CN112853538A - Wool keratin-based nano composite flexible piezoelectric material and preparation method thereof - Google Patents
Wool keratin-based nano composite flexible piezoelectric material and preparation method thereof Download PDFInfo
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Abstract
The invention relates to a wool keratin-based nano composite flexible piezoelectric material and a preparation method thereof. The flexible piezoelectric material is a core material of the flexible piezoelectric sensor, and the development of the flexible piezoelectric material with good piezoelectric performance and high sensitivity is very important. The wool keratin-based nano composite flexible piezoelectric material is prepared by taking wool keratin and polyvinyl alcohol extracted from wool as raw materials and adopting an electrostatic spinning technology. The flexible piezoelectric material prepared by the preparation method has excellent mechanical property and piezoelectric property.
Description
Technical Field
The invention belongs to the field of flexible electronic materials, and particularly relates to a wool keratin-based nano composite flexible piezoelectric material and a preparation method thereof.
Background
With the increasing aging speed of China, portable medical equipment with a real-time monitoring function is urgently needed to monitor the health of the elderly patients, and health information of the patients is transmitted to doctors through a remote transmission function. The flexible piezoelectric sensor converts mechanical signals of important parts of a human body, such as fingers, throats, wrists and the like, into electric signals by utilizing electromechanical conversion, so that the health condition of the human body is judged. The flexible piezoelectric material is a core material of the flexible piezoelectric sensor, and the development of the flexible piezoelectric material with good piezoelectric performance and high sensitivity is very important.
At present, piezoelectric materials can be mainly divided into organic piezoelectric materials and inorganic piezoelectric materials, and the inorganic piezoelectric materials (such as barium titanate and other piezoelectric ceramics) are often combined with the organic piezoelectric materials for the reasons of hardness, brittleness and the like, so that the preparation process is complex. The organic piezoelectric material is superior to the inorganic piezoelectric material in durability and flexibility. The organic piezoelectric material mainly comprises polyvinylidene fluoride and copolymers thereof, natural high molecular polymers, polypropylene and the like. Natural high molecular polymers such as collagen fibers, amino acids, and keratin have been receiving more and more attention because of their degradability. Researchers (Hanna Bishara, Alina Nanel, Maya Levanon et al. amino acids nanocrystals for piezoelectric detection of ultra-low mechanical pressure [ J ]. Materials Science & Engineering C,2019) implemented piezoelectric sensing for ultra-low pressure detection using amino acid nanocrystals and oriented growth and weak hydrogen bonding between molecules, and could output a current signal of 0.45 pA. Researchers (Sujoy Kumar Ghosh, Dipakar Man. Sustainable Energy biology for nonlinear Signal Monitoring [ J ]. ACS Sustainable chem.Eng.2017,5,8836-8843) reported in the literature that the presence of hydrogen bonds in polypeptide chains leads to piezoelectricity in collagen nanofibers, that dipoles were oriented using electric polarization, and that Piezoelectric sensors were prepared using fish collagen nanofibers, and that Piezoelectric Signal output of 0.2V could be achieved.
Wool keratin is a protein extracted from wool, exists in an alpha-helix conformation, and polypeptide chains of the protein form a three-dimensional helix structure through the combined action of salt bonds, intermolecular hydrogen bonds, ester bonds, disulfide bonds, van der waals forces and the like. Hydrogen bonds in the peptide bonds of the wool keratin can generate dipoles with certain orientation after electric polarization, and piezoelectric effect can be generated after external acting force is applied. The invention takes wool keratin and polyvinyl alcohol as raw materials for the first time, and adopts the electrostatic spinning technology to prepare the flexible piezoelectric material.
Disclosure of Invention
The invention aims to provide a wool keratin-based nano composite flexible piezoelectric material and a preparation method thereof, which can realize 2.1V piezoelectric signal output.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a preparation method of a wool keratin-based nano composite flexible piezoelectric material comprises the following steps:
the method comprises the following steps: extraction of wool keratin:
preparing 20-50 mL of wool keratin extracting solution, wherein the molar concentration of urea is 8-12 mol/L, the molar concentration of sodium sulfate partial weight is 0.5-2.5 mol/L, and the molar concentration of sodium dodecyl sulfate is 0.1-0.5 mol/L; weighing 1-2 g of wool, shearing, adding into the wool keratin extracting solution, stirring in a water bath at 60-100 ℃ for 8-12 h, and filtering out wool fiber residues to obtain wool keratin mixed solution; putting the wool keratin mixed solution into a dialysis bag for dialysis for 2-3 days, and then putting the dialysis bag into a freeze drying box for drying to obtain wool keratin;
step two: preparation of wool keratin/polyvinyl alcohol nanocomposite:
dissolving 0.1-0.3 g of wool keratin in 10-15 mL of water to obtain a wool keratin solution; dissolving 0.1-0.3 g of polyvinyl alcohol in 10-15 mL of water to obtain a polyvinyl alcohol solution; mixing 3-5 parts of the wool keratin solution and 1-3 parts of the polyvinyl alcohol solution to form a uniform spinning solution; and (2) placing the spinning solution into a 10mL syringe, wherein the syringe needle is 0.4-0.7 mm, the receiving screen is connected with a negative electrode by adopting an aluminum foil for receiving, the distance between the syringe needle and the receiving screen is 10-15 cm, the spinning voltage is 15-20 kV, and performing electrostatic spinning to obtain the wool keratin/polyvinyl alcohol nanocomposite.
The preferable technical scheme 1 comprises the following steps:
the method comprises the following steps: extraction of wool keratin:
preparing 20mL of wool keratin extracting solution, wherein the molar concentration of urea is 8mol/L, the molar concentration of sodium metabisulfite is 0.5mol/L, and the molar concentration of sodium dodecyl sulfate is 0.1 mol/L; weighing 1g of wool, shearing, adding into the wool keratin extracting solution, stirring in a water bath at 60 ℃ for 8 hours, and filtering out wool fiber residues to obtain wool keratin mixed solution; putting the wool keratin mixed solution into a dialysis bag for dialysis for 2 days, and then putting the dialysis bag into a freeze drying box for drying to obtain wool keratin;
step two: preparation of wool keratin/polyvinyl alcohol nanocomposite:
dissolving 0.1g of wool keratin in 10mL of water to obtain a wool keratin solution; dissolving 0.1g of polyvinyl alcohol in 10mL of water to obtain a polyvinyl alcohol solution; mixing 3 parts of the wool keratin solution with 1 part of the polyvinyl alcohol solution to form a uniform spinning solution; and (3) putting the spinning solution into a 10mL syringe, wherein the syringe needle is 0.5mm, the receiving screen is received by adopting an aluminum foil connected cathode, the distance between the syringe needle and the receiving screen is 15cm, the spinning voltage is 15kV, and performing electrostatic spinning to obtain the wool keratin/polyvinyl alcohol nanocomposite.
The preferable technical scheme 2 comprises the following steps:
the method comprises the following steps: extraction of wool keratin:
preparing 50mL of wool keratin extracting solution, wherein the molar concentration of urea is 12mol/L, the molar concentration of sodium metabisulfite is 2.5mol/L, and the molar concentration of sodium dodecyl sulfate is 0.5 mol/L; weighing 2g of wool, shearing, adding into the wool keratin extracting solution, stirring in a water bath at 100 ℃ for 12 hours, and then filtering out wool fiber residues to obtain wool keratin mixed solution; putting the wool keratin mixed solution into a dialysis bag for dialysis for 3 days, and then putting the dialysis bag into a freeze drying box for drying to obtain wool keratin;
step two: preparation of wool keratin/polyvinyl alcohol nanocomposite:
dissolving 0.3g of wool keratin in 15mL of water to obtain a wool keratin solution; dissolving 0.3g of polyvinyl alcohol in 15mL of water to obtain a polyvinyl alcohol solution; mixing 5 parts of the wool keratin solution with 3 parts of the polyvinyl alcohol solution to form a uniform spinning solution; and (3) putting the spinning solution into a 10mL syringe, wherein the syringe needle is 0.5mm, the receiving screen is received by adopting an aluminum foil connected cathode, the distance between the syringe needle and the receiving screen is 15cm, the spinning voltage is 20kV, and performing electrostatic spinning to obtain the wool keratin/polyvinyl alcohol nanocomposite.
Compared with the prior art, the invention has the following beneficial effects:
1) the wool keratin-based nano composite material prepared by the method can output a piezoelectric signal with the highest voltage of 2.1V, the maximum stress of the prepared wool keratin/polyvinyl alcohol nano composite material is 3.7MPa, and the piezoelectric signal of 0.2V generated by the prepared wool keratin/polyvinyl alcohol nano composite material is greatly improved relative to a flexible piezoelectric material prepared by using fish skin collagen fibers;
2) the micro-nano fiber membrane prepared by the electrostatic spinning technology has the characteristics of large specific surface area, high porosity, strong flexibility and the like, the nano fiber material prepared by the electrostatic spinning method has larger specific surface area compared with a blocky structure, and the prepared sensor has more excellent performance;
3) in China, a large amount of wool leftovers cannot be effectively utilized due to poor quality, difficult processing and the like, and about 10 ten thousand tons of thick and long wool produced every year is in a waste state; the wool leftovers are recycled and used for preparing the flexible piezoelectric material, and huge economic benefits are certainly brought to the society.
Drawings
FIG. 1 is a scanning electron micrograph of a wool keratin/polyvinyl alcohol nanocomposite
FIG. 2 shows the piezoelectric signal generated by the wool keratin/polyvinyl alcohol nanocomposite
Detailed Description
The present invention will be described in detail with reference to specific examples. These embodiments are provided to illustrate the present invention, and any techniques realized based on the above-described contents of the present invention are within the scope of the present invention. The implementation conditions used in the examples can be further adjusted according to the specific experimental environment, and the implementation conditions not mentioned are generally the conditions in routine experiments.
Example 1:
the method comprises the following steps: extraction of wool keratin:
preparing 20mL of wool keratin extracting solution, wherein the molar concentration of urea is 8mol/L, the molar concentration of sodium metabisulfite is 0.5mol/L, and the molar concentration of sodium dodecyl sulfate is 0.1 mol/L; weighing 1g of wool, shearing, adding the wool into the wool keratin extracting solution, stirring for 8 hours in a water bath at 60 ℃, filtering out wool fiber residues, putting the filtered mixed solution into a dialysis bag for dialysis for 2 days, and drying the dialyzed solution through a freeze drying box to obtain wool keratin;
step two: preparation of wool keratin/polyvinyl alcohol nanocomposite:
dissolving 0.1g of wool keratin in 10mL of hot water to obtain a wool keratin solution; dissolving 0.1g of polyvinyl alcohol in 10mL of hot water to obtain a polyvinyl alcohol solution; mixing 3 parts of wool keratin solution and 1 part of polyvinyl alcohol solution to form uniform spinning solution; and (3) putting the spinning solution into a 10mL syringe, wherein the needle head of the syringe is 0.5mm, the receiving screen is connected with a negative electrode by adopting an aluminum foil for receiving, the distance between the needle head and the receiving screen is 15cm, the spinning voltage is 15kV, and then carrying out electrostatic spinning to obtain the wool keratin/polyvinyl alcohol nanocomposite.
Example 2:
the method comprises the following steps: extraction of wool keratin:
preparing 30mL of wool keratin extracting solution, wherein the molar concentration of urea is 10mol/L, the molar concentration of sodium metabisulfite is 1.5mol/L, and the molar concentration of sodium dodecyl sulfate is 0.3 mol/L; weighing 1.5g of wool, shearing, adding into the wool keratin extracting solution, stirring in a water bath at 100 ℃ for 12 hours, filtering out wool fiber residues, putting the filtered mixed solution into a dialysis bag for dialysis for 3 days, and drying the dialyzed solution in a freeze drying box to obtain wool keratin;
step two: preparation of wool keratin/polyvinyl alcohol nanocomposite:
dissolving 0.15g of wool keratin in 15mL of hot water to obtain a wool keratin solution; dissolving 0.15g of polyvinyl alcohol in 15mL of hot water to obtain a polyvinyl alcohol solution; mixing 5 parts of wool keratin solution and 3 parts of polyvinyl alcohol solution to form uniform spinning solution; placing the spinning solution in a 10mL syringe with a syringe needle of 0.5mm, receiving with aluminum foil as negative electrode, a distance of 15cm between the needle and the receiving screen, and a spinning voltage of 17kV, and performing electrostatic spinning to obtain wool keratin/polyvinyl alcohol nanocomposite
Example 3:
the method comprises the following steps: extraction of wool keratin:
preparing 50mL of wool keratin extracting solution, wherein the molar concentration of urea is 12mol/L, the molar concentration of sodium metabisulfite is 2.5mol/L, and the molar concentration of sodium dodecyl sulfate is 0.5 mol/L; weighing 2g of wool, shearing, adding into the wool keratin extracting solution, stirring for 10h in a water bath at 80 ℃, filtering out wool fiber residues, putting the filtered mixed solution into a dialysis bag for dialysis for 3 days, and drying the dialyzed solution in a freeze drying oven to obtain wool keratin;
step two: preparation of wool keratin/polyvinyl alcohol nanocomposite:
dissolving 0.3g of wool keratin in 15mL of hot water to obtain a wool keratin solution; dissolving 0.3g of polyvinyl alcohol in 15mL of hot water to obtain a polyvinyl alcohol solution; mixing 5 parts of wool keratin solution and 3 parts of polyvinyl alcohol solution to form uniform spinning solution; placing the spinning solution in a 10mL syringe with a syringe needle of 0.5mm, receiving with aluminum foil as negative electrode, a distance of 15cm between the needle and the receiving screen, and a spinning voltage of 20kV, and performing electrostatic spinning to obtain wool keratin/polyvinyl alcohol nanocomposite
In order to show that the wool keratin-based nano composite flexible piezoelectric material is successfully prepared, the inventor carries out SEM detection and piezoelectric property detection on the material. The SEM test results are shown in figure 1, and the wool keratin/polyvinyl alcohol nanocomposite prepared by the electrostatic spinning technology is distributed in a three-dimensional network structure, which is caused by the fact that fiber layers are overlapped in the spinning process, and the fiber diameter distribution is uniform and consistent with the literature reports. The piezoelectric performance detection is that the wool keratin-based nano composite flexible piezoelectric material outputs a piezoelectric signal generated when a finger is bent, and as shown in figure 2, the maximum piezoelectric signal of 2.1V can be generated in the finger bending process. When the fingers are bent, the wool keratin-based nano composite flexible piezoelectric material generates tensile strain to generate positive voltage potential, negative voltage potential is generated during release, and the bending and releasing motion of the fingers generates measurable output signals (namely voltage), so that the wool keratin-based nano composite flexible piezoelectric material can be used for portable medical equipment and monitoring physiological signals of a human body.
The above examples are only for further detailed description of the summary of the present invention, but it should not be understood that the scope of the above-described subject matter of the present invention is limited to the above examples. Various substitutions and alterations can be made without departing from the technical idea of the invention and the technical knowledge and common means in the field, and all changes and alterations are included in the scope of the invention.
Claims (4)
1. A preparation method of a wool keratin-based nano composite flexible piezoelectric material is characterized by comprising the following steps: the method comprises the following steps:
the method comprises the following steps: extraction of wool keratin:
preparing 20-50 mL of wool keratin extracting solution, wherein the molar concentration of urea is 8-12 mol/L, the molar concentration of sodium sulfate partial weight is 0.5-2.5 mol/L, and the molar concentration of sodium dodecyl sulfate is 0.1-0.5 mol/L; weighing 1-2 g of wool, shearing, adding into the wool keratin extracting solution, stirring in a water bath at 60-100 ℃ for 8-12 h, and filtering out wool fiber residues to obtain wool keratin mixed solution; putting the wool keratin mixed solution into a dialysis bag for dialysis for 2-3 days, and then putting the dialysis bag into a freeze drying box for drying to obtain wool keratin;
step two: preparation of wool keratin/polyvinyl alcohol nanocomposite:
dissolving 0.1-0.3 g of wool keratin in 10-15 mL of water to obtain a wool keratin solution; dissolving 0.1-0.3 g of polyvinyl alcohol in 10-15 mL of water to obtain a polyvinyl alcohol solution; mixing 3-5 parts of the wool keratin solution and 1-3 parts of the polyvinyl alcohol solution to form a uniform spinning solution; and (2) placing the spinning solution into a 10mL syringe, wherein the syringe needle is 0.4-0.7 mm, the receiving screen is connected with a negative electrode by adopting an aluminum foil for receiving, the distance between the syringe needle and the receiving screen is 10-15 cm, the spinning voltage is 15-20 kV, and performing electrostatic spinning to obtain the wool keratin/polyvinyl alcohol nanocomposite.
2. The method for preparing a wool keratin-based nanocomposite flexible piezoelectric material according to claim 1, wherein: the method comprises the following steps:
the method comprises the following steps: extraction of wool keratin:
preparing 20mL of wool keratin extracting solution, wherein the molar concentration of urea is 8mol/L, the molar concentration of sodium metabisulfite is 0.5mol/L, and the molar concentration of sodium dodecyl sulfate is 0.1 mol/L; weighing 1g of wool, shearing, adding into the wool keratin extracting solution, stirring in a water bath at 60 ℃ for 8 hours, and filtering out wool fiber residues to obtain wool keratin mixed solution; putting the wool keratin mixed solution into a dialysis bag for dialysis for 2 days, and then putting the dialysis bag into a freeze drying box for drying to obtain wool keratin;
step two: preparation of wool keratin/polyvinyl alcohol nanocomposite:
dissolving 0.1g of wool keratin in 10mL of water to obtain a wool keratin solution; dissolving 0.1g of polyvinyl alcohol in 10mL of water to obtain a polyvinyl alcohol solution; mixing 3 parts of the wool keratin solution with 1 part of the polyvinyl alcohol solution to form a uniform spinning solution; and (3) putting the spinning solution into a 10mL syringe, wherein the syringe needle is 0.5mm, the receiving screen is received by adopting an aluminum foil connected cathode, the distance between the syringe needle and the receiving screen is 15cm, the spinning voltage is 15kV, and performing electrostatic spinning to obtain the wool keratin/polyvinyl alcohol nanocomposite.
3. The method for preparing a wool keratin-based nanocomposite flexible piezoelectric material according to claim 1, wherein: the method comprises the following steps:
the method comprises the following steps: extraction of wool keratin:
preparing 50mL of wool keratin extracting solution, wherein the molar concentration of urea is 12mol/L, the molar concentration of sodium metabisulfite is 2.5mol/L, and the molar concentration of sodium dodecyl sulfate is 0.5 mol/L; weighing 2g of wool, shearing, adding into the wool keratin extracting solution, stirring in a water bath at 100 ℃ for 12 hours, and then filtering out wool fiber residues to obtain wool keratin mixed solution; putting the wool keratin mixed solution into a dialysis bag for dialysis for 3 days, and then putting the dialysis bag into a freeze drying box for drying to obtain wool keratin;
step two: preparation of wool keratin/polyvinyl alcohol nanocomposite:
dissolving 0.3g of wool keratin in 15mL of water to obtain a wool keratin solution; dissolving 0.3g of polyvinyl alcohol in 15mL of water to obtain a polyvinyl alcohol solution; mixing 5 parts of the wool keratin solution with 3 parts of the polyvinyl alcohol solution to form a uniform spinning solution; and (3) putting the spinning solution into a 10mL syringe, wherein the syringe needle is 0.5mm, the receiving screen is received by adopting an aluminum foil connected cathode, the distance between the syringe needle and the receiving screen is 15cm, the spinning voltage is 20kV, and performing electrostatic spinning to obtain the wool keratin/polyvinyl alcohol nanocomposite.
4. A wool keratin-based nano composite flexible piezoelectric material is characterized in that: prepared by the preparation method of any one of claims 1 to 3.
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| CN115976739A (en) * | 2022-12-07 | 2023-04-18 | 江南大学 | Method for improving piezoelectric performance of regenerated eggshell membrane |
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Application publication date: 20210528 |