CN110681873A - Flexible strain sensor based on iron nanowires and preparation method thereof - Google Patents
Flexible strain sensor based on iron nanowires and preparation method thereof Download PDFInfo
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- CN110681873A CN110681873A CN201910984675.7A CN201910984675A CN110681873A CN 110681873 A CN110681873 A CN 110681873A CN 201910984675 A CN201910984675 A CN 201910984675A CN 110681873 A CN110681873 A CN 110681873A
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- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y15/00—Nanotechnology for interacting, sensing or actuating, e.g. quantum dots as markers in protein assays or molecular motors
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
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- B82Y40/00—Manufacture or treatment of nanostructures
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01B—MEASURING LENGTH, THICKNESS OR SIMILAR LINEAR DIMENSIONS; MEASURING ANGLES; MEASURING AREAS; MEASURING IRREGULARITIES OF SURFACES OR CONTOURS
- G01B7/00—Measuring arrangements characterised by the use of electric or magnetic techniques
- 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
- G01B7/18—Measuring arrangements characterised by the use of electric or magnetic techniques for measuring the deformation in a solid, e.g. by resistance strain gauge using change in resistance
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B22—CASTING; POWDER METALLURGY
- B22F—WORKING METALLIC POWDER; MANUFACTURE OF ARTICLES FROM METALLIC POWDER; MAKING METALLIC POWDER; APPARATUS OR DEVICES SPECIALLY ADAPTED FOR METALLIC POWDER
- B22F9/00—Making metallic powder or suspensions thereof
- B22F9/16—Making metallic powder or suspensions thereof using chemical processes
- B22F9/18—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds
- B22F9/24—Making metallic powder or suspensions thereof using chemical processes with reduction of metal compounds starting from liquid metal compounds, e.g. solutions
- B22F2009/245—Reduction reaction in an Ionic Liquid [IL]
Abstract
The invention relates to a flexible strain sensor based on iron nanowires and a preparation method thereof, belonging to the technical field of strain sensors, wherein the strain sensor comprises a PDMS (polydimethylsiloxane) matrix, an iron nanowire film and two electrode leads; the iron nanowire film is packaged in the PDMS substrate, the two electrode leads are respectively fixed at two ends of the iron nanowire film, one end of each of the two electrode leads, which is fixed with the iron nanowire film, is packaged in the PDMS substrate, and the other end of each of the two electrode leads penetrates out of the PDMS substrate and is located outside the PDMS substrate. When the iron nanowire film in the sensor is prepared, the diameter and the length-diameter ratio of the finally prepared iron nanowire can be regularly adjusted by controlling the injection speed of a reducing agent solution and the strength of an applied parallel magnetic field, so that the application requirement is met to the maximum extent, and the high-sensitivity flexible strain sensor is prepared.
Description
Technical Field
The invention belongs to the technical field of strain sensors, and particularly relates to a flexible strain sensor based on iron nanowires and a preparation method thereof.
Background
The flexible sensor has important application in the fields of artificial intelligence, next generation robots, wearable medical monitoring equipment, human body motion sensing and the like. Especially with the rapid development of artificial intelligence, sensors with high sensitivity and stability under large strain are required to facilitate communication between human users and robots.
The sensitive material is the key for improving the performance of the sensor, and at present, some nano materials with flexibility and conductivity are tried to be applied to the construction of the flexible wearable sensor in the field, and the nano materials mainly comprise graphene, carbon nano tubes, nano particles, metal nano wires and the like. However, the carbon nanotube and graphene sensors have the problems of complex preparation process and poor repeatability, and the nanoparticles have the problem of low sensing sensitivity. In contrast, metal nanowires generally have high aspect ratios, high conductivity, and flexibility, and are ideal potential materials for designing high-performance flexible tensile strain sensors. Royal jelly et al (Sheng Wang et al, Advanced Functional Materials, 2018,28(18):1707538) of the Gongxing Longgang group, university of Chinese science and technology reports that a novel multifunctional electronic skin is prepared by using silver nanowires as sensitive elements and Polyester (PET) film and Polydimethylsiloxane (PDMS) as substrates, and a Chinese patent with application number of CN201810698021.3 discloses a method for preparing a composite flexible stress sensor by using silver nanowire graphene fabric carbon. However, silver is expensive, resources are limited, and the preparation cost of the nano-wire is higher. Therefore, there is an urgent need for a metal nanowire with excellent performance and low cost.
Disclosure of Invention
In view of the above, an object of the present invention is to provide a flexible strain sensor based on iron nanowires; the other purpose is to provide a preparation method of the flexible strain sensor based on the iron nanowire.
In order to achieve the purpose, the invention provides the following technical scheme:
1. a flexible strain sensor based on iron nanowires comprises a PDMS matrix, an iron nanowire film and two electrode leads; the iron nanowire film is packaged in the PDMS substrate, the two electrode leads are respectively fixed at two ends of the iron nanowire film, one end of each of the two electrode leads, which is fixed with the iron nanowire film, is packaged in the PDMS substrate, and the other end of each of the two electrode leads penetrates out of the PDMS substrate and is located outside the PDMS substrate.
Preferably, the preparation method of the iron nanowire film is as follows:
(1) adding an iron salt solution into a reaction tank applied with a parallel magnetic field, then adding a reducing agent solution into the iron salt solution in an injection mode, reacting at room temperature after the reducing agent solution is injected, obtaining a black solid product, and cleaning and drying the black solid product to obtain the iron nanowire;
(2) and (2) dispersing the iron nanowire prepared in the step (1) in ethanol, pouring the solution on filter paper, and performing vacuum filtration to obtain the iron nanowire film.
Preferably, in the step (1), the strength of the parallel magnetic field is 10-180 mT, and the injection speed is 5-25 mL/s.
Preferably, in the step (1), the concentration of iron ions in the iron salt solution is 0.01-0.2 mol/L, the concentration of the reducing agent in the reducing agent solution is 0.8-4.8 mol/L, and the reaction time is 10-60 min.
Preferably, the ferric salt in the ferric salt solution is at least one of ferrous sulfate heptahydrate, ferric chloride, ferric sulfate, ferrous chloride or ferric nitrate; the reducing agent in the reducing agent solution is one of sodium borohydride, aluminum borohydride, potassium borohydride or hydrazine hydrate.
Preferably, in the step (1), the parallel magnetic field is applied by a permanent magnet; the injection adopts a syringe or a syringe pump.
Preferably, in the step (1), the cleaning specifically comprises: alternately cleaning with water and absolute ethyl alcohol until the pH value of the cleaning solution is neutral; the drying specifically comprises the following steps: and drying for 6-10 h at room temperature under the protection of nitrogen or argon.
Preferably, the two electrode leads are made of one of copper, silver or carbon.
2. The preparation method of the flexible strain sensor based on the iron nanowire comprises the following steps:
transferring the iron nanowire film to a semi-cured PDMS substrate, fixing two electrode leads at two ends of the iron nanowire film respectively through conductive silver adhesive, finally attaching the other semi-cured PDMS substrate to the iron nanowire film, and curing to obtain the flexible strain sensor based on the iron nanowire.
Preferably, the curing is specifically performed at 60-100 ℃ for 30-60 min.
The invention has the beneficial effects that: the invention provides a flexible strain sensor based on iron nanowires and a preparation method thereof, when an iron nanowire film in the sensor is prepared, the diameter and the length-diameter ratio of the finally prepared iron nanowires can be regularly adjusted by controlling the injection speed of a reducing agent solution and the strength of an applied parallel magnetic field, the principle of the flexible strain sensor is shown in figure 1, and as can be seen from figure 1, when iron salt meets a reducing agent, Fe meets the reducing agent2+Will be reduced to generate Fe core and a large amount of H2Bubbles, and Fe nuclei formed with H2The bubbles will combine to form a community (Fe nuclei-H)2Bubbles) to lower the surface energy, and the reaction is intensified when an excessive amount of reducing agent is injected, thereby instantaneously generating a large amount of Fe nuclei-H2Air bubbles, under the action of an external parallel magnetic field, dense Fe nuclei-H2The bubbles will be distributed along the magnetic field direction, and the Fe cores are combined with each other to form the iron nano-wires, because H exists between the iron nano-wires2The air bubbles are separated, so that the iron nanowires can be effectively prevented from being entangled or gathered, and the finally prepared iron nanowires have good monodispersity. Meanwhile, the faster the injection speed of the reducing agent solution is, the Fe nucleus-H is generated2The more bubbles, the more space between bubblesThe smaller; the higher the intensity of the external parallel magnetic field is, the Fe nucleus-H2The more orderly the bubbles are arranged, the diameter of the iron nanowire can be reduced and the length of the iron nanowire can be increased by utilizing the two factors, so that the length-diameter ratio of the iron nanowire is improved. In addition, the concentration of reactants is adjusted, the generation speed of iron cores and the self-assembly process can be further regulated, so that the diameter, the length-diameter ratio and the surface roughness of the iron nanowires are further regulated, the application requirements are met to the maximum degree, and the high-sensitivity flexible strain sensor is prepared.
Additional advantages, objects, and features of the invention will be set forth in part in the description which follows and in part will become apparent to those having ordinary skill in the art upon examination of the following or may be learned from practice of the invention. The objectives and other advantages of the invention may be realized and attained by the means of the instrumentalities and combinations particularly pointed out hereinafter.
Drawings
For the purposes of promoting a better understanding of the objects, aspects and advantages of the invention, reference will now be made to the following detailed description taken in conjunction with the accompanying drawings in which:
FIG. 1 is a schematic diagram of the aspect ratio control of iron nanowires in the present invention;
FIG. 2 is a schematic structural diagram of a flexible strain sensor based on iron nanowires in the invention;
FIG. 3 is a physical diagram of the flexible strain sensor based on iron nanowires prepared in example 1;
fig. 4 is an SEM image of iron nanowires prepared in example 1 at 1 ten thousand times;
FIG. 5 is a graph showing the trend of the relative resistance change of the flexible strain sensor based on iron nanowires according to the strain prepared in example 1;
FIG. 6 is a pictorial view of a flexible strain sensor based on iron nanowires prepared in example 2;
fig. 7 is an SEM image of iron nanowires prepared in example 2 at 1 ten thousand times;
FIG. 8 is a graph showing the trend of the relative resistance change of the flexible strain sensor based on iron nanowires according to the strain prepared in example 2;
FIG. 9 is a pictorial view of a flexible strain sensor based on iron nanowires prepared in example 3;
fig. 10 is an SEM image at 5000 x of the iron nanowires prepared in example 3;
fig. 11 is a graph of the relative resistance change trend with strain of the flexible strain sensor based on iron nanowires prepared in example 3.
Reference numbers in the figures: PDMS base member 1, iron nanowire membrane 2, electrode lead 3.
Detailed Description
The embodiments of the present invention are described below with reference to specific embodiments, and other advantages and effects of the present invention will be easily understood by those skilled in the art from the disclosure of the present specification. The invention is capable of other and different embodiments and of being practiced or of being carried out in various ways, and its several details are capable of modification in various respects, all without departing from the spirit and scope of the present invention.
Example 1
The utility model provides a flexible strain sensor based on iron nano wire, its structural schematic diagram is shown in fig. 2, the material object diagram is shown in fig. 3, this flexible strain sensor includes PDMS base member 1, iron nano wire membrane 2 and two electrode lead 3, wherein, iron nano wire membrane 2 encapsulates in PDMS base member 1, two electrode lead 3 are fixed respectively at iron nano wire membrane 2 both ends, the one end of fixing with iron nano wire membrane 2 among two electrode lead 3 encapsulates in PDMS base member 1, the other end wears out PDMS base member 1, be located outside PDMS base member 1. The flexible strain sensor is prepared by the following method:
(1) adding ferrous sulfate heptahydrate solution with the iron ion concentration of 0.08mol/L into a plastic reaction tank with permanent magnets arranged on two sides, adjusting the distance between the permanent magnets on two sides to enable the strength of a generated parallel magnetic field to be 180mT, then injecting sodium borohydride solution with the sodium borohydride concentration of 1.4mol/L into the ferrous sulfate heptahydrate solution through an injector at the speed of 25mL/s, reacting at room temperature for 30min after the sodium borohydride solution is injected, obtaining a black solid product, alternately cleaning the black solid product with water and absolute ethyl alcohol until the pH value of cleaning solution is neutral, and drying at room temperature for 8h under the protection of nitrogen to obtain the iron nanowire; an SEM image of the iron nanowire under 1 ten thousand times is shown in FIG. 4, and as can be seen from FIG. 4, the iron nanowire has a uniform structure, good dispersibility and a high length-diameter ratio;
(2) dispersing the iron nanowires prepared in the step (1) in ethanol, pouring the solution on filter paper, and performing vacuum filtration to prepare an iron nanowire film;
(3) mixing the PDMS-A component and the PDMS-B component according to A mass ratio of 10:1, stirring and dispersing, degassing for 10min at room temperature under vacuum to obtain A PDMS mixture, pouring the PDMS mixture without bubbles into an aluminum square mold, then smoothly placing the PDMS mixture into A drying oven, curing for 30min at 80 ℃ to obtain A semi-cured PDMS substrate, and preparing A semi-cured PDMS substrate by the same method;
(4) and (3) transferring the iron nanowire film prepared in the step (2) to a semi-cured PDMS substrate prepared in the step (3), fixing two copper foils at two ends of the iron nanowire film respectively through conductive silver paste, finally attaching another semi-cured PDMS substrate to the iron nanowire film, and curing at 80 ℃ for 45min to obtain the flexible strain sensor based on the iron nanowire, wherein the trend of the relative resistance change of the flexible strain sensor along with the change of strain is shown in FIG. 5, and as can be seen from FIG. 5, when the strain is 1.8%, the relative change rate of the resistance is 5.7, so that the sensitivity factor (GF ═ delta (delta R/R0)/delta epsilon) of the flexible strain sensor is 316.7.
Example 2
The utility model provides a flexible strain sensor based on iron nano wire, its structural schematic diagram is shown in fig. 2, the material object diagram is shown in fig. 6, this flexible strain sensor includes PDMS base member 1, iron nano wire membrane 2 and two electrode lead 3, wherein, iron nano wire membrane 2 encapsulates in PDMS base member 1, two electrode lead 3 are fixed respectively at iron nano wire membrane 2 both ends, the one end of fixing with iron nano wire membrane 2 among two electrode lead 3 encapsulates in PDMS base member 1, the other end wears out PDMS base member 1, be located PDMS base member 1 outside. The flexible strain sensor is prepared by the following method:
(1) adding an iron chloride solution with the iron ion concentration of 0.01mol/L into a plastic reaction tank with permanent magnets arranged on two sides, adjusting the distance between the permanent magnets on the two sides to enable the strength of a generated parallel magnetic field to be 120mT, then injecting a potassium borohydride solution with the potassium borohydride concentration of 0.8mol/L into the iron chloride solution through an injector at the speed of 15mL/s, reacting at room temperature for 10min after the injection of the potassium borohydride solution is finished to obtain a black solid product, alternately cleaning the black solid product with water and absolute ethyl alcohol until the pH value of a cleaning solution is neutral, and drying at room temperature for 6h under the protection of nitrogen to obtain an iron nanowire; an SEM image of the iron nanowire under 1 ten thousand times is shown in FIG. 7, and as can be seen from FIG. 7, the iron nanowire is good in linearity, uniform in structure, good in monodispersity and high in length-diameter ratio;
(2) dispersing the iron nanowires prepared in the step (1) in ethanol, pouring the solution on filter paper, and performing vacuum filtration to prepare an iron nanowire film;
(3) mixing the PDMS-A component and the PDMS-B component according to A mass ratio of 10:1, stirring and dispersing, degassing for 10min at room temperature under vacuum to obtain A PDMS mixture, pouring the PDMS mixture without bubbles into an aluminum square mold, then smoothly placing the PDMS mixture into A drying oven, curing for 30min at 80 ℃ to obtain A semi-cured PDMS substrate, and preparing A semi-cured PDMS substrate by the same method;
(4) transferring the iron nanowire film prepared in the step (2) to a semi-cured PDMS substrate prepared in the step (3), fixing two copper foils at two ends of the iron nanowire film respectively through conductive silver adhesive, and finally attaching the other semi-cured PDMS substrate to the iron nanowire film, curing for 60min at 60 ℃ to obtain the flexible strain sensor based on the iron nanowire, wherein the trend of the relative resistance change of the flexible strain sensor along with the change of strain is shown in FIG. 8, and as can be seen from FIG. 8, the sensitivity factor of the flexible strain sensor is 35.7, and the maximum tensile strain is 70%.
Example 3
The utility model provides a flexible strain sensor based on iron nano wire, its structural schematic diagram is shown in fig. 2, the material object diagram is shown in fig. 9, this flexible strain sensor includes PDMS base member 1, iron nano wire membrane 2 and two electrode lead 3, wherein, iron nano wire membrane 2 encapsulates in PDMS base member 1, two electrode lead 3 are fixed respectively at iron nano wire membrane 2 both ends, the one end of fixing with iron nano wire membrane 2 among two electrode lead 3 encapsulates in PDMS base member 1, the other end wears out PDMS base member 1, be located outside PDMS base member 1. The flexible strain sensor is prepared by the following method:
(1) adding an iron nitrate solution with the iron ion concentration of 0.2mol/L into a plastic reaction tank with permanent magnets arranged on two sides, adjusting the distance between the permanent magnets on the two sides to enable the strength of a generated parallel magnetic field to be 80mT, then injecting an aluminum borohydride solution with the aluminum borohydride concentration of 4.8mol/L into the iron nitrate solution at the speed of 10mL/s through an injector, reacting at room temperature for 60min after the aluminum borohydride solution is injected, obtaining a black solid product, alternately cleaning the black solid product with water and absolute ethyl alcohol until the pH value of a cleaning solution is neutral, and drying at room temperature for 10h under the protection of nitrogen to obtain an iron nanowire; an SEM image of the iron nanowire under 5000 times is shown in FIG. 10, and as can be seen from FIG. 10, the iron nanowire has good dispersibility, uniform structure and high length-diameter ratio;
(2) dispersing the iron nanowires prepared in the step (1) in ethanol, pouring the solution on filter paper, and performing vacuum filtration to prepare an iron nanowire film;
(3) mixing the PDMS-A component and the PDMS-B component according to A mass ratio of 10:1, stirring and dispersing, degassing for 10min at room temperature under vacuum to obtain A PDMS mixture, pouring the PDMS mixture without bubbles into an aluminum square mold, then smoothly placing the PDMS mixture into A drying oven, curing for 30min at 80 ℃ to obtain A semi-cured PDMS substrate, and preparing A semi-cured PDMS substrate by the same method;
(4) transferring the iron nanowire film prepared in the step (2) to a semi-cured PDMS substrate prepared in the step (3), fixing two copper foils at two ends of the iron nanowire film respectively through conductive silver adhesive, and finally attaching the other semi-cured PDMS substrate to the iron nanowire film, curing for 30min at 100 ℃ to obtain the flexible strain sensor based on the iron nanowire, wherein the trend of the relative resistance change of the flexible strain sensor along with the change of strain is shown in fig. 11, and fig. 11 shows that the sensitivity factor of the flexible strain sensor is 388.9, and the maximum tensile strain is 45%.
Finally, the above embodiments are only intended to illustrate the technical solutions of the present invention and not to limit the present invention, and although the present invention has been described in detail with reference to the preferred embodiments, it will be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions, and all of them should be covered by the claims of the present invention.
Claims (10)
1. The flexible strain sensor based on the iron nanowires is characterized by comprising a PDMS (polydimethylsiloxane) matrix, an iron nanowire film and two electrode leads; the iron nanowire film is packaged in the PDMS substrate, the two electrode leads are respectively fixed at two ends of the iron nanowire film, one end of each of the two electrode leads, which is fixed with the iron nanowire film, is packaged in the PDMS substrate, and the other end of each of the two electrode leads penetrates out of the PDMS substrate and is located outside the PDMS substrate.
2. The flexible strain sensor based on iron nanowires of claim 1, wherein the iron nanowire film is prepared by the following steps:
(1) adding an iron salt solution into a reaction tank applied with a parallel magnetic field, then adding a reducing agent solution into the iron salt solution in an injection mode, reacting at room temperature after the reducing agent solution is injected, obtaining a black solid product, and cleaning and drying the black solid product to obtain the iron nanowire;
(2) and (2) dispersing the iron nanowire prepared in the step (1) in ethanol, pouring the solution on filter paper, and performing vacuum filtration to obtain the iron nanowire film.
3. The flexible strain sensor based on iron nanowires of claim 2, wherein in step (1), the strength of the parallel magnetic field is 10-180 mT, and the injection speed is 5-25 mL/s.
4. The flexible strain sensor based on the iron nanowire as claimed in claim 3, wherein in the step (1), the concentration of iron ions in the iron salt solution is 0.01-0.2 mol/L, the concentration of the reducing agent in the reducing agent solution is 0.8-4.8 mol/L, and the reaction time is 10-60 min.
5. The flexible strain sensor based on iron nanowires of claim 4, wherein the iron salt in the iron salt solution is at least one of ferrous sulfate heptahydrate, ferric chloride, ferric sulfate, ferrous chloride or ferric nitrate; the reducing agent in the reducing agent solution is one of sodium borohydride, aluminum borohydride, potassium borohydride or hydrazine hydrate.
6. The flexible strain sensor based on iron nanowires of any of claims 2-5, wherein in step (1), the parallel magnetic field is applied by permanent magnet; the injection adopts a syringe or a syringe pump.
7. The flexible strain sensor based on iron nanowires of any one of claims 2-5, wherein in the step (1), the cleaning is specifically: alternately cleaning with water and absolute ethyl alcohol until the pH value of the cleaning solution is neutral; the drying specifically comprises the following steps: and drying for 6-10 h at room temperature under the protection of nitrogen or argon.
8. The flexible strain sensor based on iron nanowires of claim 1, wherein the two electrode leads are made of one of copper, silver or carbon.
9. The method for preparing the flexible strain sensor based on the iron nanowires, which is characterized by comprising the following steps:
transferring the iron nanowire film to a semi-cured PDMS substrate, fixing two electrode leads at two ends of the iron nanowire film respectively through conductive silver adhesive, finally attaching the other semi-cured PDMS substrate to the iron nanowire film, and curing to obtain the flexible strain sensor based on the iron nanowire.
10. The method according to claim 9, wherein the curing is carried out at 60 to 100 ℃ for 30 to 60 min.
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Application publication date: 20200114 |