CN113416285B - Preparation method and application of ionic liquid conductive elastomer - Google Patents
Preparation method and application of ionic liquid conductive elastomer Download PDFInfo
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Abstract
The invention relates to a preparation method and application of an ionic liquid conductive elastomer. The nano-sized vinyl silicon dioxide realizes homogeneous mixing of the polar ionic liquid and the nonpolar elastomer butyl acrylate monomer, and the prepared conductive elastomer has excellent conductivity. In addition, the introduction of the vinyl silicon dioxide also constructs a cross-linked polymer network, so that the mechanical property of the conductive elastomer is effectively improved, and the long-term use stability of the material is enhanced.
Description
Technical Field
The invention belongs to the technical field of conductive elastomers, and particularly relates to an ionic liquid conductive elastomer and a preparation method and application thereof.
Background
In recent years, flexible electronic devices have attracted much attention in the fields of human motion sensing and detection due to their characteristics of light weight, portability, high sensitivity, and the like. At present, various materials including hydrogel, conductive fiber film, conductive elastomer and the like are reliable candidate materials for preparing flexible electronic devices due to the excellent conductivity and flexibility of the materials. Among them, the conductive elastomer has more excellent chemical and physical stability and more excellent mechanical properties compared with materials such as hydrogel and conductive fiber membrane, so how to prepare the conductive elastomer with excellent properties becomes an important issue in the field of flexible electronics.
At present, inorganic solid conductive fillers represented by carbon nanotubes, carbon black and graphene are often used for preparing conductive elastomers. Chinese patent publication No. CN110763379B discloses a graphene conductive elastomer, a method for preparing the same, and a sensor. The invention discloses a graphene conductive elastomer which comprises an elastic matrix and a graphene three-dimensional network structure. According to the method, a porous elastic matrix is filled with a graphene three-dimensional network structure, and at least part of graphene in the graphene three-dimensional network structure is intrinsic graphene or reduced graphene oxide. However, the method for preparing the conductive elastomer by introducing the inorganic solid conductive filler can greatly affect the mechanical property of the material, so that the elongation at break of the material is greatly reduced. In addition, the inorganic filler can spontaneously agglomerate in the system due to the high surface energy of the inorganic filler to form a heterogeneous system, and the homogeneity of the material is influenced.
Compared with the traditional inorganic conductive filler, the ionic liquid has wide development prospect in the field of conductive elastomers because of the lower saturated vapor pressure and the special property of being liquid at room temperature. Chinese patent publication No. CN111205406A discloses a dielectric elastomer precursor liquid, a preparation method and applications thereof, a dielectric elastomer composite material, a flexible device, and a light-emitting device. The dielectric elastomer precursor liquid comprises an elastomer substrate, ionic liquid and a solvent, wherein the volume fraction of the ionic liquid and the solvent is 5-45%. However, in practical applications, due to the polarity difference between the ionic liquid and the elastomer matrix, a homogeneous precursor solution cannot be obtained, which is not different from practical production and is a great challenge.
Disclosure of Invention
The invention aims to solve the technical problem of providing an ionic liquid conductive elastomer and a preparation method thereof, the method overcomes the defect that the conventional elastomer cannot conduct electricity, improves the compatibility of the ionic liquid and an elastomer monomer, and effectively improves the mechanical property of the material during homogeneous preparation.
A preparation method of an ionic liquid conductive elastomer comprises the following steps:
step 1: modifying and modifying the nano silicon dioxide to obtain amino modified silicon dioxide nano particles with amino on the surface;
step 2: modifying the amino modified silica nanoparticles to obtain vinyl silica nanoparticles with vinyl on the surface;
and step 3: adding the vinyl silicon dioxide nanoparticles, the ionic liquid and butyl acrylate into a test tube, performing ultrasonic dispersion for 10min to obtain a homogeneous precursor solution, adding a photoinitiator, and performing photoinitiation for 60-120min under ultraviolet irradiation to obtain the ionic liquid conductive elastomer.
The ionic liquid conductive elastomer of the present invention may be assembled into a strain sensor.
The assembly method of the strain sensor comprises the following steps:
(1) cutting the ionic liquid conductive elastomer into 0.1cm multiplied by 2cm multiplied by 10cm to obtain M1;
(2) pasting copper foils with conductive silver paste on two sides of M1 to obtain M2;
(3) and leading out copper foils on two sides of the M2 by using copper wires to manufacture a device M3, wherein the device M3 is the strain sensor.
Advantageous effects
(1) According to the method, the vinyl silicon dioxide nanoparticles are introduced, so that the ionic liquid and the butyl acrylate are uniformly mixed, a stable conductive path is constructed, and the prepared elastomer has stable and excellent conductive performance.
(2) The vinyl functional groups on the surface of the silicon dioxide nano particles can be used as crosslinking sites, so that a crosslinked network structure is formed inside the elastomer, and the prepared elastomer has excellent mechanical properties.
(3) The conductive elastomer is prepared by uniformly mixing the ionic liquid and butyl acrylate through vinyl silicon dioxide and then carrying out photo-initiated free radical polymerization. The nano-sized vinyl silicon dioxide realizes homogeneous mixing of the polar ionic liquid and the nonpolar elastomer butyl acrylate monomer, and the prepared conductive elastomer has excellent conductivity. In addition, the introduction of the vinyl silicon dioxide also constructs a cross-linked polymer network, so that the mechanical property of the conductive elastomer is effectively improved, and the long-term use stability of the material is enhanced.
Drawings
Fig. 1 is a digital photographic image of the precursor solutions of comparative example 1, and example 2.
Fig. 2 is a stress-strain curve of examples 1 and 2.
Fig. 3 is the electrical signal sensitivity of the assembled strain sensor of example 2.
Fig. 4 is a graph of the electrical signal at different strains for the assembled strain sensor of example 2.
Fig. 5 is a graph of electrical signals for different degrees of human finger flexion for the assembled strain sensor of example 2.
FIG. 6 is a graph showing the electrical signal curves of the assembled strain sensor of example 2 for the bending of the wrist, elbow and knee of a human body.
Detailed Description
The invention will be further illustrated with reference to the following specific examples. It should be understood that these examples are for illustrative purposes only and are not intended to limit the scope of the present invention. Further, it should be understood that various changes or modifications of the present invention may be made by those skilled in the art after reading the teaching of the present invention, and such equivalents may fall within the scope of the present invention as defined in the appended claims.
A preparation method of an ionic liquid conductive elastomer comprises the following steps:
step 1: modifying and modifying the nano silicon dioxide to obtain amino modified silicon dioxide nano particles with amino on the surface;
step 2: modifying the amino modified silica nanoparticles to obtain vinyl silica nanoparticles with vinyl on the surface;
and step 3: adding the vinyl silicon dioxide nanoparticles, the ionic liquid and butyl acrylate into a test tube, performing ultrasonic dispersion for 10min to obtain a homogeneous precursor solution, adding a photoinitiator, and performing photoinitiation for 60-120min under ultraviolet irradiation to obtain the ionic liquid conductive elastomer.
Preferably, the amino-modified silica nanoparticles in step 1 of the present invention are specifically: dissolving the silicon dioxide nano-particles by using a solvent, adding a silane coupling agent, continuously heating and stirring for reaction, carrying out centrifugal precipitation, and carrying out freeze drying to obtain the amino modified silicon dioxide nano-particles.
Preferably, the solvent of the present invention is toluene; the silane coupling agent is aminopropyl trimethoxy silane.
Preferably, the silane coupling agent, the silica nanoparticles and the toluene are mixed in a mass ratio of 5: 3.5: 200 of a carrier; the reaction temperature is 90 ℃; the reaction time was 12 h.
Preferably, the vinyl silica nanoparticles in step 2 of the present invention are specifically: dissolving the amino modified silicon dioxide nano-particles by using a solvent, adding methacryloyl chloride, continuously reacting, centrifugally precipitating, and freeze-drying to obtain the vinyl silicon dioxide nano-particles.
Preferably, the solvent of the present invention is toluene.
Preferably, the mass ratio of the methacryloyl chloride to the amino-modified silica nanoparticles to the toluene is 10: 10: 200 of a carrier; the reaction temperature is 25 ℃; the reaction time was 12 h.
Preferably, in step 3 of the invention, the ionic liquid is 1-butyl-3-methylimidazolium tetrafluoroborate, and the photoinitiator is 2, 2-diethoxyacetophenone.
Preferably, in step 3 of the present invention, the addition amount of the photoinitiator is 1wt%, and the mass ratio of the vinyl silica nanoparticles, the ionic liquid, and the butyl acrylate is 20: 100: 100; the wavelength of ultraviolet light is 365nm, and the maximum light intensity is 80mW/cm -2 。
The ionic liquid conductive elastomer prepared by the invention can be assembled into a strain sensor.
Silica (30. + -.5 nm) from Shanghai Michelin Biochemical technology, Inc.; silane coupling agent (98%), methacryloyl chloride (95%), and ionic liquid (99% +) were all purchased from Shanghai Tantake technologies, Inc.; butyl acrylate (99% containing 10-60ppm MEHQ stabilizer) was purchased from Shanghai Allantin Biotech Co., Ltd; photoinitiators (> 95%) were purchased from Chishiei (Shanghai) chemical industry development Co., Ltd.
Example 1
Step 1: dissolving 3.5g of silicon dioxide and 5mL of silane coupling agent in 200mL of toluene, continuously heating and stirring in an oil bath at 90 ℃ for reaction for 12h, centrifuging, precipitating, and freeze-drying to obtain the amino modified silicon dioxide nanoparticles.
And 2, step: dissolving 1 amino modified silica nanoparticle and 1mL of methacryloyl chloride in 20mL of toluene, stirring at room temperature for reaction for 12h, performing centrifugal precipitation, and performing freeze drying to obtain the vinyl silica nanoparticle.
And step 3: dissolving 100mg of vinyl silica nanoparticles, 10mg of photoinitiator and 1mL of ionic liquid in 1mL of butyl acrylate monomer, and uniformly dispersing the mixed solution in an ultrasonic dispersion machine to obtain a precursor solution.
And 4, step 4: and pouring the precursor solution into a mold, placing the mold in an ultraviolet reactor, and carrying out photoinitiation reaction for 2 hours to prepare the ionic liquid conductive elastomer.
Example 2
Preparation was carried out according to the preparation method of example 1 except that the vinyl silica was added in an amount of 200mg to prepare example 2.
Step 1: dissolving 3.5g of silicon dioxide and 5mL of silane coupling agent in 200mL of toluene, continuously heating and stirring in an oil bath at 90 ℃ for reaction for 12h, centrifuging, precipitating, and freeze-drying to obtain the amino modified silicon dioxide nanoparticles.
Step 2: dissolving 1 amino modified silica nanoparticle and 1mL of methacryloyl chloride in 20mL of toluene, stirring at room temperature for reaction for 12h, performing centrifugal precipitation, and performing freeze drying to obtain the vinyl silica nanoparticle.
And step 3: 200mg of vinyl silicon dioxide nano particles, 10mg of photoinitiator and 1mL of ionic liquid are dissolved in 1mL of butyl acrylate monomer, and the mixed solution is placed in an ultrasonic dispersion machine to be uniformly dispersed, so that precursor solution is obtained.
And 4, step 4: and pouring the precursor solution into a mold, placing the mold in an ultraviolet reactor, and carrying out photoinitiation reaction for 2 hours to prepare the ionic liquid conductive elastomer.
Comparative example 1
(1) And dissolving the photoinitiator and the ionic liquid in a butyl acrylate monomer, and uniformly dispersing the mixed solution in an ultrasonic dispersion machine to obtain a precursor solution.
(2) And pouring the precursor solution into a mold, placing the mold in an ultraviolet light reactor, and carrying out photoinitiation reaction for 2 hours to obtain the comparative example 1.
Figure 1 shows digital photographic images of the precursor solutions of comparative example 1, example 1 and example 2. In the comparative example, significant delamination of the solution occurred due to the difference in polarity between butyl acrylate and the ionic liquid. With the introduction of the vinyl silica, both the example 1 and the example 2 are homogeneous solutions, which shows that the compatibility of butyl acrylate and the ionic liquid is improved, and the vinyl silica plays a role of a surfactant. (solutions were all dyed by methylene blue, thus appearing blue)
Fig. 2 shows stress-strain curves of examples 1 and 2. With increasing vinyl silica, example 2 exhibited a higher tensile modulus than example 1. The vinyl functional group on the vinyl silicon dioxide can construct an effective cross-linked network system in the system, so that the mechanical property of the material is improved. Comparative example 1 photo initiation was not performed because no solution was available in the military.
Figure 3 shows the response sensitivity of the strain sensor assembled from example 2. The device can make a sensitive response to the external strain, and the response time is only 240 milliseconds. The excellent sensing sensitivity is mainly caused by the uniform dispersion of the conductive ionic liquid in the material.
Fig. 4 shows the electrical signal curves at different strains for the strain sensor assembled from example 2. The device shows stable and recyclable electric signal curves under different strains of 50% -200%, which indicates that the device has stable sensing performance.
Fig. 5 shows the electrical signal curves for different degrees of human finger flexion for the strain sensor assembled from example 2. Under the condition that the finger is bent by 30 degrees, 60 degrees and 90 degrees respectively, the resistance of the device is gradually increased, and a stable and recyclable electric signal curve is displayed, which proves that the device has stable performance in the field of human body dynamic monitoring.
Fig. 6 shows the electrical signal curves of the strain sensor assembled in example 2 for the bending of the wrist, elbow and knee of a human body. When different parts are bent, the deformation of the sensing device is different due to the difference of the motion amplitude of the human body, so that the electric signals are obviously different. The bending part can be estimated through the difference of different signal peak values, which proves that the device has important application value in the field of human body dynamic monitoring.
Claims (9)
1. The preparation method of the ionic liquid conductive elastomer is characterized by comprising the following steps of:
step 1: modifying and modifying the nano silicon dioxide to obtain amino modified silicon dioxide nano particles with amino on the surface;
step 2: modifying the amino modified silica nanoparticles to obtain vinyl silica nanoparticles with vinyl on the surface;
and step 3: adding the vinyl silicon dioxide nanoparticles, the ionic liquid and butyl acrylate into a test tube, performing ultrasonic dispersion for 10min to obtain a homogeneous precursor solution, adding a photoinitiator, and performing photoinitiation for 60-120min under ultraviolet irradiation to obtain the ionic liquid conductive elastomer.
2. The method for preparing the ionic liquid conductive elastomer according to claim 1, wherein the amino-modified silica nanoparticles in the step 1 are specifically: dissolving the silicon dioxide nano-particles by using a solvent, adding a silane coupling agent, continuously heating and stirring for reaction, carrying out centrifugal precipitation, and carrying out freeze drying to obtain the amino modified silicon dioxide nano-particles.
3. The method for preparing an ionic liquid conductive elastomer according to claim 2, wherein the solvent is toluene; the silane coupling agent is aminopropyl trimethoxy silane.
4. The method for preparing the ionic liquid conductive elastomer according to claim 3, wherein the mass ratio of the silane coupling agent to the silica nanoparticles to the toluene is 5: 3.5: 200 of a carrier; the reaction temperature is 90 ℃; the reaction time was 12 h.
5. The method for preparing the ionic liquid conductive elastomer according to claim 1, wherein the vinyl silica nanoparticles in the step 2 are specifically: dissolving the amino modified silicon dioxide nano-particles by using a solvent, adding methacryloyl chloride, continuously reacting, centrifugally precipitating, and freeze-drying to obtain the vinyl silicon dioxide nano-particles.
6. The method for preparing an ionic liquid conductive elastomer according to claim 5, wherein the solvent is toluene.
7. The preparation method of the ionic liquid conductive elastomer as claimed in claim 6, wherein the mass ratio of the methacryloyl chloride to the amino-modified silica nanoparticles to the toluene is 10: 10: 200 of a carrier; the reaction temperature is 25 ℃; the reaction time was 12 h.
8. The method for preparing the ionic liquid conductive elastomer as claimed in claim 1, wherein the ionic liquid in the step 3 is 1-butyl-3-methylimidazolium tetrafluoroborate, and the photoinitiator is 2, 2-diethoxyacetophenone.
9. The method for preparing the ionic liquid conductive elastomer according to claim 1, wherein in the step 3, the addition amount of the photoinitiator is 1wt%, the vinyl silica nanoparticles are 100mg or 200mg, the ionic liquid is 1ml, and the butyl acrylate is 1 ml; the wavelength of ultraviolet light is 365nm, and the maximum light intensity is 80mW/cm -2 。
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