CN116145304B - A non-polarized cotton cellulose/PVDF composite piezoelectric fabric and its preparation method and application - Google Patents
A non-polarized cotton cellulose/PVDF composite piezoelectric fabric and its preparation method and application Download PDFInfo
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- 229920000742 Cotton Polymers 0.000 title claims abstract description 94
- 229920002981 polyvinylidene fluoride Polymers 0.000 title claims abstract description 86
- 229920002678 cellulose Polymers 0.000 title claims abstract description 85
- 239000001913 cellulose Substances 0.000 title claims abstract description 85
- 239000002033 PVDF binder Substances 0.000 title claims abstract description 84
- 239000004744 fabric Substances 0.000 title claims abstract description 59
- 239000002131 composite material Substances 0.000 title claims abstract description 57
- 238000002360 preparation method Methods 0.000 title claims description 12
- KWGKDLIKAYFUFQ-UHFFFAOYSA-M lithium chloride Chemical compound [Li+].[Cl-] KWGKDLIKAYFUFQ-UHFFFAOYSA-M 0.000 claims abstract description 36
- 238000009987 spinning Methods 0.000 claims abstract description 35
- 239000000835 fiber Substances 0.000 claims abstract description 28
- 239000002904 solvent Substances 0.000 claims abstract description 20
- 238000000034 method Methods 0.000 claims abstract description 18
- 230000015271 coagulation Effects 0.000 claims abstract description 15
- 238000005345 coagulation Methods 0.000 claims abstract description 15
- 238000001994 activation Methods 0.000 claims abstract description 14
- 230000004913 activation Effects 0.000 claims abstract description 13
- 238000009941 weaving Methods 0.000 claims abstract description 11
- 238000010907 mechanical stirring Methods 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 7
- 238000009792 diffusion process Methods 0.000 claims abstract description 4
- 238000002156 mixing Methods 0.000 claims abstract description 3
- 238000005406 washing Methods 0.000 claims abstract description 3
- 238000007872 degassing Methods 0.000 claims abstract 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical group OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 claims description 24
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 238000003756 stirring Methods 0.000 claims description 9
- 238000004090 dissolution Methods 0.000 claims description 5
- 238000006116 polymerization reaction Methods 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims 2
- 239000002699 waste material Substances 0.000 abstract description 11
- 230000000694 effects Effects 0.000 abstract description 6
- 239000002994 raw material Substances 0.000 abstract description 2
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 description 23
- 238000002166 wet spinning Methods 0.000 description 13
- 230000005684 electric field Effects 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 4
- 239000000203 mixture Substances 0.000 description 4
- 230000001112 coagulating effect Effects 0.000 description 3
- 239000006184 cosolvent Substances 0.000 description 3
- 239000000463 material Substances 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 238000005303 weighing Methods 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical group CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 238000005265 energy consumption Methods 0.000 description 2
- 230000010287 polarization Effects 0.000 description 2
- 239000011540 sensing material Substances 0.000 description 2
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000009954 braiding Methods 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 238000005520 cutting process Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000003247 decreasing effect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000010438 heat treatment Methods 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 238000002329 infrared spectrum Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000010248 power generation Methods 0.000 description 1
- 230000035945 sensitivity Effects 0.000 description 1
- 230000001953 sensory effect Effects 0.000 description 1
- 230000028016 temperature homeostasis Effects 0.000 description 1
- 238000010998 test method Methods 0.000 description 1
- 239000004753 textile Substances 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
Classifications
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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
- D01F8/02—Conjugated, i.e. bi- or multicomponent, artificial filaments or the like; Manufacture thereof from cellulose, cellulose derivatives, or proteins
-
- 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
- D01D1/00—Treatment of filament-forming or like material
- D01D1/02—Preparation of spinning solutions
-
- 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
- D01D5/06—Wet spinning methods
-
- 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
-
- D—TEXTILES; PAPER
- D03—WEAVING
- D03D—WOVEN FABRICS; METHODS OF WEAVING; LOOMS
- D03D15/00—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used
- D03D15/20—Woven fabrics characterised by the material, structure or properties of the fibres, filaments, yarns, threads or other warp or weft elements used characterised by the material of the fibres or filaments constituting the yarns or threads
- D03D15/292—Conjugate, i.e. bi- or multicomponent, fibres or filaments
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- Engineering & Computer Science (AREA)
- Textile Engineering (AREA)
- Mechanical Engineering (AREA)
- Chemical & Material Sciences (AREA)
- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Artificial Filaments (AREA)
Abstract
一种无极化棉纤维素/PVDF复合压电织物的制备方法，包括：将棉纤维素置于恒温烘箱中烘干至恒重，加入DMAc溶剂活化处理；将棉纤维素溶于LiCl/DMAc体系中，得到棉纤维素溶液；将PVDF溶于DMAc溶剂中，得到PVDF溶液；将棉纤维素溶液和PVDF溶液在机械搅拌下共混，所得共混液进行高压脱泡处理，得到棉纤维素/PVDF复合纺丝液；将棉纤维素/PVDF复合纺丝液从喷丝帽挤出，并浸入凝固浴中以通过溶剂的双扩散作用使纤维凝固成型，再经过洗涤并干燥处理，得到棉纤维素/PVDF复合压电纤维；将棉纤维素/PVDF复合压电纤维采用经纬织法编织得到无极化棉纤维素/PVDF复合压电织物。本发明以废旧棉浆粕(棉纤维素)为原料，采用预活化工艺随后将其溶解在LiCl/DMAc体系中，操作简单，且实现了废旧棉的再利用。
A method for preparing a non-polarized cotton cellulose/PVDF composite piezoelectric fabric comprises: placing cotton cellulose in a constant temperature oven and drying it to constant weight, adding DMAc solvent for activation treatment; dissolving cotton cellulose in a LiCl/DMAc system to obtain a cotton cellulose solution; dissolving PVDF in a DMAc solvent to obtain a PVDF solution; blending the cotton cellulose solution and the PVDF solution under mechanical stirring, and subjecting the obtained blended solution to high-pressure degassing treatment to obtain a cotton cellulose/PVDF composite spinning solution; extruding the cotton cellulose/PVDF composite spinning solution from a spinneret, and immersing it in a coagulation bath to coagulate and form the fiber through the double diffusion effect of the solvent, and then washing and drying to obtain a cotton cellulose/PVDF composite piezoelectric fiber; weaving the cotton cellulose/PVDF composite piezoelectric fiber by warp and weft weaving to obtain a non-polarized cotton cellulose/PVDF composite piezoelectric fabric. The invention uses waste cotton pulp (cotton cellulose) as a raw material, adopts a pre-activation process and then dissolves it in a LiCl/DMAc system, is simple to operate, and realizes the reuse of waste cotton.
Description
Technical Field
The invention relates to the field of wearable fabrics and intelligent sensing, in particular to an electrodeless cotton cellulose/PVDF composite piezoelectric fabric, and a preparation method and application thereof.
Background
The new electronic textile technology is pushing innovative applications for garments, telemedicine, thermoregulation, sensory experience or coming tremendous revolution in reality and even the world of the meta-universe. The intelligent fabric (also called as electronic fabric) refers to fibers and fabrics embedded with electronic devices or electronic functions, and has the characteristics of automatic heating and cooling, data acquisition and transmission, power generation, touch sensing and the like.
The traditional sensor generally has the problems of large mass, rigidity, battery replacement and the like, utilizes the piezoelectric effect to develop the self-powered sensing fabric, solves the problems that the traditional wearable electronic equipment depends on external power supply, has single function, has lower sensitivity and the like, and provides a new solution for realizing the multifunctional integrated wearable equipment. In addition, most piezoelectric materials need to induce a piezoelectric effect by polarizing an external high-voltage electric field to induce a piezoelectric phase transition of a non-piezoelectric phase in the piezoelectric material, which inevitably causes a loss of energy, so that the application is limited, and thus further improvement is required.
Disclosure of Invention
Based on the above, the invention provides an electrodeless cotton cellulose/PVDF composite piezoelectric fabric, a preparation method and application thereof, and the stretching force in the wet spinning process is utilized to promote the non-piezoelectric phase to the piezoelectric phase in the piezoelectric material PVDF to be converted, so that the piezoelectric effect can be generated without external electric field polarization, and the technical problem of energy loss caused by external electric field polarization in the prior art for realizing self-powered sensing materials by utilizing the piezoelectric effect is solved.
In order to achieve the above purpose, the invention provides a preparation method of an electrodeless cotton cellulose/PVDF composite piezoelectric fabric, which comprises the following steps:
s1, placing cotton cellulose with the polymerization degree of 500-650 in a constant-temperature oven at 50 ℃ to be dried to constant weight, and adding DMAc solvent for activation treatment;
S2, dissolving the cotton cellulose treated in the step S1 in a LiCl/DMAc system to obtain a cotton cellulose solution, wherein preferably, the mass fraction of LiCl in the DMAc system is 10%, the dissolution of the activated cotton cellulose in the LiCl/DMAc system adopts high-speed mechanical stirring, the rotating speed is more than or equal to 1500rpm, the stirring time is 60-90 min, and the solution is placed in a constant-temperature oven at 25 ℃ for standing for 12h for standby after the completion;
s3, dissolving PVDF with the molecular weight of 40-60 ten thousand in a DMAc solvent to obtain a PVDF solution;
s4, blending the cotton cellulose solution and the PVDF solution under mechanical stirring according to the mass ratio of the cotton cellulose to the PVDF of 7:10-9:10, and performing high-pressure defoaming treatment on the obtained blend to obtain the cotton cellulose/PVDF composite spinning solution;
S5, extruding the cotton cellulose/PVDF composite spinning solution from a spinning cap under the conditions of 25-30 ℃ and 50-100 kg/cm 3 of spinning pressure and 4-5 m/min of spinning speed, immersing the spinning solution into a coagulating bath to coagulate and form fibers through double diffusion of a solvent, and washing and drying the fibers to obtain the cotton cellulose/PVDF composite piezoelectric fibers, wherein preferably 5 bath fibers for the coagulating bath are sequentially provided with 1# bath, 2# bath, 3# bath and 4# bath as water, 40 ℃ and 5# bath as methanol, and the temperature is room temperature;
s6, weaving the cotton cellulose/PVDF composite piezoelectric fiber by adopting a warp-weft weaving method to obtain the non-polarized cotton cellulose/PVDF composite piezoelectric fabric.
As a further preferable technical scheme of the invention, in the step S1, the activation treatment temperature of the cotton cellulose is 50-70 ℃ and the activation treatment time is 6-12 hours. The activation treatment can reduce the dissolution temperature of cotton cellulose in a LiCl/DMAc system in the subsequent steps, and also improves the dissolution effect of cellulose and the uniformity degree in a solvent system.
As a further preferable technical scheme of the invention, cotton cellulose activated by DMAc in the step S1 is placed in a vacuum oven at 50-60 ℃ for drying.
As a further preferable technical scheme of the invention, in the step S2, the solid content of LiCl in a LiCl/DMAc system is 6% -10%, and the dissolution temperature is 50 ℃.
As a further preferable technical scheme of the invention, in the step S4, the concentration of the cotton cellulose solution is 3% -4%, and the concentration of the PVDF solution is 20%.
As a further preferable technical scheme of the invention, in the step S4, the mechanical stirring speed is 1000-1500 rpm, the stirring time is 30min, and the defoaming pressure is 0.4-0.6 MPa.
In a further preferable embodiment of the present invention, in step S5, the specification of the spinning nozzle is 20 holes×0.2mm, the components of the coagulation bath are water, and the temperature of the coagulation bath is 25 to 60 ℃.
As a further preferable technical scheme of the present invention, in step S6, the fiber bundles of the cotton cellulose/PVDF composite piezoelectric fiber are cut off before braiding, each section is 5m, and then twisted.
According to another scheme of the invention, the invention also provides the electrodeless cotton cellulose/PVDF composite piezoelectric fabric, which is prepared by the preparation method of the electrodeless cotton cellulose/PVDF composite piezoelectric fabric.
According to the electrodeless cotton cellulose/PVDF composite piezoelectric fabric and the preparation method thereof, the following beneficial effects can be achieved by adopting the technical scheme:
(1) The invention takes waste cotton pulp (cotton cellulose) as raw material, adopts a preactivation process and then dissolves the waste cotton pulp in a LiCl/DMAc system, thus not only being simple to operate, but also realizing the reutilization of waste cotton.
(2) The cotton cellulose/PVDF composite spinning solution prepared by the invention has good spinnability, the coagulating bath is water and methanol, wherein the water is a green pollution-free solvent, and the methanol can be recycled.
(3) The electrodeless cotton cellulose/PVDF composite piezoelectric fabric prepared by the invention has excellent piezoelectric sensing performance, the peak open-circuit voltage and the peak short-circuit current of the fabric can respectively reach 10V and 1 mu A, and the fabric is still stable after 3000 times of cyclic tests, thereby meeting the requirement of self-powered sensing and further reducing energy consumption.
Drawings
The invention will be described in further detail with reference to the drawings and the detailed description.
FIG. 1 is a flow chart of wet spinning of composite piezoelectric fibers.
Fig. 2 is a diagram of cotton cellulose/PVDF composite piezoelectric fabric.
FIG. 3 is an infrared spectrum of a cotton cellulose/PVDF composite piezoelectric fabric.
Fig. 4 is an X-ray diffraction pattern of a cotton cellulose/PVDF composite piezoelectric fabric.
Fig. 5 is a graph showing the open circuit voltage (a) and short circuit current (b) test results for a composite piezoelectric fabric of cotton cellulose, pvdf=8:10 (mass ratio).
Fig. 6 is a graph of 3000 cycles of test results for a cotton cellulose, pvdf=8:10 (mass ratio) composite piezoelectric fabric.
Fig. 7 shows the fiber break strength for different cotton cellulose and PVDF ratios.
FIG. 8 is an open circuit voltage of a piezoelectric fabric at 10N force at different spinning pressures
The achievement of the objects, functional features and advantages of the present invention will be further described with reference to the accompanying drawings, in conjunction with the embodiments.
Detailed Description
The following describes specific embodiments of the present invention in detail with reference to the drawings. It should be understood that the detailed description and specific examples, while indicating and illustrating the invention, are not intended to limit the invention.
Unless defined otherwise, technical terms used in the following examples have the same meaning as commonly understood by one of ordinary skill in the art to which the inventive concepts pertain. The test reagents used in the following examples are all conventional biochemical reagents unless otherwise specified, and the test methods are all conventional methods unless otherwise specified.
Example 1
(1) 3.6G of absolute dry waste cotton pulp (cotton cellulose) with the polymerization degree of 543 is weighed and placed in a 250ml beaker, 30g of N, N-dimethylacetamide (DMAc) solvent is added, the mixture is activated for 6 hours at the temperature of 60 ℃, the residual DMAc solvent in the pulp is removed and recovered after the activation is finished, and then the activated cotton pulp is placed in a vacuum oven at the temperature of 60 ℃ to be dried to constant weight.
(2) Dissolving 3.6g of waste cotton pulp activated in the step (1) in 86.4g of LiCl/DMAc cosolvent, wherein the mass fraction of LiCl is 8%, mechanically stirring at the room temperature for 40min at the rotating speed of 1500rpm to obtain a cellulose solution with the mass fraction of 4%, weighing 2.52g of polyvinylidene fluoride (PVDF) with the molecular weight of 50 ten thousand, adding the polyvinylidene fluoride into 10.08gDMAc, and stirring at the temperature of 50 ℃ for 8h to obtain the PVDF solution with the mass fraction of 20%.
(3) The cellulose solution and PVDF solution obtained in the step (2) are uniformly mixed through mechanical stirring and are subjected to high-pressure defoaming treatment, wherein the cotton cellulose is PVDF=7:10 (mass ratio), and then the cotton cellulose/PVDF composite piezoelectric fiber is prepared by a wet spinning technology, wherein 5 coagulation baths for spinning are arranged, namely 1# bath, 2# bath, 3# bath and 4# bath are water, the temperature is 40 ℃, the 5# bath is methanol, the temperature is room temperature, the specification of a spinning cap for spinning is 20 holes multiplied by 0.2mm, the spinning pressure is 75kg/cm 2, and the spinning speed is 5m/min. The process flow of the wet spinning technique is shown in figure 1.
(4) Cutting the obtained fiber bundles into 5m sections, twisting, and then manually weaving into a fabric by adopting a warp-weft weaving method to obtain the electrodeless cotton cellulose/PVDF composite piezoelectric fabric as shown in figure 2.
The composite piezoelectric fabric prepared by wet spinning in example 1 was subjected to a piezoelectric sensing test, and under a 10N cyclic pressure, the open-circuit voltage and the short-circuit current were measured to be 4V and 0.5 μa, respectively, and then the structure was characterized, as shown in fig. 3 and fig. 4, in comparison with the original PVDF, the non-piezoelectric α -phase of PVDF in the cotton cellulose/PVDF piezoelectric fabric formed by wet spinning was almost disappeared, and the content of the piezoelectric β -phase was greatly increased.
As a control group of example 1, the same preparation method as in example 1 was used, and only the last coagulation bath in wet spinning was replaced with ethanol by methanol, so that the fiber spinnability was deteriorated.
Example 2
(1) 3.6G of absolute dry waste cotton pulp with the polymerization degree of 543 is weighed and placed in a 250ml beaker, 30g of DMAc solvent is added, the mixture is activated for 6 hours at the temperature of 60 ℃, the residual DMAc solvent in the pulp is removed after the activation is finished, the DMAc solvent is recovered, and then the cotton pulp after the activation treatment is placed in a vacuum oven at the temperature of 60 ℃ and dried to constant weight.
(2) Dissolving 3.6g of waste cotton pulp activated in the step (1) in 86.4g of LiCl/DMAc cosolvent, wherein the mass fraction of LiCl is 8%, mechanically stirring at the room temperature for 40min at the rotating speed of 1500rpm to obtain a cellulose solution with the mass fraction of 4%, weighing 2.88g of PVDF with the molecular weight of 50 ten thousand, adding the PVDF into 11.52g of DMAc, and stirring for 8h at the temperature of 50 ℃ to obtain a PVDF solution with the mass fraction of 20%.
(3) The solution prepared in the step (2) is uniformly mixed by mechanical stirring and is subjected to high-pressure defoaming treatment, and then the cotton cellulose/PVDF composite piezoelectric fiber is prepared by a wet spinning technology, wherein 5 coagulation baths for spinning are arranged, namely 1# bath, 2# bath, 3# bath and 4# bath are water at the temperature of 40 ℃, methanol is arranged in the 5# bath at the temperature of room temperature, the specification of a spinning cap for spinning is 20 holes multiplied by 0.2mm, the spinning pressure is 75kg/cm 2, and the spinning speed is 5m/min.
(4) The obtained fiber bundles are cut into 5m sections and twisted, and then are woven into fabrics by hand by adopting a warp-weft weaving method, namely the non-polarized cotton cellulose/PVDF composite piezoelectric fabrics.
The composite piezoelectric fabric prepared by wet spinning in example 2 was subjected to a piezoelectric sensing test, and the open circuit voltage and the short circuit current thereof were respectively 7V and 0.7 μa as measured at a 10N cycle pressure in fig. 5, which were higher than those generated at the same pressure in example 1, and remained stable through 3000 cycles of the test, as shown in fig. 6. Next, the structure is characterized, as shown in fig. 3 and 4, in the cotton cellulose/PVDF piezoelectric fabric subjected to wet spinning forming, the non-piezoelectric α phase of PVDF almost disappears, and the content of the piezoelectric β phase is greatly improved, and the content of the piezoelectric β phase of the composite piezoelectric fabric is higher than that of the fabric in example 1.
As a control group of example 2, the same preparation method as in example 2 was adopted, and only the temperature of the coagulation bath water was set to 60 ℃ and 80 ℃ respectively, and the content of the piezoelectric β phase in the prepared composite piezoelectric fiber was hardly changed, and from the viewpoints of energy saving and double diffusion of the solvent in the coagulation bath, the temperature of the coagulation bath water was 40 ℃ more suitable, the energy consumption was lower, and the preparation method was more suitable for industrial production.
Example 3
(1) 3.6G of absolute dry waste cotton pulp with the polymerization degree of 543 is weighed and placed in a 250ml beaker, 30g of DMAc solvent is added, the mixture is activated for 6 hours at the temperature of 60 ℃, the residual DMAc solvent in the pulp is removed after the activation is finished, the DMAc solvent is recovered, and then the cotton pulp after the activation treatment is placed in a vacuum oven at the temperature of 60 ℃ and dried to constant weight.
(2) Dissolving 3.6g of waste cotton pulp activated in the step (1) in 86.4g of LiCl/DMAc cosolvent, wherein the mass fraction of LiCl is 8%, mechanically stirring at the room temperature for 40min at the rotating speed of 1500rpm to obtain a cellulose solution with the mass fraction of 4%, weighing 3.24g of PVDF with the molecular weight of 50 ten thousand, adding the PVDF into 12.96g of DMAc, and stirring for 8h at the temperature of 50 ℃ to obtain a PVDF solution with the mass fraction of 20%.
(3) The solution prepared in the step (2) is uniformly mixed by mechanical stirring and is subjected to high-pressure defoaming treatment, and then the cotton cellulose/PVDF composite piezoelectric fiber is prepared by a wet spinning technology, wherein 5 coagulation baths for spinning are arranged, namely 1# bath, 2# bath, 3# bath and 4# bath are water at the temperature of 40 ℃, methanol is arranged in the 5# bath at the temperature of room temperature, the specification of a spinning cap for spinning is 20 holes multiplied by 0.2mm, the spinning pressure is 75kg/cm 2, and the spinning speed is 5m/min.
(4) The obtained fiber bundles are cut into 5m sections and twisted, and then are woven into fabrics by hand by adopting a warp-weft weaving method, namely the non-polarized cotton cellulose/PVDF composite piezoelectric fabrics.
The composite piezoelectric fabric prepared by wet spinning in example 3 was subjected to a piezoelectric sensing test, and the open circuit voltage and the short circuit current thereof were measured to be 10V and 1 μa, respectively, at a 10N cyclic pressure, which were higher than those generated at the same pressure in example 2. Next, the structure is characterized, as shown in fig. 3 and fig. 4, in the cotton cellulose/PVDF piezoelectric fabric formed by wet spinning, the non-piezoelectric α phase of PVDF almost disappears, and the content of the piezoelectric β phase is greatly increased, and in the composite piezoelectric fabric, the content of the piezoelectric β phase is higher than that of the fabric in example 2, and it can be seen that the content of the piezoelectric β phase increases with increasing PVDF content, and as shown in fig. 7, it can be seen that with further increasing PVDF content, the breaking strength of the piezoelectric fiber decreases.
As a control group of example 3, the same preparation method as in example 3 was employed, and the spinning pressure was changed to 110kg/cm 3 alone, and the open circuit voltage and open circuit current generated by the prepared piezoelectric fabric were only half of those of the original ones, 5V and 0.5. Mu.A, respectively. Further, the open circuit voltage of the piezoelectric fabric at 10N force at different spinning pressures as shown in fig. 8 was obtained by changing only the spinning pressure on the basis of example 3, and it was found that the open circuit voltage and the short circuit current of the fabric were increased and then decreased as the spinning pressure was increased, and the open circuit voltage and the short circuit current of the fabric reached the maximum values of 10V and 1 μa, respectively, when the spinning pressure was 75kg/cm 3. Therefore, the piezoelectric fabric of the present invention can generate considerable voltage and current without being polarized by an external high-voltage electric field, so that the piezoelectric fabric is used as a self-powered sensing material without being polarized by an external electric field.
While particular embodiments of the present invention have been described above, it will be appreciated by those skilled in the art that these are merely illustrative, and that many variations or modifications may be made to the embodiments without departing from the principles and spirit of the invention, the scope of which is defined only by the appended claims.
Claims (10)
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Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101550614A (en) * | 2009-05-07 | 2009-10-07 | 新疆大学 | Method of using non-adhesive method to prepare cellulose base fiber |
| KR101429542B1 (en) * | 2013-02-19 | 2014-08-14 | 국방과학연구소 | Method for producing piezoelectric properties enhanced poly(vinylidene fluoride) piezoelectric fiber using wet spinning |
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| US10828400B2 (en) * | 2014-06-10 | 2020-11-10 | The Research Foundation For The State University Of New York | Low temperature, nanostructured ceramic coatings |
| US9762176B2 (en) * | 2015-07-14 | 2017-09-12 | Maxmillian Minichetti | Hybrid photovoltaic and piezoelectric fiber |
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