CN110330747B - Preparation method and application of large-strain superelasticity PVA/MCNTS hydrogel - Google Patents
Preparation method and application of large-strain superelasticity PVA/MCNTS hydrogel Download PDFInfo
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- CN110330747B CN110330747B CN201910477009.4A CN201910477009A CN110330747B CN 110330747 B CN110330747 B CN 110330747B CN 201910477009 A CN201910477009 A CN 201910477009A CN 110330747 B CN110330747 B CN 110330747B
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Abstract
The invention provides a preparation method and application of a large-strain superelasticity PVA/MCNTS hydrogel, wherein the preparation method comprises the following steps of 01, preparing disordered MCNTS powder by adopting chemical vapor deposition; 02. acidifying, separating, drying and grinding MCNTS powder; 03. preparing a PVA aqueous solution, adding the MCNTS powder treated in the step 02 into the PVA aqueous solution, heating in a water bath and stirring to fully disperse the MCNTS powder, and preparing a PVA/MCNTS mixed solution; 04. and (3) pouring the PVA/MCNTS mixed solution in the step (03) into a mould, and then freezing and unfreezing for multiple times to obtain the PVA/MCNTS hydrogel. The polyvinyl alcohol/multi-walled carbon nanotube hydrogel prepared by the invention has uniform components, simultaneously has large tensile strain and compressive strain, has superelasticity and sensitive factors in the tensile process and the compressive process, and can be used as a strain sensor in the field of flexible and stretchable devices due to the excellent performance of the hydrogel.
Description
Technical Field
The invention relates to the technical field of nano material preparation, in particular to a preparation method and application of a large-strain superelasticity PVA/MCNTS hydrogel, which can be used as a strain sensor and applied to the field of flexible wearable electronic devices.
Background
With the development of scientific technology and artificial intelligence, the demand of flexible wearable electronic devices is increasing. Currently, most flexible wearable devices employ an organic polymer flexible substrate and a conductive media filler. The carbon nanotube is a typical one-dimensional tubular nano material, has good electrical conductivity, thermal conductivity and good mechanical properties, and is widely applied to strain sensors. Polyvinyl alcohol, an organic polymer with good biocompatibility, has great tensile strain and toughness, but the irrecoverability during the stretching process limits its ability to serve as a substrate for a strain sensor. The polyvinyl alcohol hydrogel prepared by adopting the freezing cycle has a large number of three-dimensional physical cross-linked networks, so that the polyvinyl alcohol hydrogel has high strain and good elasticity, but the polyvinyl alcohol hydrogel has poor conductivity.
Disclosure of Invention
The invention provides a preparation method and application of a large-strain superelasticity PVA/MCNTS hydrogel, wherein PVA is polyvinyl alcohol, MCNTS is a multi-wall carbon nano tube, and the conductive capacity of the traditional hydrogel is greatly improved by compounding multi-wall carbon nano tube powder in the polyvinyl alcohol hydrogel.
The technical scheme of the invention is realized as follows: a preparation method of a large-strain superelasticity PVA/MCNTS hydrogel comprises the following steps:
01. preparing disordered MCNTS powder by adopting chemical vapor deposition;
02. soaking MCNTS powder in 20% dilute nitric acid for 12h, washing the acidified MCNTS powder to neutrality by a suction filter, performing solid-liquid separation, drying the separated MCNTS in a vacuum drying oven at 60 ℃ for 12h, and grinding the dried MCNTS powder into finer particles by a mortar;
03. adding PVA powder into water, heating and stirring in a water bath to prepare a PVA aqueous solution, adding MCNTS powder treated in the step 02 into the PVA aqueous solution, heating and stirring in the water bath to fully disperse the MCNTS powder, and preparing a PVA/MCNTS mixed solution;
04. and (3) pouring the PVA/MCNTS mixed solution in the step (03) into a mould, and then freezing and unfreezing for multiple times to obtain the PVA/MCNTS hydrogel.
Further, in step 01, a CVD tube furnace was used, 100ml of dichlorobenzene was used as a carbon source, 0.6g of ferrocene was used as a catalyst, and disordered MCNTS powder was grown on the wall of the quartz tube at a reaction temperature of 850 ℃ in an atmosphere of 2000sccm hydrogen-argon mixed gas. The multi-walled carbon nanotube prepared by the method has good conductivity and disorder property, and provides possibility for the subsequent synthesis of hydrogel with uniform components.
Further, in step 03, 10g of PVA powder was added to 90ml of water, and heated and stirred in a water bath at 85 ℃ for 3 hours in a water bath to prepare a 10 wt.% PVA aqueous solution, and the MCNTS powder treated in step 02 was added to the PVA aqueous solution, and heated and stirred in a water bath at 65 ℃ for 3 hours to be sufficiently dispersed, thereby preparing a PVA/MCNTS mixed solution.
Further, in step 04, the PVA/MCNTS mixed solution of step 03 is poured into a cylindrical mold, and then frozen in a refrigerator for 12 hours and then thawed at room temperature for 12 hours, and the freezing/thawing process is repeated a plurality of times to prepare the PVA/MCNTS mixed solution.
The application of the large-strain superelasticity PVA/MCNTS hydrogel as a tensile strain sensor or a pressure sensor.
Further, the tensile strain sensor or the pressure sensor is used for a flexible wearable electronic device.
The invention has the beneficial effects that: according to the invention, the multi-walled carbon nanotube powder and the polyvinyl alcohol hydrogel are compounded, so that the conductivity of the original polyvinyl alcohol hydrogel is improved, and the high-strain super-elastic polyvinyl alcohol/multi-walled carbon nanotube hydrogel is prepared. When the multi-wall carbon nanotube powder and the polyvinyl alcohol aqueous solution are mixed, the problem of uneven distribution of the carbon tubes can be well solved by heating and stirring in a water bath.
In the preparation process, the original multi-walled carbon nanotube has hydrophobicity, and the surface of the multi-walled carbon nanotube generates hydrophilic groups after acidification, so that the multi-walled carbon nanotube has hydrophilic capacity; the method is characterized in that a mixed solution of polyvinyl alcohol and multi-walled carbon nanotubes is heated in a water bath, the polyvinyl alcohol aqueous solution is a viscous liquid at normal temperature and is not beneficial to the diffusion movement of multi-walled carbon nanotube powder, the mixed solution of polyvinyl alcohol and multi-walled carbon nanotubes is heated in the water bath, the diffusion capacity of the multi-walled carbon nanotubes in the solution is improved, and the method is the key for preparing the hydrogel with uniform components. The method of the freezing circulation can be that polyvinyl alcohol is physically crosslinked to prepare three-dimensional stretchable compressible super-elastic hydrogel with uniform components, disordered multi-wall carbon nano-tubes are uniformly distributed in the hydrogel, direct current conducting capacity is provided for the hydrogel, and super-elasticity and high-sensitivity factors are provided in the stretching process and the compression process.
The polyvinyl alcohol/multi-walled carbon nanotube hydrogel with uniform components is successfully obtained through acidification, grinding and water bath, can be stretched and compressed, has large strain, superelasticity and high sensitivity factors in the stretching process and the compressing process, and has a great application prospect in flexible wearable devices, particularly strain sensors.
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In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only some embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the drawings without creative efforts.
FIG. 1 is a schematic diagram of the preparation process of the present invention;
FIG. 2 is a scanning electron micrograph of a PVA/MCNTS hydrogel prepared according to the present invention;
FIG. 3 is a stress-strain curve of the PVA/MCNTS hydrogel prepared by the present invention undergoing a snap test;
FIG. 4 is a stress-strain plot of the PVA/MCNTS hydrogel prepared by the present invention subjected to a tensile cycle;
FIG. 5 is a stress-strain plot of a PVA/MCNTS hydrogel prepared according to the present invention undergoing a compression cycle;
FIG. 6 is a graph of a force-electricity test performed on the PVA/multiwalled carbon nanotube hydrogel prepared by the present invention.
Wherein: MCNTS powder 1, a beaker 2, PVA aqueous solution 3, a water bath 4, a dropper 5, a mould 6 and PVA/MCNTS hydrogel 7 after freezing circulation.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be obtained by a person skilled in the art without inventive effort based on the embodiments of the present invention, are within the scope of the present invention.
As shown in FIG. 1, a method for preparing a large-strain superelasticity PVA/MCNTS hydrogel comprises the following steps:
01. adopting a CVD tube furnace, taking 100ml of dichlorobenzene as a carbon source and 0.6g of ferrocene as a catalyst, and growing disordered MCNTS powder on the wall of a quartz tube at the reaction temperature of 850 ℃ in the atmosphere of 2000sccm hydrogen-argon mixed gas;
02. soaking MCNTS powder in 20% dilute nitric acid for 12h, washing the acidified MCNTS powder to neutrality by a suction filter, performing solid-liquid separation, drying the separated MCNTS in a vacuum drying oven at 60 ℃ for 12h, and grinding the dried MCNTS powder into finer particles by a mortar;
03. adding 10g of PVA powder into 90ml of water, heating and stirring for 3 hours in a water bath kettle at 85 ℃ in a water bath to prepare 10 wt.% of PVA aqueous solution, adding MCNTS powder treated in the step 02 into the PVA aqueous solution, heating for 3 hours in a water bath at 65 ℃ to fully disperse the MCNTS powder, and preparing PVA/MCNTS mixed solution;
04. and (3) filling the PVA/MCNTS mixed solution in the step 03 into a cylindrical mold, freezing the mold in a refrigerator for 12 hours, then unfreezing the mold at room temperature for 12 hours, and repeating the freezing/unfreezing process for multiple times to prepare the PVA/MCNTS hydrogel, wherein a scanning electron microscope photo of the PVA/MCNTS hydrogel is shown in figure 2.
In step 03, MCNTS powder is added in an amount of between 0.2g and 1.0g, such as 0.2g, 0.6g or 1.0g, and the volume of the aqueous solution of polyvinyl alcohol is 30 ml.
The present invention will be described in detail with reference to examples.
Example 1
10g of PVA powder was added to 90ml of water, and the mixture was heated and stirred in a water bath at 85 ℃ for 3 hours to obtain a PVA water-soluble solution. Preparing MCNTS powder through chemical vapor deposition, acidifying, drying and grinding the MCNTS powder, adding 0.2g of the MCNTS powder into 30ml of PVA solution, heating and stirring in a water bath at 65 ℃ for 3h, filling the PVA/MCNTS mixed solution into a mold, freezing for 12h in a refrigerator, then unfreezing for 12h at room temperature, and repeating the freezing and unfreezing process for multiple times to obtain the PVA/MCNTS hydrogel.
Example 2
10g of PVA powder was added to 90ml of water, and the mixture was heated and stirred in a water bath at 85 ℃ for 3 hours to obtain a PVA water-soluble solution. Preparing MCNTS powder through chemical vapor deposition, acidifying, drying and grinding the MCNTS powder, adding 0.6g of the MCNTS powder into 30ml of PVA solution, heating and stirring in a water bath at 65 ℃ for 3h, filling the PVA/MCNTS mixed solution into a mold, freezing for 12h in a refrigerator, then unfreezing for 12h at room temperature, and repeating the freezing and unfreezing process for multiple times to obtain the PVA/MCNTS hydrogel.
Example 3
10g of PVA powder was added to 90ml of water, and the mixture was heated and stirred in a water bath at 85 ℃ for 3 hours to obtain a PVA water-soluble solution. Preparing MCNTS powder through chemical vapor deposition, acidifying, drying and grinding the MCNTS powder, adding 1.0g of the MCNTS powder into 30ml of PVA solution, heating and stirring in a water bath at 65 ℃ for 3h, filling the PVA/MCNTS mixed solution into a mould, freezing for 12h in a refrigerator, then unfreezing for 12h at room temperature, and repeating the freezing and unfreezing process for multiple times to obtain the PVA/MCNTS hydrogel.
Comparative example 1
Adding 10g of PVA powder into 90ml of water, heating and stirring in a water bath at 85 ℃ for 3h, filling the obtained PVA aqueous solution into a mould, freezing in a refrigerator for 12h, then unfreezing at room temperature for 12h, and repeating the freezing and unfreezing process for multiple times to obtain the PVA hydrogel.
The examples 1 to 3 and comparative example 1 were taken out of the mold, fixed to the jig of a stretcher, and subjected to a tensile test at a tensile rate of 10mm/min, respectively. Let the hydrogel have an original length of l0The pre-cleavage length is l, according to ε ═ l0)/l0Strain values were calculated as 100%. The stress-strain curve is shown in FIG. 3, wherein the cross-sectional area of the hydrogel is s and the pre-fracture load is F, and the stress value is calculated according to σ ═ F/s, but the strain of the hydrogel is less than 300% when MCNTS is added at 1.0 g.
The conductivity measurements were performed for examples 1-3 using a multimeter to measure the resistance R individually, with the example between the multimeter beam probes being l and the hydrogel cross-sectional area being s, and the conductivity was calculated from σ ═ l/Rs. The results of the conductivity tests performed on examples 1-3 are shown in the following table:
| sample (I) | Conductivity (S/km) |
| Example 1 | 15.14530 |
| Example 2 | 15.57002 |
| Example 3 | 18.65908 |
A cyclic stretching experiment was performed on example 2 to cyclically stretch at 50%, 100%, 200%, 300% tensile strain for 5 cycles at a stretching rate of 2 cycles per minute, and the stress-strain curve of the stretching cycle is shown in fig. 4.
Example 2 was subjected to a cyclic compression test at 10%, 20%, 30%, 40%, 50% cyclic compression for 5 cycles at a compression rate of 2 cycles per minute, with the stress-strain curve for the compression cycle shown in figure 5.
Example 2 was subjected to a force-electricity test with 300% cyclic elongation at high strain at a rate of two cycles per minute and the rate of change of resistance during elongation was measured, the curve of which is shown in figure 6.
The tests show that the prepared PVA/MCNTS hydrogel has the advantages of large tensile strain, large bending strain, high superelasticity and the like, the addition of the disordered multi-wall carbon nano tubes improves the conductive capacity of the hydrogel, the hydrogel has high sensitive factors in the stretching and compressing processes, and the PVA/MCNTS hydrogel is favorably used as a tensile strain sensor or a pressure sensor to be applied to a flexible wearable electronic device.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that fall within the spirit and principle of the present invention are intended to be included therein.
Claims (4)
1. A preparation method of a large-strain superelasticity PVA/MCNTS hydrogel is characterized by comprising the following steps:
01. adopting a CVD tube furnace, taking 100mL of dichlorobenzene as a carbon source and 0.6g of ferrocene as a catalyst, and growing disordered MCNTS powder on the wall of a quartz tube at the reaction temperature of 850 ℃ in the atmosphere of 2000sccm hydrogen-argon mixed gas;
02. soaking MCNTS powder in 20% dilute nitric acid for 12h to obtain acidified MCNTS powder, washing the acidified MCNTS powder to be neutral by a suction filter, performing solid-liquid separation, drying the separated MCNTS in a vacuum drying oven at 60 ℃ for 12h, and grinding the dried MCNTS powder into finer particles;
03. adding 10g of PVA powder into 90mL of water, heating and stirring for 3h in a water bath kettle at 85 ℃ in a water bath for preparing 10 wt.% of PVA aqueous solution, adding 0.2g-1.0g of MCNTS powder treated in the step 02 into 30mL of PVA aqueous solution, heating and stirring for 3h in a water bath at 65 ℃ for fully dispersing, and preparing PVA/MCNTS mixed solution;
04. and (3) pouring the PVA/MCNTS mixed solution in the step (03) into a mould, and then freezing and unfreezing for multiple times to obtain the PVA/MCNTS hydrogel.
2. The method of claim 1, wherein in step 04, the PVA/MCNTS mixed solution obtained in step 03 is poured into a cylindrical mold, and then frozen in a refrigerator for 12h, and then thawed at room temperature for 12h, and the freezing/thawing process is repeated several times to obtain the PVA/MCNTS hydrogel.
3. Use of the large strain superelastic PVA/MCNTS hydrogel of claim 1 or 2 as a tensile strain sensor or a pressure sensor.
4. Use of the tensile strain sensor or pressure sensor of claim 3 for a flexible wearable electronic device.
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| 《MWCNTs增强聚乙二醇-聚乙烯醇复合水凝胶的制备及性能》;徐朝阳等;《复合材料学报》;20171231;全文 * |
| 《Polyvinyl alcohol wrapped multiwall carbon nanotube (MWCNTs) network on fabrics for wearable room temperature ethanol sensor》;Maity, D;《Sensors and Actuators B: Chemical》;20181231;全文 * |
| <碳纳米管基聚合物水凝胶研究进展>;程亚玮,李欢军,张公正;<中国科技论文>;20130830;全文 * |
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