CN115559019A - Elastic piezoresistive strain sensing fiber and preparation method and application thereof - Google Patents
Elastic piezoresistive strain sensing fiber and preparation method and application thereof Download PDFInfo
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/04—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers
- D01F8/10—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from synthetic polymers with at least one other macromolecular compound obtained by reactions only involving carbon-to-carbon unsaturated bonds as constituent
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/12—Stretch-spinning methods
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01D—MECHANICAL METHODS OR APPARATUS IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS
- D01D5/00—Formation of filaments, threads, or the like
- D01D5/24—Formation of filaments, threads, or the like with a hollow structure; Spinnerette packs therefor
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- D—TEXTILES; PAPER
- D01—NATURAL OR MAN-MADE THREADS OR FIBRES; SPINNING
- D01F—CHEMICAL FEATURES IN THE MANUFACTURE OF ARTIFICIAL FILAMENTS, THREADS, FIBRES, BRISTLES OR RIBBONS; APPARATUS SPECIALLY ADAPTED FOR THE MANUFACTURE OF CARBON FILAMENTS
- D01F8/00—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof
- D01F8/18—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from other substances
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/18—Measuring force or stress, in general using properties of piezo-resistive materials, i.e. materials of which the ohmic resistance varies according to changes in magnitude or direction of force applied to the material
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Abstract
The invention discloses an elastic piezoresistive strain sensing fiber and a preparation method and application thereof, wherein the sensing fiber has a coaxial structure, the outer layer of the sensing fiber is hydrogenated styrene-butadiene block copolymer hollow SEBS fiber prepared by a prefabricated part-hot stretching process, and the inner layer of the sensing fiber is a composite metal layer obtained by injecting copper particle doped gallium-based liquid metal obtained by internalization under the action of voltage into a hollow channel of the SEBS fiber. The preparation method is simple, high in production efficiency and suitable for large-scale production; the sensing fiber prepared by the method can be stretched and compressed, the electrical property of the sensing fiber is changed regularly in a larger stress range, and the sensing fiber has high sensitivity and good circulation stability and has good application prospect in the aspect of piezoresistive strain sensors; and the sensing fiber can be heated to more than 80 ℃ within 2min under the condition of applying 0.1-1V direct current voltage, has good joule heating effect and has potential application prospect in the aspect of preparing electric heaters.
Description
Technical Field
The invention relates to the technical field of flexible sensing material preparation, in particular to an elastic piezoresistive strain sensing fiber and a preparation method and application thereof.
Background
With the development of intelligent robots, wearable intelligent electronic products, human health monitoring and other fields, flexible and wearable sensing materials become research hotspots. The elastic conductor has high stretchability, and the resistance of the elastic conductor can change when the elastic conductor is stretched and compressed, so that the elastic conductor can respond to behavior actions or external stimuli, and has a good application prospect on wearable intelligent electronic products.
The patent CN110184731B discloses a fabric sensor with a negative pressure resistance effect and application thereof, the sensing effect of human body physiological information detection is realized by soaking various fabrics in a conductive material, although the elasticity of a base material is utilized in the method, the conductive material on the surface of the fabric is easy to fall off in the strain process, and the sensitivity of the corresponding sensor is gradually weakened; patent CN113804097a uses multilayer elastic composite layer to stably limit the high-efficiency conductive substance in the structure, the stretching performance is provided by elastic polymer material, in order to avoid the influence of the material on the conductivity, the ratio of the conductive substance needs to be increased, and the complex multilayer structure is not strong for capturing the human motion signal compared with the fabric. The elastic sensing material prepared based on the fabric or sheet flexible substrate cannot be applied to the small strain sensing field due to the limitation of sensitivity, and the integratability is poor. In order to improve the sensitivity and multifunctional integration of sensing functional materials, patent CN107167180B discloses an elastic fiber sensor and a preparation method thereof, wherein elastic fibers are impregnated in different functional materials to obtain elastic fibers with surfaces coated with tin dioxide/reduced graphene oxide composite materials, and the elastic fibers have the functions of strain sensing, gas sensing and photosensitive sensing, but the sensing materials prepared by compounding the functional materials and a substrate by an impregnation method generally have the problem of poor stability. Therefore, there is a need for an elastic sensing material with high sensitivity and good stability to meet the performance requirements of wearable intelligent electronic products for elastic sensing materials.
Disclosure of Invention
The invention aims to solve the technical problem of providing an elastic piezoresistive strain sensing fiber and a preparation method and application thereof.
In order to solve the technical problems, the invention provides the following technical scheme:
the invention provides an elastic piezoresistive strain sensing fiber, which has a coaxial structure, wherein an outer layer of the sensing fiber is a hydrogenated styrene-butadiene block copolymer hollow fiber, and an inner layer of the sensing fiber is copper particles doped with gallium-based liquid metal.
Further, the hydrogenated styrene-butadiene block copolymer hollow fiber is prepared by a hot drawing method, and the inner layer is obtained by injecting copper particles doped with gallium-based liquid metal into a hollow channel of the hydrogenated styrene-butadiene block copolymer hollow fiber.
Further, the hydrogenated styrene-butadiene block copolymer hollow fiber has a cross section of any regular or irregular shape, preferably a circle or a square.
Further, the hollow channel is of any regular or irregular shape, preferably circular or square.
Further, the cross section of the hollow channel is positioned in the central part of the cross section of the hollow fiber.
Furthermore, the area ratio of the cross section of the hollow fiber to the cross section of the hollow channel is 1.75-5.3 mm 2 ：1.256×10 5 μm 2 ～2.826×10 5 μm 2 。
The invention provides a method for preparing the elastic piezoresistive strain sensing fiber, which comprises the following steps:
(1) Adding copper powder and gallium-based liquid metal into a sodium hydroxide solution, and internalizing under the action of voltage to obtain copper particles doped with the gallium-based liquid metal; placing a mold filled with hydrogenated styrene-butadiene block copolymer (SEBS) particles in a vulcanizing machine, performing vulcanization treatment to obtain a solid rod, and drilling a round hole in the center of one end of the solid rod to obtain a prefabricated member;
(2) Putting the prefabricated member prepared in the step (1) into a wire drawing tower, and carrying out hot drawing treatment by taking one end of the prefabricated member without a round hole as an initial section to obtain a hydrogenated styrene-butadiene block copolymer hollow fiber; injecting the copper particle doped gallium-based liquid metal prepared in the step (1) into a hollow channel of the hydrogenated styrene-butadiene block copolymer hollow fiber, and sealing two ends to obtain the elastic piezoresistive strain sensing fiber.
Further, in the step (1), adding copper powder and gallium-based liquid metal into a sodium hydroxide solution, after layering, respectively fixing graphite electrodes of a direct current power supply in the gallium-based liquid metal and the sodium hydroxide solution, applying voltage, stirring the gallium-based liquid metal, and internalizing to obtain the copper particle doped gallium-based liquid metal.
Further, the mass ratio of the copper powder to the gallium-based liquid metal is 1:8 to 15.
Furthermore, the concentration of the sodium hydroxide solution is 1-1.5 mol/L.
Further, in the internalization process, the voltage is 5-7V, and the internalization time is 30-45 min.
Further, after the internalization is finished, the gallium-based liquid metal layer and the sodium hydroxide layer are separated, and the separated liquid metal is washed by deionized water and then dried in vacuum to obtain the stable copper particle doped gallium-based liquid metal.
Further, the temperature of the vacuum drying is 60-80 ℃, and the time is 3-5 h.
Further, in the step (1), the temperature of the vulcanization treatment is 190-220 ℃, and the pressure is 8-12MPa.
Furthermore, in the step (1), drying treatment is required before vulcanization of the SEBS particles, wherein the drying treatment temperature is 55-70 ℃, and the drying treatment time is 10-12 h.
Further, in the step (2), the inside of the drawing tower comprises an upper temperature zone, a middle temperature zone and a lower temperature zone, wherein the temperature of the upper temperature zone is 70-100 ℃, the temperature of the middle temperature zone is 190-210 ℃, and the temperature of the lower temperature zone is 170-190 ℃.
Furthermore, the advancing speed of the prefabricated rod in the hot drawing process is 0.8-4 mm/min, and the drawing speed is 1-5 m/min.
In one embodiment of the invention, in the step (1), the length of the solid rod is 15-20 cm, the cross section is square, the side length of the cross section is 20-30 mm, and the diameter of the round hole is 6-10 mm.
Further, in the step (2), the hydrogenated styrene-butadiene block copolymer hollow fiber has a square cross section, the side length of the cross section is 1.5 to 2.3mm, and the diameter of the hollow channel is 200 to 300 μm.
Further, the part without hollow pore channels at the lower end of the fiber is removed after hot drawing.
And further, inserting a lead into the hollow channel of the fiber, and sealing two ends to obtain the elastic piezoresistive strain sensing fiber.
The invention provides an application of the elastic piezoresistive strain sensing fiber in the first aspect in wearable intelligent electronic products and intelligent temperature-adjusting textiles.
The invention has the beneficial effects that:
1. according to the invention, a hydrogenated styrene-butadiene block copolymer is subjected to a hot stretching process to prepare a hollow fiber with a hollow channel, uniform copper particles obtained by internalization are doped with gallium-based liquid metal and injected into the hollow channel of the hollow fiber to obtain a stretchable and compressible multifunctional conductive elastic fiber with a coaxial structure, wherein the breaking tensile strain of the fiber is up to 850%; the preparation method has the advantages of simple and easily-controlled preparation process and high production efficiency, is suitable for large-scale production, and compared with the processes of dipping, coating and the like, the elastic fiber with the coaxial structure prepared by the preparation method can effectively protect the liquid metal in the inner layer through the fiber in the outer layer so as to avoid factors such as oxidation and the like from influencing the fluidity of the liquid metal and the conductivity of the liquid metal, thereby ensuring the sensitivity and the cycling stability of the sensing fiber.
2. The elastic fiber prepared by the invention has good elasticity and strain sensitivity, the hollow channel of the outer layer fiber is used for protecting and limiting the flow behavior of the liquid metal in different stress states, and when the fiber is stretched, the composite liquid metal in the channel is thinned in the length direction, the side length is reduced, the sectional area is reduced, and the resistance is increased; when the fiber is compressed, the collapse of the local channels causes a change in the electrical conductivity properties; under the tensile and compression states, the electrical property of the elastic fiber can be changed regularly in a large stress range, the long-term stability is shown, the elastic fiber can keep the long-term stable small-deformation sensing performance under the action of 1000 times of stretching under the frequency of 1Hz and 3000 times of pressure under the frequency of 1.5Hz, and the elastic fiber can be used as a strain sensor and has a good application prospect in wearable intelligent electronic products.
3. The elastic fiber prepared by the invention can be used as a strain sensor, has good thermal conductivity, can be heated to more than 80 ℃ within 2min after being applied with 0.1-1V voltage, shows stable Joule heat effect, and can realize rapid heating, thereby having potential application prospect in the aspects of intelligent temperature-adjusting textiles and the like.
Drawings
FIG. 1 is a schematic view of the process for preparing copper particles doped with liquid metal in example 1;
FIG. 2 is a schematic view of a process for preparing a sensor fiber in example 1;
fig. 3 is a scanning electron microscope image of the copper particles doped with gallium-based liquid metal prepared in example 1;
FIG. 4 is a side scanning electron microscope image of a sensing fiber prepared in example 1;
FIG. 5 is a cross-sectional scanning electron microscope image of a sensing fiber prepared in example 1;
FIG. 6 is a stress-strain curve during drawing of a sensing fiber prepared in example 1;
FIG. 7 is a tensile strain sensing performance curve of the sensing fiber prepared in example 1;
FIG. 8 is a compressive strain sensing performance curve of the sensing fiber prepared in example 1;
FIG. 9 is a temperature profile of the sensing fiber prepared in example 1 under an applied voltage;
FIG. 10 is a strain-conductivity curve for a sensing fiber prepared in example 1 and an undoped copper particle fiber prepared in comparative example 1;
fig. 11 is a strain-strain coefficient curve of the sensing fiber prepared in example 1 and the undoped copper particle fiber prepared in comparative example 1.
Description of the reference numerals: 1. a graphite electrode; 2. NaOH solution; 3. a liquid metal; 4. copper powder; 5. SEBS prefabricated member; 6. a wire drawing tower; 7. SEBS hollow fiber; 8. copper particles are doped with gallium-based liquid metal; 9. a sensing fiber; 10. fibers undoped with copper particles.
Detailed Description
Unless defined otherwise, all technical and scientific terms used herein have the same meaning as commonly understood by one of ordinary skill in the art to which this invention belongs. The terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used herein, the term "and/or" includes any and all combinations of one or more of the associated listed items.
The present invention is further described below in conjunction with the following figures and specific examples so that those skilled in the art may better understand the present invention and practice it, but the examples are not intended to limit the present invention.
The following raw material information used in the examples and comparative examples is as follows:
SEBS, model YH-503T, available from Zhongpetrochemical Baling petrochemical Co., ltd;
gallium-based liquid metal, model No. GF25498514-1EA, available from sigma aldrich (shanghai) trade ltd;
copper powder, model C103836-100g, available from Shanghai Allantin Biotechnology Ltd;
NaOH, available from Shanghai Aladdin Biotechnology Ltd under the designation 1310-73-2.
Example 1
The embodiment relates to a preparation method of an elastic piezoresistive strain sensing fiber, which comprises the following specific steps:
(1) Preparation of copper particle doped gallium-based liquid metal: 20g of gallium-based liquid metal and 2g of copper powder were added to 1mol/L of NaOH solution, respectively. Then, graphite electrodes of a direct current power supply are respectively fixed in the gallium-based liquid metal and the NaOH solution. After applying 5V, the liquid metal was gently stirred to accelerate the internalization process of the copper particles. The entire internalization process takes approximately 30 minutes. Finally, after separating the liquid metal, washing the liquid metal by deionized water, and drying the liquid metal in a vacuum oven at 70 ℃ for 3 hours to obtain stable copper particle doped gallium-based liquid metal;
preparing a prefabricated part: the SEBS granules were dried in an oven at 60 ℃ for 12 hours. And then placing the mold filled with the SEBS particles into a vulcanizing machine for hot pressing for 30 minutes, wherein the vulcanizing temperature of the vulcanizing machine is 200 ℃, and the pressure of the vulcanizing machine is 10MPa, so as to prepare a solid rod, and the size of the solid preform is 25mm multiplied by 15cm. And finally, drilling a round hole in the center of the solid rod to manufacture the SEBS prefabricated part, wherein the diameter of the round hole is 8mm.
(2) Preparing elastic piezoresistive strain sensing fibers: and (2) putting the SEBS prefabricated member with the round hole into a wire drawing tower, heating, and then carrying out hot drawing treatment by taking one end without the round hole of the prefabricated member as an initial section, wherein the prefabricated member is pushed in the wire drawing tower at the speed of 1mm/min and the wire drawing speed is 1m/min to obtain SEBS hollow fibers, and then injecting copper particle doped gallium-based liquid metal into the hollow channel of the SEBS fibers by using an injector. And finally, inserting copper wires into two ends of the hollow channel and sealing the two ends by using glue to prepare the elastic piezoresistive strain sensing fiber.
The scanning electron microscope image of the copper particle doped gallium-based liquid metal prepared in this example is shown in fig. 3, and the gallium and copper metal in the liquid metal realize uniform distribution under the polarization effect.
Scanning electron microscope images of the side surface and the cross section of the elastic piezoresistive strain sensing fiber prepared in the embodiment are respectively shown in fig. 4 and fig. 5, and it can be known from the figures that the SEBS fiber prepared by the hot stretching method has uniform thickness, the side length of the SEBS fiber is 1.77mm, the cross section of the SEBS fiber is well maintained, the injected copper particle doped gallium-based liquid metal is fully filled in the channel, and the diameter of the cross section of the hollow channel is 228.7 μm.
1. Mechanical Properties
The sensing fiber prepared in the embodiment with the length of 100mm is taken to test the stress-strain curve in the stretching process, corresponding data are obtained by testing through a universal material testing machine, and the stretching speed is 100mm/min. As shown in FIG. 6, the sensing fiber prepared in this example has a tensile strain at break of up to 850%, corresponding to a stress at break of over 5MPa, and exhibits excellent mechanical properties.
2. Strain sensing performance
In this embodiment, a digital multimeter and an electronic stepper were used to perform strain sensing performance testing on the optical fiber, and the sensing fiber prepared in this embodiment with a length of 40mm was used as a test sample.
Sensing tensile strain: the sample was repeatedly stretched over a range of tensile strain (150%) and the change in resistance and the sensing stability were recorded. As shown in FIG. 7, the relative resistance change of the sample was maintained in a stable range after 1000 cycles under the stretching action at a frequency of 1Hz, and the resistance change amount (. DELTA.R) after stretching and the initial resistance (R) were measured 0 ) The ratio of (A) to (B) is-120%.
Compressive strain sensing: the sample was repeatedly compressed within a fixed pressure range (0.12 MPa) and its resistance change and sensing stability were recorded. As shown in FIG. 8, the relative resistance change is highly stable after 3000 cycles under the compression effect of the frequency of 1.5Hz, and the resistance change (Δ R) and the initial resistance (R) after compression are both stable 0 ) The ratio of (A) to (B) is-150%.
3. Electric heating effect
The sensing fiber prepared in the embodiment with the length of 40mm is used as a test sample, leads at two ends are connected with a direct current power supply, and the electrothermal effect test is carried out by applying different direct current voltages (0.1-1V). The test result is shown in FIG. 9, the sensing fiber has a relatively obvious temperature rising behavior at the weak point supply (less than or equal to 0.2V), the direct current voltage is raised from 0 to 1V within 2min, and the temperature of the sensing fiber is raised from room temperature (23 ℃) to more than 80 ℃, thereby showing good electrothermal effect and thermal conductivity.
Comparative example 1
The comparative example relates to preparation of an elastic piezoresistive strain sensing fiber, the preparation method is consistent with that of the embodiment, only the inner layer liquid metal is different, and the elastic fiber is prepared by directly filling hollow channels of the hollow fiber with gallium-based liquid metal.
Sensitivity contrast
The sensing fibers prepared in example 1 and comparative example 1 with the length of 100mm are respectively taken as test samples, and the change conditions of the conductivity and the strain coefficient of different samples under the stretching action of 0-400 percent are researched. As shown in fig. 10 and 11 (fig. 9 is the sensing fiber prepared in example 1, fig. 10 is the sensing fiber prepared in comparative example 1), the conductivity σ (σ = L/(RS), L is the length of the material, R is the resistance value, and S is the area) of the sample increases with the increase of the strain value, and the conductivity change value of the sensing fiber prepared in example 1 is much larger than that of the sensing fiber prepared in comparative example 1, which indicates that the electrical conductivity of the strain sensing fiber in a tensile state can be improved by introducing copper particles into the gallium-based liquid metal according to the present invention; FIG. 11 shows the change of the strain coefficient GF with strain (GF = (Δ R/R) for different samples 0 ) [ epsilon ]. DELTA.R is the amount of resistance change, R 0 Which is the initial resistance, epsilon is the strain), it can be seen from the graph that the difference of the strain coefficients among different samples increases with the increase of the strain value, and when the strain increases to 400%, the strain coefficient of the sensing fiber prepared in example 1 increases to-664% compared with the sensing fiber prepared by undoped copper particles, which also shows that the introduction of the copper particles into the gallium-based liquid metal can effectively improve the strain sensitivity of the sensing fiber.
The above-mentioned embodiments are merely preferred embodiments for fully illustrating the present invention, and the scope of the present invention is not limited thereto. The equivalent substitution or change made by the technical personnel in the technical field on the basis of the invention is all within the protection scope of the invention. The protection scope of the invention is subject to the claims.
Claims (10)
1. An elastic piezoresistive strain sensing fiber is characterized in that the sensing fiber has a coaxial structure, the outer layer of the sensing fiber is a hydrogenated styrene-butadiene block copolymer hollow fiber, and the inner layer of the sensing fiber is copper particle doped gallium-based liquid metal.
2. A method of making an elastic piezoresistive strain sensing fibre according to claim 1, characterised in that it comprises the steps of:
(1) Adding copper powder and gallium-based liquid metal into a sodium hydroxide solution, and internalizing under the action of voltage to obtain copper particles doped with the gallium-based liquid metal; placing the die filled with the hydrogenated styrene-butadiene block copolymer particles in a vulcanizing machine, vulcanizing to obtain a solid rod, and drilling a circular hole in the center of one end of the solid rod to prepare a prefabricated member;
(2) Putting the prefabricated member prepared in the step (1) into a wire drawing tower, and carrying out hot drawing treatment by taking one end of the prefabricated member without a round hole as an initial section to obtain a hydrogenated styrene-butadiene block copolymer hollow fiber; injecting the copper particle doped gallium-based liquid metal prepared in the step (1) into a hollow channel of the hydrogenated styrene-butadiene block copolymer hollow fiber, and sealing two ends to obtain the elastic piezoresistive strain sensing fiber.
3. The preparation method according to claim 2, wherein in the step (1), copper powder and gallium-based liquid metal are added into a sodium hydroxide solution, after layering, graphite electrodes of a direct current power supply are respectively fixed in the gallium-based liquid metal and the sodium hydroxide solution, voltage is applied, the gallium-based liquid metal is stirred, and internalization is carried out to obtain the copper particle doped gallium-based liquid metal.
4. The production method according to claim 2 or 3, wherein the mass ratio of the copper powder to the gallium-based liquid metal is 1:8 to 15; the concentration of the sodium hydroxide solution is 1-1.5 mol/L.
5. The method according to claim 2 or 3, wherein the voltage is 5 to 7V and the time for internalization is 30 to 45min.
6. The production method according to claim 2, wherein in the step (1), the temperature of the vulcanization treatment is 190 to 220 ℃ and the pressure is 8 to 12MPa.
7. The method according to claim 2, wherein in the step (2), the drawing tower comprises an upper temperature zone, a middle temperature zone and a lower temperature zone, the temperature of the upper temperature zone is 70-100 ℃, the temperature of the middle temperature zone is 190-210 ℃, and the temperature of the lower temperature zone is 170-190 ℃.
8. The method according to claim 2, wherein in the step (2), the advancing speed of the preform during the hot drawing process is 0.8 to 4mm/min, and the drawing speed is 1 to 5m/min.
9. The preparation method according to claim 2, wherein in the step (1), the length of the solid rod is 15 to 20cm, the section is square, the side length of the section is 20 to 30mm, and the diameter of the circular hole is 6 to 10mm; in the step (2), the section of the hydrogenated styrene-butadiene block copolymer hollow fiber is square, the side length of the section is 1.5-2.3 mm, and the diameter of the hollow channel is 200-300 mu m.
10. Use of the elastic piezoresistive strain sensing fiber according to claim 1 in wearable smart electronics, smart temperature regulating textiles.
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