CN108707252B - Nano composite ionic liquid gel material, preparation thereof and strain sensor based on material - Google Patents
Nano composite ionic liquid gel material, preparation thereof and strain sensor based on material Download PDFInfo
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- CN108707252B CN108707252B CN201810548926.2A CN201810548926A CN108707252B CN 108707252 B CN108707252 B CN 108707252B CN 201810548926 A CN201810548926 A CN 201810548926A CN 108707252 B CN108707252 B CN 108707252B
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- ionic liquid
- liquid gel
- ferroferric oxide
- nano composite
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- CXQXSVUQTKDNFP-UHFFFAOYSA-N octamethyltrisiloxane Chemical compound C[Si](C)(C)O[Si](C)(C)O[Si](C)(C)C CXQXSVUQTKDNFP-UHFFFAOYSA-N 0.000 description 1
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Abstract
The invention discloses a preparation method of a high-tensile self-repairing multifunctional nano composite ionic liquid gel material. The ionic liquid gel material has high tensile property and self-repairing property, and also has self-adhesion property, electric conductivity, magnetic responsiveness, flame retardance and a wide working temperature range. Meanwhile, the invention provides a resistance-type strain sensor based on the multifunctional nano composite ionic liquid gel material, which can detect great strain and small strain, has higher sensitivity and solves the problem that the traditional strain sensor cannot detect great strain.
Description
Technical Field
The invention belongs to the technical field of high polymer materials and flexible electronics, and particularly relates to a nano composite ionic liquid gel material, a preparation method thereof and a strain sensor based on the material.
Background
The ionic liquid gel is a viscoelastic high molecular material which swells a large amount of ionic liquid in a three-dimensional polymer network of the ionic liquid gel. Due to the advantages of thermal stability, chemical inertness, almost no saturated vapor pressure, good conductivity, wide electrochemical window and the like, the ionic liquid gel has wide application prospect in the fields of capacitors, energy batteries, sensors, drivers and the like. The ionic liquid gel inevitably causes damage during long-term use, thereby causing wrong information and even life danger. The self-repairing ionic liquid gel is an intelligent material with the characteristics of repairing a damaged structure of a high molecular network structure and a gel function. Endows the ionic liquid gel with self-repairing performance, and provides an economical and convenient new method for greatly improving the use safety and the service life of the material.
The ionic liquid gel has a contradiction between the mechanical property and the self-repairing property. In order to improve the self-repairing performance of the ionic liquid gel, the mechanical property of the ionic liquid gel is sacrificed. Among the ionic liquid gels reported at present, the ionic liquid gel with self-repairing performance has the problem of very poor mechanical property and bears larger stress; however, the ionic liquid gel which can bear certain stress and deform often does not have the self-repairing function. These drawbacks have greatly limited the application of ionic liquid gels in emerging technology fields, particularly in flexible electronics where there is a need for deformation. At present, no research report exists on a preparation method of a multifunctional ionic liquid gel material with both high tensile property and self-repairing property and a strain sensor based on the material. With the advent and rapid development of flexible electronic products, flexible and stretchable strain sensors are increasingly in demand. Therefore, the ionic liquid gel material with excellent mechanical property and self-repairing property obtained by chemical design has important engineering significance and is a problem to be solved urgently in the field of flexible electronics.
Disclosure of Invention
In order to overcome the defects of the prior art, the invention aims to provide a high-tensile self-repairing multifunctional nano composite ionic liquid gel material, a preparation method thereof and a strain sensor based on the material, wherein the technical principle of the preparation method is as follows: the ionic liquid gel has the characteristics of autonomy (no external condition stimulation) and repeated self-repairing property, is broken in the stretching process, and can form reversible metal coordination bonds again after being released, so that the composite ionic liquid gel has excellent mechanical property and self-repairing property.
The ionic liquid gel has excellent tensile property, the elongation can reach 14 times, and the ionic liquid gel has quick and efficient self-repairing property, the conductivity of the ionic liquid gel can be repaired by 100% within 0.5 second at room temperature, and the tensile stress self-repairing of 90.0% -97.6% and the tensile length self-repairing of 92.0% -98.4% can be completed within 4 hours. In addition, temperature can also affect the self-healing properties of ionic liquid nanocomposite gels. The glass transition temperature of the ionic liquid nano composite gel is very low (-51 ℃), so that the material can realize self-repairing at a lower temperature (for example, -25 ℃), and the self-repairing performance is improved when the temperature is increased (for example 60 ℃). Meanwhile, the ionic liquid nano composite gel is assembled into a resistance type sensor, so that the application of the ionic liquid nano composite gel as a strain sensor in the field of flexible electronics is realized. The material overcomes the contradiction between the tensile property and the self-repairing property of a high polymer material, and provides a new thought for the synthesis of a multifunctional novel self-repairing flexible conductive material with excellent performance and the preparation of a large-deformation flexible tension sensor.
In order to achieve the purpose, the invention adopts the technical scheme that:
a nano-composite ionic liquid gel material comprises ferroferric oxide nanoparticles and a polymer, wherein the polymer can form a dynamic reversible coordination bond with Fe (III) ions on the surfaces of the ferroferric oxide nanoparticles.
The polymer accounts for 0.1-10 wt% of the content of the ferroferric oxide nano particles.
The invention also provides a preparation method of the nano composite ionic liquid gel material and a strain sensor based on the material, and the method specifically comprises the following steps
and 2, preparing a reaction mixed solution. Adding a high-molecular monomer, an initiator and the polymer-coated ferroferric oxide nanoparticles obtained in the step (1) into an ionic liquid, and uniformly mixing to obtain a mixed solution;
and 3, preparing the nano composite ionic liquid gel. And pouring the mixed solution into a glass plate mold, and irradiating under an ultraviolet lamp (for 6-20 hours) or heating under the ultraviolet lamp (for 1-10 hours) to prepare the nano composite ionic liquid gel material doped with the ferroferric oxide nano particles.
Wherein the polymer is alginate, polyvinyl alcohol (PVA), Polyacrylamide (PAM), polymethacrylic acid (PMAA), Polyhydroxyethylmethacrylate (PHEMA), polyvinyl acetate (PVAc), Polyacrylonitrile (PAN), Polystyrene (PS) or polyvinylpyrrolidone (PVP).
The high molecular monomer is alginate (Alg), acrylamide (AAm), methacrylic acid (MAA), 2-Methacrylamide (MAA), Acrylic Acid (AA), butyl Acrylate (N-butyl Acrylate, BA), Ethyl Acrylate (Ethyl Acrylate, AA), isopropyl acrylamide (N-isopropylacrylamide, NIPAm), hydroxyethyl methacrylate (HEMA), acrylonitrile (acrylonitrile, AN), styrene (styrene, ST) or N-Vinyl pyrrolidone (N-Vinyl-2-pyrrolidone, NVP).
The ionic liquid is imidazole ionic liquid, pyridine ionic liquid, quaternary phosphorus ionic liquid, quaternary ammonium ionic liquid, pyrrolidine ionic liquid, piperidine ionic liquid, ionic liquid with benzyl, sulfonic ionic liquid, hydroxyl ionic liquid, carboxyl ionic liquid, alkenyl ionic liquid, halogen ionic liquid, tetrafluoroborate ionic liquid, hexafluorophosphate ionic liquid or amino acid ionic liquid. For example, 1-methylimidazolium tetrafluoroborate, 1-ethyl-3-methylimidazolium ethyl sulfate, 1-ethyl-2, 3-dimethylimidazolium p-methylbenzenesulfonate, N-ethylpyridinium bromide, N-ethyl-3-methylpyridinium hexafluorophosphate, ethyltriphenylphosphine perchlorate, tetrabutylammonium trifluoromethanesulfonate, N-ethyl, methylpyrrolidine thiocyanate, N-ethyl, methylpiperidine hydrogensulfate, 1-benzyl-3-methylimidazolium hexafluorophosphate, 1-sulfopropyl-3-methylimidazolium inner salt, 1-hydroxybutyl-2, 3-dimethylimidazolium bromide, 1-carboxymethyl-3-methylimidazolium bistrifluoromethylsulfimide, 1-vinyl-3-methylimidazolium dicyanamide salt, or tetramethylquaternary ammonium glycine ionic liquid.
The initiator is ammonium persulfate, potassium persulfate, sodium persulfate, 2-hydroxy-2-methyl-1-phenyl acetone, methyl benzoylformate or alkyl iodonium salt.
In the step 1, the amount of the polymer is 0.1-10 wt% of the ferroferric oxide nano particles, in the step 2, the amount of the high molecular monomer is 1-50 wt% of the nano composite ionic liquid gel material, the amount of the ferroferric oxide nano particles coating the polymer is 0.1-30 wt% of the nano composite ionic liquid gel material, the amount of the initiator is 0.01-10 wt% of the high molecular monomer, and the amount of the ionic liquid is 10-90 wt% of the nano composite ionic liquid gel material.
In addition, the nano composite ionic liquid gel is cut into a required shape to be used as a strain sensor. The nano composite ionic liquid gel material can be used for a resistance type strain sensor, and the nano composite ionic liquid gel is cut into a required shape and is connected with an electrode material to be used as the strain sensor. The principle of the strain sensor provided by the invention is a piezoresistive strain sensor, namely, the change of the relative resistance value of the ionic liquid gel material is in a linear or exponential relationship with the change of strain.
The nano composite ionic liquid gel material can be applied to the field of flexible electronics.
The principle of the invention is as follows:
the high-tensile self-repairing multifunctional nano composite ionic liquid gel network is formed on the basis of dynamic reversible coordination bonds. The coordination bonds are derived from the dynamic interaction of Fe (III) ions on the surfaces of the ferroferric oxide nanoparticles and carboxylate radicals on polymer macromolecular chains, and the reversible dissociation/combination of the dynamic bonds enables the ionic liquid gel to have the characteristic of repeated self-repairing without external condition stimulation; in addition, the ferroferric oxide nano particles are doped to endow the gel with the magnetic response characteristic; and the multifunctional nano composite ionic liquid gel also has the excellent characteristics of the ionic liquid, such as wide temperature working range, electric conductivity, flame retardance and wide electrochemical window. The strain sensor based on the nano composite ionic liquid gel belongs to a resistance type strain sensor, namely, the relative resistance change of a material is in a linear or exponential relationship with the change of strain.
Compared with the prior art, the invention has the beneficial effects that:
compared with other ionic liquid gel materials, the nano-composite ionic liquid gel prepared by the invention has the characteristics of high stretchability and self-repairing, the tensile strain of the nano-composite ionic liquid gel can reach 1400%, the self-repairing is efficient without external condition stimulation (at room temperature, the conductivity of the nano-composite ionic liquid gel can be repaired 100% within 0.5 second, and the tensile stress self-repairing of 90.9% and the tensile length self-repairing of 92.86% can be completed within 4 hours), and the nano-composite ionic liquid gel also has magnetic responsiveness and can be driven under the action of a magnetic field, and the conductivity level is 0.01-1S/m. When the nano composite ionic liquid gel material is applied to a strain sensor, the nano composite ionic liquid gel material can be attached to a measured object with any curved surface, the problem that the traditional strain sensor is short in strain length is solved, the application measurement range of the strain sensor is expanded, and high sensitivity (GF = 3-20, obtained by GF = Delta R/R/calculation, wherein Delta R represents a resistance change value when strain occurs, R is a resistance change value when strain occurs, and R is a resistance change value0Representing the resistance value in the absence of strain).
Drawings
FIG. 1 is a multifunctional Fe3O4Design and preparation flow chart and force of @ PAA/PAA ionic liquid gelSchematic representation of chemical properties and free-form properties.
Fig. 2 is a high stretchability (2 a) and self-repairability (2 b) display diagram of the nanocomposite ionic liquid gel material of the present invention.
Fig. 3 is a schematic diagram of the results of the stretching (3 a) and self-repairing performance test (3 b) of the sample of the nanocomposite sodium alginate ionic liquid gel of the invention by an electron tensile machine, corresponding to example 1.
FIG. 4 is the self-adhesion and conductivity of nanocomposite polymethacrylic acid ionic liquid nanocomposite gels.
FIG. 5 is pressure sensing of nanocomposite polyacrylamide ionic liquid nanocomposite gels.
Detailed Description
The following examples are provided to explain embodiments of the present invention in detail.
The invention relates to a high-tensile self-repairing multifunctional nano composite ionic liquid gel material and a strain sensor based on the material.
Example 1
Referring to 1a, 1b, 1c and 1d of fig. 1, the preparation process of the high-stretch self-repair multifunctional nanocomposite ionic liquid gel material of the invention is as follows:
And 2, preparing a reaction mixed solution. Adding 20wt% of macromolecular sodium alginate and 2.5wt% of ferroferric oxide nano particles coated with the sodium alginate into 1-methylimidazole tetrafluoroborate seed liquid, adding 2.5wt% of initiator ammonium persulfate relative to the macromolecular sodium alginate, and uniformly mixing to obtain a mixed solution.
And 3, preparing the nano composite ionic liquid gel. Pouring the mixed solution into a glass plate mold with a silica gel gasket, and heating the glass plate mold in a thermostat for 1 hour to prepare nano composite ionic liquid gel doped with ferroferric oxide nano particles; it has excellent mechanical properties and free-form formability as shown in 1e of fig. 1.
The resulting nanocomposite ionic liquid gels in dumbbell shape were subjected to tensile testing using an electronic tensile machine, as shown in 2a of fig. 2. The nano composite ionic liquid gel can be stretched to 14 times of the original length, and the tensile breaking strength reaches 40 kPa. The nano composite ionic liquid gel is cut off by a scalpel blade, after self-repairing is carried out for 4 hours at room temperature, a repairing performance test is carried out by an electronic tensile machine, and the nano composite ionic liquid gel can finish the self-repairing of 90.9% of tensile stress and 92.86% of tensile length. The sensor is applied to the balloon and responds well to the expansion of the balloon. As the balloon expands, the resistance of the sensor becomes progressively greater, and the expansion of the balloon volume can be evaluated, as shown in fig. 2 b.
Example 2
The preparation process of the high-tensile self-repairing multifunctional nano composite ionic liquid gel material comprises the following steps:
And 2, preparing a reaction mixed solution. Adding 30wt% of high molecular monomer vinyl acetate and 1.5wt% of ferroferric oxide nano particles coated with polyvinyl acetate into 1-ethyl-2, 3-dimethyl imidazole p-methyl benzene sulfonate ionic liquid, adding 5wt% of initiator methyl benzoylformate relative to the high molecular vinyl acetate, and uniformly mixing to obtain a mixed solution.
And 3, preparing the nano composite ionic liquid gel. Pouring the mixed solution into a glass plate mold with a silica gel gasket, and irradiating for 7 hours by ultraviolet light to prepare the nano composite ionic liquid gel doped with the ferroferric oxide nano particles;
tensile test of the obtained dumbbell-shaped nano-composite ionic liquid gel by an electronic tensile machine is shown in 3a of figure 3, the nano-composite ionic liquid gel can be stretched to 11 times of the original length, and the tensile breaking strength reaches 71.3 kPa. The nano composite ionic liquid gel is cut off by a surgical blade, after self-repairing is carried out for 4 hours at room temperature, a self-repairing performance test is carried out by an electronic tensile machine, and the nano composite ionic liquid gel can complete 70.46% of tensile stress self-repairing and 75.4% of tensile length self-repairing. Applied to the finger, has good response to the bending of the finger. The finger is bent at different angles, and different resistance changes occur, so that a good response is made to the bending degree of the finger, as shown in fig. 3 b.
Example 3
The preparation process of the high-tensile self-repairing multifunctional nano composite ionic liquid gel material comprises the following steps:
And 2, preparing a reaction mixed solution. Adding 40wt% of macromolecular methacrylic acid and 9wt% of ferroferric oxide nano particles coated with the polymethacrylic acid into 1-hydroxybutyl-2, 3-dimethyl imidazole bromide sub liquid, adding 0.5wt% of initiator sodium persulfate relative to the macromolecular methacrylic acid, and uniformly mixing to obtain a mixed solution.
And 3, preparing the nano composite ionic liquid gel. Pouring the mixed solution into a glass plate mold with a silica gel gasket, and heating the glass plate mold in a thermostat for 1 hour to prepare nano composite ionic liquid gel doped with ferroferric oxide nano particles;
the adhesion strength of the resulting nanocomposite ionic liquid gel in a dumbbell shape was subjected to tensile test using an electron tensile machine, as shown in 4a, 4b, 4c of fig. 4. The adhesive strength of the nano-composite ionic liquid gel to PDMS is 207.4 +/-24.98N/m, and the adhesive strength of the nano-composite ionic liquid gel to a Cu sheet is 347.3 +/-6.97N/m. Increasing the strain, the brightness of the LED lamp darkened, indicating the sensing ability of the sensor during strain. The conductivity of the self-healing sample was restored to that of the original sample at 0.5s by cutting the nanocomposite ionic liquid gel 20 times with a scalpel blade as shown in 4e, 4f of fig. 4. .
Example 4
The preparation process of the high-tensile self-repairing multifunctional nano composite ionic liquid gel material comprises the following steps:
And 2, preparing a reaction mixed solution. Adding 35wt% of macromolecular polyacrylamide and 19wt% of the polyacrylamide-coated ferroferric oxide nanoparticles into 1-vinyl-3-methylimidazol dicyanamide molecular liquid, adding 7wt% of initiator alkyl iodonium salt relative to the mass fraction of the macromolecular acrylamide, and uniformly mixing to obtain a mixed solution.
And 3, preparing the nano composite ionic liquid gel. Pouring the mixed solution into a glass plate mold with a silica gel gasket, and performing ultraviolet illumination for 13 hours to prepare the nano composite ionic liquid gel doped with the ferroferric oxide nano particles;
the obtained nano composite ionic liquid gel is self-assembled into a stress strain sensor, and GF before and after the gel with the strain less than 800 percent is healed is respectively 3.82 and 3.96; the strain was between 800% and 1000% and the GF before and after gel healing was 19.6 and 20.2 respectively as shown in 5a of fig. 5. Compared with other materials, the ionic liquid gel self-assembly stress strain sensor has high sensitivity and large deformation as shown in 5b and 5c of figure 5. The application of the sensor to the balloon responds well to inflation of the balloon and to finger flexion as shown in 5d, 5e of figure 5.
In further embodiments, the polymer coated with ferroferric oxide may also be polyvinyl alcohol, polyacrylic acid, polyhydroxyethylmethacrylate, polyacrylonitrile, polystyrene, polyvinylpyrrolidone, or the like. The high molecular monomer is not limited to alginate, vinyl acetate, methacrylic acid, acrylamide, but may be other carboxylic acids with similar properties, such as acrylic acid, butyl acrylate, ethyl acrylate, acrylonitrile, styrene, vinyl pyrrolidone, hydroxyethyl methacrylate, and the like. The ionic liquid solvent may also be other types of ionic liquids, for example, ethyl 1-ethyl-3-methylimidazole sulfate, N-ethylpyridine bromide, N-ethyl-3-methylpyridine hexafluorophosphate, ethyltriphenylphosphine perchlorate, tetrabutylammonium trifluoromethanesulfonate, N-ethyl, methylpyrrolidine thiocyanate, N-ethyl, methylpiperidine hydrogensulfate, 1-benzyl-3-methylimidazole hexafluorophosphate, 1-sulfopropyl-3-methylimidazole inner salt, 1-carboxymethyl-3-methylimidazole bistrifluoromethanesulfonylimide, methyl quaternary ammonium glycine ionic liquid, and the like.
The invention prepares the ionic liquid gel material with high stretchability and self-repairability for the first time, and the multifunctional ionic liquid gel material also has magnetic responsiveness, electrical conductivity, flame retardance and a wide temperature working range. The ionic liquid gel material has wide application prospect in the field of flexible electronics.
The invention also provides a strain sensor based on the material, which comprises the following components:
the nano composite ionic liquid gel is cut into a strip shape to be used as a piezoresistive strain sensor, and the relative resistance value of the material can be correspondingly changed in the process of strain, so that the nano composite ionic liquid gel is used for sensing the mechanical deformation of an object.
Finally, it should be noted that: the above embodiments are only used to illustrate the technical solution of the present invention, and not to limit the same; while the invention has been described in detail and with reference to the foregoing embodiments, it will be understood by those skilled in the art that: the technical solutions described in the foregoing embodiments may still be modified, or some or all of the technical features may be equivalently replaced; and the modifications or the substitutions do not make the essence of the corresponding technical solutions depart from the scope of the technical solutions of the embodiments of the present invention.
Claims (4)
1. A preparation method of a nano composite ionic liquid gel material is characterized by comprising the following steps:
step 1, coating ferroferric oxide nano particles
Under the protection of nitrogen, adding polymethacrylic acid which is 5wt% of the weight of the ferroferric oxide nano particles under slow stirring at 80 ℃, continuously stirring for 60 minutes to obtain a suspended aqueous solution of the ferroferric oxide nano particles coated with the polymethacrylic acid, collecting the nano particles by using a magnet, drying and weighing;
step 2, preparation of reaction mixture
Adding methacrylic acid 40wt% and the ferroferric oxide nano particles coated with the polymethacrylic acid 9wt% relative to the total mass into 1-hydroxybutyl-2, 3-dimethyl imidazole bromide ionic liquid, adding initiator sodium persulfate 0.5wt% relative to the mass fraction of the methacrylic acid, and uniformly mixing to obtain mixed liquid;
step 3, preparation of nano composite ionic liquid gel
Pouring the mixed solution into a glass plate mold clamped with a silica gel gasket, and heating the glass plate mold in a thermostat for 1 hour to prepare the nano composite ionic liquid gel doped with the ferroferric oxide nano particles, wherein methacrylic acid and Fe (III) ions on the surfaces of the ferroferric oxide nano particles form dynamic reversible coordination bonds.
2. A strain sensor prepared from the nano-composite ionic liquid gel material obtained by the preparation method of claim 1.
3. The strain sensor of claim 2, wherein the nanocomposite ionic liquid gel is cut into a desired shape and adhesively bonded to the electrode material.
4. The application of the nano composite ionic liquid gel material obtained by the preparation method of claim 1 in the field of flexible electronics.
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