CN115449101A - High-conductivity and high-environmental-stability strain sensing film and preparation method thereof - Google Patents
High-conductivity and high-environmental-stability strain sensing film and preparation method thereof Download PDFInfo
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- G01B7/16—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge
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Abstract
The invention discloses a high-conductivity and high-environmental-stability strain sensing film and a preparation method thereof, wherein the sensing film forms an integrated multilayer composite structure comprising: the conducting layer is enriched on the lower layer of the membrane, an isolation network layer is arranged above the conducting layer, and the outermost surface layer of the whole sensing membrane is a compact protective layer. The invention has excellent environmental stability, can realize continuous and stable conductive signal transmission even if the interference of complex environment is caused, and particularly has the characteristics of better waterproof performance, higher mechanical property, extremely high conductivity, excellent strain sensing performance, good repeatability and the like. The invention can be applied to various complicated environments including underwater, and effectively broadens and promotes the application of the strain sensing film in a plurality of fields such as the preparation of intelligent sensing equipment, strain sensing monitoring equipment, underwater real-time monitoring equipment, underwater artificial intelligence technology and the like.
Description
Technical Field
The invention relates to the technical field of conductor materials, in particular to a strain sensing film with high conductivity and high environmental stability and a preparation method thereof.
Background
In recent years, flexible strain sensing films have attracted attention due to their great potential in the fields of electronic soft mechanical devices, artificial intelligence technology, human health and motion monitoring, and the like. Conventional strain sensing films based on metal or semiconductor materials have narrow strain ranges (strain is generally less than 5%) and high stiffness, which cannot meet the requirements of intelligent wearable devices. The flexible electronic device has the characteristics of unique ductility, information transmission, low-cost manufacturing process and the like, and is concerned in the fields of information, energy, medical treatment, national defense and the like.
At present, the mainstream design idea of the flexible strain sensor is to convert the deformation of the sensor into the change of the conductivity. It is common practice to incorporate conductive nanomaterials (e.g., carbon black, graphene, carbon nanotubes, metal nanowires, flakes, particles, etc.) into elastomeric polymers such as rubbers, gels, etc. as sensing materials. By this approach, flexible sensors with a more controllable sensing range compared to conventional sensors have been achieved. However, the interaction between the commonly used conductive nano-materials (such as carbon black, graphene, carbon nanotubes, etc.) and the elastic polymer is generally weak, and it is difficult to construct a uniformly dispersed, completely continuous three-dimensional conductive network in the matrix. In order to improve the conductivity and sensitivity of the flexible sensor, the amount of the conductive nano material is increased, which causes a problem in production cost. Therefore, it is still a challenge to prepare a flexible sensor with a larger sensing range and higher sensitivity while reducing the amount of expensive conductive nano-materials.
While the coated flexible sensor that has been commercially produced at present has obvious advantages in terms of conductive stability and production cost, the interaction between the commonly used coated conductive nano-materials (such as carbon black, graphene, carbon nanotubes, metal nanowires, sheets, particles, etc.) and the elastic substrate is generally weak, and mostly van der waals force or hydrogen bond interaction, which makes the coated flexible sensor have great limitations in wear resistance and use environment. In addition, the conductive coating layer and the elastic base layer do not have uniform changes in elongation under the same external force, which makes it difficult to transmit a stable strain signal as a stable strain sensor.
And as the human society gradually steps into the 5G information era, higher requirements are put forward on flexible sensing materials in order to meet the applicability of the artificial intelligence technology in various environments. For example, when people use flexible wearable equipment in complex environments such as high humidity or apply artificial intelligence technology to deep sea detection, the environmental stability of the material becomes the key of the technology, but because the complex environment greatly interferes with electric signals and corrodes the base material, for example, most of traditional flexible sensors absorb water and swell in water, the mechanical property becomes poor, and even the sensing property is completely lost, the development of the sensors in the fields facing the complex environment and underwater application is seriously hindered.
The prior literature on multilayer electrically conductive sensing films is retrieved as follows:
1. a high-strength high-conductivity laminated silicone rubber composite material and a preparation method thereof; application No.: CN202111359209.3; and (3) abstract: a high-strength high-conductivity layered silicone rubber composite material and a preparation method thereof are disclosed, wherein a carbon cloth/silicone rubber conducting layer A, a rubber conducting layer C taking silver-plated copper powder as a conducting filler, and a silicone rubber tensile layer B taking nickel nanowires and graphene as reinforcement are adopted; and alternately paving the conducting layer and the tensile layer into a mould to form a multilayer ABC multilayer structure, and carrying out hot-press vulcanization and two-stage vulcanization to form the rubber sheet. The method has the advantages of simple technical route, low cost, no interface problem between layers, and good mechanical property and excellent conductivity of the obtained conductive rubber material. The density of ABC three-layer conductive silicone rubber with the thickness of 2mm is as low as 1.8g/cm & lt 3 & gt, the resistivity can be as low as 0.01 omega-cm, the tensile strength can reach more than 4.12MPa, the right-angle tearing strength can reach more than 12.9N/mm, and the X-band electromagnetic shielding effectiveness can reach more than 50 dB. The material can be applied to electronic devices and aircrafts and used as an electromagnetic shielding sealing material with high conductivity and high strength requirements.
2. A multilayer anisotropic conductive film and a method for producing the same; application No.: CN200610021066.4; and (3) abstract: an Anisotropic conductive Film (ACAF-Anisotropic conductive Action Film) having a functional multilayer structure and a method for manufacturing the same, comprising a resin surface monomer coating layer, a metal particle sub-layer, and a low temperature hot melt resin layer with good insulation property, wherein the monomer layer is: butyl acrylate, methyl acrylate, diethylene glycol acrylate, 2-ethyl per caproic acid tetramethyl butyl ester, the metal particle resin layer and the low temperature hot melt resin layer are as follows: the high-precision ACAF is obtained by coating copolymer of phenoxy resin, novolac epoxy resin, acrylate rubber, styrene-butadiene rubber elastomer, long-chain imidazole derivative, mike Luo Poer AV conductive particles and toluene/ethyl acetate mixed solvent on different resins, and the chemical property, the physical property and the electrical property of the ACAF can meet the bonding and packaging connection requirements of 0.18-0.13 micron chips and high-density COF circuits.
In the prior document, the multilayer conductive rubber film is prepared in the forms of coating, hot-press compounding and the like, the integrity is poor, the interlayer can not be tightly combined, and the defects are still existed.
Disclosure of Invention
The invention provides a high-conductivity and high-environmental-stability strain sensing membrane, which has excellent environmental stability, can realize continuous and stable conductive signal transmission even if the interference of complex environment is caused, and particularly has the characteristics of better waterproof performance, higher mechanical property, extremely high conductivity, excellent strain sensing performance, good repeatability and the like. The invention can be applied to various complicated environments including underwater, and effectively broadens and promotes the application of the strain sensing film in a plurality of fields such as the preparation of intelligent sensing equipment, strain sensing monitoring equipment, underwater real-time monitoring equipment, underwater artificial intelligence technology and the like.
The technical scheme of the invention is as follows:
high electrically conductive, high environmental stability's strain sensing membrane, the multilayer composite structure that the sensing membrane formed an organic whole includes: the conducting layer is enriched on the lower layer of the membrane, an isolation network layer is arranged above the conducting layer, and the outermost surface layer of the whole sensing membrane is a compact protective layer.
The conducting layer is formed by uniformly depositing nano conducting filler at the bottom of the elastic matrix.
The isolation network layer is formed by dispersing a biomass dispersing agent in an elastic matrix.
The elastic matrix comprises one or a mixture of more of natural rubber, epoxidized natural rubber, styrene butadiene rubber, nitrile butadiene rubber or silicon rubber.
The biomass dispersant comprises: sodium lignosulfonate, calcium lignosulfonate, and other lignin derivatives; chitosan, carboxymethyl chitosan and other chitosan derivatives; carboxymethyl cellulose and other carboxymethyl cellulose derivatives; one or more of the above.
The preparation method of the high-environmental-stability strain conductance sensing film comprises the following steps:
(1) Under the condition of room temperature, taking a biomass dispersing agent, and mixing and stirring the biomass dispersing agent and deionized water uniformly to obtain a biomass dispersing solution; adding the nano conductive filler into the biomass dispersion solution, and uniformly mixing to obtain a conductive mixed solution;
(2) Stirring an elastic matrix raw material, slowly adding the conductive mixed liquid obtained in the step (1) into the elastic matrix raw material in a stirring state, then carrying out vacuum defoaming, pouring into a film-forming mould, standing, and putting into a constant-temperature oven for drying to obtain a flexible sensing film;
(3) And (3) immersing the flexible sensing film obtained in the step (2) into deionized water, taking out the flexible sensing film, and drying the flexible sensing film in a forced air drying oven to constant weight to obtain the sensing film.
Calculating according to parts by weight: 15 parts of a biomass dispersing agent; 100 parts of deionized water; 1-7 parts of nano conductive filler; 100 parts of elastic matrix raw material; the solid content of the raw material emulsion of the elastic matrix is 50 wt percent.
The principle of the invention is as follows:
the invention relates to a high-conductivity and high-environmental-stability strain sensing film, which is an integrated layered structure and comprises the following parts from an inner layer to a surface: the conductive layer with ultrahigh conductivity is formed by uniformly depositing nano conductive filler at the bottom of the elastic matrix, so that ultrahigh conductivity is provided; the enhanced isolation network layer formed by dispersing the biomass auxiliary dispersing agent in the elastomer matrix can provide a good protection effect for the whole material; and a compact rubber water-resistant layer formed on the surface layer of the sensing film after water-resistant treatment, so as to provide hydrophobicity for the material.
The biomass auxiliary dispersing agent is the key for assisting the uniform deposition of the nano conductive filler and forming the conductive layer, the conductive filler is firstly mutually dispersed in a solution instead of an agglomeration state, and the biomass auxiliary dispersing agent does not provide strong interaction to enable the conductive filler to maintain a uniformly dispersed state in a latex solution in the film forming process, but assists the deposition of the conductive filler and finally forms a conductive enrichment layer. Meanwhile, the biomass auxiliary dispersing agent also forms a continuous network penetrating through the whole material, thereby providing great mechanical strength improvement for the material. The continuous network structure construction process is as follows: the main body of the rubber composite material is prepared by biomass material and rubber latex, wherein the biomass material is positioned on the interface of latex particles and is not randomly arranged in a matrix. During the film forming process, under the influence of the volume exclusion effect, latex particles are mutually close to each other and extruded, and biomass molecules filled in gaps are dispersed among the latex particles and form a continuous isolation network. Meanwhile, in order to solve the problem that natural polymers in a natural polymer/rubber composite material are easy to dissolve in water, so that the whole material is difficult to be practically applied in a water environment, a part of natural polymers on the surface of the material are removed by soaking in water for a short time, and then a high-temperature heating means is used for promoting the rubber layer on the surface of the material to be healed to form a compact protective thin layer of pure rubber, wherein the process is called a water-resistant treatment process. The method is based on the treatment method that natural macromolecules in a natural macromolecule/rubber composite material are uniformly dispersed or form an isolation network structure, the biomass material on the surface of the composite material is dissolved first instead of being dissolved completely by short-time soaking treatment, then the composite film is taken out in time, rubber on the surface of the composite film is promoted to extend and cover by heating, and finally a rubber protective layer covering the whole composite film is formed.
The invention has the beneficial effects that:
1. the high-conductivity and high-environmental-stability strain sensing membrane has excellent environmental stability, can realize continuous and stable conductive signal transmission even under the interference of complex environment, and particularly has the characteristics of better waterproof performance, higher mechanical property, extremely high conductivity, excellent strain sensing performance, good repeatability and the like.
2. The preparation method of the invention needs mild environment, does not need harsh conditions for production, and can be suitable for being converted into large-scale industrial production.
3. The invention has high environmental stability, especially excellent waterproof performance, so that the application of the strain sensing film in the fields of preparing intelligent sensing equipment, strain sensing monitoring equipment, underwater real-time monitoring equipment, electronic skin, underwater real-time monitoring action change equipment, underwater artificial intelligent equipment and the like can be effectively widened and promoted; wide application range and great potential.
4. The invention can use less conductive material, prepare flexible material with excellent conductivity, and reduce the manufacturing cost of the flexible material greatly.
Drawings
FIG. 1 is a schematic view of a cut-away multilayer structure according to the present invention; as can be seen from fig. 1, the integrated layered structure comprises: the innermost layer is a conducting layer with ultrahigh conductivity, which is formed by uniformly depositing nano conducting filler at the bottom of a carboxylic styrene butadiene rubber matrix, and the thickness of the conducting layer is about 10 to 100 micrometers; the middle layer is a reinforced isolation network layer formed by dispersing sodium lignosulfonate in carboxylic styrene butadiene rubber; the surface layer is a compact rubber water-resistant layer formed on the surface layer of the sensing film after water-resistant treatment, and the thickness of the compact rubber water-resistant layer is about 10 microns;
FIG. 2 is a scanning electron micrograph of a cross-section of example 3 after cold extraction; (conductive layer region);
FIG. 3 is a scanning electron micrograph of a cross-section of example 3 after cold extraction; (conductive layer and isolated network layer regions);
FIG. 4 is a schematic representation of a scanning electron microscope showing the cross-section of example 3 after cold extraction; (isolated network layer and dense protection layer regions);
FIG. 5 shows the mechanical property curves for example 1 (XSBR/rSL-1 AgNWs), example 2 (XSBR/rSL-3 AgNWs), example 3 (XSBR/rSL-5 AgNWs), example 4 (XSBR/rSL-7 AgNWs) according to the present invention;
FIG. 6 shows the mechanical property test comparisons between comparative example 6 pure carboxylated styrene-butadiene rubber film (XSBR), comparative example 1 (XSBR/rSL), comparative example 2 (XSBR/5 AgNWs) and example 3 (XSBR/rSL-5 AgNWs);
FIG. 7 shows a comparison of mechanical properties of comparative example 1 (XSBR/rSL) and comparative example 3 (XSBR/rSL-5 AgNWs) after soaking in water for 4 hours, 1 day, and 7 days;
FIG. 8 is a comparative picture of comparative example 3 and example 3 after soaking in water for 7 days;
FIG. 9 shows the stress-strain curves of example 3 after soaking in water for various periods of time;
FIG. 10 is a graph showing the trend of the conductivity of example 4;
FIG. 11 is a graph showing sensitivity factor (GF) curves at different elongations for example 3;
FIG. 12 shows the response time of example 3;
FIG. 13 shows the frequency dependence of example 3 on 0.5% strain;
FIG. 14 is a graph showing the resistance change in the underwater finger bending motion monitoring according to example 3;
FIG. 15 is a graph showing the resistance change in the air monitored by the finger bending movement in example 3;
in the drawings, the names of reference numbers are: 11-a conductive layer; 12-an isolated network layer; 13-dense protective layer.
Detailed Description
Example one
Step (1): dispersing 1.5g of sodium lignosulfonate in 100ml of deionized water, and uniformly stirring to obtain a sodium lignosulfonate solution; and adding the silver nanowire 0.1 g into the sodium lignosulfonate solution and uniformly mixing to obtain the sodium lignosulfonate/silver nanowire mixed solution.
Step (2): slowly adding the obtained sodium lignosulfonate/silver nanowire mixed solution into 20g of carboxylic styrene butadiene rubber emulsion under a stirring state, and continuously stirring for 30 minutes at the rotation speed of 600-1000rpm; then vacuum defoaming is carried out in a planetary vacuum defoaming machine, the rotating speed is 1600 multiplied by 2400rpm, and the time is 5 minutes. Pouring the mixture into a film forming mould for standing, and then putting the mixture into a constant-temperature oven at 40 ℃ for drying to obtain the carboxylic styrene-butadiene rubber/sodium lignosulfonate/silver nanowire flexible film;
and (3): and (3) taking the dried carboxylic styrene butadiene rubber/sodium lignosulfonate/silver nanowire flexible film obtained in the step (2), immersing the film in deionized water for 4 hours, taking out the composite film, and drying the composite film in a 60 ℃ oven to constant weight.
Example two
The difference from the embodiment 1 is that: in the step (1), adding the silver nanowire 0.3 g into the sodium lignosulfonate solution and uniformly mixing to obtain the sodium lignosulfonate/silver nanowire mixed solution.
EXAMPLE III
The difference from the example 1 is that: in the step (1), the silver nanowire 0.5g is added into the sodium lignosulfonate solution and mixed evenly to obtain the sodium lignosulfonate/silver nanowire mixed solution.
Example four
The difference from the embodiment 1 is that: in the step (1), 0.7g of silver nanowire is added into the sodium lignosulfonate solution and uniformly mixed to obtain the sodium lignosulfonate/silver nanowire mixed solution.
Comparative example 1
Dispersing 1.5g of sodium lignosulfonate in 100ml of deionized water, and uniformly stirring to obtain a sodium lignosulfonate solution; slowly adding the obtained sodium lignosulfonate solution into 20g of carboxylic styrene-butadiene rubber emulsion under the stirring state, and continuously stirring for 30 minutes at the rotation speed of 600-1000rpm. Then vacuum defoaming is carried out in a planetary vacuum defoaming machine, the rotating speed is 1600 multiplied by 2400rpm, and the time is 5 minutes. And pouring the mixture into a film forming mould for standing, and then putting the film forming mould into a constant-temperature oven at 40 ℃ for drying to obtain the carboxylic styrene butadiene rubber/sodium lignosulphonate flexible composite film.
Comparative example No. two
0.5g of silver nanowires is dispersed by 100ml of deionized water, and then directly added into 20g of carboxylic styrene butadiene rubber emulsion, and continuously stirred for 30min. And then vacuum defoaming is carried out in a planetary vacuum defoaming machine, the solution is poured into a film forming mold for standing, and then the film is placed into a constant temperature oven at 40 ℃ for drying until the weight is constant, so as to obtain the carboxylic styrene butadiene rubber/silver nanowire film.
Comparative example No. three
Step (1): dispersing 1.5g of sodium lignosulfonate in 100ml of deionized water, and uniformly stirring to obtain a sodium lignosulfonate solution; adding the silver nanowire 0.5g into the sodium lignosulfonate solution and uniformly mixing to obtain a sodium lignosulfonate/silver nanowire mixed solution;
step (2): slowly adding the obtained sodium lignosulfonate/silver nanowire mixed solution into 20g of carboxylic styrene butadiene rubber emulsion under the stirring state, continuously stirring, then carrying out vacuum defoaming in a planetary vacuum defoaming machine, pouring into a film forming mold for standing, and then putting into a constant-temperature oven at 40 ℃ for drying until the weight is constant to obtain the carboxylic styrene butadiene rubber/sodium lignosulfonate/silver nanowire flexible film.
Comparative example No. four
The difference from example 3 is that: and (3) taking the dried carboxylic styrene butadiene rubber/sodium lignosulfonate/silver nanowire flexible film obtained in the step (2), and soaking in deionized water for 1 day.
Comparative example five
The difference from example 3 is that: and (3) taking the dried carboxylic styrene butadiene rubber/sodium lignosulfonate/silver nanowire flexible film obtained in the step (2), and soaking in deionized water for 7 days.
Comparative example VI
20g of carboxylic styrene-butadiene latex is subjected to vacuum defoaming in a planetary vacuum defoaming machine, poured into a film forming mold for standing, and then placed into a constant-temperature oven at 40 ℃ for drying until the weight is constant, so that the carboxylic styrene-butadiene rubber film is obtained.
The application example is as follows:
the mechanical property comparison test process and method are as follows:
a material to be tested is taken and cut into dumbbell-shaped test pieces with the length, width and height of 75 multiplied by 4 multiplied by 0.5mm by a dumbbell-shaped cutter, and a tensile test is carried out on a stretching machine, wherein the stretching speed is 50mm/min.
The mechanical test results obtained are given in the following table:
As can be seen from the combination of FIG. 5 and FIG. 6, the stress of the ordinary carboxylated styrene-butadiene rubber is about 4.3MPa, and the elongation is about 370%;
the stress of the carboxylic styrene butadiene rubber/sodium lignosulfonate composite film is about 9.0 MPa, and the elongation is about 360%;
the stress of the carboxylic styrene-butadiene rubber/sodium lignosulfonate/silver nanowire composite film without water-resistant treatment is about 10.2MPa, and the elongation is about 350%;
the stress of the carboxyl styrene-butadiene rubber/sodium lignosulfonate/silver nanowire sensing film subjected to the water-resistant treatment is about 10.5MPa, and the elongation is about 350%;
therefore, the mechanical property of the composite film is greatly improved by adding the sodium lignosulfonate, and the mechanical property of the whole material is not negatively influenced by adding the silver nanowires due to the formation of the integrated layered structure; the whole mechanical property of the sensing film is not influenced by the water-resistant treatment process.
Hydrophobicity comparison test procedure and method are as follows:
the gravimetric method is used for testing the weight loss rate of the sensing membrane before and after the sensing membrane is soaked in deionized water for different time in the water-resistant treatment process. The weight loss rate calculation method is as follows: firstly, placing a sample cut by a cutter in a constant-temperature oven at 40 ℃ to be dried to constant weight to obtain the initial mass of the sample, then soaking the sample in a sample bottle filled with deionized water and respectively standing for 4 hours, 1 day and 7 days, then taking out the sample and drying to constant weight to obtain the mass of the soaked sample. The weight loss ratio (Wr) calculation formula is as follows:
in the formula, m 0 Is the initial weight of the composite rubber film, m 1 The dry mass after soaking. The results for each of the above samples are the average of three tests.
(1) The flexible sensing membrane of example 3 was cut into samples of 50 × 10 × 0.5mm in length, width and height by a cutter, and immersed in a sample bottle containing deionized water, and the solubility behavior was continuously observed and the weight loss rate after immersion for various periods of time was measured.
(2) The flexible film of comparative example 3 was cut into samples each having a length, width and height of 50X 10X 0.5mm by a cutter, and immersed in a sample bottle containing deionized water, and the solubility behavior thereof was continuously observed and the weight loss rate thereof after immersion for various periods of time was measured.
The test results are shown in the following table:
watch two
As can be seen from Table two, the sensor film without water-resistant treatment (XSBR/rSL-5 AgNWs) underwent a small weight loss of about 2.1% when soaked in water for 4 hours, indicating that the soaking treatment for a short time can dissolve the sodium lignosulfonate on the surface layer of the sensor film in water. The weight loss rate is obviously increased along with the prolonging of the soaking time, the weight loss rate reaches 10.9 percent after soaking for one day, the weight loss rate of the composite membrane basically reaches 15.3 percent of the maximum value after soaking for 7 days, namely the content of the sodium lignin sulfonate in the composite material.
On the contrary, the carboxylic styrene-butadiene rubber/sodium lignosulfonate/silver nanowire composite membrane after the water-resistant treatment is soaked in water for 7 days, and the quality is kept basically stable. Example 3 the weight loss rate after seven days of soaking only reached 1.7%. This shows that the carboxylic styrene-butadiene rubber/sodium lignosulfonate/silver nanowire sensing film after the water-resistant treatment can keep long-term stability in the water environment.
FIG. 8 is a physical representation of comparative example 3 (XSBR/rSL-5 AgNWs without water-resistant treatment) and example 3 (XSBR/rSL-5 AgNWs) after being soaked in an aqueous solution for 1 day, and the aqueous solution of the carboxylated styrene-butadiene rubber/sodium lignosulfonate/silver nanowire composite film without water-resistant treatment turns brown, which is the color of sodium lignosulfonate dissolved in water. And the soaking solution of the carboxylic styrene butadiene rubber/sodium lignosulfonate/silver nanowire sensing film after water treatment is still clear and transparent.
FIG. 9 is a comparison of mechanical properties of the flexible strain sensing film of example 3 after soaking in water for 1 day, 3 days, and 7 days, respectively. As can be seen from the figure, the mechanical properties of the flexible sensing film are not substantially changed along with the prolonging of the soaking time, and the strain sensing film after soaking for 7 days still has the strain of 10.2MPa and the elongation of 355 percent. This result indicates that the flexible sensing membrane has very high stability in water and still maintains high mechanical strength.
FIG. 10 is a conductivity test of the upper and lower surfaces of a flexible strain sensing membrane. The upper and lower faces of the sensing membrane exhibited complete absence based on the formation of an integral layered structureThe same conductive capability. As example 4 (XSBR/rSL-7 AgNWs), the conductivity of the conductive layer reached 1500S/m, while the conductivity of the bulk layer structure (isolated network layer) remained at 1X 10 -7 And (5) S/m. The conductive layer with ultrahigh conductivity can effectively transmit electric signals in a more complex environment, and the main body layer with higher resistance can provide good protection for the conductive layer.
FIG. 11 is a graph of sensitivity factors of flexible strain sensing films under water at different stretch ratios. When the tensile strain is less than 50%, the relative resistance change is proportional to the elongation, and the sensitivity factor GF 1 About 4.96. Sensitivity factor GF when the strain is greater than 100% 2 About 44. The reliability and the accuracy of the flexible strain sensor for testing the human motion are ensured.
Fig. 12 is a response time of the flexible strain sensing film to 0.5% strain when stretched at a stretcher stretching rate of 500mm/min, and it can be seen that the response stretching time is respectively 115 milliseconds, ensuring a rapid response to external stimuli.
Fig. 13 is a graph of the stretch-release cycle at 0.5% strain for a flexible strain sensing film, and it can be seen that the sensor responds stably to a tensile force at 0.5% strain, and is consistent in relative resistance change, exhibiting high reliability to mechanical deformation.
FIG. 14 shows that when the flexible strain sensing film is fixed at the finger joint and the finger bending motion detection is performed in an underwater environment, the relative resistance changes of the finger under different bending degrees show obvious differences, and the flexible strain sensing film has good discrimination for the finger bending motion in the underwater environment.
Fig. 15 shows that when the flexible strain sensing film is fixed at the finger joint and the finger bending motion detection is performed in the air environment, the relative resistance changes of the finger under different bending degrees show obvious differences, and the flexible strain sensing film has good discrimination for the finger bending motion in the air environment.
Various embodiments of the present invention have been described above with respect to carboxylated styrene-butadiene rubber/sodium lignosulfonate/silver nanowire flexible sensing films. The foregoing description is exemplary rather than exhaustive and is not limited to the disclosed embodiments. Many modifications and variations will be apparent to those of ordinary skill in the art without departing from the scope and spirit of the described embodiments. The terminology used herein is chosen in order to best explain the principles of the embodiments, the practical application, or improvements made to the technology in the marketplace, or to enable others of ordinary skill in the art to understand the embodiments disclosed herein.
Claims (10)
1. A highly conductive, highly environmentally stable strain sensing film characterized in that the sensing film forms an integral multilayer composite structure comprising: the conducting layer is enriched on the lower layer of the membrane, an isolation network layer is arranged above the conducting layer, and the outermost surface layer of the whole sensing membrane is a compact protective layer.
2. The high environmental stability strain conductance sensing film according to claim 1, wherein said conductive layer is formed by uniformly depositing nano conductive filler on the bottom of the elastic matrix.
3. The highly conductive, highly environmentally stable strain sensing film of claim 1, wherein the isolating network layer is formed by dispersing a biomass dispersing agent in an elastomeric matrix.
4. A highly conductive, highly environmentally stable strain sensing film according to claim 2 or 3, wherein said elastomeric matrix comprises one or more blends of natural rubber, epoxidized natural rubber, styrene butadiene rubber, nitrile butadiene rubber or silicone rubber.
5. The highly conductive, highly environmentally stable strain sensing film of claim 3, wherein the biomass dispersant comprises: sodium lignosulfonate, calcium lignosulfonate, and other lignin derivatives; chitosan, carboxymethyl chitosan and other chitosan derivatives; carboxymethyl cellulose and other carboxymethyl cellulose derivatives or one or more mixtures thereof.
6. The highly conductive and environmentally stable strain sensing film of claim 2, wherein the nano conductive filler is one or a combination of two or more of carbon nanotubes, graphene, MXenes, conductive carbon black, metal nanowires, metal nanoparticles, or metal nanosheets.
7. The highly conductive, highly environmentally stable strain sensing film of claim 1, wherein the method of making comprises the steps of:
under the condition of room temperature, taking a biomass dispersing agent, and mixing and stirring the biomass dispersing agent and deionized water uniformly to obtain a biomass dispersing solution; adding the nano conductive filler into the biomass dispersion solution, and uniformly mixing to obtain a conductive mixed solution;
stirring an elastic matrix raw material, slowly adding the conductive mixed liquid obtained in the step (1) into the elastic matrix raw material in a stirring state, then carrying out vacuum defoaming, pouring into a film-forming mould, standing, and putting into a constant-temperature oven for drying to obtain a flexible sensing film;
and (3) immersing the flexible sensing film obtained in the step (2) into deionized water, taking out the flexible sensing film, and drying the flexible sensing film in a forced air drying oven to constant weight to obtain the sensing film.
8. The method for preparing a highly conductive and environmentally stable strain sensing film according to claim 7, wherein the method comprises the following steps: 15 parts of biomass dispersing agent; 100 parts of deionized water; 1-7 parts of nano conductive filler; the raw material of the elastic matrix is 100 parts.
9. The method for preparing the highly conductive and environmentally stable strain sensing film according to claim 6, wherein in the step (3), the soaking reaction time is 4 to 24 hours; the drying temperature of the air-blast drying oven is 40-60 ℃, and the drying time is 24-48 hours.
10. The highly conductive and environmentally stable strain sensing film as claimed in claim 1, wherein the film is applied to electronic skin, underwater environment real-time monitoring motion change equipment and underwater artificial intelligence equipment.
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| AU2020101386A4 (en) * | 2020-07-16 | 2020-08-20 | Shaanxi University Of Science & Technology | A Biomimetic multifunctional flexible sensor based on skin collagen aggregate and its manufacturing method |
| CN113861538A (en) * | 2021-09-30 | 2021-12-31 | 华南理工大学 | Self-repairing conductive ring oxidized natural rubber composite material and preparation method thereof |
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| AU2020101386A4 (en) * | 2020-07-16 | 2020-08-20 | Shaanxi University Of Science & Technology | A Biomimetic multifunctional flexible sensor based on skin collagen aggregate and its manufacturing method |
| CN113861538A (en) * | 2021-09-30 | 2021-12-31 | 华南理工大学 | Self-repairing conductive ring oxidized natural rubber composite material and preparation method thereof |
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