CN111171573A - Preparation method of super-hydrophobic strain sensor composite material - Google Patents
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Abstract
The invention discloses a preparation method of a super-hydrophobic strain sensor composite material. According to the invention, fluorinated polydimethylsiloxane is introduced to serve as a building block, and then the super-hydrophobic stretchable sensor is prepared on the basis of a mixture of the fluorinated polydimethylsiloxane, perfluoropolyether and carbon nanotubes. The prepared samples showed stable response, remained superhydrophobic even after extensive cyclic stretching, scraping, hand rubbing, sandpaper abrasion, heat treatment at 200 ℃, acid/base/salt attack and high-speed drop/water jet, and had excellent mechanical strength and liquid impact resistance. In addition, as a wearable strain sensor, the sample can maintain excellent sensitivity, durability and repeatability when detecting finger or wrist bending, neck bending and blinking, and provides a reliable basis for the development of the strain gauge sensor.
Description
Technical Field
The invention belongs to the technical field of preparation of super-hydrophobic composite materials, and particularly relates to a preparation method of a composite material of a super-hydrophobic strain sensor based on fluorinated polydimethylsiloxane.
Background
At present, the stretchable sensor has great potential application value in the fields of artificial skin, human motion detection, electronics and the like. Generally stretchable sensors can be prepared by incorporating conductive fillers (e.g. metal nanomaterials, graphene, carbon nanotubes) into an elastomeric polymer. Carbon nanotubes, in particular, have been widely used in stretchable sensing applications due to the excellent electrical and mechanical properties of the conductive materials. While the CNT-based strain sensor shows both high sensitivity (-35) and excellent stretchability (45%). However, strain sensors are susceptible to degradation when subjected to harsh environments such as moisture, acidic, and alkaline environments. And strain sensors with superhydrophobic properties are receiving increasing attention. Since superhydrophobicity is achieved by a combination of low surface energy materials and micro or nano-scale textures, most artificial superhydrophobic materials cannot withstand mechanical abrasion due to destruction of micro or nano structures. Furthermore, poor resistance to high velocity water jets or droplet impingement is another key factor that prevents the practical application of superhydrophobic materials. In recent years, many efforts have been made to construct superhydrophobic wearable sensors. Despite significant advances, there are still few superhydrophobic scalable sensors with excellent mechanical strength and excellent chemical resistance.
Disclosure of Invention
The invention aims to provide a preparation method of a composite material of a super-hydrophobic strain sensor based on fluorinated polydimethylsiloxane
A preparation method of a super-hydrophobic strain sensor composite material comprises the following steps:
(1) dissolving heptafluorobutyric acid in tetrahydrofuran, stirring for 0.7-1.5h, adding tetraethoxysilane, stirring for 2.5-3.5h, and naturally drying the mixed solution in an evaporation pan to obtain a fluorinated curing agent;
(2) dissolving perfluorooctyl triethoxysilane in dimethylformamide, stirring the solution for 1.5-3h, adding carbon nanotubes, performing ultrasonic treatment for 20-40min, magnetically stirring for 4-8h, pouring the solution into an evaporation dish, naturally drying in the air, and collecting to obtain hydrophobic carbon nanotube powder;
(3) dispersing carbon nanofibers in tetrahydrofuran, adding polydimethylsiloxane, stirring for 1-3h, and performing ultrasonic treatment for 20-40min to obtain a polydimethylsiloxane solution;
(4) dispersing a fluorinated curing agent in tetrahydrofuran, stirring for 0.5-1.5h, and then mixing a polydimethylsiloxane solution with a fluorinated curing agent suspension by ultrasonic treatment for 20-40 min;
(5) adding perfluoropolyether into the suspension, adding dibutyltin dilaurate as a curing catalyst, carrying out ultrasonic treatment on the solution for 3-8min, and stirring for 4-6 h; the perfluoropolyether is used for the polyfluorinated carbon nanotube to improve the mechanical flexibility;
(6) casting the solution prepared in the step (5) into a Teflon mold, making the solution semi-solidified after 15-25min at room temperature, then uniformly spreading hydrophobic carbon nanotube powder on the surface of a semi-solidified sample by means of a copper net, after 6-9h, completely solidifying the sample, and taking out the obtained super-hydrophobic strain sensor composite material from the mold; the hydrophobic carbon nanotube powder was uniformly spread on the surface of the semi-cured sample to ensure the stretchability of the material.
The dosage mass ratio of the heptafluorobutyric acid, the tetrahydrofuran and the tetraethoxysilane in the step (1) is 3: (20-40): (3-8).
The mass ratio of the perfluorooctyl triethoxysilane to the dimethylformamide to the carbon nano tube in the step (2) is 1: (40-60): (0.5-2).
The mass ratio of the carbon nanofibers, tetrahydrofuran and polydimethylsiloxane in the step (3) is 3: (40-60): (40-60).
The using amount mass ratio of the perfluoropolyether to the dibutyltin dilaurate in the step (5) is (3-5): 1.
the mesh size of the copper mesh is 200 #.
The invention has the beneficial effects that: the invention reduces the surface energy without sacrificing the stretchability by grafting the fluorine group to the polydimethylsiloxane backbone, further improves the hydrophobicity by perfluoropolyether, and effectively improves the mechanical flexibility and liquid impact resistance. Finally, carbon nanotubes are introduced into the KFS polymer to achieve superhydrophobicity and carbon nanotube powder is sprinkled on the semi-cured KFS polymer to make it stable superhydrophobicity also after stretching. The sample remained superhydrophobic even after 1000 cycles of stretching to 200% strain, and the mechanical strength of the prepared superhydrophobic material was qualitatively evaluated by scratch and hand rub tests. The super-hydrophobicity was not lost except for the abrasion resistance test of the sandpaper for 300 cycles (60m) and the chemical corrosion attack and the thermal attack, confirming that it has excellent mechanical strength and thermal stability. In addition, it is obtained by high-speed water drop and water jet test to have excellent impact resistance. In summary, the polyfluorination strategy imparts unprecedented liquid impact resistance and excellent mechanical properties to the polydimethylsiloxane matrix. Meanwhile, as a wearable strain sensor, the sample can keep excellent sensitivity, durability and repeatability when detecting bending of fingers or wrists, bending of necks and blinking of eyes, and provides a reliable basis for development of a super-hydrophobic strain gauge sensor.
Drawings
Fig. 1 is a schematic diagram of a strain gauge sensor and a schematic diagram of a sample after being stretched by 100% and 200%.
Fig. 2 shows contact angles and rolling angles of strain gauge sensors under different tensile conditions.
Fig. 3 is a scanning electron micrograph of a strain gauge sensor.
FIG. 4 is a water contact angle and a water roll angle of a strain gauge sensor after scratching, finger wiping, abrasive paper abrasion, and taped glass.
Fig. 5 is a water drop and water impact experiment of a strain gauge sensor.
Fig. 6 is a graph showing the change in resistance of a strain gauge sensor after cyclic stretching and the real-time change in relative resistance to detect human behavior.
Detailed Description
The present invention is further described with reference to the following figures and specific examples, but it should be understood that the scope of the present invention is not limited to the specific embodiments.
Example 1
A preparation method of a super-hydrophobic strain sensor composite material comprises the following steps:
(1) dissolving 0.3g of heptafluorobutyric acid in 3g of tetrahydrofuran, stirring for 1h, then adding 0.5g of tetraethoxysilane, stirring for 3h, and naturally drying the mixed solution in an evaporation pan to obtain a fluorinated curing agent;
(2) dissolving 0.2g of perfluorooctyl triethoxysilane in 10g of dimethylformamide, stirring the solution for 2 hours, then adding 0.2g of carbon nanotubes, carrying out ultrasonic treatment on the solution based on the carbon nanotubes for 30 minutes in order to ensure uniformity, carrying out magnetic stirring for 6 hours, then pouring the solution based on the carbon nanotubes into an evaporation dish, naturally drying in the air, synthesizing and collecting to obtain hydrophobic carbon nanotube powder;
(3) dispersing 0.3g of carbon nanofibers for polymer toughening in 5g of tetrahydrofuran, then adding 5g of polydimethylsiloxane and stirring for 2h and carrying out ultrasonic treatment for 30min to form a polydimethylsiloxane solution;
(4) dispersing 0.8g of fluorinated curing agent in 3g of tetrahydrofuran, stirring for 1h, and then mixing polydimethylsiloxane solution and fluorinated curing agent suspension by ultrasonic treatment for 30 min;
(5) adding 0.2g of perfluoropolyether into the suspension, further adding 0.05g of dibutyltin dilaurate as a curing catalyst, finally carrying out ultrasonic treatment on the solution for 5min and stirring for 5 h;
(6) the final solution was cast into a teflon mold, and after 20min at room temperature, it became semi-cured, and then hydrophobic carbon nanotube powder was uniformly spread on the surface of the semi-cured sample by means of a copper mesh (200#), and after 8h, the sample was completely cured and taken out of the mold to obtain the desired superhydrophobic strain sensor composite.
Example 2
A preparation method of a super-hydrophobic strain sensor composite material comprises the following steps:
(1) dissolving 0.3g of heptafluorobutyric acid in 3.5g of tetrahydrofuran, stirring for 1.2h, then adding 0.5g of tetraethoxysilane, stirring for 3h, and naturally drying the mixed solution in an evaporation pan to obtain a fluorinated curing agent;
(2) dissolving 0.2g of perfluorooctyl triethoxysilane in 12g of dimethylformamide, stirring the solution for 1.8h, then adding 0.2g of carbon nanotubes, carrying out ultrasonic treatment on the solution based on the carbon nanotubes for 30min in order to ensure uniformity, magnetically stirring for 6h, then pouring the solution based on the carbon nanotubes into an evaporation dish, naturally drying in the air, and synthesizing and collecting to obtain hydrophobic carbon nanotube powder;
(3) dispersing 0.3g of carbon nanofibers for polymer toughening in 6g of tetrahydrofuran, then adding 5g of polydimethylsiloxane and stirring for 2h and carrying out ultrasonic treatment for 30min to form a polydimethylsiloxane solution;
(4) dispersing 0.8g of fluorinated curing agent in 3g of tetrahydrofuran and stirring for 1.2h, and then mixing polydimethylsiloxane solution and fluorinated curing agent suspension by ultrasonic treatment for 30 min;
(5) adding 0.2g of perfluoropolyether into the suspension, further adding 0.08g of dibutyltin dilaurate as a curing catalyst, finally carrying out ultrasonic treatment on the solution for 5min and stirring for 5 h;
(6) the final solution was cast into a teflon mold, and after 25min at room temperature, it became semi-cured, then hydrophobic carbon nanotube powder was uniformly spread on the surface of the semi-cured sample by means of a copper mesh (200#), and after 7h, the sample was completely cured and taken out of the mold to obtain the desired superhydrophobic strain sensor composite.
Example 3
A preparation method of a super-hydrophobic strain sensor composite material comprises the following steps:
(1) dissolving 0.25g of heptafluorobutyric acid in 3g of tetrahydrofuran, stirring for 0.9h, then adding 0.5g of tetraethoxysilane, stirring for 3h, and naturally drying the mixed solution in an evaporation pan to obtain a fluorinated curing agent;
(2) dissolving 0.25g of perfluorooctyl triethoxysilane in 12g of dimethylformamide, stirring the solution for 2.5 hours, then adding 0.25g of carbon nanotubes, carrying out ultrasonic treatment on the solution based on the carbon nanotubes for 30 minutes in order to ensure uniformity, magnetically stirring for 5 hours, then pouring the solution based on the carbon nanotubes into an evaporation dish, naturally drying in the air, and synthesizing and collecting to obtain hydrophobic carbon nanotube powder;
(3) dispersing 0.3g of carbon nanofibers for polymer toughening in 6g of tetrahydrofuran, then adding 6g of polydimethylsiloxane and stirring for 2.5h and carrying out ultrasonic treatment for 30min to form a polydimethylsiloxane solution;
(4) dispersing 0.7g of fluorinated curing agent in 3g of tetrahydrofuran and stirring for 1.5h, and then mixing polydimethylsiloxane solution and fluorinated curing agent suspension by ultrasonic treatment for 30 min;
(5) adding 0.3g of perfluoropolyether into the suspension, further adding 0.04g of dibutyltin dilaurate as a curing catalyst, finally carrying out ultrasonic treatment on the solution for 5min and stirring for 5 h;
(6) the final solution was cast into a teflon mold, and after 30min at room temperature, it became semi-cured, then hydrophobic carbon nanotube powder was uniformly spread on the surface of the semi-cured sample by means of a copper mesh (200#), and after 9h, the sample was completely cured and taken out of the mold to obtain the desired superhydrophobic strain sensor composite.
Example 4
A preparation method of a super-hydrophobic strain sensor composite material comprises the following steps:
(1) dissolving 0.35g of heptafluorobutyric acid in 5g of tetrahydrofuran, stirring for 1h, then adding 0.5g of tetraethoxysilane, stirring for 2.5h, and naturally drying the mixed solution in an evaporation pan to obtain a fluorinated curing agent;
(2) dissolving 0.18g of perfluorooctyl triethoxysilane in 10g of dimethylformamide, stirring the solution for 2.3h, then adding 0.18g of carbon nanotubes, carrying out ultrasonic treatment on the solution based on the carbon nanotubes for 30min in order to ensure uniformity, magnetically stirring for 6.5h, then pouring the solution based on the carbon nanotubes into an evaporation dish, naturally drying in the air, and synthesizing and collecting to obtain hydrophobic carbon nanotube powder;
(3) dispersing 0.35g of carbon nanofibers for polymer toughening in 5.5g of tetrahydrofuran, then adding 5g of polydimethylsiloxane and stirring for 2h and carrying out ultrasonic treatment for 30min to form a polydimethylsiloxane solution;
(4) dispersing 0.7g of fluorinated curing agent in 3.2g of tetrahydrofuran and stirring for 1.2h, then mixing the polydimethylsiloxane solution with the fluorinated curing agent suspension by ultrasonic treatment for 30 min;
(5) adding 0.2g of perfluoropolyether into the suspension, further adding 0.07g of dibutyltin dilaurate as a curing catalyst, finally carrying out ultrasonic treatment on the solution for 5min and stirring for 5 h;
(6) the final solution was cast into a teflon mold, and after 18min at room temperature, it became semi-cured, then hydrophobic carbon nanotube powder was uniformly spread on the surface of the semi-cured sample by means of a copper mesh (200#), and after 8h, the sample was completely cured and taken out of the mold to obtain the desired superhydrophobic strain sensor composite.
The strain gauge sensor prepared in example 1 was used as a detection target, the actual diagram of the strain gauge sensor is shown as a in fig. 1, and b and c in fig. 1 show that water droplets (10L) on the sample remained nearly circular and were very likely to roll off after the sample was stretched by 100% and 200%, respectively.
D in fig. 2 indicates that when the tensile specimen is increased from 0% to 200%, neither the contact angle nor the rolling angle shows a significant change, indicating that the superhydrophobicity of the specimen is retained even after the tensile treatment.
Fig. 3 analyzes electron microscope images of samples of different strains to detect changes in surface structure. By further comparing the electron microscope images, fig. 4, the layered structure is maintained despite the large distance between the microscopic projections. Thus, the sample can still remain superhydrophobic. Fig. 5 shows that the mechanical strength of the prepared superhydrophobic material was qualitatively evaluated by scratch and hand rub tests, and further the sample was ground at a weight of 200g (3.2KPa), and after 300 cycles (60m) of grinding, superhydrophobicity was not lost. While the test piece was pressed with an adhesive tape (3M Scotch600) under a load of 1kg weight (24.50KPa), and then peeled off, indicating that the test piece had excellent mechanical strength. Fig. 6 tests the effect of free-dripping water droplets and continuous water spray from nozzles of different diameters on horizontal and inclined samples and shows that the samples have excellent impact resistance. Fig. 6 further tests the low strain performance of the samples and the cyclic variation of the electrical resistance from 0% to 10% over 10000 cycles, indicating excellent durability and repeatability. Meanwhile, the prepared samples are attached to different joints of a human body, and the change difference of each joint can be detected from the difference between each cycle, so that the real-time monitoring effect is realized.
The above disclosure is only for a few specific embodiments of the present invention, but the present invention is not limited thereto, and any variations that can be made by those skilled in the art are intended to fall within the scope of the present invention.
Claims (6)
1. The preparation method of the super-hydrophobic strain sensor composite material is characterized by comprising the following steps of:
(1) dissolving heptafluorobutyric acid in tetrahydrofuran, stirring for 0.7-1.5h, adding tetraethoxysilane, stirring for 2.5-3.5h, and naturally drying the mixed solution in an evaporation pan to obtain a fluorinated curing agent;
(2) dissolving perfluorooctyl triethoxysilane in dimethylformamide, stirring the solution for 1.5-3h, adding carbon nanotubes, performing ultrasonic treatment for 20-40min, magnetically stirring for 4-8h, pouring the solution into an evaporation dish, naturally drying in the air, and collecting to obtain hydrophobic carbon nanotube powder;
(3) dispersing carbon nanofibers in tetrahydrofuran, adding polydimethylsiloxane, stirring for 1-3h, and performing ultrasonic treatment for 20-40min to obtain a polydimethylsiloxane solution;
(4) dispersing a fluorinated curing agent in tetrahydrofuran, stirring for 0.5-1.5h, and then mixing a polydimethylsiloxane solution with a fluorinated curing agent suspension by ultrasonic treatment for 20-40 min;
(5) adding perfluoropolyether into the suspension, adding dibutyltin dilaurate as a curing catalyst, carrying out ultrasonic treatment on the solution for 3-8min, and stirring for 4-6 h;
(6) and (3) casting the solution prepared in the step (5) into a Teflon mold, making the solution semi-solidified after 15-25min at room temperature, then uniformly spreading hydrophobic carbon nanotube powder on the surface of the semi-solidified sample by means of a copper net, completely solidifying the sample after 6-9h, and taking out the obtained super-hydrophobic strain sensor composite material from the mold.
2. The preparation method of the superhydrophobic strain sensor composite material according to claim 1, wherein the dosage mass ratio of the heptafluorobutyric acid, the tetrahydrofuran and the tetraethoxysilane in the step (1) is 3: (20-40): (3-8).
3. The preparation method of the superhydrophobic strain sensor composite material according to claim 1, wherein the amount by mass ratio of the perfluorooctyltriethoxysilane, the dimethylformamide and the carbon nanotube in the step (2) is 1: (40-60): (0.5-2).
4. The preparation method of the superhydrophobic strain sensor composite material according to claim 1, wherein the carbon nanofibers, the tetrahydrofuran and the polydimethylsiloxane in the step (3) are used in an amount of 3: (40-60): (40-60).
5. The preparation method of the superhydrophobic strain sensor composite material according to claim 1, wherein the amount mass ratio of the perfluoropolyether to dibutyltin dilaurate in the step (5) is (3-5): 1.
6. the method of claim 1, wherein the mesh size of the copper mesh is 200 #.
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