CN112629718A - Three-dimensional layered MXene-wood sponge electrode and preparation method and application thereof - Google Patents
Three-dimensional layered MXene-wood sponge electrode and preparation method and application thereof Download PDFInfo
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L1/00—Measuring force or stress, in general
- G01L1/20—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress
- G01L1/22—Measuring force or stress, in general by measuring variations in ohmic resistance of solid materials or of electrically-conductive fluids; by making use of electrokinetic cells, i.e. liquid-containing cells wherein an electrical potential is produced or varied upon the application of stress using resistance strain gauges
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- A—HUMAN NECESSITIES
- A61—MEDICAL OR VETERINARY SCIENCE; HYGIENE
- A61B—DIAGNOSIS; SURGERY; IDENTIFICATION
- A61B5/00—Measuring for diagnostic purposes; Identification of persons
- A61B5/68—Arrangements of detecting, measuring or recording means, e.g. sensors, in relation to patient
- A61B5/6801—Arrangements of detecting, measuring or recording means, e.g. sensors, in relation to patient specially adapted to be attached to or worn on the body surface
- A61B5/6802—Sensor mounted on worn items
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- G—PHYSICS
- G01—MEASURING; TESTING
- G01L—MEASURING FORCE, STRESS, TORQUE, WORK, MECHANICAL POWER, MECHANICAL EFFICIENCY, OR FLUID PRESSURE
- G01L9/00—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means
- G01L9/02—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of variations in ohmic resistance, e.g. of potentiometers, electric circuits therefor, e.g. bridges, amplifiers or signal conditioning
- G01L9/04—Measuring steady of quasi-steady pressure of fluid or fluent solid material by electric or magnetic pressure-sensitive elements; Transmitting or indicating the displacement of mechanical pressure-sensitive elements, used to measure the steady or quasi-steady pressure of a fluid or fluent solid material, by electric or magnetic means by making use of variations in ohmic resistance, e.g. of potentiometers, electric circuits therefor, e.g. bridges, amplifiers or signal conditioning of resistance-strain gauges
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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
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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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
- H01G11/22—Electrodes
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
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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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
-
- 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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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/13—Energy storage using capacitors
Abstract
The invention relates to an MXene-wood sponge electrode with a three-dimensional layered structure and a preparation method and application thereof. Selectively removing lignin and hemicellulose components in the wood cell wall, and then impregnating and coating MXene nanosheets to prepare the anisotropic MXene-wood sponge. The MXene-wood sponge coated with the MXene nanosheets has excellent resilience performance and electrochemical performance, and the sensitivity, the working range and the linear sensing range of the MXene-wood sponge, the electrochemical performance of a super capacitor and the like are researched to realize self-powered sensing.
Description
Technical Field
The invention belongs to the technical field of flexible wearable electronic equipment and new materials, and particularly relates to an MXene-wood sponge electrode with a three-dimensional layered structure, a preparation method and application thereof, and particularly relates to an MXene-wood sponge electrode with a three-dimensional layered structure, a preparation method thereof and a self-powered pressure sensor assembled by using the electrode.
Background
In recent years, the growing interest in human health detection has driven the research into wearable, portable and self-powered smart devices, and in particular flexible sensors. Currently, many researchers are concerned with studying sensors that have both high sensitivity and a wide linear operating range. However, there are few reports of achieving both performance requirements simultaneously. Therefore, new materials and reasonable structures are the key to solving this problem. We have found that a book-like layered structure is more beneficial in improving the overall performance of the sensor. The plant materials, including wood, leaves and flowers, are abundant, renewable, cheap and nontoxic natural biological materials. These properties make it possible to replace conventional elastomeric substrate materials in the production of sustainable, environmentally friendly flexible sensors. The balsa wood as an important plant material has the characteristics of sustainability and richness. The chemically treated balsa wood has rich porous structure and satisfactory high-pressure retraction elastic performance. At present, the material has many reports on the aspects of oil-water separation, heat insulation, sensors, transparent composite materials and the like.
MXene is a two-dimensional layered ternary carbide/nitride nano conductive material similar to graphene, and has excellent metal-grade conductive performance and outstanding mechanical properties. It is needless to say that the preparation of flexible electrodes has a great potential in the fabrication of piezoresistive sensors. In order to prepare the self-powered compressible pressure sensor, the invention selects a liquid treatment and impregnation method, converts rigid non-conductive bulk wood blocks into flexible compressible wood sponge, impregnates MXene nanosheets to prepare MXene-wood sponge with a layered structure, selectively removes lignin and hemicellulose components in wood cell walls, and then impregnates and coats the MXene nanosheets to prepare the anisotropic MXene-wood sponge. The MXene nanosheet MXene-wood sponge coated with the MXene nanosheets has excellent resilience performance and electrochemical performance, the electrode performance of the MXene-wood sponge is explored, and the MXene nanosheet MXene-wood sponge is applied to a self-powered pressure sensor to achieve self-powered sensing.
Disclosure of Invention
Aiming at the defects in the prior art or the defects of research contents, the invention aims to provide an MXene-wood sponge electrode with a three-dimensional layered structure and a preparation method thereof, which are applied to a self-powered sensor, wherein Basa wood is treated sequentially through a two-step method of sodium chlorite and sodium hydroxide to obtain a wood sponge with excellent resilience, and then MXene nanosheets are loaded on a three-dimensional skeleton of the wood sponge to obtain the MXene-wood sponge electrode. A wood sponge electrode with a three-dimensional layered structure is used as a template to prepare the layered MXene-wood sponge self-powered sensor. The electrode is assembled into the self-powered sensor, can realize stable detection under 0-50% strain, is also stable to detection of different frequencies, has excellent air permeability and tailorability, and is very suitable for wearable pressure sensors.
In order to achieve the above purpose, one aspect of the present invention provides a method for preparing an MXene-wood sponge electrode with a three-dimensional layered structure, which comprises the steps of sequentially cutting and chemically treating natural wood in a growth direction to obtain a wood sponge skeleton, and coating the prepared wood sponge with an MXene nanosheet.
As a further preferred aspect of the present invention, the natural wood is balsa wood.
As a further preferred mode of the present invention, the chemical treatment is to remove lignin and hemicellulose components selectively from cell walls, and then to perform freeze-drying to prepare the anisotropic wood sponge.
As a further preferred aspect of the invention, the process for removing the lignin and hemicellulose components is: after the mixed solution is infiltrated, the mixed solution is dialyzed by deionized water to remove residual chemical substances, and the hemicellulose is completely removed through treatment.
In a further preferred embodiment of the present invention, the mixed solution is NaClO2Sodium acetate, acetic acid and deionized water are mixed by mild stirring to obtain NaClO2The content was 3wt%, and the pH of the mixed solution was about 4.6.
As a further preferred aspect of the present invention, the process of completely removing hemicellulose is: and (3) treating the intermediate product with a sodium hydroxide solution to achieve the aim of completely removing hemicellulose, and finally obtaining the required wood sponge.
As a further preferred aspect of the present invention, the coating process of the MXene nanosheet is as follows: wood sponges were infiltrated with an aqueous MXene dispersion in a vacuum oven, then placed on a copper plate, pre-cooled in liquid nitrogen for freezing, and then freeze-dried on a freeze dryer.
In a further preferred embodiment of the present invention, the MXene nanosheets in the MXene aqueous dispersion are Ti3C2TxA sheet layer with a size of 500-1000 nm.
As a further preferable mode of the invention, the MXene nanosheets in the MXene aqueous dispersion are obtained by selectively etching a MAX phase of a precursor by hydrochloric acid and lithium fluoride; in the MAX phase of the precursor, M is transition metal, A is mainly III group element or IV group element, and X is C element or N element; the precursor MAX phase is preferably Ti3AlC2And selectively etching to remove the Al phase.
As a further optimization of the invention, the etching is carried out by adding lithium fluoride into hydrochloric acid, and the single-layer film is formed by centrifugal cleaning and hand-shaking stripping.
In another aspect of the invention, the MXene-wood sponge electrode with the three-dimensional layered structure prepared by the preparation method is also protected.
In another aspect of the invention, the application of the MXene-wood sponge electrode with the three-dimensional layered structure in preparing a sensor is also protected, and the sensor is a self-powered pressure sensor, preferably a piezoresistive pressure sensor.
In general, compared with the prior art, the MXene-wood sponge self-powered sensor preparation method has the advantages that the sensing component is MXene-wood sponge, the preparation process is simple, and large-area production can be realized. The MXene-wood sponge electrode has good reversible compressibility and shows huge application potential in materials of flexible sensors. The wood sponge containing the holocellulose component has eco-friendly and biocompatible properties, and can be used for manufacturing MXene-wood sponges in various shapes, and the sponge can be completely restored to the original level after stress is released, so that the application of the sponge in a pressure sensor is very favorable. In addition, wood is earth-abundant as a plant material, structurally sound, sustainable, biocompatible, biodegradable, and available on a large scale. Therefore, the MXene-wood sponge preparation process is simple, large-scale preparation can be realized, and the environment is friendly.
In addition, the invention provides a new material (namely MXene-wood sponge electrode with a three-dimensional layered structure) capable of obtaining the self-powered sensor, the Basa sand wood with extremely low density and strong porosity anisotropy is selected as a raw material, and the natural wood is sequentially treated by a two-step method of sodium chlorite and sodium hydroxide to prepare the compressible and eco-friendly wood sponge. The MXene-wood sponge with a layered structure is prepared by adopting a direct impregnation process to impregnate the MXene dispersion liquid, and is applied to a self-powered piezoresistive pressure sensor. The sensor has good sensitivity (GF = 1.31), can realize stable detection under 0-50% strain, is also stable to detection of different frequencies, has excellent air permeability, and is very suitable for wearable pressure sensors.
Therefore, the MXene-wood sponge self-powered sensor with the three-dimensional layered structure can effectively avoid complicated operation processes, and the wood sponge with good reversible compressibility is finally formed by utilizing the vertical hollow pore channel structure of natural wood, so that the self-powered sensor can be prepared by simple assembly. The coated MXene nanosheet MXene-wood sponge has excellent resilience performance and electrochemical performance, the sensitivity, the working range and the linear sensing range of the sponge, the electrochemical performance of a super capacitor and the like are researched, and self-powered sensing is realized.
Drawings
The following is further described with reference to the accompanying drawings:
FIG. 1 is a process flow diagram of the present invention;
FIG. 2 is a graph of sensing performance at different strains;
FIG. 3 is a representation of a sensing linear region;
FIG. 4 shows different frequency sensing performance;
FIG. 5 is a cyclic voltammogram of MXene-wood sponge;
FIG. 6 is a graph showing the charge and discharge curves of MXene-wood sponge;
fig. 7 is a graph of rate capability of MXene-wood sponge.
Detailed Description
In order to make the objects, embodiments and advantages of the present invention more apparent and clear, the following description is provided with reference to the accompanying drawings. It is to be noted that the following description is only intended to illustrate the present invention, but not to limit the present invention. In addition, the technical features involved in the embodiments of the present invention described below may be combined with each other as long as they do not conflict with each other.
The MXene-wood sponge electrode is applied to a self-powered sensor, rigid non-conductive bulk wood blocks are converted into flexible and compressible wood sponge through cutting and chemical treatment methods, and MXene nanosheets are impregnated to obtain a three-dimensional layered structure, and a specific process flow diagram is shown in FIG. 1.
Example 1
Preparing MXene-wood sponge electrode with three-dimensional layered structure for self-powered sensor, comprising the following steps:
(1) cutting the balsa wood according to the growth direction;
(2) chemical treatment
Selective removal of lignin and hemicellulose components in cell walls: after soaking the mixed solution (pH is approximately equal to 4.6) for 10 hours at 100 ℃, dialyzing the mixed solution with deionized water for 12 hours to remove residual chemical substances; the mixed solution is prepared from NaClO2Sodium acetate, acetic acid and deionized water are obtained by mild stirring and mixing;
and then the hemicellulose is thoroughly removed through treatment: treating the intermediate product with 8% sodium hydroxide solution at 80 deg.C for about 10 hr to completely remove hemicellulose, and freeze drying to obtain anisotropic wood sponge;
(3) adding MXene nanosheets to coat the wood sponge: the wood sponge is permeated by MXene aqueous dispersion for 2 hours in a vacuum oven, then placed on a copper plate, precooled and frozen in liquid nitrogen, and then freeze-dried on a freeze dryer to obtain the wood sponge.
The concentration of the MXene aqueous dispersion is 4 mg/ml; the MXene nano-sheet in the MXene aqueous dispersion is Ti3C2TxA sheet layer having a size of 1000 nm; the MXene nanosheet is obtained by selectively etching a MAX phase of a precursor through hydrochloric acid and lithium fluoride; in the MAX phase of the precursor, M is transition metal, A is mainly III group element or IV group element, and X is C element or N element; the precursor MAX phase is preferably Ti3AlC2Selectively etching to remove Al phase; the etching is carried out by adding 1 g of lithium fluoride into 20 ml (9M) of hydrochloric acid, selectively etching for 24 h, centrifuging and washing to pH value at 3500 r>And 6, manually shaking to peel the film into a single-layer film.
The performance test results of the prepared MXene-wood sponge electrode with the three-dimensional structure are shown in FIGS. 2-7.
Fig. 2 shows that the sensing signal of the MXene-wood sponge sensor is very stable under different compression at the same frequency, and the rate of change of the resistance correspondingly increases with the increasing compression deformation, and shows a linear increase. The waveform and peak of the curve are very consistent during each strain cycle, indicating satisfactory stability of the sensing performance. Even after continuous cycling from 10% -50% compression, the resistance returns to the initial value after the stress is removed. This shows that the sensor has a good recovery capability even after cycling and large deformations, which has a very reliable long-term use.
Fig. 3 is a sensitivity test of an MXene-wood sponge sensor, the change in resistance is linear in the range of 10% -50%, and the whole test process becomes a full linear change. The resistance drops linearly with increasing strain, which is very useful for real utility testing. And the slope is 1.31, namely the sensitivity of the sensor is 1.31, and the performance of the sensor is very excellent in a compression type pressure sensor.
Fig. 4 shows the relative resistance change of the MXene-wood sponge sensor at different frequencies at 15% compression. The output signal of the MXene-wood sponge sensor is very stable at 0.2 to 4 Hz. As the frequency increases, the waveform change of the output signal is almost the same, which is probably due to the strong interaction between the MXene sheet and the wood sponge. The interconversion between different frequencies still has stable signal output and stable waveform change, which shows that the MXene-wood sponge sensor has super-strong frequency stability. Therefore, the MXene-wood sponge sensor has the advantages of good sensitivity, high stability and wide working range.
FIGS. 5, 6, and 7 show that MXene-wood sponge supercapacitor electrochemical performance is tested by using polyvinyl alcohol/sulfuric acid (PVA/H)2SO4) The gel electrolyte is used for preparing a solid MXene-wood sponge supercapacitor. The electrochemical workstation measures different current density ranges of 1-30 mA/cm2CV, GCD and area capacitance below. As shown in FIG. 5, the CV curve of MXene-wood sponge supercapacitor has a stable voltage window at scan speed of 1mv/s to 20 mv/s. The GCD measured in fig. 6 has a shape of a curve depending on the applied charge and discharge current at a current of 1mA to 20mA, and the charge and discharge curve is very symmetrical. In addition, the maximum area capacitance of the MXene-wood sponge supercapacitor was 178 microfarads/cm at a current density of 1 ma/cm, and the area capacitance of the capacitor slightly decreased as the current density increased (fig. 7). Quasi-rectangular CV curve and symmetrical charge of MXene-wood sponge super capacitorThe discharge curve shows that the material has good double-layer electrochemical behavior and rate performance.
It will be understood by those skilled in the art that the foregoing is only a preferred embodiment of the present invention, and is not intended to limit the invention, and that any modification, equivalent replacement, or improvement made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (10)
1. A preparation method of an MXene-wood sponge electrode with a three-dimensional layered structure is characterized in that natural wood is cut and chemically treated according to the growth direction in sequence to obtain a wood sponge framework, and then MXene nanosheets are added to coat the prepared wood sponge to obtain the MXene-wood sponge electrode.
2. A method according to claim 1, wherein said natural wood is balsa wood.
3. The method according to claim 1, wherein the chemical treatment is to selectively remove lignin and hemicellulose components from cell walls, and then to freeze-dry to prepare the anisotropic wood sponge.
4. The method of claim 3, wherein the removing of the lignin and hemicellulose components is performed by: after the mixed solution is infiltrated, the mixed solution is dialyzed by deionized water to remove residual chemical substances, and the hemicellulose is completely removed through treatment.
5. The method according to claim 4, wherein the mixed solution is NaClO2Sodium acetate, acetic acid and deionized water are mixed by mild stirring to obtain NaClO2The content was 3wt%, and the pH of the mixed solution was about 4.6.
6. The method according to claim 4, wherein the process of completely removing hemicellulose is: and (3) treating the intermediate product with a sodium hydroxide solution to achieve the aim of completely removing hemicellulose, and finally obtaining the required wood sponge.
7. The preparation method of claim 1, wherein the step of adding MXene nanosheets for coating comprises: wood sponges were infiltrated with an aqueous MXene dispersion in a vacuum oven, then placed on a copper plate, pre-cooled in liquid nitrogen for freezing, and then freeze-dried on a freeze dryer.
8. The preparation method of claim 7, wherein the MXene nanosheets in the MXene aqueous dispersion are Ti3C2TxA sheet layer with a size of 500-1000 nm; the MXene nanosheets in the MXene aqueous dispersion are obtained by selectively etching a precursor MAX phase through hydrochloric acid and lithium fluoride; in the MAX phase of the precursor, M is transition metal, A is mainly III group element or IV group element, and X is C element or N element; the precursor MAX phase is preferably Ti3AlC2Selectively etching to remove Al phase; the etching is carried out by adding lithium fluoride into hydrochloric acid for etching, and the single-layer film is formed by centrifugal cleaning and hand-shaking stripping.
9. MXene-wood sponge electrode of three-dimensional layered structure prepared according to the preparation method of any one of claims 1 to 8.
10. Use of the MXene-wood sponge electrode of three-dimensional layered structure according to claim 9 for the preparation of sensors, wherein said sensors are self-powered pressure sensors, preferably of piezoresistive type.
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| CN113801438A (en) * | 2021-11-16 | 2021-12-17 | 北京石墨烯技术研究院有限公司 | Heat-conducting and insulating composite material and preparation method and application thereof |
| CN113881098A (en) * | 2021-09-14 | 2022-01-04 | 中国林业科学研究院木材工业研究所 | Conductive wooden sponge with piezoresistive effect and preparation method and application thereof |
| CN114890453A (en) * | 2022-06-10 | 2022-08-12 | 南京林业大学 | Method for preparing self-supporting electrode by using MXene modified carbonized wood/metal oxide composite |
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Application publication date: 20210409 |