CN115101356A - Wood-based high-density solid electrode and preparation method thereof - Google Patents
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- 238000002360 preparation method Methods 0.000 title claims abstract description 9
- 239000007787 solid Substances 0.000 title claims abstract description 6
- 238000007731 hot pressing Methods 0.000 claims abstract description 23
- 238000005087 graphitization Methods 0.000 claims abstract description 16
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000010411 cooking Methods 0.000 claims abstract description 12
- 238000005520 cutting process Methods 0.000 claims abstract description 12
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 240000007182 Ochroma pyramidale Species 0.000 claims description 18
- 239000007772 electrode material Substances 0.000 claims description 16
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 claims description 13
- 229910052938 sodium sulfate Inorganic materials 0.000 claims description 13
- 235000011152 sodium sulphate Nutrition 0.000 claims description 13
- 238000004108 freeze drying Methods 0.000 claims description 11
- 238000005406 washing Methods 0.000 claims description 11
- 238000001035 drying Methods 0.000 claims description 8
- 238000004519 manufacturing process Methods 0.000 claims description 8
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 6
- 238000002791 soaking Methods 0.000 claims description 6
- 239000002131 composite material Substances 0.000 claims description 5
- 239000000835 fiber Substances 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 4
- GEHJYWRUCIMESM-UHFFFAOYSA-L sodium sulfite Chemical compound [Na+].[Na+].[O-]S([O-])=O GEHJYWRUCIMESM-UHFFFAOYSA-L 0.000 abstract 2
- 230000002378 acidificating effect Effects 0.000 abstract 1
- 238000005470 impregnation Methods 0.000 abstract 1
- 235000010265 sodium sulphite Nutrition 0.000 abstract 1
- 239000004964 aerogel Substances 0.000 description 28
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 18
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- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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, LIGHT-SENSITIVE OR TEMPERATURE-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, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/32—Carbon-based
- H01G11/34—Carbon-based characterised by carbonisation or activation of carbon
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
- H01G11/32—Carbon-based
- H01G11/44—Raw materials therefor, e.g. resins or coal
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Abstract
The invention discloses a wood-based high-density solid electrode and a preparation method thereof; the method comprises the following steps: (1) cutting wood into block bodies with the same size; (2) cooking the cut wood pieces with an acidic sodium sulfite solution to obtain delignified wood pieces; (3) the method comprises the following steps of (1) realizing effective loading of graphene oxide on a steamed wood block by using a vacuum impregnation technology, and then carrying out hot pressing under a hot press; (4) and heating the hot-pressed wood blocks to 900 ℃ in an oxygen-free environment to obtain the high-density solid electrode. The invention utilizes abundant similar tracheid structure and fiber direction characteristics in the wood, and greatly improves the volume specific capacitance of the wood by hot pressing and graphitization technology.
Description
Technical Field
The invention relates to the field of wood for a supercapacitor, in particular to a wood-based high-density solid-state electrode and a preparation method thereof.
Background
In recent years, with the gradual reduction of fossil fuels and the continuous enhancement of environmental awareness, sustainable development gradually becomes a main development mode.
Compared with fossil fuels, the bio-based materials have the advantages of abundant reserves, wide sources, greenness, renewability, a few points and the like, and corresponding energy storage equipment is required to fully utilize novel renewable energy. However, the traditional energy storage technology is difficult to achieve ideal energy density, and is not favorable for the green and sustainable development of energy storage equipment.
Therefore, the development of efficient electrochemical energy storage systems with high energy and high power characteristics to meet the needs of today's and future society for inexpensive, flexible, lightweight energy storage devices has become a hot area of current scientific research. Supercapacitors, also referred to as electrochemical capacitors, are considered the most promising development in mobile energy storage technology because of their advantages of ultra-fast power supply capability, high energy density and long cycle life.
The wood is used as a renewable, recyclable and naturally degradable material, has a fixed space capable of accommodating other particles or powder, polymers and other structural units, most of the space originates from a conduit and a sieve pipe left by the life activities of the wood, and provides a great development space for the performance improvement and the functionalization of the wood.
Meanwhile, due to the porous structure and the unique texture characteristics of the wood, the wood has certain radial compression performance, and an important opportunity is provided for constructing the light and thin wood-based polyelectrolyte composite energy storage material.
However, the current wood-based supercapacitor materials still have the defect that the light weight, the thinness and the high capacitance cannot be achieved at the same time. In addition, the use of toxic substances and relatively complicated process flow in the preparation process are also important problems restricting practical application.
Therefore, it is urgent to prepare a wood-based electrode material having light weight and excellent electrochemical properties using conventional instruments and a simple processing method.
Disclosure of Invention
The present invention has been made to overcome the above-mentioned drawbacks and disadvantages of the prior art, and an object of the present invention is to provide a wood-based high-density solid-state electrode and a method for manufacturing the same.
According to the invention, graphene oxide is doped into wood with a porous structure by adopting a vacuum infiltration method, and then hot pressing and graphitization treatment are carried out on the wood by utilizing the texture characteristics of the wood. The prepared wood-based electrode material has both higher density and reasonable pore size distribution, and is an ideal material for a supercapacitor electrode;
the invention is realized by the following technical scheme:
a method for preparing a wood-based high-density solid-state electrode comprises the following steps:
the method comprises the following steps: cutting the balsawood into blocky structures to obtain balsawood blocks;
step two: vacuum soaking the cut balsawood blocks in a sodium sulfate solution, cooking and washing to obtain porous wood;
step three: hot-pressing the porous wood obtained in the step two by using a hot press; naturally drying after hot pressing; obtaining naturally dried porous wood;
step four: vacuum soaking the porous wood obtained in the step two in a graphene oxide solution, and freeze-drying after loading is finished; obtaining a wood @ graphene oxide composite material;
step five: carrying out hot pressing on the wood @ graphene oxide composite material obtained in the fourth step by using a hot press, and naturally drying after the hot pressing is finished; obtaining hot-pressed wood;
step six: and (4) carrying out graphitization treatment on the porous wood naturally dried in the third step and the hot-pressed wood obtained in the fifth step in an oxygen-free environment to complete the preparation of the wood-based high-density solid electrode.
In the first step, the volume of the balsa blocks is 2 multiplied by 2 cm.
In the second step, the concentration of sodium sulfate is 0.4M, and the pH value is adjusted to 4.6 by acetic acid.
In the third step, the pressure of hot pressing is 0-1MP, and the time is 6-12 h.
In the fourth step, the vacuum degree of vacuum soaking is-1 MP, and the time is 5-10 min.
In the fifth step, the hot pressing pressure is 0-1MP, and the time is 0-24 h.
In the sixth step, the graphitization treatment conditions are as follows: heating to 250 deg.C at 5 deg.C/min, maintaining for 120min, heating to 900 deg.C at 5 deg.C/min, and maintaining for 120 min.
The invention takes the wood fiber biomass balsawood as the raw material, effectively breaks through the pipeline structure of the wood by utilizing the chemical delignification method, and creates favorable conditions for doping and hot pressing of the graphite oxide. The multistage pore structure of wood is effectively designed by combining graphitization treatment, and a high-speed channel is provided for transmission of ions and electrons. The treated three-dimensional wood structure has a large number of micropores and macroporous structures arranged along the growth direction, so that graphene oxide can uniformly permeate into the interior of the three-dimensional wood structure. The hierarchical porous structure in wood effectively increases the specific surface area of the electrode, so that the rapid passing of electrons is facilitated.
The super capacitor electrode material prepared by the method has strong potential as an energy storage and conversion electrode material with high energy/power density, low cost and green.
Compared with the prior art, the method has the advantages that the internal pipeline of the wood is firstly opened, the graphene is oxidized in a vacuum permeation mode, and the three-dimensional electrode material with high energy density and micro volume is prepared by utilizing hot pressing and oxygen-free graphene treatment. The three-dimensional graphene oxide carbon electrode material directly prepared by the method at least has the following advantages:
(1) conventional preparation equipment is adopted, and the required equipment does not need to be modified;
(2) the preparation process is simple, the cost is low, and the environment is protected;
(3) the abundant pipeline characteristics in wood are ingeniously utilized to dope graphene oxide, and meanwhile, the natural texture structure characteristics are utilized, and the hierarchical porous structure is adjusted through hot pressing.
Drawings
Fig. 1 is a scanning electron microscope image of the wood-based aerogel prepared in example 1 of the present invention.
Detailed Description
The present invention will be described in further detail with reference to specific examples.
Example 1:
(1) cutting the balsawood into regular block structures with the length, width and thickness of 2 multiplied by 2 cm;
(2) cooking the wood obtained in the step (1) in a 0.4M sodium sulfate solution for 8 hours, then washing the wood with 50% ethanol/water and deionized water for several times, and finally freeze-drying to obtain regular wood aerogel;
(3) and (4) carrying out anaerobic graphitization treatment on the wood aerogel obtained in the step (3) in a tubular furnace under the condition that the temperature is raised to 250 ℃ at the normal temperature at the speed of 5 ℃/min, preserving the heat for 120min, then continuously raising the temperature to 900 ℃ at the speed of 5 ℃/min, preserving the heat for 120min, and finally naturally cooling to room temperature to obtain the product, namely the three-dimensional wood-based electrode material.
Example 2:
(1) cutting balsawood into regular blocky structures with the length, width and thickness of 2 multiplied by 2;
(2) cooking the wood obtained in the step (1) in a 0.4M sodium sulfate solution for 8 hours, then washing the wood with 50% ethanol/water and deionized water for several times, and finally freeze-drying to obtain regular wood aerogel;
(3) and (3) carrying out hot pressing on the wood hydrogel obtained in the step (2) for 8 hours in a direction perpendicular to the fiber direction by using a hot press 100MP to obtain the wood aerogel with the length, width and thickness of 2 multiplied by 1.6 cm.
(4) And (4) carrying out anaerobic graphitization treatment on the wood aerogel obtained in the step (3) in a tubular furnace under the condition that the temperature is raised to 250 ℃ at the normal temperature at the speed of 5 ℃/min, preserving the heat for 120min, then continuously raising the temperature to 900 ℃ at the speed of 5 ℃/min, preserving the heat for 120min, and finally naturally cooling to room temperature to obtain the product, namely the three-dimensional wood-based electrode material.
Example 3:
(1) cutting the balsawood into regular block structures with the length, width and thickness of 2 multiplied by 2;
(2) cooking the wood obtained in the step (1) in a 0.4M sodium sulfate solution for 8 hours, then washing the wood with 50% ethanol/water and deionized water for several times, and finally freeze-drying to obtain regular wood aerogel;
(3) and (3) carrying out hot pressing on the wood hydrogel obtained in the step (2) in a direction perpendicular to the fiber direction by using a hot press 100MP for 12 times to obtain the wood aerogel with the length, width and thickness of 2 multiplied by 1.0 cm.
(4) And (4) carrying out anaerobic graphitization treatment on the wood aerogel obtained in the step (3) in a tubular furnace under the condition that the temperature is raised to 250 ℃ at the normal temperature at the speed of 5 ℃/min, preserving the heat for 120min, then continuously raising the temperature to 900 ℃ at the speed of 5 ℃/min, preserving the heat for 120min, and finally naturally cooling to room temperature to obtain the product, namely the three-dimensional wood-based electrode material.
Example 4
(1) Cutting the balsawood into regular block structures with the length, width and thickness of 2 multiplied by 2;
(2) cooking the wood obtained in the step (1) in a 0.4M sodium sulfate solution for 8 hours, then washing the wood with 50% ethanol/water and deionized water for several times, and finally freeze-drying to obtain regular wood aerogel;
(3) and (3) carrying out hot pressing on the wood hydrogel obtained in the step (2) for 16 hours in a direction perpendicular to the fiber direction by using a hot press 100MP to obtain the wood aerogel with the length, width and thickness of 2 multiplied by 0.8 cm.
(4) And (4) carrying out anaerobic graphitization treatment on the wood aerogel obtained in the step (3) in a tubular furnace under the condition that the temperature is raised to 250 ℃ at the normal temperature at the speed of 5 ℃/min, preserving the heat for 120min, then continuously raising the temperature to 900 ℃ at the speed of 5 ℃/min, preserving the heat for 120min, and finally naturally cooling to room temperature to obtain the product, namely the three-dimensional wood-based electrode material.
Example 5:
(1) cutting balsawood into regular blocky structures with the length, width and thickness of 2 multiplied by 2;
(2) cooking the wood obtained in the step (1) in a 0.4M sodium sulfate solution for 8 hours, then washing the wood with 50% ethanol/water and deionized water for several times, and finally freeze-drying to obtain regular wood aerogel;
(3) and (3) carrying out hot pressing on the wood hydrogel obtained in the step (2) for 24 hours in a direction perpendicular to the fiber direction by using a hot press 100MP to obtain the wood aerogel with the length, width and thickness of 2 multiplied by 0.4 cm.
(4) And (4) carrying out anaerobic graphitization treatment on the wood aerogel obtained in the step (3) in a tubular furnace under the condition that the temperature is raised to 250 ℃ at the normal temperature at the speed of 5 ℃/min, preserving the heat for 120min, then continuously raising the temperature to 900 ℃ at the speed of 5 ℃/min, preserving the heat for 120min, and finally naturally cooling to room temperature to obtain the product, namely the three-dimensional wood-based electrode material.
Example 6:
(1) cutting balsawood into regular blocky structures with the length, width and thickness of 2 multiplied by 2;
(2) cooking the wood obtained in the step (1) in a 0.4M sodium sulfate solution for 8 hours, then washing the wood with 50% ethanol/water and deionized water for several times, and finally freeze-drying to obtain regular wood aerogel;
(3) vacuum-dipping the wood hydrogel obtained in the step (2) in 1mg/mL GO solution for 5-10min, and finally freezing and drying to obtain wood @ GO aerogel;
(4) and (4) carrying out anaerobic graphitization treatment on the wood aerogel obtained in the step (3) in a tubular furnace under the condition that the temperature is raised to 250 ℃ at the normal temperature at the speed of 5 ℃/min, preserving the heat for 120min, then continuously raising the temperature to 900 ℃ at the speed of 5 ℃/min, preserving the heat for 120min, and finally naturally cooling to room temperature to obtain the product, namely the three-dimensional wood-based electrode material.
Example 7:
(1) cutting the balsawood into regular block structures with the length, width and thickness of 2 multiplied by 2;
(2) cooking the wood obtained in the step (1) in a 0.4M sodium sulfate solution for 8 hours, then washing the wood with 50% ethanol/water and deionized water for several times, and finally freeze-drying to obtain regular wood aerogel;
(3) vacuum-dipping the wood hydrogel obtained in the step (2) in 2mg/mL GO solution for 5-10min, and finally freezing and drying to obtain wood @ GO aerogel;
(4) and (4) carrying out anaerobic graphitization treatment on the wood aerogel obtained in the step (3) in a tubular furnace under the condition that the temperature is raised to 250 ℃ at the normal temperature at the speed of 5 ℃/min, preserving the heat for 120min, then continuously raising the temperature to 900 ℃ at the speed of 5 ℃/min, preserving the heat for 120min, and finally naturally cooling to room temperature to obtain the product, namely the three-dimensional wood-based electrode material.
Example 8:
(1) cutting the balsawood into regular block structures with the length, width and thickness of 2 multiplied by 2;
(2) cooking the wood obtained in the step (1) in a 0.4M sodium sulfate solution for 8 hours, then washing the wood with 50% ethanol/water and deionized water for several times, and finally freeze-drying to obtain regular wood aerogel;
(3) vacuum-dipping the wood hydrogel obtained in the step (2) in a GO solution of 5mg/mL for 5-10min, and finally freezing and drying to obtain wood @ GO aerogel;
(4) and (4) carrying out anaerobic graphitization treatment on the wood aerogel obtained in the step (3) in a tubular furnace under the condition that the temperature is raised to 250 ℃ at the normal temperature at the speed of 5 ℃/min, preserving the heat for 120min, then continuously raising the temperature to 900 ℃ at the speed of 5 ℃/min, preserving the heat for 120min, and finally naturally cooling to room temperature to obtain the product, namely the three-dimensional wood-based electrode material.
Example 9:
(1) cutting the balsawood into regular block structures with the length, width and thickness of 2 multiplied by 2;
(2) cooking the wood obtained in the step (1) in a 0.4M sodium sulfate solution for 8 hours, then washing the wood with 50% ethanol/water and deionized water for several times, and finally freeze-drying to obtain regular wood aerogel;
(3) vacuum-dipping the wood hydrogel obtained in the step (2) in a GO solution of 2mg/mL for 5-10min, and finally freezing and drying to obtain wood @ GO aerogel;
(4) and (4) carrying out hot pressing on the wood hydrogel obtained in the step (3) for 16 hours in a direction perpendicular to the fiber direction by using a hot press 100MP to obtain the wood @ GO aerogel with the length, width and thickness of 2 multiplied by 0.8 cm.
(5) And (4) carrying out anaerobic graphitization treatment on the wood aerogel obtained in the step (4) in a tubular furnace under the condition that the temperature is raised to 250 ℃ at the normal temperature at the speed of 5 ℃/min, preserving the heat for 120min, then continuously raising the temperature to 900 ℃ at the speed of 5 ℃/min, preserving the heat for 120min, and finally naturally cooling to room temperature to obtain the product, namely the three-dimensional wood-based electrode material.
As described above, the present invention can be preferably realized.
The embodiments of the present invention are not limited to the above-described embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and they are included in the scope of the present invention.
Claims (8)
1. A method for preparing a wood-based high-density solid-state electrode is characterized by comprising the following steps:
the method comprises the following steps: cutting the balsawood into blocky structures to obtain balsawood blocks;
step two: vacuum soaking the cut balsawood blocks in a sodium sulfate solution, cooking and washing to obtain porous wood;
step three: hot-pressing the porous wood obtained in the step two by using a hot press; naturally drying after hot pressing; obtaining naturally dried porous wood;
step four: vacuum soaking the porous wood obtained in the step two in a graphene oxide solution, and freeze-drying after loading is finished; obtaining a wood @ graphene oxide composite material;
step five: carrying out hot pressing on the wood @ graphene oxide composite material obtained in the fourth step by using a hot press, and naturally drying after the hot pressing is finished; obtaining hot-pressed wood;
step six: and (4) carrying out graphitization treatment on the porous wood naturally dried in the third step and the hot-pressed wood obtained in the fifth step in an oxygen-free environment to complete the preparation of the wood-based high-density solid electrode.
2. The method for producing a wood-based high-density solid-state electrode according to claim 1, wherein:
in the first step, the volume of the balsa blocks is 2 multiplied by 2 cm.
3. The method for producing a wood-based high-density solid-state electrode according to claim 1, wherein:
in the second step, the concentration of sodium sulfate is 0.4M, and the pH value is adjusted to 4.6 by acetic acid.
4. The method for producing a wood-based high-density solid-state electrode according to claim 3, wherein:
in the third step, the pressure of hot pressing is 0-1MP, and the time is 6-12 h.
5. The method for producing a wood-based high-density solid-state electrode according to claim 4, wherein:
in the fourth step, the vacuum degree of vacuum soaking is-1 MP, and the time is 30 min.
6. The method for producing a wood-based high-density solid-state electrode according to claim 5, wherein:
in the fifth step, the pressure of hot pressing is 0-1MP, and the time is 6-12 h.
7. The method for producing a wood-based high-density solid-state electrode according to claim 6, wherein:
in the sixth step, the graphitization treatment conditions are as follows: heating to 250 deg.C at 5 deg.C/min, maintaining for 120min, heating to 900 deg.C at 5 deg.C/min, and maintaining for 120 min.
8. A wood-based electrode material characterized by being obtained by the production method according to any one of claims 1 to 7.
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