CN109764979B - Ion paper, ion electronic type flexible pressure sensor and preparation method thereof - Google Patents

Ion paper, ion electronic type flexible pressure sensor and preparation method thereof Download PDF

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Publication number
CN109764979B
CN109764979B CN201811551798.3A CN201811551798A CN109764979B CN 109764979 B CN109764979 B CN 109764979B CN 201811551798 A CN201811551798 A CN 201811551798A CN 109764979 B CN109764979 B CN 109764979B
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ionic
ion
liquid
paper
cellulose
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CN109764979A (en
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常煜
彭涛
李森
王连建
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Titanium Shenzhen Technology (Shenzhen) Co., Ltd.
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Tai Shen Technology Shenzhen Co ltd
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Priority to PCT/CN2018/123781 priority patent/WO2020124628A1/en
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    • BPERFORMING OPERATIONS; TRANSPORTING
    • B41PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41MPRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M1/00Inking and printing with a printer's forme
    • B41M1/12Stencil printing; Silk-screen printing
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B41PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41MPRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M5/00Duplicating or marking methods; Sheet materials for use therein
    • BPERFORMING OPERATIONS; TRANSPORTING
    • B41PRINTING; LINING MACHINES; TYPEWRITERS; STAMPS
    • B41MPRINTING, DUPLICATING, MARKING, OR COPYING PROCESSES; COLOUR PRINTING
    • B41M7/00After-treatment of prints, e.g. heating, irradiating, setting of the ink, protection of the printed stock
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H11/00Pulp or paper, comprising cellulose or lignocellulose fibres of natural origin only
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H19/00Coated paper; Coating material
    • D21H19/10Coatings without pigments
    • D21H19/14Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H19/00Coated paper; Coating material
    • D21H19/10Coatings without pigments
    • D21H19/14Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12
    • D21H19/20Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12 comprising macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • DTEXTILES; PAPER
    • D21PAPER-MAKING; PRODUCTION OF CELLULOSE
    • D21HPULP COMPOSITIONS; PREPARATION THEREOF NOT COVERED BY SUBCLASSES D21C OR D21D; IMPREGNATING OR COATING OF PAPER; TREATMENT OF FINISHED PAPER NOT COVERED BY CLASS B31 OR SUBCLASS D21G; PAPER NOT OTHERWISE PROVIDED FOR
    • D21H19/00Coated paper; Coating material
    • D21H19/10Coatings without pigments
    • D21H19/14Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12
    • D21H19/20Coatings without pigments applied in a form other than the aqueous solution defined in group D21H19/12 comprising macromolecular compounds obtained by reactions only involving carbon-to-carbon unsaturated bonds
    • D21H19/22Polyalkenes, e.g. polystyrene
    • GPHYSICS
    • G01MEASURING; TESTING
    • G01LMEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
    • G01L1/00Measuring force or stress, in general
    • G01L1/14Measuring force or stress, in general by measuring variations in capacitance or inductance of electrical elements, e.g. by measuring variations of frequency of electrical oscillators

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  • Chemical & Material Sciences (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Physics & Mathematics (AREA)
  • General Physics & Mathematics (AREA)
  • Compositions Of Macromolecular Compounds (AREA)

Abstract

The invention provides ion paper which is made of a cellulose-reinforced ion gel composite material, wherein the cellulose-reinforced ion gel composite material comprises a liquid ion material, a polymer and cellulose, and the weight percentages of the liquid ion material, the polymer and the cellulose are as follows, wherein the total weight of the cellulose-reinforced ion gel composite material is 100 percent: 1-80% of a liquid ionic material; 1-80% of a polymer; 19-80% of cellulose, wherein the cellulose is selected from papermaking cellulose. The cellulose-reinforced ionic gel composite material is used as a preparation raw material of the ionic paper, so that the ionic paper is endowed with excellent ion conductivity, shearability, printability and foldability, and the obtained ionic paper can be used as a functional material of a flexible pressure sensor to prepare the flexible pressure sensor with high sensitivity and foldability.

Description

Ion paper, ion electronic type flexible pressure sensor and preparation method thereof
Technical Field
The invention belongs to the technical field of sensors, and particularly relates to ion paper and a preparation method of an ion electronic type flexible pressure sensor made of an ion gel composite material.
Background
Because people expect the bionic touch sensing technology more strongly in the application fields of future intelligent robot technology, medical artificial limbs, nerve repair, consumer electronics and the like, the research on novel portable, foldable, attachable and wearable flexible electronic devices is widely concerned by researchers at home and abroad and quickly becomes one of the most important science and technology frontier research fields at present. For the needs of these emerging applications, flexible materials have gained intense attention and widespread use by researchers with their good adaptability to different surface materials and shapes. Therefore, flexible pressure sensing technology has been developed, and various flexible pressure sensing technologies and devices have been developed, and have been applied to wearable medical health monitoring equipment, robot bionic touch, touch artificial limb and other fields.
The traditional non-flexible pressure sensing element adopts non-bendable materials such as a metal cantilever beam and a silicon-based stress sheet. Different from the flexible pressure sensor, a polymer film, a fiber structure material, and the like are often used as a material for constructing the sensor. The flexible pressure sensor mainly comprises an electrode and a functional material layer, wherein the electrode is made of high-conductivity metal, conductive carbon material, conductive ceramic material and conductive polymer material, and forms a specific circuit pattern. The functional material layer mainly includes a conductor material, a dielectric material, a piezoelectric material, a triboelectric material, an ionic material, etc. according to different mechanisms, and the corresponding flexible sensing mechanisms are also mainly classified into piezoresistive type, parallel plate capacitive type, piezoelectric type, triboelectric type, and ion type.
The off-electronic pressure sensor is a novel pressure sensing technology based on the principle of interface double-electric-layer capacitance. Such pressure sensors use materials rich in freely mobile anions and cations, such as high boiling point solutions of electrolytes, ionic liquids, polyelectrolytes, ionic liquid gels, and the like. When a voltage is applied to the ionic material, positive ions and negative ions in the ionic material rapidly move towards the two poles under the action of an electric field, and compact charge layers, namely electric double layers, are formed on the surfaces of the two electrodes respectively. The double electric layers are a nano-scale capacitor structure formed by ion arrangement, and the capacitance per unit area is more than 1000 times that of the traditional parallel plate capacitor because the distance between positive ions and negative ions is extremely short. For the same ion material, the interface capacitance is mainly in positive correlation with the contact area between the electrode and the ion material, and according to the point, the ion type pressure sensor increases the contact area between the ion material and the electrode under the action of pressure, and the sensor capacitance is correspondingly increased. The interface capacitance type pressure sensing mechanism is a brand new sensing mechanism different from the existing resistance type, capacitance type and piezoelectric type sensing. Because the value of interface capacitance can reach hundreds of nF or even uF level, compared with a parallel plate capacitive sensor with dozens of pF, the sensitivity of the sensor is improved by more than 1000 times, and the sensor has strong anti-interference capability on capacitance noise of human bodies and environments. Compared with a piezoresistive pressure sensor, the interface capacitive pressure sensor has better linear responsivity in a certain pressure range and higher signal-to-noise ratio, and compared with conductive materials such as graphene and carbon nanotubes, the ionic material can be prepared into the forms of solution, ink, slurry and the like, and can be prepared into an ionic material layer more conveniently through various processing modes such as dip coating, blade coating, ink jetting, printing and the like. Compared with piezoelectric and triboelectric pressure sensors, the interface capacitance type pressure sensor can detect static pressure while having quick mechanical response speed. The off-electronic pressure sensing technology has developed various forms, including various flexible pressure sensing forms based on polymer films, nano fabrics, ionic gel elastomers, surface-applied ultrathin coatings and the like. However, although the linear responsivity of the current electronic pressure sensor is greatly improved compared with that of the piezoresistive pressure sensor, the distance is completely linear and has a certain difference, and in addition, the sensor is also insufficient in the aspect of foldability.
Disclosure of Invention
The invention aims to provide ion paper, and aims to solve the problem that the response linearity and foldability of the conventional off-electronic pressure sensor are insufficient.
The invention also aims to provide a preparation method of the ion-electron type flexible pressure sensor made of the ion gel composite material.
In order to achieve the purpose, the invention adopts the following technical scheme:
the invention provides an ion paper, which is made of a cellulose-reinforced ion gel composite material, wherein the cellulose-reinforced ion gel composite material comprises a liquid ion material, a polymer and cellulose, and the weight percentages of the liquid ion material, the polymer and the cellulose are as follows, based on 100 percent of the total weight of the cellulose-reinforced ion gel composite material:
1-80% of a liquid ionic material;
1-80% of a polymer;
19 to 80 percent of cellulose,
wherein the cellulose is selected from papermaking cellulose, and the polymer is selected from polymers capable of forming gel materials with the liquid ionic material.
The invention provides an ion-electron type flexible pressure sensor, which is a foldable flexible pressure sensor and comprises an electrode area and an ion area, wherein at least the ion area is made of a cellulose reinforced ion gel composite material, the cellulose reinforced ion gel composite material comprises a liquid ion material, a polymer and cellulose, and the weight percentages of the liquid ion material, the polymer and the cellulose are as follows, wherein the total weight of the cellulose reinforced ion gel composite material is 100 percent:
1-80% of a liquid ionic material;
1-80% of a polymer;
19 to 80 percent of cellulose,
wherein the cellulose is selected from papermaking cellulose, and the polymer is selected from polymers capable of forming gel materials with the liquid ionic material.
The third aspect of the present invention provides a method for manufacturing an off-electronic flexible pressure sensor, including the steps of:
providing an ion paper substrate, and preparing a patterned electrode on the ion paper substrate according to a preset electrode pattern, wherein the ion paper substrate is the ion paper;
arranging an adhesive at the designed part of the ion paper substrate, and folding the ion paper substrate to ensure that the ion area and the electrode area are attached face to form a preset electrode pattern, so as to obtain the foldable electronic flexible pressure sensor; or
The preparation method of the flexible pressure sensor comprises the following steps:
providing a paper substrate made of cellulose materials, printing electrode materials in a preset electrode area of the paper substrate according to a preset electrode pattern, and printing ion ink in a preset ion area of the paper substrate to form an electrode area and an ion area; wherein the ionic ink contains a liquid ionic material, a polymer, and an additive;
and arranging an adhesive at the designed part of the paper substrate, and folding the paper substrate to ensure that the ion area and the electrode area are attached face to form a preset electrode pattern, thereby obtaining the foldable electronic flexible pressure sensor.
The ionic paper provided by the invention is made of a cellulose-reinforced ionic gel composite material, and the cellulose-reinforced ionic gel composite material comprises a liquid ionic material, a polymer and cellulose. The liquid ionic material is used as a matrix functional material, and the ionic paper is endowed with excellent ion conduction performance; the polymer is used for fixing the liquid ionic material in the ionic paper and preventing the liquid ionic material from diffusing or separating out; the introduction of the cellulose provides a fibrous microstructure, provides a rough surface for sensing pressure changes when the ionic paper is used as a sensor, and simultaneously endows the ionic paper with excellent folding performance. In addition, the ionic paper prepared by using the liquid ionic material, the polymer and the cellulose as raw materials according to the proportion requirement has good response linearity.
In conclusion, the cellulose-reinforced ionic gel composite material is used as a raw material for preparing the ionic paper, so that the ionic paper can be endowed with excellent ion conductivity, printability, weather resistance, foldability and response linearity, and the obtained ionic paper can be used as a functional material of a flexible pressure sensor to prepare the foldable, shearable and printable flexible pressure sensor.
The ion-electron type flexible pressure sensor provided by the invention comprises an electrode area and an ion area, wherein at least the ion area is made of the ion paper. Since the ion paper has excellent ion conductivity, shearability, printability and foldability, foldability and sensitivity of the flexible pressure sensor can be improved.
According to the preparation method of the ion-electron type flexible pressure sensor, provided by the invention, the ion paper is directly used as the substrate to prepare the patterned electrode, and then folding treatment is carried out; or firstly respectively depositing an electrode material and ionic ink containing a liquid ionic material, a polymer and an additive on a paper substrate made of a cellulose material, forming an electrode area and an ion area, and then carrying out folding treatment, thereby not only endowing the obtained flexible pressure sensor with excellent foldability, but also having higher sensitivity. In addition, by the method, the two-dimensional or multi-dimensional flexible pressure sensor can be prepared by folding.
Drawings
FIG. 1 is a schematic flow chart illustrating a process for manufacturing a first flexible pressure sensor according to an embodiment of the present invention;
FIG. 2 is a schematic flow chart illustrating a manufacturing process of a second flexible pressure sensor according to an embodiment of the present invention;
FIG. 3 is a pressure-capacitance curve diagram of a two-dimensional ion-electron type flexible pressure sensor provided in embodiment 1 of the present invention;
fig. 4 is a schematic diagram of a three-dimensional off-electronic flexible pressure sensor according to embodiment 2 of the present invention.
Detailed Description
In order to make the technical problems, technical solutions and advantageous effects to be solved by the present invention more clearly apparent, the present invention is further described in detail below with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
In the description of the present invention, it is to be understood that the terms "first", "second" and the like are used for descriptive purposes only and are not to be construed as indicating or implying relative importance or implying any number of technical features indicated. Thus, a feature defined as "first" or "second" may explicitly or implicitly include one or more of that feature. In the description of the present invention, "a plurality" means two or more unless specifically defined otherwise.
The paper is an aggregate material with natural cellulose or artificial cellulose as a main component, and has the characteristics of special fibrous microstructure, degradability, high biocompatibility and low cost. In addition, paper also has a variety of properties not completely possessed by other materials, such as printability, cuttability, bondability, and foldability. In view of this, it is preferable that,
the first aspect of the embodiments of the present invention provides an ion paper, where the ion paper is made of a cellulose-reinforced ion gel composite material, the cellulose-reinforced ion gel composite material includes a liquid ion material, a polymer, and cellulose, and the liquid ion material, the polymer, and the cellulose are in the following weight percentages, where the total weight of the cellulose-reinforced ion gel composite material is 100%:
1-80% of a liquid ionic material;
1-80% of a polymer;
19 to 80 percent of cellulose,
wherein the cellulose is selected from papermaking cellulose, and the polymer is selected from polymers capable of forming gel materials with the liquid ionic material.
The ionic paper provided by the embodiment of the invention is made of a cellulose-reinforced ionic gel composite material, and the cellulose-reinforced ionic gel composite material comprises a liquid ionic material, a polymer and cellulose. The liquid ionic material is used as a matrix functional material, and the ionic paper is endowed with excellent ion conduction performance; the polymer is used for fixing the liquid ionic material in the ionic paper and preventing the liquid ionic material from diffusing or separating out; the introduction of the cellulose provides a fibrous microstructure, provides a rough surface for sensing pressure changes when the ionic paper is used as a sensor, and simultaneously endows the ionic paper with excellent folding performance. In addition, the ionic paper prepared by using the liquid ionic material, the polymer and the cellulose as raw materials according to the proportion requirement has good response linearity.
In conclusion, the cellulose-reinforced ionic gel composite material is used as a raw material for preparing the ionic paper, so that the ionic paper can be endowed with excellent ion conductivity, printability, shearability, foldability and response linearity, and the obtained ionic paper can be used as a functional material of a flexible pressure sensor to prepare the foldable, shearable and printable flexible pressure sensor.
Specifically, the liquid ionic material is used as a matrix functional material, and the ionic paper is endowed with excellent ion conductivity, so that a functional guarantee is provided for preparing the ion-electron type pressure sensor by adopting the ionic paper. In some embodiments, the liquid ionic material is selected from at least one of an ionic liquid, an ionic liquid solution, and a solid electrolyte solution, and a solvent in the ionic liquid solution or the solid electrolyte solution is retained in the ionic paper.
Specifically, the ionic liquid is an ionic compound which is in a liquid state at the temperature of 10-35 ℃. In some embodiments, the ionic liquid may be selected from at least one of imidazole ionic liquid, quaternary ammonium salt ionic liquid, pyridine ionic liquid, pyrrole ionic liquid and piperidine ionic liquid, but is not limited thereto. The preferred ionic liquid type is liquid at normal temperature (10-35 ℃) and has better ion conductivity, so that the obtained ionic paper can effectively play the function when being used as an off-electronic sensor.
The ionic liquid high-boiling-point organic solution is a solution formed by dissolving an ionic liquid in a high-boiling-point high-polarity organic solvent (which can be understood as adding high-boiling-point high-polarity organic solvents with different content to the ionic liquid to form a corresponding ionic liquid solution), and the high-boiling-point high-polarity organic solvent is an organic solvent which has a boiling point of not less than 200 ℃ and contains at least one of hydroxyl, amino, ester, amide and carboxyl in a molecular structure. In this case, the high-boiling point and high-polarity organic solvent has a high boiling point and is not easily volatilized, and since the solvent has a large polarity, the ionic compound having a large polarity per se can be effectively dissolved. In some embodiments, in the ionic liquid solution, the ionic liquid is at least one selected from imidazole ionic liquids, quaternary ammonium salt ionic liquids, pyridine ionic liquids, pyrrole ionic liquids, and piperidine ionic liquids; the high-boiling-point high-polarity organic solvent is at least one selected from dibutyl phthalate, tributyl citrate, N-methyl pyrrolidone, dimethyl sulfoxide, glycerol and ethylene glycol. The preferred ionic liquid type is liquid at normal temperature (10-35 ℃) and has better ion conductivity, so that the obtained ionic paper can effectively play the function when being used as an off-electronic sensor. The preferable organic solvent type has good solubility to the ionic liquid, and more importantly, the organic solvent has a high boiling point and is not easy to volatilize, and the organic solvent can be properly retained in the ionic paper when the ionic paper is prepared and used as an ion conduction medium, so that the ion conduction effect of the ionic liquid is further improved. More preferably, the weight percentage of the ionic liquid is 50-70% and the weight percentage of the high-boiling point and high-polarity organic solvent is 30-50% based on 100% of the total weight of the ionic liquid solution, and in this case, the prepared ionic paper has more excellent ion conductivity.
The solid electrolyte high-boiling-point organic solution is a solution formed by an ionic compound which is in a solid state at the temperature of 10-35 ℃ in a high-boiling-point high-polarity organic solvent, and the high-boiling-point high-polarity organic solvent has a boiling point of not less than 200 ℃ and contains at least one of hydroxyl, amido, ester, amido and carboxyl in a molecular structure. In this case, the high-boiling point and high-polarity organic solvent has a high boiling point and is not easily volatilized, and since the solvent has a large polarity, the ionic compound having a large polarity per se can be effectively dissolved. In some embodiments, in the solid electrolyte solution, the ionic compound is selected from at least one of a small molecule electrolyte (non-polymer small molecule electrolyte), a polymer electrolyte; the high-boiling-point high-polarity organic solvent is at least one selected from dibutyl phthalate, tributyl citrate, N-methyl pyrrolidone, dimethyl sulfoxide, glycerol and ethylene glycol. The preferable organic solvent type has good solubility to the ionic compound, and more importantly, the organic solvent has high boiling point and is not easy to volatilize, and the organic solvent can be properly retained in the ionic paper when the ionic paper is prepared and used as an ion conduction medium to further improve the ion conduction effect of the ionic compound. More preferably, the weight percentage of the ionic compound is 50-70% and the weight percentage of the high-boiling point and high-polarity organic solvent is 30-50% based on 100% of the total weight of the solid electrolyte and high-boiling point organic solution, and then the prepared ion paper has more excellent ion conductivity.
In the embodiment of the present invention, the weight percentage of the liquid ionic material is 1% to 80%, specifically 1%, 5%, 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, and 80%, based on 100% of the total weight of the cellulose-reinforced ionic gel composite material.
The polymer is used to fix the liquid ionic material in the ionic paper, preventing it from diffusing or leaching out. Particularly, when the ionic paper is used as a base material of the flexible pressure sensor of the ion-electron type, under the action of the polymer, the liquid ionic material and the polymer form gel to be fixed, so that the ionic material cannot be diffused or separated out, and the problem that the sensitivity of the flexible pressure sensor of the ion-electron type is reduced due to the fact that the content of the liquid ionic material is reduced after the liquid ionic material is diffused to an electrode area or separated out is solved. In addition, the polymer can fix the liquid ionic material, so that the safety of the ionic paper (some liquid ionic materials have certain toxicity) can be improved, and further, when the ionic paper is used for the ion-electron type flexible sensor, the weather resistance of the ion-electron type flexible sensor is improved. In an embodiment of the present invention, the polymer is selected from polymers capable of forming a gel material with the liquid ionic material.
Specifically, the polymer is selected from at least one of hydroxyl, carboxyl, amide, amino, nitro, halogen atoms, ester, cyano and carbamate contained in the polymer monomer. The polymer formed by the monomer containing the active functional group has stronger polarity and has better fixation effect on the liquid ionic material.
In some embodiments, the polymer is selected from at least one of polyvinyl alcohol, polyurethane, polyamide, polyvinylidene fluoride, polyacrylate. The polymer has stronger polarity, can be combined with a liquid ionic material, and restrains the liquid ionic material from being diffused, transferred or separated out in the ionic paper.
In a preferred embodiment, the polymer is selected to have better stability and better match with the liquid ionic material during gel formation, depending on the solubility of the liquid ionic material used. In some embodiments, a glycerol solution of a hydrophilic liquid ionic material lithium hexafluorophosphate is preferably combined with polyvinyl alcohol to form a gel, a dibutyl phthalate solution of hydrophobic lithium trifluoromethanesulfonate is preferably combined with a polyacrylate polymer to form a gel, and a liquid ionic material 1-butyl-3-methylimidazolium trifluoromethanesulfonate having moderate hydrophilicity and hydrophobicity is preferably combined with a polyurethane polymer to form a gel. The polyvinyl alcohol contains hydroxyl, the polyurethane contains a carbamate group, the polyamide contains an amide group, the polyvinylidene fluoride contains a halogen atom group, and the polyacrylate contains an ester group. The combination of the preferable combinations has better matching property with each other, thereby forming gel and obtaining the gel with better stability.
In the embodiment of the present invention, the weight percentage of the polymer is 1% to 80%, specifically 1%, 5%, 10%, 15%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, and 80%, based on 100% of the total weight of the cellulose-reinforced ionic gel composite.
In the embodiment of the invention, another important raw material of the ion paper is cellulose, and the cellulose can be natural cellulose or artificial cellulose. It is noted that the cellulose must be papermaking cellulose, so that the formed ion paper has high biocompatibility, degradability, printability, shearability, bondability and foldability. In particular, the introduction of the cellulose can form the ion paper with a fibrous microstructure on the surface, so that the ion paper can effectively sense when being used as a sensor material.
In some embodiments, the cellulose may be selected from, but not limited to, tree plant fibers, bast fibers, mineral fibers, synthetic papermaking fibers, and the like, preferably tree plant fibers.
In the embodiment of the present invention, the weight percentage of the cellulose is 19% to 80%, specifically 19%, 20%, 25%, 30%, 35%, 40%, 45%, 50%, 55%, 60%, 65%, 70%, 75%, and 80%, based on 100% of the total weight of the cellulose-reinforced ionic gel composite material. If the weight of the cellulose is too low, the obtained ion paper is not obvious in pressure change sensing when used as a sensor material due to insufficient surface roughness, so that the comprehensive performance of the sensor is reduced. As a preferred embodiment, the weight percentage of the cellulose is 20-50% based on 100% of the total weight of the cellulose-reinforced ionic gel composite material, and the obtained ionic paper has good sensitivity, high resolution and high response speed when used as a sensor material.
In a second aspect, the present invention provides an ion-electron type flexible pressure sensor, which is a foldable flexible pressure sensor and includes an electrode region and an ion region, wherein at least the ion region is made of a cellulose-reinforced ionic gel composite material, and the cellulose-reinforced ionic gel composite material includes a liquid ionic material, a polymer and cellulose, and the weight percentages of the liquid ionic material, the polymer and the cellulose are as follows, based on 100% of the total weight of the cellulose-reinforced ionic gel composite material:
1-80% of a liquid ionic material;
1-80% of a polymer;
19 to 80 percent of cellulose,
wherein the cellulose is selected from papermaking cellulose, and the polymer is selected from polymers capable of forming gel materials with the liquid ionic material.
The ion-electron type flexible pressure sensor provided by the embodiment of the invention is a foldable ion-electron type pressure sensor and comprises an electrode area and an ion area, wherein at least the ion area is made of the ion paper. Since the ion paper has excellent ion conductivity, shearability, printability and foldability, foldability and sensitivity of the flexible pressure sensor can be improved.
In some embodiments, the flexible pressure sensor of the foldable-release electronic type includes an ionomeric paper substrate and a patterned electrode bonded to the ionomeric paper substrate. The region where the patterned electrode is located forms an electrode region, and the region outside the patterned electrode forms an ion region. Further, the ion region and the electrode region are folded oppositely to form a folding flexible pressure sensor.
In some embodiments, the foldable-ion electronic flexible pressure sensor includes a paper substrate, and patterned electrodes formed on the paper substrate, and a patterned ionic paper pattern bonded to the paper substrate and outside of the patterned electrodes. Further, the ion region and the electrode region are folded oppositely to form a folding flexible pressure sensor.
In the embodiment of the invention, the cellulose-reinforced ionic gel composite material is the material for preparing the ionic paper. Wherein, the selection of the liquid ionic material, the polymer and the cellulose is the same as that of the ionic paper.
Specifically, the liquid ionic material is selected from at least one of ionic liquid, ionic liquid high boiling point organic solution and solid electrolyte high boiling point organic solution, wherein,
the ionic liquid is an ionic compound which is in a liquid state at the temperature of 10-35 ℃;
the ionic liquid high-boiling-point organic solution is formed by dissolving ionic liquid in a high-boiling-point high-polarity organic solvent, and the high-boiling-point high-polarity organic solvent has a boiling point of not less than 200 ℃ and contains at least one of hydroxyl, amido, ester, amido and carboxyl in a molecular structure;
the solid electrolyte high-boiling-point organic solution is a solution formed by an ionic compound which is in a solid state at the temperature of 10-35 ℃ in a high-boiling-point high-polarity organic solvent, and the high-boiling-point high-polarity organic solvent has a boiling point of not less than 200 ℃ and contains at least one of hydroxyl, amido, ester, amido and carboxyl in a molecular structure.
Preferably, the ionic liquid solution is at least one selected from imidazole ionic liquids, quaternary ammonium salt ionic liquids, pyridine ionic liquids, pyrrole ionic liquids and piperidine ionic liquids.
Preferably, in the ionic liquid solution, the ionic liquid is at least one selected from imidazole ionic liquid, quaternary ammonium salt ionic liquid, pyridine ionic liquid, pyrrole ionic liquid and piperidine ionic liquid; the high-boiling-point high-polarity organic solvent is at least one selected from dibutyl phthalate, tributyl citrate, N-methyl pyrrolidone, dimethyl sulfoxide, glycerol and ethylene glycol.
Preferably, in the solid electrolyte solution, the ionic compound is at least one selected from small molecule electrolyte and polymer electrolyte; the high-boiling-point high-polarity organic solvent is at least one selected from dibutyl phthalate, tributyl citrate, N-methyl pyrrolidone, dimethyl sulfoxide, glycerol and ethylene glycol.
In particular, the polymer is selected from polymers capable of forming a gel material with the liquid ionic material.
Preferably, the polymer is selected from at least one of hydroxyl, carboxyl, amide, amino, nitro, halogen atoms, ester, cyano and carbamate contained in the polymer monomer.
Preferably, the polymer is at least one selected from polyvinyl alcohol, polyurethane, polyamide, polyvinylidene fluoride and polyacrylate.
The off-electronic flexible pressure sensor provided by the embodiment of the invention has the advantages of high sensitivity, high signal-to-noise ratio, high anti-interference performance and the like of an off-electronic flexible pressure sensing mechanism, and also has the characteristics of low cost, high biocompatibility, degradability, printability, shearability, bondability and foldability of paper.
The off-electronic flexible pressure sensor provided by the embodiment of the invention can be prepared by the following method.
In one embodiment, as shown in fig. 1 and 3, the method for manufacturing the ion-beam flexible pressure sensor comprises the following steps:
s01, providing an ion paper base material, and preparing a patterned electrode on the ion paper base material according to a preset electrode pattern, wherein the ion paper base material is the ion paper provided by the embodiment of the invention;
and S02, arranging an adhesive at the designed part of the ion paper substrate, and folding the ion paper substrate to ensure that the ion area and the electrode area are attached face to form a preset electrode pattern, so as to obtain the foldable flexible pressure sensor.
Specifically, in step S01, the ion paper substrate is the ion paper according to the embodiment of the present invention, and can be prepared by various methods.
In some embodiments, the method of making the ionic paper substrate is:
s111, weighing the components according to the formula of the ionic paper, and dispersing the liquid ionic material, the polymer and the cellulose in water or an organic solvent to form slurry.
Specifically, the formula of the ion paper is as described above, and is not repeated here for saving space.
After weighing the formulation components, the ionic material, polymer and cellulose in liquid form are dispersed in water or an organic solvent to form a slurry containing the ionic material. Wherein the organic solvent is an organic solvent capable of dispersing the liquid ionic material, the polymer and the cellulose, and in some embodiments, the organic solvent is selected from alcohols, sulfones, amides, esters, and the like.
S112, depositing the slurry on the surface of a substrate, drying to remove the solvent, and stripping the formed ionic paper from the substrate.
And depositing the slurry on the surface of a substrate, drying to remove the solvent, and stripping the formed film layer from the substrate to obtain the ion paper substrate. Wherein, the solvent can be removed by heating.
The method for forming the ionic paper base material by depositing the slurry on the surface of the base has various modes, and in some specific embodiments, the slurry is directly coated on the surface of the base, and after drying and removing the solvent, the formed film layer is peeled off from the base, so that the ionic paper base material is obtained. In some embodiments, the cellulosic fibers are scooped from the slurry using a screen to form a layer of cellulosic slurry on the screen, and the desired ionomeric paper material is obtained after heating to evaporate the dry solvent and then stripping off the screen.
In some embodiments, the method of making the ionic paper substrate is:
s211, dissolving a liquid ionic material and a polymer in water or an organic solvent to form slurry, and preparing the slurry into a liquid ionic coating.
In the embodiment of the invention, the liquid ionic material and the polymer are dissolved in water or an organic solvent according to a ratio of 1-80: 1-80 to form slurry. Further, depositing the slurry on a substrate to form a liquid ionic coating.
S212, providing a paper substrate made of cellulose materials, soaking the paper substrate into the liquid-state ion coating, and drying to remove the solvent to prepare the ion paper.
In the embodiment of the invention, the paper substrate of the cellulose material is dipped into the liquid ion coating, that is, the cellulose material of the paper substrate can be dipped into the liquid ion coating, so that the coating contains a certain content of the cellulose material, and finally, the ion paper with the paper property is formed.
Specifically, the method for dipping the paper substrate into the liquid ion coating can be as follows: soaking a paper base material of a cellulose material into the ionic coating by a dip coating method, uniformly pulling, and heating to volatilize the solvent to obtain the required ionic paper material.
Wherein, the solvent can be removed by heating.
In some embodiments, the method of making the ionic paper substrate is:
dissolving a liquid ionic material, a polymer and an additive in water or an organic solvent to form ionic ink, printing the ionic ink on a paper substrate made of a cellulose material, and drying to remove the solvent to prepare the ionic paper.
Wherein, the additive is an additive capable of improving the performance of the film layer, and comprises but is not limited to a defoaming agent and a leveling agent; the deposition method includes but is not limited to conventional deposition methods such as screen printing, ink-jet printing, blade coating, etc.; drying to remove the solvent may be by heating.
After providing the ionized paper substrate, preparing a patterned electrode on the ionized paper substrate according to a preset electrode pattern. Specifically, the conductive material for preparing the patterned electrode may be selected from, but not limited to, at least one of conductive silver paste, conductive carbon paste, nano-silver conductive ink, and conductive polymer ink.
After the patterned electrode is prepared on the ionized paper substrate, forming an electrode area in the area where the patterned electrode is located; the regions other than the electrodes are patterned to form ion regions.
In the step S02, an adhesive is disposed on the designed portion of the ion paper substrate, in the embodiment of the present invention, the designed portion is understood as a functional region where the sensor performs a sensing function, and if the area of the sensor is large, the adhesive is disposed inside the sensor at a gap portion except for the one-turn position of the edge of the sensor, so as to ensure the tight adhesion of the sensor after the bonding and packaging. In some embodiments, the adhesive is a liquid adhesive, and the liquid adhesive is deposited on the designed part of the paper substrate; in some embodiments, the adhesive is a double-sided tape, and in this case, the double-sided tape is directly adhered to the design portion of the paper substrate.
Further, the ion paper substrate is folded through an adhesive, so that the ion area and the electrode area are attached to each other in a face-to-face mode to form a preset electrode pattern, and the foldable flexible pressure sensor is obtained. Of course, it should be understood that, according to the design of the off-electronic flexible pressure sensor, a special folding design can be performed, and a three-dimensional folding structure with a pressure sensing function on the surface can be obtained.
As shown in fig. 2, the method for manufacturing the flexible pressure sensor includes the following steps:
D01. providing a paper substrate made of cellulose materials, printing electrode materials in a preset electrode area of the paper substrate according to a preset electrode pattern, and printing ion ink in a preset ion area of the paper substrate to form an electrode area and an ion area; wherein the ionic ink contains a liquid ionic material, a polymer, and an additive;
D02. and arranging an adhesive at the designed part of the paper substrate, and folding the paper substrate to ensure that the ion area and the electrode area are attached face to form a preset electrode pattern, thereby obtaining the foldable flexible pressure sensor.
Specifically, in the step D01, the paper substrate made of the cellulose material is conventional paper. According to a preset electrode pattern, printing an electrode material on a preset electrode area of the paper substrate, and printing ion ink on a preset ion area of the paper substrate to form an electrode area and an ion area. Electrode materials used for printing the electrode patterns include, but are not limited to, conductive silver paste, conductive carbon paste, nano-silver conductive ink and conductive polymer ink; the ionic ink used for printing the ionic region is an aqueous solution of a liquid ionic material and a polymer or an organic solution of the liquid ionic material and the polymer. In the organic solution of the liquid ionic material and the polymer, the organic solvent is selected from organic solvents capable of dissolving the liquid ionic material and the polymer, and includes, but is not limited to, alcohols, sulfones, amides, esters, and the like. Furthermore, the ionic ink also contains additives, namely the ionic ink contains a liquid ionic material, a polymer and additives. The additive is an additive capable of improving the performance of the film layer, and includes but is not limited to an antifoaming agent and a leveling agent.
Printing an electrode material on a preset electrode area of the paper substrate, and printing ionic ink on a preset ion area of the paper substrate, wherein the printing method comprises but is not limited to screen printing, ink-jet printing and blade coating, and drying after printing to remove a solvent.
Then, the ion ink is printed on the surface of the conventional paper material by the printing modes such as silk screen printing, ink jet printing and the like, and after the solvent is heated and volatilized, the required ion pattern area is obtained.
In the step D02, an adhesive is disposed on the designed portion of the paper substrate, in the embodiment of the present invention, the designed portion is understood as a functional area where the sensor performs a sensing function, and if the area of the sensor is large, the adhesive is disposed inside the sensor at a gap portion except for the one-circle position of the edge of the sensor, so as to ensure that the sensor is tightly attached after being bonded and packaged. In some embodiments, the adhesive is a liquid adhesive, and the liquid adhesive is deposited on the designed part of the paper substrate; in some embodiments, the adhesive is a double-sided tape, and in this case, the double-sided tape is directly adhered to the design portion of the paper substrate.
Further, the paper substrate is folded through an adhesive, so that the ion area and the electrode area are attached to each other in a face-to-face mode to form a preset electrode pattern, and the foldable flexible pressure sensor is obtained. Of course, it should be understood that, according to the design of the off-electronic flexible pressure sensor, a special folding design can be performed, and a three-dimensional folding structure with a pressure sensing function on the surface can be obtained.
According to the preparation method of the flexible pressure sensor, provided by the embodiment of the invention, the ion paper is directly used as the substrate to prepare the patterned electrode, and then folding treatment is carried out; or firstly respectively depositing an electrode material and ionic ink containing a liquid ionic material, a polymer and an additive on a paper substrate made of a cellulose material, forming an electrode area and an ion area, and then carrying out folding treatment, so that the obtained flexible pressure sensor is endowed with excellent foldability, and has better weather resistance and higher sensitivity. In addition, by the method provided by the embodiment of the invention, the two-dimensional or multi-dimensional flexible pressure sensor can be prepared by folding.
The following description will be given with reference to specific examples.
Example 1
A preparation method of a foldable off-electronic flexible pressure sensor comprises the following steps:
uniformly mixing 1-butyl-3-methylimidazole bistrifluoromethanesulfonimide salt ionic liquid, polyvinylidene fluoride and azomethylpyrrolidone in a mass ratio of 1:2:20 to prepare an ionic coating;
immersing the dust-free paper into the ionic coating, uniformly lifting at a speed of 1mm/s, and then placing the dust-free paper on the surface of the flexible polyester film;
placing the dust-free paper dipped with the ionic coating in a blast oven, drying for 3 hours at the temperature of 100 ℃, and taking out to obtain ionic paper;
conducting screen printing conductive silver paste on a designed area on the surface of the ion paper to form a specific electrode pattern;
adhering a pressure-sensitive double-sided adhesive to a design area on the surface of the ion paper; folding the ion paper to enable the electrodes/the ion paper/the electrodes to be in face-to-face contact with each other to form a sandwich structure;
and leading the electrodes out to a test circuit through the anisotropic conductive adhesive tape to obtain the required two-dimensional ion-electron type flexible pressure sensor.
The two-dimensional ion-electron type flexible pressure sensor prepared in example 1 was subjected to a performance test, and a pressure-capacitance curve thereof is shown in fig. 3. As can be seen from fig. 3, the two-dimensional ion-electron type flexible pressure sensor prepared in example 1 has excellent response linearity.
Example 2
A preparation method of a foldable off-electronic flexible pressure sensor comprises the following steps:
1-ethyl-3-methylimidazole hexafluoromethanesulfonate ionic liquid, polyether polyurethane 75A, fumed silica and dimethyl sulfoxide are mixed according to a mass ratio of 1:1: 0.1: 6, preparing the ionic ink;
at 80g/m2Printing conductive carbon paste on the design area through a screen printing method to obtain an interdigital electrode pattern and form an electrode area; at 80g/m2Printing ion ink on the design area by a screen printing method to form an ion area;
at 80g/m2Printing a pressure-sensitive acrylic adhesive emulsion on the design area by a screen printing method to form an adhesive area; placing the printed paper in a blast oven, and drying for 3 hours at the temperature of 100 ℃;
through folding, the electrode area is in face-to-face contact with the ion area to form a pressure sensing unit; through special folding design, a three-dimensional folding structure with a pressure sensing function on the surface can be obtained.
The two-dimensional ion-electron type flexible pressure sensor prepared in example 2 is shown in fig. 4.
Example 3
A preparation method of a foldable off-electronic flexible pressure sensor comprises the following steps:
uniformly mixing 1-butyl-3-methylimidazole bis (trifluoromethanesulfonimide) salt ionic liquid, polyvinyl alcohol, natural poplar cellulose and water in a mass ratio of 1:2:3:150 to prepare slurry;
coating the slurry on a substrate, drying for 3 hours in a blast oven at the temperature of 100 ℃, and taking out to obtain the ion paper;
conducting screen printing conductive silver paste on a designed area on the surface of the ion paper to form a specific electrode pattern;
adhering a pressure-sensitive double-sided adhesive to a design area on the surface of the ion paper; folding the ion paper to enable the electrodes/the ion paper/the electrodes to be in face-to-face contact with each other to form a sandwich structure;
and leading the electrodes out to a test circuit through the anisotropic conductive adhesive tape to obtain the required two-dimensional ion-electron type flexible pressure sensor.
Example 4
A preparation method of a foldable off-electronic flexible pressure sensor comprises the following steps:
uniformly mixing a 10 wt% glycerol solution of lithium trifluoromethanesulfonate, polyvinyl alcohol and water according to a ratio of 1:1:8 to prepare ionic ink;
coating ion ink on the dust-free paper, placing the dust-free paper coated with the ion ink in a blast oven, drying for 3 hours at the temperature of 100 ℃, and taking out to obtain the ion paper;
conducting screen printing conductive silver paste on a designed area on the surface of the ion paper to form a specific electrode pattern;
adhering a pressure-sensitive double-sided adhesive to a design area on the surface of the ion paper; folding the ion paper to enable the electrodes/the ion paper/the electrodes to be in face-to-face contact with each other to form a sandwich structure;
and leading the electrodes out to a test circuit through the anisotropic conductive adhesive tape to obtain the required two-dimensional ion-electron type flexible pressure sensor.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents and improvements made within the spirit and principle of the present invention are intended to be included within the scope of the present invention.

Claims (10)

1. The ionic paper is characterized by being made of a cellulose reinforced ionic gel composite material, wherein the cellulose reinforced ionic gel composite material comprises a liquid ionic material, a polymer and cellulose, and the liquid ionic material, the polymer and the cellulose are contained in the following weight percentages based on the total weight of the cellulose reinforced ionic gel composite material as 100 percent:
1-80% of a liquid ionic material;
1-80% of a polymer;
19 to 80 percent of cellulose,
wherein the cellulose is selected from papermaking cellulose, and the polymer is selected from polymers capable of forming gel materials with the liquid ionic material.
2. The ionic paper of claim 1, wherein the liquid ionic material is selected from at least one of an ionic liquid, an ionic liquid high boiling point organic solution, a solid electrolyte high boiling point organic solution, wherein,
the ionic liquid is an ionic compound which is in a liquid state at the temperature of 10-35 ℃;
the ionic liquid high-boiling-point organic solution is formed by dissolving ionic liquid in a high-boiling-point high-polarity organic solvent, and the high-boiling-point high-polarity organic solvent has a boiling point of not less than 200 ℃ and contains at least one of hydroxyl, amido, ester, amido and carboxyl in a molecular structure;
the solid electrolyte high-boiling-point organic solution is a solution formed by an ionic compound which is in a solid state at the temperature of 10-35 ℃ in a high-boiling-point high-polarity organic solvent, and the high-boiling-point high-polarity organic solvent has a boiling point of not less than 200 ℃ and contains at least one of hydroxyl, amido, ester, amido and carboxyl in a molecular structure.
3. The ionic paper of claim 2, wherein the ionic liquid is at least one selected from imidazole ionic liquids, quaternary ammonium salt ionic liquids, pyridine ionic liquids, pyrrole ionic liquids and piperidine ionic liquids; and/or
In the ionic liquid solution, the ionic liquid is at least one selected from imidazole ionic liquid, quaternary ammonium salt ionic liquid, pyridine ionic liquid, pyrrole ionic liquid and piperidine ionic liquid; the high-boiling-point high-polarity organic solvent is selected from at least one of dibutyl phthalate, tributyl citrate, N-methyl pyrrolidone, dimethyl sulfoxide, glycerol and ethylene glycol; and/or
In the solid electrolyte high-boiling-point organic solution, the ionic compound is selected from at least one of small molecule electrolyte and polymer electrolyte; the high-boiling-point high-polarity organic solvent is at least one selected from dibutyl phthalate, tributyl citrate, N-methyl pyrrolidone, dimethyl sulfoxide, glycerol and ethylene glycol.
4. The ionic paper according to claim 3, wherein the ionic compound in the solid electrolyte solution is at least one selected from the group consisting of lithium trifluoromethanesulfonate, lithium hexafluorophosphate and polystyrene sulfonic acid.
5. The ionic paper of claim 1, wherein the polymer is selected from the group consisting of a polymer monomer containing at least one of a hydroxyl group, a carboxyl group, an amide group, an amino group, a nitro group, a halogen atom, an ester group, a cyano group, and a carbamate group.
6. The ionic paper of claim 5, wherein the polymer is selected from at least one of polyvinyl alcohol, polyurethane, polyamide, polyvinylidene fluoride, and polyacrylate.
7. An off-electronic flexible pressure sensor is a foldable flexible pressure sensor and comprises an electrode area and an ion area, wherein at least the ion area is made of a cellulose reinforced ionic gel composite material, the cellulose reinforced ionic gel composite material comprises a liquid ionic material, a polymer and cellulose, and the weight percentages of the liquid ionic material, the polymer and the cellulose are as follows based on 100 percent of the total weight of the cellulose reinforced ionic gel composite material:
1-80% of a liquid ionic material;
1-80% of a polymer;
19 to 80 percent of cellulose,
wherein the cellulose is selected from papermaking cellulose, and the polymer is selected from polymers capable of forming gel materials with the liquid ionic material.
8. A preparation method of an off-electronic flexible pressure sensor is characterized by comprising the following steps:
providing an ion paper substrate, and preparing a patterned electrode on the surface of the ion paper substrate according to a preset electrode pattern, wherein the ion paper substrate is the ion paper of any one of claims 1 to 6;
and arranging an adhesive at the designed part of the ion paper substrate, and folding the ion paper substrate to ensure that the ion area and the electrode area are attached face to form a preset electrode pattern, thereby obtaining the foldable electronic flexible pressure sensor.
9. The method of manufacturing an ion-beam flexible pressure sensor according to claim 8, wherein the method of manufacturing the ion paper substrate comprises:
weighing the components according to the formula of the ionic paper of any one of claims 1 to 6, and dispersing the liquid ionic material, the polymer and the cellulose in water or an organic solvent to form slurry;
depositing the slurry on the surface of a substrate, drying to remove the solvent, and stripping the formed ionic paper from the substrate; or
Dissolving a liquid ionic material and a polymer in water or an organic solvent to form slurry, and preparing the slurry into a liquid ionic coating;
providing a paper substrate of cellulosic material, dipping the paper substrate into the liquid ionic coating, and drying to remove the solvent to prepare ionic paper; or
Dissolving a liquid ionic material, a polymer and an additive in water or an organic solvent to form ionic ink, printing the ionic ink on a paper substrate made of a cellulose material, and drying to remove the solvent to prepare the ionic paper.
10. A preparation method of an off-electronic flexible pressure sensor is characterized by comprising the following steps:
providing a paper substrate made of cellulose materials, printing electrode materials on preset electrode areas of the paper substrate according to a preset electrode pattern, and printing ion ink on preset ion areas of the paper substrate to form electrode areas and ion areas made of the ion paper according to any one of claims 1 to 6; wherein the ionic ink contains a liquid ionic material, a polymer, and an additive;
and arranging an adhesive at the designed part of the paper substrate, and folding the paper substrate to ensure that the ion area and the electrode area are attached face to form a preset electrode pattern, thereby obtaining the ion-electron type foldable flexible pressure sensor.
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