CN114835931B - Interface-enhanced multilayer composite conductive gel and preparation method thereof - Google Patents

Interface-enhanced multilayer composite conductive gel and preparation method thereof Download PDF

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CN114835931B
CN114835931B CN202210322272.8A CN202210322272A CN114835931B CN 114835931 B CN114835931 B CN 114835931B CN 202210322272 A CN202210322272 A CN 202210322272A CN 114835931 B CN114835931 B CN 114835931B
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CN114835931A (en
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彭争春
徐秀茹
何楚斌
陈宇轩
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Shenzhen University
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Abstract

The invention discloses an interface-enhanced multilayer composite conductive gel and a preparation method thereof. The multilayer composite conductive gel comprises n gel layers and n-1 interface layers, wherein the n gel layers and the n-1 interface layers are alternately laminated, and the first gel layer, the first interface layer, the second gel layer, the second interface layer, … …, the n-1 interface layer and the n-1 interface layer are sequentially arranged along the lamination direction, wherein n is an integer greater than or equal to 2. The interface layer is used as a bonding interface between gel layers, and an interlocking structural unit is constructed between adjacent gel layers, so that the multi-layer composite conductive gel has excellent stretchability, good tensile strength, good elastic modulus and higher toughness, and also has excellent interface stability and good fatigue resistance. As a tensile strain sensor, it also has good conductivity, sensitive strain sensing performance, a wide strain response range, and excellent response stability.

Description

Interface-enhanced multilayer composite conductive gel and preparation method thereof
Technical Field
The invention relates to the technical field of conductive gel, in particular to an interface-enhanced multilayer composite conductive gel and a preparation method thereof.
Background
Conductive gels are three-dimensional polymer networks, physically or chemically crosslinked, with network structures resembling human cell matrices, most gels have similar young's modulus to muscle and skin tissue, good mechanical flexibility, environmental stability, biocompatibility, and thus find wide research and application in flexible conductive materials such as wearable electrodes, energy conversion and storage devices, sensors, implantable medical and biological devices, actuators. As an emerging conductive gel structure, the conductive gel with gradient modulus is similar to a gradual change structure from high modulus to low modulus from epidermis to dermis in a human skin structure, and is expected to have a great improvement effect on the sensitivity and the range of sensor signals.
However, the preparation method of the gradient modulus gel reported at present often realizes the gradient modulus by an electric field induction method or a particle sedimentation method and the like. For example, researchers reported a multi-stage gradient modulus ionogel polymer material (ADVANCED MATERIALS,2021,2008486) that achieved a gradient change in modulus from 0.3kPa to 2.5 MPa. However, this work is mainly achieved by applying a single electric field across the precursor solution during the preparation process to induce charged material in the precursor to accumulate in the vicinity of the electric field electrodes to form a gradient concentration and to undergo a curing crosslinking reaction. CN109096504B disclosed in the chinese patent office mainly prepares gradient gel with different sedimentation rates of particles such as hydrophobic white carbon black, hydrophobic silica, hydrophobic polymer particles, hydrophobic carbon nanoparticles, hydrophobic metal silica particles, hydrophobic aerogel particles, etc. in the gel. The above method, although realizing a gel material with gradient modulus gradient, has the following problems: the application of the electric field has certain limitation, so that the specific modulus combination and distribution in the material have the defect of unknown property; also, gradient modulus gels, which rely on differences in sedimentation velocity of the material, have uncontrollable material modulus depending on particle sedimentation.
In addition, CN113769120A, CN112457449a discloses a preparation scheme of a bilayer gel in the literature published by the chinese patent office, and mainly adopts a method of polymerizing one layer and then polymerizing the other layer, so that the two layers of gel are combined together. Such bilayer gels tend to have a poor interface, which results in poor stability during use, greatly affecting their useful life and limiting their field of application.
Accordingly, the prior art is still in need of improvement and development.
Disclosure of Invention
In view of the above-mentioned shortcomings of the prior art, the present invention aims to provide an interface-enhanced multi-layer composite conductive gel and a preparation method thereof, which aims to solve the problem of unstable interface between the gel layers.
The technical scheme of the invention is as follows:
The interface-enhanced multilayer composite conductive gel comprises n gel layers and n-1 interface layers, wherein the n gel layers and the n-1 interface layers are alternately laminated, and sequentially comprise a first gel layer, a first interface layer, a second gel layer, a second interface layer, … …, an n-1 interface layer and an n-1 interface layer along the lamination direction, wherein n is an integer greater than or equal to 2;
each interface layer independently comprises an interface conductive agent, and the interface conductive agent is a micro-nano material.
Optionally, the n gel layers have a mechanical modulus from large to small: the first gel layer is greater than the second gel layer is greater than … … and greater than the nth gel layer.
Optionally, the multilayer composite conductive gel is composed of a first gel layer, a first interface layer and a second gel layer which are sequentially stacked.
Optionally, each interface layer independently comprises an interface conductive agent, wherein the interface conductive agent is one or more selected from metal salts, metal nano materials (such as nano silver wires, nano silver particles, nano silver sheets and the like), conductive polymers containing doping agents and conductive carbon materials;
the thickness of each interface layer is between 50 nanometers and 50 micrometers.
Optionally, each gel layer has a thickness between 100 nanometers and 10 millimeters.
The preparation method of the interface-enhanced multilayer composite conductive gel comprises the following steps:
Preparing a first gel layer;
sequentially preparing a first interface layer, a second gel layer, a second interface layer, … …, an n-1 interface layer and an n gel layer on the first gel layer to obtain the multilayer composite conductive gel, wherein n is an integer greater than or equal to 2.
Alternatively, the preparation method of each gel layer is independently selected from one of a template method, a spin coating method, a spray coating method and a printing method,
The preparation method of each interface layer is independently selected from one of a template method, a spin coating method, a spraying method and a printing method.
Optionally, n is 2, and the preparation method of the multilayer composite conductive gel comprises the following steps:
mixing 100 parts of a first solvent, 5-50 parts of a first polymer precursor, 0.1-10 parts of a first cross-linking agent, 0-20 parts of a first conductive agent and 0.01-20 parts of a first modulus regulator to obtain a first precursor solution;
Stirring the first precursor solution, and then carrying out prepolymerization for 1-60 minutes under the condition of heating at 25-90 ℃ or ultraviolet irradiation to obtain a first gel layer;
Taking interface conductive agent dispersion liquid on the first gel layer to form a first interface layer;
Mixing 100 parts of a second solvent, 5-50 parts of a second polymer precursor, 0.1-10 parts of a second crosslinking agent, 0-20 parts of a second conductive agent and 0.01-20 parts of a second modulus regulator to obtain a second precursor solution;
stirring the second precursor solution, and then taking the second precursor solution on the first interface layer, and carrying out prepolymerization for 1-60 minutes under the condition of heating at 25-90 ℃ or ultraviolet irradiation to form a second gel layer.
Optionally, the first polymer precursor and the second polymer precursor are each independently selected from one or more of acrylamide (abbreviated as AAm), N-methylolacrylamide (abbreviated as NMA), dimethylacrylamide, and polyvinyl alcohol;
The first crosslinking agent and the second crosslinking agent are respectively and independently selected from one or more of N, N' -dimethyl diacrylamide, polyethylene glycol diacrylate, methacryloylated gelatin, acryloylated xanthan gum and ammonium persulfate;
the first conductive agent and the second conductive agent are each independently selected from one or more of metal salts, metal nanomaterials, conductive polymers containing dopants, conductive carbon materials;
The metal salt is one or more selected from potassium chloride (KCl), sodium chloride (NaCl), calcium chloride (CaCl 2), copper chloride (CuCl 2) and ferric chloride (FeCl 3);
The metal nano material is one or more selected from nano silver wires, nano silver particles, nano silver sheets, nano gold wires, nano gold particles, nano gold sheets, nano copper wires, nano copper particles and nano copper sheets;
The conductive polymer is selected from one or more of Polyaniline (PANi), polypyrrole (Ppy) and poly 3, 4-ethylenedioxythiophene (PEDOT);
the doping agent is selected from one or more of poly (styrenesulfonic acid), hydrochloric acid, sulfuric acid and citric acid;
The first modulus modifier and the second modulus modifier are each independently selected from one or more of polyvinylpyrrolidone (abbreviated PVP), carboxylated cellulose nanowhiskers (abbreviated C-CNWs), carboxymethyl chitosan, metal oxide micro-nanoparticles.
The metal oxide micro-nano particles are selected from one or more of silicon dioxide, titanium dioxide, barium titanate, ferroferric oxide, zinc oxide, nickel oxide and other metal oxide micro-nano particles.
The first solvent and the second solvent are respectively and independently selected from one or more of deionized water, ethanol, methanol, isopropanol, isobutanol, glycerol and ethylene glycol.
Optionally, the interfacial conductive agent dispersion is composed of an interfacial conductive agent and an interfacial solvent;
The interface conductive agent is one or more selected from metal salt, metal nano material (such as nano silver wire, nano silver particle, nano silver sheet, nano gold wire, nano gold particle, nano gold sheet, nano copper wire, nano copper particle, nano copper sheet, etc.), conductive polymer containing doping agent, conductive carbon material (such as conductive carbon black, conductive carbon nano tube, conductive graphene, etc.);
the conductive polymer is selected from one or more of Polyaniline (PANi), polypyrrole (Ppy), poly 3, 4-ethylenedioxythiophene (PEDOT) and the like;
The interfacial solvent is one or more selected from deionized water, ethanol, methanol, isopropanol, isobutanol, glycerol and ethylene glycol.
The beneficial effects are that: the invention introduces an interface layer between the gel layers, which acts as a bonding interface between the gel layers, creating interlocking structural units between adjacent gel layers. The interfacial strength and stability of the double-layer gel can be enhanced by introducing the interfacial layer, so that the multi-layer composite conductive gel containing the interfacial layer has excellent stretchability, good tensile strength, good elastic modulus and higher toughness. Due to modulus matching between gel layers, an interface interlocking network and patch effect of interfaces, the multilayer composite conductive gel has excellent interface stability and good fatigue resistance. As a tensile strain sensor, it also has good conductivity, sensitive strain sensing performance, a wide strain response range, and excellent response stability.
Drawings
Fig. 1 is a schematic structural diagram of an interface-enhanced multi-layer composite conductive gel.
Fig. 2 is a stress-strain curve of a bilayer conductive gel with and without an added interfacial layer.
Fig. 3 is a cyclic stretching response of a bilayer conductive gel with and without an added interfacial layer.
Fig. 4 is a peel strength test of a bilayer conductive gel with and without an added interfacial layer.
FIG. 5 shows a strain sensing test of a double-layer conductive gel with and without an additional interfacial layer.
Detailed Description
The invention provides an interface-enhanced multilayer composite conductive gel and a preparation method thereof. The present invention will be described in further detail below in order to make the objects, technical solutions and effects of the present invention more clear and distinct. It should be understood that the specific embodiments described herein are for purposes of illustration only and are not intended to limit the scope of the invention.
The embodiment of the invention provides an interface-enhanced multilayer composite conductive gel, which comprises n gel layers and n-1 interface layers, wherein the n gel layers and the n-1 interface layers are alternately laminated, and sequentially comprise a first gel layer, a first interface layer, a second gel layer, a second interface layer, … …, an n-1 interface layer and an n gel layer along the lamination direction, wherein n is an integer greater than or equal to 2;
each interface layer independently comprises an interface conductive agent, and the interface conductive agent is a micro-nano material.
For example, when n is 5, the multi-layer composite conductive gel includes 5 gel layers and 4 interface layers, wherein the 5 gel layers and the 4 interface layers are alternately laminated, and the first gel layer 11, the first interface layer 12, the second gel layer 13, the second interface layer 14, the third gel layer 15, the third interface layer 16, the fourth gel layer 17, the fourth interface layer 18, and the fifth gel layer 19 are sequentially laminated along the lamination direction, as shown in fig. 1.
In this embodiment, the multi-layer composite conductive gel comprises a series of gel layers, and an interface layer introduced between the gel layers. The interfacial layer serves as a bonding interface between the gel layers, and an interlocking structural unit is constructed between adjacent gel layers. This is because effective hydrogen bonds and covalent bonds (e.g., hydrogen bonds between the PAAM host polymer segment and PEDOT: PSS) can be formed between the interfacial layer and the polymer material and other materials of the adjacent gel, and at the same time, since the interfacial layer material is micro-nano structure, a layer of interfacial structure with a rough surface can be formed, further increasing the contact area between the adjacent gel and the interfacial layer. The two functions effectively improve the contact area and the mutual bonding force between the adjacent gel layers by introducing the interface layer. The multi-layer composite conductive gel containing the interface layer of the embodiment has excellent stretchability, good tensile strength, good elastic modulus and higher toughness. Due to modulus matching between gel layers, an interface interlocking network and patch effect of interfaces, the multilayer composite conductive gel of the embodiment has excellent interface stability and good fatigue resistance. As a tensile strain sensor, it also has good conductivity, sensitive strain sensing performance, a wide strain response range, and excellent response stability.
In one embodiment, the n gel layers have a mechanical modulus from large to small: the first gel layer is greater than the second gel layer is greater than … … and greater than the nth gel layer. The n gel layers are arranged from the bottom layer to the top layer according to the size of the mechanical modulus, so that the multi-layer composite conductive gel has the characteristic of gradual change of modulus. Due to modulus matching between gel layers, an interface interlocking network and patch effect of interfaces, the multilayer composite conductive gel of the embodiment has excellent interface stability and good fatigue resistance.
In one embodiment, the multi-layer composite conductive gel is composed of a first gel layer, a first interface layer and a second gel layer which are sequentially stacked. That is, the multilayer composite conductive gel of the present embodiment is composed of a double-layer gel layer and an interface layer between the double-layer gel layers. The interfacial layer acts as a bonding interface between the gel layer and the gel layer, creating interlocking structural units between the double layer gel layer. The conductive gel of the double-layer structure containing the interface layer of this example has excellent stretchability, good tensile strength, good elastic modulus and higher toughness. The conductive gel of the embodiment has excellent interface stability and good fatigue resistance due to modulus matching between two gel layers, an interface interlocking network and a patch effect of an interface. As a tensile strain sensor, it also has good conductivity, sensitive strain sensing performance, a wide strain response range, and excellent response stability.
In one embodiment, each interface layer independently includes an interface conductive agent, which may be selected from one or more of a metal salt, a metal nanomaterial, a conductive polymer containing a dopant, a conductive carbon material, and the like. Wherein the metal salt is selected from one or more of potassium chloride (KCl), sodium chloride (NaCl), calcium chloride (CaCl 2), copper chloride (CuCl 2), ferric chloride (FeCl 3) and the like; the metal nano material can be one or more selected from nano silver wires, nano silver particles, nano silver flakes, nano gold wires, nano gold particles, nano gold flakes, nano copper particles, nano copper wires, nano copper sheets and the like; the conductive polymer is selected from one or more of Polyaniline (PANi), polypyrrole (Ppy) and poly 3, 4-ethylenedioxythiophene (PEDOT); the doping agent is selected from one or more of poly (styrenesulfonic acid), hydrochloric acid, sulfuric acid and citric acid. Wherein the materials of the interface layers of the layers can be the same or different.
In one embodiment, the thickness of each interfacial layer is between 50 nanometers and 50 microns, such as 50 nanometers, 0.01 microns, 3 microns, 10 microns, 20 microns, etc. The thickness of each interface layer can be the same or different. Further, the thickness of each interface layer is the same.
In one embodiment, each gel layer has a thickness of between 100 nanometers and 10 millimeters, such as a thickness of 100 nanometers, 500 nanometers, 800 nanometers, 1 micrometer, 10 micrometers, 1 millimeter, 10 millimeters, or the like. Wherein the thickness of each gel layer can be the same or different. Further, the thickness of each interface layer is the same.
The embodiment of the invention provides a preparation method of the interface-enhanced multilayer composite conductive gel, which comprises the following steps:
Preparing a first gel layer;
and sequentially preparing a first interface layer, a second gel layer, a second interface layer, … …, an n-1 interface layer and an n gel layer on the first gel layer to obtain the conductive gel, wherein n is an integer greater than or equal to 2.
In one embodiment, the method of preparing each gel layer is independently selected from one of a stencil method, a spin coating method, a spray coating method, a printing method, and the like.
The template method is to use a template of a fixed shape to surround the periphery of the gel layer, and to obtain a desired shape and thickness by pouring an appropriate amount of gel precursor solution and then solidifying.
The spin coating method is to spin-coat an appropriate amount of gel precursor solution on a substrate, followed by curing to obtain a desired shape and thickness.
The spraying method is to spray a proper amount of gel precursor solution on a substrate and then cure the gel precursor solution to obtain a required shape and thickness.
The printing method is to print gel precursor solution on a substrate in different shapes by using printing technologies such as 3D printing, screen printing or ink-jet printing, and then solidifying to obtain the required gel layer.
In one embodiment, the method of preparing the interfacial layer of each layer is independently selected from one of a template method, a spin coating method, a spray coating method, a printing method, and the like.
In one embodiment, n is 2, and the preparation method of the multilayer composite conductive gel comprises the following steps:
mixing 100 parts of a first solvent, 5-50 parts of a first polymer precursor, 0.1-10 parts of a first cross-linking agent, 0-20 parts of a first conductive agent and 0.01-20 parts of a first modulus regulator to obtain a first precursor solution;
Stirring the first precursor solution, and then carrying out prepolymerization for 1-60 minutes under the condition of heating at 25-90 ℃ or ultraviolet irradiation to obtain a first gel layer;
Taking interface conductive agent dispersion liquid on the first gel layer to form a first interface layer;
Mixing 100 parts of a second solvent, 1-50 parts of a second polymer precursor, 0.01-10 parts of a second crosslinking agent, 0-20 parts of a second conductive agent and 0.01-20 parts of a second modulus regulator to obtain a second precursor solution;
stirring the second precursor solution, and then taking the second precursor solution on the first interface layer, and carrying out prepolymerization for 1-60 minutes under the condition of heating at 25-90 ℃ or ultraviolet irradiation to form a second gel layer.
In this embodiment, the interfacial conductive agent dispersion liquid is composed of an interfacial conductive agent and an interfacial solvent. In one embodiment, the interfacial conductive agent is selected from one or more of metal salts, metal nanomaterials, conductive polymers containing dopants, conductive carbon materials, and the like. Wherein the metal salt is selected from one or more of potassium chloride (KCl), sodium chloride (NaCl), calcium chloride (CaCl 2), copper chloride (CuCl 2) and ferric chloride (FeCl 3); the metal nano material can be one or more selected from nano silver wires, nano silver particles, nano silver flakes, nano gold wires, nano gold particles, nano gold flakes, nano copper particles, nano copper wires, nano copper sheets and the like; the conductive polymer is selected from one or more of Polyaniline (PANi), polypyrrole (Ppy) and poly 3, 4-ethylenedioxythiophene (PEDOT); the doping agent is selected from one or more of poly (styrenesulfonic acid), hydrochloric acid, sulfuric acid and citric acid.
In one embodiment, the interfacial solvent is selected from one or more of deionized water, ethanol, methanol, isopropanol, isobutanol, and the like.
In one embodiment, the first and second polymer precursors are each independently selected from one or more of acrylamide, N-methylolacrylamide, dimethylacrylamide, polyvinyl alcohol, and the like.
In one embodiment, the first and second crosslinking agents are each independently selected from one or more of N, N' -dimethyl diacrylamide, polyethylene glycol diacrylate, methacryloylated gelatin, acrylated xanthan gum, ammonium persulfate, and the like.
In one embodiment, the first and second conductive agents are each independently selected from one or more of a metal salt, a metal nanomaterial, a conductive polymer containing a dopant, a conductive carbon material, and the like.
Wherein the metal salt is selected from one or more of potassium chloride (KCl), sodium chloride (NaCl), calcium chloride (CaCl 2), copper chloride (CuCl 2) and ferric chloride (FeCl 3); the metal nano material is one or more selected from nano silver wires, nano silver particles, nano silver sheets, nano gold wires, nano gold particles, nano gold sheets, nano copper wires, nano copper particles and nano copper sheets; the conductive polymer is selected from one or more of Polyaniline (PANi), polypyrrole (Ppy) and poly 3, 4-ethylenedioxythiophene (PEDOT); the doping agent is selected from one or more of poly (styrenesulfonic acid), hydrochloric acid, sulfuric acid and citric acid.
In one embodiment, the first and second modulus modifiers are each independently selected from one or more of polyvinylpyrrolidone (PVP), carboxylated cellulose nanowhiskers, carboxymethyl chitosan, metal-oxide micro-nanoparticles, and the like. Wherein the metal oxide micro-nano particles are selected from one or more of silicon dioxide, titanium dioxide, barium titanate, ferroferric oxide, zinc oxide, nickel oxide and other metal oxide micro-nano particles.
The embodiment of the invention provides a method for applying the interface-enhanced multilayer composite conductive gel to stretchable electronic equipment, soft robots and wearable equipment.
The invention is further illustrated by the following specific examples.
Example 1
This example proposes a bilayer composite conductive gel with an aqueous dispersion of poly (styrenesulfonic acid) -doped poly (3, 4-ethylenedioxythiophene) (PEDOT: PSS) microspheres (PEDOT: PSS microspheres 3 microns in diameter) as an interface, the preparation steps of the bilayer composite conductive gel being as follows:
first, a PANC precursor solution and PAVK precursor solution were prepared:
PANC precursor solution: 5.00g deionized water as solvent, 1.20g AAm polymer precursor, 0.05g NMA polymer precursor, 0.10g C-CNWs as modulus modifier were weighed into a glass beaker and subsequently stirred continuously at 70℃for 4 hours to dissolve all materials completely.
PAVK precursor solution: 5.00g deionized water as solvent, 1.20g AAm as polymer precursor, 0.10g PVP as modulus modifier, 0.03g KCl as conductive agent, 0.001g acrylated xanthan gum as crosslinking agent were weighed into a glass beaker and stirred for 2 hours to dissolve the mixture completely.
Then, 0.03g of PANC precursor solution is taken, 0.03g of ammonium persulfate is added as a cross-linking agent, the mixture is poured into a template after being uniformly stirred, and the template is put into an oven at 80 ℃ for pre-polymerization for 7 minutes, so that the PANC pre-polymerized gel layer is obtained. Next, 300. Mu.l of PEDOT/PSS aqueous dispersion (PEDOT: PSS concentration 1.2 wt%) was measured with a pipette and transferred to a spray gun. And after adjusting the distance and the speed of the spray gun, spraying the PANC prepolymer gel layer to form a PEDOT-PSS interface layer, wherein the thickness of the interface layer is 6 microns. Finally, 0.03g of ammonium persulfate cross-linking agent is added into the precursor solution of 0.03g PAVK g, and the mixture is poured onto the PEDOT/PSS interface layer after being uniformly stirred. And then, putting the mixture into an oven at 80 ℃ to be completely polymerized for 40 minutes for template method curing to form PAVK/PEDOT: PSS/PANC double-layer composite conductive gel.
Comparative example 1
This comparative example proposes a PANC monolayer conductive gel prepared by the following steps:
5.00g deionized water solvent, 1.20g AAm polymer precursor, 0.05g NMA polymer precursor, 0.10g C-CNWs modulus modifier were weighed into a glass beaker and stirred continuously at 70℃for 4 hours to allow complete dissolution of all materials. Then 0.03g of ammonium persulfate cross-linking agent is added, after being stirred uniformly, the mixture is poured into a template and put into an oven at 80 ℃ to be completely polymerized for 40 minutes, so as to form PANC single-layer conductive gel.
Comparative example 2
This comparative example proposes a PAVK single layer conductive gel prepared by the following steps:
5.00g deionized water as solvent, 1.20g AAm as polymer precursor, 0.10g PVP as modulus modifier, 0.03g KCl as conductive agent, 0.001g acrylated xanthan gum as crosslinking agent were weighed into a glass beaker and stirred for 2 hours to dissolve the mixture completely. Then 0.03g of ammonium persulfate cross-linking agent is added, after being stirred uniformly, the mixture is poured into a template and put into an oven at 80 ℃ to be completely polymerized for 40 minutes, so as to form PAVK single-layer conductive gel.
Comparative example 3
The comparative example proposes PAVK/PANC double-layer conductive gel, and the preparation steps of the conductive gel are as follows:
first, a PANC precursor solution and PAVK precursor solution were prepared:
PANC precursor solution: 5.00g deionized water as solvent, 1.20g AAm polymer precursor, 0.05g NMA polymer precursor, 0.10g C-CNWs as modulus modifier were weighed into a glass beaker and subsequently stirred continuously at 70℃for 4 hours to dissolve all materials completely.
PAVK precursor solution: 5.00g deionized water as solvent, 1.20g AAm as polymer precursor, 0.10g PVP as modulus modifier, 0.03g KCl as conductive agent, 0.001g acrylated xanthan gum as chemical cross-linking agent were weighed into a glass beaker and stirred for 2 hours to dissolve the mixture completely.
Then, 0.03g of PANC precursor solution is taken, 0.03g of ammonium persulfate cross-linking agent is added, the mixture is poured into a template after being stirred uniformly, and the template is put into an oven at 80 ℃ for pre-polymerization for 7 minutes, so that PANC pre-polymerized gel layer is obtained. Next, 0.03g of ammonium persulfate cross-linking agent was added to the precursor solution of 0.03g PAVK, and after stirring uniformly, poured onto the PANC pre-polymerized gel layer. Then, the mixture is put into an oven at 80 ℃ to be completely polymerized for 40 minutes for template method curing, and PAVK/PANC double-layer conductive gel is formed.
The conductive gels of example 1 and comparative examples 1 to 3 described above were tested and the test results were as follows:
FIG. 2 is a stress-strain curve of PANC, PAVK single layer conductive gel and PAVK/PANC and PAVK/PEDOT PSS/PANC double layer conductive gel. As shown in fig. 2 (a), the mechanical properties of the PANC single layer conductive gel are greater than those of the PAVK single layer conductive gel, and the mechanical properties of the PAVK/PANC double layer conductive gel prepared from these two layers of conductive gel lie between them. Subsequently, the introduction of the PEDOT/PSS interface layer can effectively enhance the interface toughness and the interface strength of PAVK/PANC double-layer conductive gel, so that the PAVK/PEDOT/PSS/PANC double-layer conductive gel has good mechanical properties (shown in (b) of fig. 2), the breaking strain is 1763.85%, the tensile strength is 0.92MPa, the elastic modulus is 69.16KPa, and the toughness is 9.27MJ/m 3.
FIG. 3 shows the cyclic stretching response of PAVK/PANC and PAVK/PEDOT: PSS/PANC bilayer conductive gels. As shown in fig. 3, when the PAVK/PANC double-layer conductive gel was tested for cyclic tensile response without any interface treatment, it was found to be less stable and only able to respond less than 2500 cycles. After the PEDOT-PSS interface layer is introduced, PAVK/PEDOT-PSS/PANC double-layer conductive gel can stably respond more than 12500 stretching loading-unloading cycles, which shows that the introduction of the PEDOT-PSS interface layer improves the interface strength and the interface stability of the PVAK/PANC double-layer conductive gel (see shown in figure 4).
FIG. 5 is a strain sensing test of PAVK/PEDOT: PSS/PANC bilayer conductive gel. The relationship between the applied strain during stretching and the relative resistance change of the sample is shown in fig. 5 (a), and a linear fit is performed. From the results, PAVK/PEDOT PSS/PANC bilayer conductive gel can respond to strain with a broad linear response range (0-445%). Through linear fitting results, a strain range of 0-445% can be obtained, and the strain coefficient (GF) is 4.28; for a strain range of 445-905%, the GF value increases to 9.71; after the strain reaches 1600%, the GF value reaches a maximum value of 18.14. The relative resistance change of the PANC/PEDOT: PSS/PAVK bilayer gel showed stable response peak shapes under both small and large strains (FIG. 5 (b)), indicating that the gel had good reproducibility and high sensitivity. Furthermore, PAVK/PEDOT PSS/PANC bilayer conductive gel was subjected to more than 12500 load-unload stretching cycles from 0 to 200% strain (FIG. 5 (c)). Experimental results show that PAVK/PEDOT-PSS/PANC double-layer gel has excellent cycle stability and durability.
Table 1 below shows the mechanical properties of the individual single-layer gels in comparison with the double-layer gels. As can be taken from table 1, the PANC monolayer gel exhibits the properties of a hard hydrogel, such as high modulus, high tensile strength, but lower ductility. PAVK single layer gels exhibit typical soft gel properties such as low modulus, low tensile strength, low toughness, but strong stretchability. After the two single-layer gels are compounded, the prepared PANC/PAVK double-layer conductive gel has good mechanical property and modulus adaptability. Subsequently, PEDOT and PSS interface layer are further introduced, so that the mechanical property of the double-layer hydrogel is further improved. In summary, by compounding the high modulus PANC monolayer gel with the low modulus PAVK monolayer gel and introducing the PEDOT: PSS interfacial layer, the PAVK/PEDOT: PSS/PANC composite bilayer gel combines soft water gel properties (good ductility and moderate modulus) with hard water gel properties (maintaining a certain strength and toughness), has a breaking strain of 1763.85%, a tensile strength of 0.92MPa, an elastic modulus of 69.16kPa, and a toughness of 9.27MJ/m 3.
TABLE 1
In summary, the invention provides a multilayer structure conductive gel with excellent mechanical interface stability, fatigue resistance, electrical stability and strain sensitivity. The multi-layer conductive gel is composed of a series of gel layers, and interlocking structural units are constructed between the two layers of gel by a prepolymerization technique and a spray technique. The conductive gel with the double-layer structure containing the PEDOT and PSS interface has excellent stretchability, good tensile strength, good elastic modulus and higher toughness. The resulting double-layer conductive gel exhibits excellent interfacial stability and good fatigue resistance due to modulus matching between the two-layer gels, interfacial interlocking network, and the patch effect of PEDOT: PSS. As a tensile strain sensor, it also exhibits good conductivity (not less than 1.76S/m), sensitive strain sensing performance (at least up to a strain coefficient of 10.46), a broad strain response range (0-445%) and excellent response stability (> 12,500 cycles). The above-described double-layer structured conductive gel with PEDOT: PSS interface can be used for promising materials for use in stretchable electronics, soft robots, and next generation wearable devices.
It is to be understood that the invention is not limited in its application to the examples described above, but is capable of modification and variation in light of the above teachings by those skilled in the art, and that all such modifications and variations are intended to be included within the scope of the appended claims.

Claims (9)

1. The interface-enhanced multilayer composite conductive gel is characterized by comprising n gel layers and n-1 interface layers, wherein the n gel layers and the n-1 interface layers are alternately laminated, and sequentially comprise a first gel layer, a first interface layer, a second gel layer, a second interface layer, … …, an n-1 interface layer and an n gel layer along the lamination direction, wherein n is an integer greater than or equal to 2;
each interface layer is independently composed of an interface conductive agent, wherein the interface conductive agent is a micro-nano material;
the interface conductive agent is selected from one or more of metal salt, conductive polymer and conductive polymer containing doping agent; the thickness of each interface layer is between 50 nanometers and 50 micrometers.
2. The interface enhanced multi-layer composite conductive gel of claim 1, wherein the n-layer gel layer has a mechanical modulus from large to small: the first gel layer is greater than the second gel layer is greater than … … and greater than the nth gel layer.
3. The interface-enhanced multilayer composite conductive gel of claim 1 or 2, wherein the multilayer composite conductive gel is composed of a first gel layer, a first interface layer, and a second gel layer, which are sequentially stacked.
4. The interface enhanced multi-layer composite conductive gel of claim 1, wherein each gel layer has a thickness between 100 nanometers and 10 millimeters.
5. A method of preparing the interface-enhanced multi-layer composite conductive gel of any one of claims 1-4, comprising the steps of:
Preparing a first gel layer;
sequentially preparing a first interface layer, a second gel layer, a second interface layer, … …, an n-1 interface layer and an n gel layer on the first gel layer to obtain the multilayer composite conductive gel, wherein n is an integer greater than or equal to 2.
6. The method for preparing the interface-enhanced multi-layer composite conductive gel according to claim 5, wherein the method for preparing each layer of gel layer is independently selected from one of a template method, a spin coating method, a spray coating method and a printing method, and the method for preparing each layer of interface layer is independently selected from one of a template method, a spin coating method, a spray coating method and a printing method.
7. The method for preparing an interface-enhanced multi-layer composite conductive gel according to claim 5, wherein n is 2, the method for preparing the multi-layer composite conductive gel comprising:
mixing 100 parts of a first solvent, 5-50 parts of a first polymer precursor, 0.1-10 parts of a first cross-linking agent, 0-20 parts of a first conductive agent and 0.01-20 parts of a first modulus regulator to obtain a first precursor solution;
Stirring the first precursor solution, and then carrying out prepolymerization for 1-60 minutes under the condition of heating at 25-90 ℃ or ultraviolet irradiation to obtain a first gel layer;
Taking interface conductive agent dispersion liquid on the first gel layer to form a first interface layer;
Mixing 100 parts of a second solvent, 1-50 parts of a second polymer precursor, 0.01-10 parts of a second crosslinking agent, 0-20 parts of a second conductive agent and 0.01-20 parts of a second modulus regulator to obtain a second precursor solution;
stirring the second precursor solution, and then taking the second precursor solution on the first interface layer, and carrying out prepolymerization for 1-60 minutes under the condition of heating at 25-90 ℃ or ultraviolet irradiation to form a second gel layer.
8. The method for preparing an interface-enhanced multilayer composite conductive gel according to claim 7, wherein the first polymer precursor and the second polymer precursor are each independently selected from one or more of acrylamide, N-methylolacrylamide, dimethylacrylamide, polyvinyl alcohol;
The first crosslinking agent and the second crosslinking agent are respectively and independently selected from one or more of N, N' -dimethyl diacrylamide, polyethylene glycol diacrylate, methacryloylated gelatin, acryloylated xanthan gum and ammonium persulfate;
the first conductive agent and the second conductive agent are each independently selected from one or more of a metal salt, a conductive polymer containing a dopant;
The first modulus regulator and the second modulus regulator are respectively and independently selected from one or more of polyvinylpyrrolidone, carboxylated cellulose nanowhisker, carboxymethyl chitosan and metal oxide micro-nano particles;
The first solvent and the second solvent are respectively and independently selected from one or more of deionized water, ethanol, methanol, isopropanol, isobutanol, glycerol and ethylene glycol.
9. The method for preparing an interface-enhanced multi-layer composite conductive gel according to claim 7, wherein the interface conductive agent dispersion liquid is composed of an interface conductive agent and an interface solvent;
The interface conductive agent is selected from one or more of metal salt, conductive polymer and conductive polymer containing doping agent;
The interfacial solvent is one or more selected from deionized water, ethanol, methanol, isopropanol, isobutanol, glycerol and ethylene glycol.
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Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108417296A (en) * 2018-03-20 2018-08-17 常州大学 A kind of stretchable conductive material of round-the-clock self-healing and preparation method thereof
CN113769120A (en) * 2021-09-18 2021-12-10 北京脑陆科技有限公司 Preparation method of double-layer conductive hydrogel
CN113773445A (en) * 2021-08-31 2021-12-10 北京工业大学 Preparation method and application of hydrogel flexible touch sensor

Patent Citations (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108417296A (en) * 2018-03-20 2018-08-17 常州大学 A kind of stretchable conductive material of round-the-clock self-healing and preparation method thereof
CN113773445A (en) * 2021-08-31 2021-12-10 北京工业大学 Preparation method and application of hydrogel flexible touch sensor
CN113769120A (en) * 2021-09-18 2021-12-10 北京脑陆科技有限公司 Preparation method of double-layer conductive hydrogel

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