the operation for 10 times to obtain a silver nanowire transparent conductive film of a glass substrate as an embedded structure;
(2) Respectively weighing the polyurethane 6210 and the polyurethane 6290 according to mass ratios of 1, 10, 1, 5, 1;
(3) Weighing 1g of polyurethane with different moduli obtained in the step (2), respectively mixing the polyurethane with 0.5g of acrylic acid (5-ethyl-1, 3-dioxane-5-yl) methyl ester and 0.15g of photoinitiator, uniformly stirring, centrifuging to remove bubbles, spin-coating the surface of the silver nanowire transparent conductive film obtained in the step (1) with the moduli from high to low in sequence, wherein the rotating speed is 900rpm, the spin-coating time is 60s, and carrying out ultraviolet curing for 3 min to obtain the film;
(4) And (4) peeling the film from the glass substrate in the step (3) to obtain the transparent stress sensor.
Fig. 2 is a working curve of the transparent stress sensor of the present embodiment, showing the working range and sensitivity of the device of the present invention.
Fig. 3 shows the service life of the transparent stress sensor of this embodiment, and the resistance changes are kept stable for 1000 cycles and 4000 cycles in the stretch-release cycle with strain of 40%.
FIG. 4 is a graph showing the transmittance of the transparent stress sensor according to the embodiment, wherein the transmittance and the sheet resistance decrease as the thickness of the transparent conductive film increases; therefore, the larger the thickness of the transparent conductive film is, the smaller the square resistance and the light transmittance are; conversely, the greater the sheet resistance and the light transmittance; in fig. 4, the sheet resistance increases, and accordingly, the thickness of the transparent conductive film decreases and the light transmittance increases.
Example 2
A printable transparent stress sensor, similar to the procedure of example 1, except that the nano-conductive material is selected from two-dimensional transition metal nitride (MXene), prepared by the following steps:
(1) Preparing a transparent conductive layer: weighing 100 muL of MXene/water dispersion with the concentration of 10 mg/mL, printing on a glass sheet by using an ink-jet printer, heating at 60 ℃ for 1 min, and repeatedly operating for 5 times to obtain an MXene transparent conductive film of a glass substrate;
(2) Respectively weighing the following components in mass ratio of 1;
(3) Respectively weighing 4g of polyurethane obtained in the step (2), 2g of acrylic acid (5-ethyl-1, 3-dioxane-5-yl) methyl ester and 0.6g of photoinitiator, mixing the polyurethane, the acrylic acid (5-ethyl-1, 3-dioxane-5-yl) methyl ester and the photoinitiator, uniformly stirring, vacuumizing to remove bubbles, sequentially performing screen printing on the surface of the Mxene transparent conductive film obtained in the step (1) by using a screen printing plate according to the modulus from high to low, and performing ultraviolet curing for 5 min to obtain an elastic film with a modulus gradient and an embedded transparent conductive layer;
(4) And peeling off the glass substrate to obtain the transparent stress sensor.
Example 3
A printable transparent stress sensor is similar to the step of the embodiment 1, except that a nano conductive material is selected from copper nanowires, an elastic substrate material is selected from polydimethylsiloxane PDMS part A and PDMS part B, and the sensor is prepared by the following steps:
(1) Preparing a transparent conductive layer: weighing 100 muL of copper nanowire/water dispersion with the concentration of 5 mg/mL, carrying out blade coating on a glass sheet by using a Meyer rod, heating for 1 min at 60 ℃, and repeatedly operating for 5 times to obtain the copper nanowire transparent conductive film with the glass substrate.
(2) Respectively weighing polydimethylsiloxane PDMS part A and PDMS part B with the mass ratio of 10;
(3) Weighing 10g of PDMS obtained in the step (2), vacuumizing to remove bubbles, blade-coating the surface of the copper nanowire transparent conductive film obtained in the step (1) with a Meyer bar in sequence from high modulus to low modulus, and heating and curing at 60 ℃ for 2h to obtain an elastic film embedded with a transparent conductive layer and having modulus gradient;
(4) And peeling the film from the glass substrate to obtain the transparent stress sensor. The structure is shown in figure 1, and comprises a conductive layer and an elastic substrate, wherein the conductive layer is a transparent conductive layer 1 composed of conductive nano materials; the elastic substrate is three layers of elastic substrate layers with modulus gradient structures, namely a high-modulus elastic substrate layer 2, a medium-modulus elastic substrate layer 3 and a low-modulus elastic substrate layer 4.
Example 4
A printable transparent stress sensor, similar to the procedure of example 1, except that the nano conductive material is selected from two-dimensional transition metal nitride (MXene), the elastic base material is selected from polydimethylsiloxane PDMS part A and PDMS part B, and the sensor is prepared by the following steps:
(1) Preparing a transparent conductive layer: weighing 100 mL of MXene/water dispersion with the concentration of 8 mg/mL, soaking a glass sheet in the MXene/water dispersion for 10 min, heating and drying at 80 ℃, and repeatedly operating for 7 times to obtain an Mxene transparent conductive film of the glass substrate as an embedding structure;
(2) Respectively weighing 10 parts of PDMS part A and PDMS part B;
(3) Respectively weighing 5g of PDMS obtained in the step (2), sequentially performing screen printing on the surface of the MXene transparent conductive film obtained in the step (1) by using a screen printing plate according to the modulus from high to low, and heating for 1 h at 80 ℃ to obtain an elastic film with a modulus gradient and a transparent conductive layer embedded;
(4) And peeling the film from the glass substrate to obtain the transparent stress sensor.
Example 5
A printable transparent stress sensor, similar to the procedure of example 1, except that the nano conductive material is selected from graphene, is prepared by the following steps:
(1) Preparing a transparent conductive layer: preparing graphene/DMF dispersion liquid with the concentration of 6 mg/mL by using Dimethylformamide (DMF) as a solvent, weighing 10 mL of graphene/DMF dispersion liquid, performing screen printing on a glass sheet, heating and drying at 40 ℃, and repeatedly operating for 3 times to obtain the graphene transparent conductive film with the glass substrate;
(2) Respectively weighing the following components in mass ratio of 1;
(3) Respectively weighing 2g of polyurethane obtained in the step (2), 1g of acrylic acid (5-ethyl-1, 3-dioxane-5-yl) methyl ester and 0.3g of photoinitiator, mixing the polyurethane, the acrylic acid (5-ethyl-1, 3-dioxane-5-yl) methyl ester and the photoinitiator, uniformly stirring, sequentially coating the surface of the graphene transparent conductive film obtained in the step (1) with a slit coating machine according to the modulus from high to low, and carrying out ultraviolet curing for 10 min to obtain an elastic film which is embedded with the transparent conductive layer and has modulus gradient;
(4) And peeling the film from the glass substrate to obtain the transparent stress sensor.
Application example
A screen fingerprint unblock, transparent wearable equipment for flexible touch-sensitive screen, perhaps, be used for surveying human motion signal, including pulse beat type micro deformation signal and finger or knee bend type major strain signal.
As shown in fig. 5, the present invention can be used as a pulse beat sensor, and has high detection sensitivity for the micro deformation signals of pulse beat.
The present invention also has an excellent effect of detecting the bending motion of the knee joint as shown in fig. 6.
The above embodiments are merely illustrative of the present invention and should not be limited to the contents shown in the embodiments. The specific substances in the product components disclosed in the technical scheme of the invention can be implemented by the invention, and the technical effects are the same as those obtained in the examples, and the examples are not separately illustrated. Therefore, it is intended that all equivalents and modifications which are within the spirit of the disclosure be protected by the accompanying claims.
Claims (13)
1. A printable transparent stress sensor comprising a conductive layer and an elastic substrate, characterized in that: the conducting layer is a transparent conducting layer made of conducting nano materials; the elastic substrate is two or more transparent elastic layers with modulus gradient structures, and the transparent conductive layer is embedded in the elastic substrate and connected with the highest modulus layer.
2. The printable transparent stress sensor according to claim 1, wherein: with the increase of the thickness of the transparent conductive film, the light transmittance of the transparent stress sensor is reduced correspondingly when the sheet resistance is less than 50 Ω · sq -1 When the light transmittance is higher than 80%.
3. The printable transparent stress sensor and method of claim 1, wherein the elastomeric substrate is: styrenic block copolymer-type thermoplastic elastomer: SBS, SEBS, SIS; a polyurethane; a silicone elastomer: polydimethylsiloxane; one or more of polyethylene terephthalate, poly 4-methylpentene, polyvinyl alcohol, polyamide thermoplastic elastomer, ethylene-vinyl acetate copolymer, polyacrylate and polyolefin thermoplastic elastomer.
4. Printable transparent stress sensor according to claim 1 or 3, characterized in that: the modulus of the elastomer substrate with the modulus gradient gradually decreases from one side close to the transparent conductive layer to the other side.
5. The printable transparent stress sensor and the method for making the same according to claim 1, wherein the nano conductive material is selected from the group consisting of:
zero-dimensional metal nanoparticles, one of gold, silver, copper, iron, chromium, nickel, aluminum, tungsten, platinum, gallium, indium, gallium-indium alloy and gallium-indium-tin alloy metal nanoparticles, with the particle size of 1-1000 nm; and/or the presence of a gas in the atmosphere,
one-dimensional metal nanowires, wherein the metal nanowires are one of gold, silver, copper, iron, nickel, platinum, palladium and aluminum, the diameter of the metal nanowires is 1-300 nm, and the length of the metal nanowires is 2-100 microns; and/or the presence of a gas in the atmosphere,
graphene, two-dimensional transition metal carbide or nitride (MXene), which is a two-dimensional structure similar to graphene and has a chemical general formula of M n+1 X n T z N = 1, 2, 3, wherein M is an early transition metal element, X is carbon or nitrogen, T is a surface-linked-F, -OH reactive functional group, including Ti 2 C、Ti 3 C 2 、Ti 3 CN、V 2 C、Nb 2 C、TiNbC、Nb 4 C 3 、Ta 4 C 3 、(Ti 0.5 Nb 0.5 ) 2 C or (V) 0.5 Cr 0.5 ) 3 C 2 One kind of (1).
6. A method of making a printable transparent stress sensor according to any one of claims 1 to 5, comprising:
(1) Mixing the conductive nano material with a solvent, uniformly dispersing the conductive nano material by ultrasonic oscillation, and preparing a transparent conductive film on a glass substrate by a printing method;
(2) Taking two or more than two elastomer materials with larger modulus difference and close elongation at break, mixing the elastomer materials according to different proportions to obtain elastomer solutions or precursor solutions with different moduli as elastomer base materials;
(3) Spreading the elastomer solution or precursor solution obtained in the step (2) on the surface of the conductive film in sequence from high modulus to low modulus, heating to evaporate the solvent or curing to form an elastic matrix with modulus gradient, wherein the elastic matrix is embedded with the transparent conductive film;
(4) And (4) tearing the elastic matrix embedded with the transparent conductive film from the glass substrate in the step (3) to obtain the transparent stress sensor.
7. The printable transparent stress sensor and the manufacturing method thereof according to claim 6, wherein in the step (1), the printing method of the conductive film is as follows: screen printing, ink jet printing, blade coating, stencil printing, gravure printing, relief printing, offset printing, spin coating, dip coating, meyer rod coating, spray coating, slot coating, microcontact printing, direct writing printing.
8. A printable transparent stress sensor and method of manufacture according to claim 6 or 7, characterized by the following steps:
(1) Preparing a transparent conductive layer: selecting silver nanowires as a conductive nano material, dissolving the silver nanowires in ethanol, dispersing the silver nanowires uniformly by ultrasonic oscillation to obtain silver nanowire/ethanol dispersion liquid with the concentration of 2 mg/mL, weighing 100 muL of the silver nanowire/ethanol dispersion liquid, spin-coating the silver nanowire/ethanol dispersion liquid on a glass sheet by a printing method, wherein the rotating speed is 800 rpm, the spin-coating time is 15 s, heating is carried out at 60 ℃ for 1 min, and repeating the operation for 10 times to obtain a silver nanowire transparent conductive film of a glass substrate as an embedded structure;
(2) Respectively weighing the polyurethane 6210 and the polyurethane 6290 according to mass ratios of 1, 10, 1, 5, 1;
(3) Weighing 1g of polyurethane with different moduli obtained in the step (2), respectively mixing the polyurethane with 0.5g of acrylic acid (5-ethyl-1, 3-dioxane-5-yl) methyl ester and 0.15g of photoinitiator, uniformly stirring, centrifuging to remove bubbles, spin-coating the surface of the silver nanowire transparent conductive film obtained in the step (1) with the moduli from high to low in sequence, wherein the rotating speed is 900rpm, the spin-coating time is 60s, and carrying out ultraviolet curing for 3 min to obtain the film;
(4) And (4) peeling the film from the glass substrate in the step (3) to obtain the transparent stress sensor.
9. A printable transparent stress sensor and method of manufacture according to claim 6 or 7, characterized by the following steps:
(1) Preparing a transparent conductive layer: weighing 100 muL of MXene/water dispersion with the concentration of 10 mg/mL, printing on a glass sheet by using an ink-jet printer, heating at 60 ℃ for 1 min, and repeatedly operating for 5 times to obtain an MXene transparent conductive film of the glass substrate;
(2) Respectively weighing the following components in mass ratio of 1;
(3) Respectively weighing 4g of polyurethane obtained in the step (2), 2g of acrylic acid (5-ethyl-1, 3-dioxane-5-yl) methyl ester and 0.6g of photoinitiator, mixing the polyurethane, the acrylic acid (5-ethyl-1, 3-dioxane-5-yl) methyl ester and the photoinitiator, uniformly stirring, vacuumizing to remove bubbles, sequentially performing screen printing on the surface of the Mxene transparent conductive film obtained in the step (1) by using a screen printing plate according to the modulus from high to low, and performing ultraviolet curing for 5 min to obtain an elastic film with a modulus gradient and an embedded transparent conductive layer;
(4) And peeling off the glass substrate to obtain the transparent stress sensor.
10. A printable transparent stress sensor and method of manufacture according to claim 6 or 7, characterized by the following steps:
(1) Preparing a transparent conductive layer: weighing 100 muL of copper nanowire/water dispersion with the concentration of 5 mg/mL, carrying out blade coating on a glass sheet by using a Meyer rod, heating for 1 min at 60 ℃, and repeatedly operating for 5 times to obtain the copper nanowire transparent conductive film with the glass substrate.
(2) Respectively weighing polydimethylsiloxane PDMS part A and PDMS part B with the mass ratio of 10;
(3) Weighing 10g of PDMS obtained in the step (2), vacuumizing to remove bubbles, blade-coating the surface of the copper nanowire transparent conductive film obtained in the step (1) with a Meyer bar in sequence from high modulus to low modulus, and heating and curing at 60 ℃ for 2h to obtain an elastic film embedded with a transparent conductive layer and having modulus gradient;
(4) And peeling the film from the glass substrate to obtain the transparent stress sensor. The structure is shown in figure 1, and comprises a conductive layer and an elastic substrate, wherein the conductive layer is a transparent conductive layer 1 composed of conductive nano materials; the elastic substrate is three layers of elastic substrate layers with modulus gradient structures, namely a high-modulus elastic substrate layer 2, a medium-modulus elastic substrate layer 3 and a low-modulus elastic substrate layer 4.
11. A printable transparent stress sensor and method of manufacture according to claim 6 or 7, characterized by the following steps:
(1) Preparing a transparent conductive layer: weighing 100 mL of MXene/water dispersion with the concentration of 8 mg/mL, soaking a glass sheet in the water dispersion for 10 min, heating and drying at 80 ℃, and repeatedly operating for 7 times to obtain an Mxene transparent conductive film of a glass substrate as an embedding structure;
(2) Weighing 10 parts of PDMS part A and PDMS part B;
(3) Respectively weighing 5g of PDMS obtained in the step (2), sequentially performing screen printing on the surface of the MXene transparent conductive film obtained in the step (1) by using a screen printing plate according to the modulus from high to low, and heating at 80 ℃ for 1 h to obtain an elastic film embedded with the transparent conductive layer and having modulus gradient;
(4) And peeling the film from the glass substrate to obtain the transparent stress sensor.
12. A printable transparent stress sensor and method of manufacture according to claim 6 or 7, characterized by the following steps:
(1) Preparing a transparent conductive layer: preparing graphene/DMF dispersion liquid with the concentration of 6 mg/mL by using Dimethylformamide (DMF) as a solvent, weighing 10 mL of graphene/DMF dispersion liquid, performing screen printing on a glass sheet, heating and drying at 40 ℃, and repeatedly operating for 3 times to obtain the graphene transparent conductive film with the glass substrate;
(2) The following components are weighed according to the mass ratio of 1;
(3) Respectively weighing 2g of polyurethane obtained in the step (2), 1g of acrylic acid (5-ethyl-1, 3-dioxane-5-yl) methyl ester and 0.3g of photoinitiator, mixing the polyurethane, the acrylic acid (5-ethyl-1, 3-dioxane-5-yl) methyl ester and the photoinitiator, uniformly stirring, sequentially coating the surface of the graphene transparent conductive film obtained in the step (1) with a slit coating machine from high modulus to low modulus, and carrying out ultraviolet curing for 10 min to obtain an elastic film which is embedded with a transparent conductive layer and has modulus gradient;
(4) And peeling the film from the glass substrate to obtain the transparent stress sensor.
13. Use of the printable transparent stress sensor according to any of the claims 1 to 5, characterized by screen fingerprint unlocking for flexible touch screens, transparent wearable devices, or for detecting human body movement signals, including pulse beat type micro-deformation signals and finger or knee bend type macro-strain signals.
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