CN114613617A - Preparation method of wood-based micro supercapacitor - Google Patents
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- CN114613617A CN114613617A CN202210301539.5A CN202210301539A CN114613617A CN 114613617 A CN114613617 A CN 114613617A CN 202210301539 A CN202210301539 A CN 202210301539A CN 114613617 A CN114613617 A CN 114613617A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
Abstract
The invention discloses a method for preparing a wood-based micro supercapacitor, which comprises the following steps: slicing the wood along the direction parallel to the growth direction to obtain a longitudinal-section wood substrate; immersing the substrate into a delignification solution, and heating to carry out delignification treatment; freeze-drying the delignified wood substrate, and then pressing the delignified wood substrate by using a cold press to obtain a paper substrate; then the MWCNT/PEDOT: the PSS conductive ink is transferred to a paper substrate in an ink-jet printing mode; and then 0.5mL of polyvinyl alcohol/sulfuric acid electrolyte is poured on the obtained paper base material, and the paper base material is dried to obtain the wood-based micro supercapacitor. The method has the advantages of simple preparation process, mild reaction conditions, contribution to industrial production, small influence of the obtained product on the environment, and wide application in the fields of flexible electronics, energy storage and the like.
Description
Technical Field
The invention relates to a preparation method of a super capacitor, in particular to a preparation method of a wood-based micro super capacitor, and belongs to the field of electrochemical energy storage devices.
Background
With the rapid development of wearable electronic products, in addition to the inherent properties of wearable electronic products such as flexibility, stretchability, sensitivity, mechanical durability and the like, people also put higher demands on comfort and environmental performance of the wearable electronic products. The environment-friendly disposable electronic product can be thrown into the garbage can after use without generating electronic garbage, and is considered as a potential electronic product. Among them, planar Micro Supercapacitors (MSCs) have attracted great research interest as compact energy storage elements. Generally, as a miniature energy storage element (generally, a planar interdigital structure), the MSC has a great potential in small electronic devices and self-powered intelligent systems due to its high power density, fast charging rate and long cycle life. Planar interdigitated electrodes with submillimeter-scale features reduce the migration distance of ions in the electrolyte. Therefore, an important feature is that the energy density and power density of these devices are improved. A large number of paper-based MSCs have been reported due to the low cost, environmental friendliness and recyclability of paper. All conventional paper is made by pulping, bleaching and wet forming techniques. The pulping and bleaching process not only consumes a large amount of energy, but also causes environmental pollution. Therefore, there is a strong need to find a new environment-friendly substrate for preparing MSC.
The natural wood serving as a sustainable and abundant carbon resource has a unique three-dimensional microstructure, and is provided with hierarchical communication channels in the growth direction for transporting water and ions to cultivate the growth of trees. Efforts have been made to utilize the structure of wood to make various functional materials such as electrodes for batteries and supercapacitors, membrane separators and lightweight structural materials. The top-down strategy can preserve the anisotropic structure of the wood, thereby producing a mechanically robust substrate that is well suited for electronic products. More specifically, wood-based films are highly attractive as flexible electronic substrates due to their high mechanical properties, flexibility and degradability.
To prepare environmentally friendly MSCs, in addition to an environmentally friendly substrate, the environmental friendliness of the active material and the manufacturing process is required. Currently, the most commonly used materials include carbon nanotubes (MWCNTs), graphene, metal oxides, metal nanoparticles, and conductive polymers, of which MWVNTs and conductive polymers are of widespread interest. The MWCNT has narrow pore size distribution, high specific surface area utilization rate, high conductivity and high stability, and can provide stableAn electric double layer capacitor; conductive polymers have been receiving attention because of their excellent electrochemical activity, mechanical responsiveness, light weight, and flexibility. In particular poly-3, 4-ethylenedioxythiophene: polystyrene sulfonate (PEDOT: PSS) has the advantages of good mechanical property, processability, high conductivity, low intrinsic thermal conductivity and the like, and can improve the specific capacitance of an electrode when being used as a pseudocapacitance material. Therefore, the method for preparing the composite active material by combining the two materials and preparing the composite electrode on the wood substrate by combining a certain process load is a promising method. In terms of manufacturing processes, inkjet printing is considered a sustainable technology because it combines a number of advantages, such as pure additive processing, direct (maskless) patterning, relatively high resolution, minimal waste of materials, good scalability and excellent compatibility with a variety of active materials. Particularly, due to the hierarchical structure of the wood fiber, the wood obtained after the treatment is a high-quality base material for ink-jet printing, and the surface of the wood contains a large number of hydroxyl active sites, so that the wood can be conveniently combined with an active material, and a printing pattern can be quickly formed. Patent CN202010806015.2 discloses a method for preparing an interdigital paper-based micro supercapacitor, which comprises the steps of firstly, making an interdigital micro-pattern groove on filter paper by using a photoresist method; sequentially carrying out suction filtration on the conductive silver adhesive and MXene/carbon nano tube slurry on the interdigital micropattern by using a vacuum suction filtration method; final coating with polyvinyl alcohol/sulfuric acid (PVA/H)2SO4) Gel electrolyte is dried at room temperature to obtain a micro capacitor; patent CN110265227B discloses a preparation method of a self-repairing miniature supercapacitor, wherein a hydrogel polyelectrolyte monomer is coated in a groove and polymerized to obtain a hydrogel polyelectrolyte template; injecting an electrode material into the groove by a printing technology; and finally, packaging by using a self-repairing electrolyte membrane to obtain the miniature super capacitor. The preparation method has complex preparation process and does not consider the degradability and environmental protection of devices. Therefore, the invention of a wood-based micro supercapacitor is a very urgent subject.
Disclosure of Invention
Aiming at the defects of the prior art, the invention aims to provide a novel wood-based micro supercapacitor preparation method which is green, environment-friendly, simple and feasible. The prepared micro super capacitor has good electrochemical performance, excellent flexibility and degradability.
Specifically, the invention is achieved by the following technical scheme:
a preparation method of a wood-based micro supercapacitor comprises the following steps:
(1) the wood was sliced parallel to the growth direction to obtain a wood substrate having a longitudinal section.
(2) And (2) immersing the wood substrate obtained in the step (1) into a delignification solution, wherein the delignification solution is a sodium chlorite solution and a sodium hydroxide solution, the pH value of the sodium chlorite solution and the sodium hydroxide solution is adjusted to 4.6 by using acetic acid, taking out the wood substrate after the reaction is finished, washing the wood substrate by using ethanol and deionized water, and then freezing and drying the treated wood substrate.
(3) And (3) pressing the wood substrate obtained in the step (2) by using a cold press.
(4) 1mL of PEDOT: PSS solution and 0.5g of MWCNT powder were poured into 2mL of ethylene glycol solution and stirred to obtain a mixed ink, and then the mixed ink was printed on the wood substrate obtained in the step (3) with a printer.
(5) 0.5ml of VA/H2SO4And (4) pouring electrolyte on the wood substrate obtained in the step (4), and drying to obtain the wood-based micro supercapacitor.
Preferably, the wood in step (1) is selected from less dense wood, such as balsa wood, poplar wood, paulownia wood, fir wood, etc.
Preferably, the thickness of the wood substrate in step (1) is 1-2mm, most preferably 1.5 mm.
Preferably, the wood substrate obtained in step (1) is washed with deionized water and then dried under vacuum at 60 ℃ for 24 hours for later use.
Preferably, the reaction sequence of the wood in the delignification solution in the step (2) is that the wood is firstly reacted in a sodium chlorite solution with the pH value adjusted to 4.6 by acetic acid for 6 hours and then reacted in a sodium hydroxide solution for 6 hours.
Preferably, the concentration of the sodium hydroxide solution in step (2) is 1 to 5mol/L, and most preferably 2.5 mol/L.
Preferably, the sodium hydroxide and sodium chlorite used in step (2) are both analytical grade.
Preferably, the reaction in step (2) is carried out under water bath conditions.
Preferably, the washing in the step (2) is washing with ethanol and deionized water in sequence.
Preferably, the washing described in step (2) needs to be repeated three times.
Preferably, the washing in step (2) is 3 minutes at a time.
Preferably, the freeze-drying in step (2) is vacuum freeze-drying.
Preferably, the freeze-drying time of step (2) is 24 h.
Preferably, the cold press described in step (3) is a small cold press.
Preferably, the pressing pressure in step (3) is 5 MPa.
Preferably, the pressing time in step (3) is 10 min.
Preferably, PEDOT: PSS and MWCNT in step (4) are both analytically pure grades.
Preferably, the stirring in step (4) is magnetic stirring.
Preferably, the stirring time in the step (4) is 10 h.
Preferably, the printing interval in the step (4) is 5 min.
Preferably, PVA and H as described in step (5)2SO4Are all analytical grade.
Preferably, PVA and H in step (5)2SO4The amounts of (A) were 0.5mL and 0.14mL, respectively.
Preferably, the casting pitch in step (5) is 10 μm.
Preferably, the drying in step (5) is natural drying.
Preferably, the drying time in step (5) is 2 days.
According to the method, lignin and hemicellulose of wood are removed, and then the wood is subjected to freeze drying and cold pressing to obtain the base material, the paper base material has the advantages of high strength and environmental friendliness, and the MWCNT/PEDOT: PSS ink is printed on the paper base material by adopting an ink-jet printing method, so that the wood-based micro supercapacitor with excellent electrochemical performance is obtained. Compared with the prior art, the invention has the following advantages and excellent effects:
(1) in the process of preparing the miniature super capacitor, the substrate material is natural wood with wide sources, environmental protection and low cost, and the traditional paper with complex preparation process is replaced, so that the energy is saved and the cost is reduced.
(2) The method for printing by adopting the ink jet has the advantages of relatively high resolution, minimized material waste, good expandability and the like, and the prepared wood-based micro supercapacitor has good application prospect.
Drawings
FIG. 1 is a schematic view of voltammetric cycle
Detailed Description
In order to make up for the above deficiencies, the invention provides a method for manufacturing a wood-based micro supercapacitor, so as to solve the problems in the background art. The technical solutions of the present invention will be further described below with reference to specific examples, but the scope of protection and embodiments of the present invention are not limited thereto.
Example 1:
(1) barsha was sliced parallel to the growth direction to obtain a wood substrate having a thickness of 1.5mm and a length and width dimension of 10X 10 mm.
(2) Repeatedly washing the wood substrate obtained in the step (1) with deionized water, and then placing the wood substrate in a vacuum drying oven at 60 ℃ for 12h for later use.
(3) And (3) sequentially putting the sample in the step (2) into a sodium chlorite solution and a sodium hydroxide solution, wherein the pH value of the sodium chlorite solution and the sodium hydroxide solution is adjusted to 4.6 by acetic acid, and heating the sample in a water bath for 6 hours.
(4) And (4) washing the wood substrate obtained in the step (3) with ethanol and deionized water in sequence, and repeating for 3 times.
(5) And (4) freeze-drying the wood substrate obtained in the step (4) at-45 ℃ for 2 days.
(6) And (3) pressing the wood substrate obtained in the step (5) for 10min at the pressure of 2MPa by using a cold press.
(7) 1mL of poly-3, 4-ethylenedioxythiophene: pouring the polystyrene sulfonate solution and 0.5g of carbon nanotube powder into 2mL of ethylene glycol solution and stirring to obtain mixed ink, and then printing the mixed ink on the wood substrate obtained in the step (6) by using a printer.
(8) And (4) pouring 0.5mL of polyvinyl alcohol/sulfuric acid electrolyte on the wood substrate obtained in the step (7), and drying to obtain the wood-based micro supercapacitor.
(9) The obtained wood-based micro super capacitor has excellent electrochemical performance, as shown in figure 1, the specific capacitance of the obtained wood-based micro super capacitor reaches 1.81mF/cm at the scanning rate of 150mV/s2。
Example 2:
(1) the poplar was sliced parallel to the growth direction to obtain a wood substrate with a thickness of 1.5mm and a length and width dimension of 10X 10 mm.
(2) Repeatedly washing the wood substrate obtained in the step (1) with deionized water, and then placing the wood substrate in a vacuum drying oven at 60 ℃ for 12h for later use.
(3) And (3) sequentially putting the sample obtained in the step (2) into a sodium chlorite solution and a sodium hydroxide solution, wherein the pH value of the sodium chlorite solution and the sodium hydroxide solution is adjusted to 4.6 by acetic acid, and heating the samples in a water bath for 6 hours.
(4) And (4) washing the wood substrate obtained in the step (3) with ethanol and deionized water in sequence, and repeating for 3 times.
(5) And (4) freeze-drying the wood substrate obtained in the step (4) at-45 ℃ for 2 days.
(6) And (3) pressing the wood substrate obtained in the step (5) for 10min at the pressure of 2MPa by using a cold press.
(7) 1mL of poly-3, 4-ethylenedioxythiophene: pouring the polystyrene sulfonate solution and 0.5g of carbon nanotube powder into 2mL of ethylene glycol solution and stirring to obtain mixed ink, and then printing the mixed ink on the wood substrate obtained in the step (6) by using a printer.
(8) And (4) pouring 0.5mL of polyvinyl alcohol/sulfuric acid electrolyte on the wood substrate obtained in the step (7), and drying to obtain the wood-based micro supercapacitor.
(9) The obtained wood-based micro super capacitor has excellent electrochemical performance, and the specific capacitance of the obtained wood-based micro super capacitor reaches 1.76mF/cm at the scanning rate of 150mV/s2。
Example 3:
(1) paulownia wood was sliced parallel to the growth direction to obtain a wood substrate having a thickness of 1.5mm and a length and width dimension of 10 x 10 mm.
(2) Repeatedly washing the wood substrate obtained in the step (1) with deionized water, and then placing the wood substrate in a vacuum drying oven at 60 ℃ for 12h for later use.
(3) And (3) sequentially putting the sample in the step (2) into a sodium chlorite solution and a sodium hydroxide solution, wherein the pH value of the sodium chlorite solution and the sodium hydroxide solution is adjusted to 4.6 by acetic acid, and heating the sample in a water bath for 6 hours.
(4) And (4) washing the wood substrate obtained in the step (3) with ethanol and deionized water in sequence, and repeating for 3 times.
(5) And (4) freeze-drying the wood substrate obtained in the step (4) at-45 ℃ for 2 days.
(6) And (3) pressing the wood substrate obtained in the step (5) for 10min at the pressure of 2MPa by using a cold press.
(7) 1mL of poly-3, 4-ethylenedioxythiophene: pouring the polystyrene sulfonate solution and 0.5g of carbon nanotube powder into 2mL of ethylene glycol solution and stirring to obtain a mixed ink, and then printing the mixed ink onto the wood substrate obtained in step (6) by using a printer.
(8) And (4) pouring 0.5mL of polyvinyl alcohol/sulfuric acid electrolyte on the wood substrate obtained in the step (7), and drying to obtain the wood-based micro supercapacitor.
(9) The obtained wood-based micro super capacitor has excellent electrochemical performance, and the specific capacitance of the obtained wood-based micro super capacitor reaches 1.74mF/cm at the scanning rate of 150mV/s2。
Example 4:
(1) fir wood was sliced parallel to the growth direction to obtain wood substrates 1.5mm in thickness and 10 x 10mm in length and width.
(2) Repeatedly washing the wood substrate obtained in the step (1) with deionized water, and then placing the wood substrate in a vacuum drying oven at 60 ℃ for 12h for later use.
(3) And (3) sequentially putting the sample obtained in the step (2) into a sodium chlorite solution and a sodium hydroxide solution, wherein the pH value of the sodium chlorite solution and the sodium hydroxide solution is adjusted to 4.6 by acetic acid, and heating the samples in a water bath for 6 hours.
(4) And (4) washing the wood substrate obtained in the step (3) with ethanol and deionized water in sequence, and repeating for 3 times.
(5) And (4) freeze-drying the wood substrate obtained in the step (4) at-45 ℃ for 2 days.
(6) And (3) pressing the wood substrate obtained in the step (5) for 10min at the pressure of 2MPa by using a cold press.
(7) 1mL of poly-3, 4-ethylenedioxythiophene: pouring the polystyrene sulfonate solution and 0.5g of carbon nanotube powder into 2mL of ethylene glycol solution and stirring to obtain mixed ink, and then printing the mixed ink on the wood substrate obtained in the step (6) by using a printer.
(8) And (4) pouring 0.5mL of polyvinyl alcohol/sulfuric acid electrolyte on the wood substrate obtained in the step (7), and drying to obtain the wood-based micro supercapacitor.
(9) The obtained wood-based micro super capacitor has excellent electrochemical performance, and the specific capacitance of the obtained wood-based micro super capacitor reaches 1.87mF/cm at the scanning rate of 150mV/s2。
Claims (7)
1. A method for preparing a wood-based micro supercapacitor is characterized by comprising the following steps:
(1) slicing the wood along the direction parallel to the growth direction to obtain a wood substrate with a longitudinal section, wherein the thickness of the wood substrate is 1-2 mm;
(2) immersing the wood substrate obtained in the step (1) into a delignification solution, wherein the delignification solution is a sodium chlorite solution and a sodium hydroxide solution, the pH value of the sodium chlorite solution and the sodium hydroxide solution is adjusted to 4.6 by using acetic acid, taking out the wood substrate after the reaction is finished, washing the wood substrate by using ethanol and deionized water, and then freeze-drying the treated wood substrate;
(3) pressing the wood substrate obtained in the step (2) by using a cold press;
(4) 1mL of poly-3, 4-ethylenedioxythiophene: pouring the polystyrene sulfonate solution and 0.5g of carbon nano tube powder into 2mL of glycol solution and stirring to obtain mixed ink, and then printing the mixed ink on the wood substrate obtained in the step (3) by using a printer;
(5) and (4) pouring 0.5mL of polyvinyl alcohol/sulfuric acid electrolyte on the wood substrate obtained in the step (4), and drying to obtain the wood-based micro supercapacitor.
2. The method according to claim 1, wherein the wood substrate in the step (1) has a thickness of 1.5mm and a length and width dimension of 10 x 10 mm.
3. The method according to claim 1, wherein the concentration of the sodium hydroxide solution in the step (2) is 2.5 mol/L.
4. The method according to claim 1, wherein the freeze-drying in step (2) is a freeze-drying at-45 ℃ for 36 hours in a freeze-dryer.
5. The method of claim 1, wherein the pressure of the cold press in step (3) is 5Mpa, and the reaction time is 10 min.
6. The method according to claim 1, wherein the stirring time in the step (4) is 10 hours.
7. The method according to claim 1, wherein the drying in the step (5) is natural drying for 2 days.
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