CN111463028A - rGO-L iOH micro-spring/wood composite electrode material, and preparation method and application thereof - Google Patents
rGO-L iOH micro-spring/wood composite electrode material, and preparation method and application thereof Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 62
- 238000002360 preparation method Methods 0.000 title claims abstract description 22
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 61
- 229910021389 graphene Inorganic materials 0.000 claims abstract description 54
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000003990 capacitor Substances 0.000 claims abstract description 26
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 23
- 238000000034 method Methods 0.000 claims abstract description 22
- XGZVUEUWXADBQD-UHFFFAOYSA-L lithium carbonate Chemical compound [Li+].[Li+].[O-]C([O-])=O XGZVUEUWXADBQD-UHFFFAOYSA-L 0.000 claims abstract description 21
- 229910052808 lithium carbonate Inorganic materials 0.000 claims abstract description 21
- 239000011148 porous material Substances 0.000 claims abstract description 21
- 239000004964 aerogel Substances 0.000 claims abstract description 19
- 239000008367 deionised water Substances 0.000 claims abstract description 19
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 19
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 16
- 238000004108 freeze drying Methods 0.000 claims abstract description 12
- 239000011261 inert gas Substances 0.000 claims abstract description 9
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 claims description 40
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 36
- 229960000583 acetic acid Drugs 0.000 claims description 20
- 239000012362 glacial acetic acid Substances 0.000 claims description 20
- UKLNMMHNWFDKNT-UHFFFAOYSA-M sodium chlorite Chemical compound [Na+].[O-]Cl=O UKLNMMHNWFDKNT-UHFFFAOYSA-M 0.000 claims description 20
- 229960002218 sodium chlorite Drugs 0.000 claims description 20
- 238000010438 heat treatment Methods 0.000 claims description 18
- 238000007664 blowing Methods 0.000 claims description 15
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- 238000010298 pulverizing process Methods 0.000 claims 1
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- 239000002028 Biomass Substances 0.000 description 2
- WHXSMMKQMYFTQS-UHFFFAOYSA-N Lithium Chemical compound [Li] WHXSMMKQMYFTQS-UHFFFAOYSA-N 0.000 description 2
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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
- H01G11/22—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
-
- 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
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
-
- 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
- H01G11/32—Carbon-based
- H01G11/44—Raw materials therefor, e.g. resins or coal
Abstract
The invention provides an rGO-L iOH micro-spring/wood composite electrode material, and a preparation method and application thereof, wherein the method comprises the step 1 of carrying out ultrasonic crushing on lithium carbonate, graphene oxide and deionized water, and then carrying out freeze drying to obtain L iCO3And GO, step 2, L iCO3Removing water in the aerogel with GO, then preserving heat for 2-5 h at 1000-1200 ℃ in nitrogen or inert gas to obtain an rGO-L iOH micro spring, and step 3, expanding the rGO-L iOH micro spring into a pore channel of carbonized delignified wood to obtain three-dimensional high specific capacitance, high elasticity, high porosity and high specific capacitanceSurface area of electrode material. The electrode material can be further assembled into a flexible capacitor or a wearable capacitor, which can then drive any electronic device within the range of the capacitor.
Description
Technical Field
The invention belongs to the technical field of biomass energy, and particularly relates to an rGO-L iOH micro-spring/wood composite electrode material, and a preparation method and application thereof.
Background
The super capacitor has the advantages of flexible capacity configuration, easiness in realization of modular design, long cycle service life, wide working temperature range, environmental friendliness, no maintenance and the like, and the characteristics enable the super capacitor to be more suitable for harsh working environments. In recent years, with the development of carbon nanotechnology, the manufacturing cost of the super capacitor is continuously reduced, and the power density and the energy density of the super capacitor are continuously improved, which will further expand and accelerate the application of the super capacitor in the aspect of novel power energy storage.
Among the electrode materials of the super capacitor, the carbon electrode material is the most used electrode material due to the advantages of the carbon electrode material such as porosity, high specific surface area structure, good conductivity, wide pore size distribution and the like. Chemical Vapor Deposition (CVD) is a classical method of synthesizing carbon materials. In fact, a regular, ordered, low defect carbon material can be obtained by CVD high temperature reduction. Therefore, aiming at the problem that the developed carbon material is difficult to produce on a large scale, wood widely distributed in nature is taken as a natural carbon source, the wood without lignin has excellent double electric layer characteristics after being reduced by a high-temperature reduction method, namely a CVD method, and meanwhile, the natural biomass carbon source has higher cycling stability and can provide high cycling stability for the composite material. The material also has certain elastic characteristic, because the large-area pipeline structure left by the wood with the lignin removed is similar to an arch structure, and the structure has certain elastic stability in composition, so that the material is applied to the preparation of the electrode material of the super capacitor, the large-scale preparation of the capacitor material is possible on the premise of not influencing the performance of the capacitor material, and the capacitor has circular elastic stability.
Therefore, the electrode material with high specific capacitance, high elasticity, high porosity and high specific surface area is hopefully prepared by utilizing the double electric layer characteristics and arch-structure pore channels of the carbonized wood, but the report of the aspect is not available at present.
Disclosure of Invention
Aiming at the problems in the prior art, the invention provides the rGO-L iOH micro-spring/wood composite electrode material, the preparation method and the application thereof, the process is simple, the design is novel, the obtained electrode material provides effective pore channels and larger specific surface area for the infiltration of electrolyte and the storage of electrons, so that the energy density, the power density and the charge/discharge stability of the material are improved, and meanwhile, the arched structure of wood and reduced graphene oxide supported by lithium hydroxide jointly form a 3D composite material with high elasticity.
The invention is realized by the following technical scheme:
the preparation method of the rGO-L iOH micro-spring/wood composite electrode material comprises the following steps,
step 2, L iCO3Removing water in the aerogel with GO, and then preserving heat for 2-5 hours at 1000-1200 ℃ in nitrogen or inert gas to obtain an rGO-L iOH micro spring;
and 3, inflating the rGO-L iOH micro spring into a pore channel of the carbonized delignified wood to obtain the rGO-L iOH micro spring/wood composite electrode material.
Preferably, in the step 1, the ratio of lithium carbonate to deionized water is (0.1-0.3) mol: (150-400) ml.
Preferably, the mixed system in the step 1 is subjected to ultrasonic crushing by using an ultrasonic cell crusher, and the required time is 10-30 min;
the working frequency of the ultrasonic cell crusher is 20-24 KHz, the ultrasonic power is 200-600W, and the temperature is 25-40 ℃.
Preferably, the mixed system in the step 1 is freeze-dried for 2-4 hours at-50 to-5 ℃.
Preferably, in step 2, L iCO is added3And keeping the temperature of the aerogel and GO at 130-300 ℃ for 2-4 h, and then keeping the temperature at 1000-1200 ℃.
Preferably, in the step 2, the wood chips are soaked in a mixed system composed of sodium chlorite, glacial acetic acid and deionized water and stirred, then the wood chips are sequentially frozen and freeze-dried, and finally the carbonized delignified wood is obtained by heat preservation for 3-6 hours at 650-800 ℃ in nitrogen or inert gas at the heating rate of 3-15 ℃/min.
Preferably, in step 3, the rGO-L iOH micro-spring is ultrasonically dispersed in ethanol or ethanol solution with volume fraction of more than or equal to 90%, the micro-spring is blown into the pore channel of the carbonized delignified wood by a double-row pipe air pumping and blowing method, and the rGO-L iOH micro-spring/wood composite electrode material is obtained after the ethanol is volatilized.
An rGO-L iOH micro-spring/wood composite electrode material prepared by the preparation method of the rGO-L iOH micro-spring/wood composite electrode material.
An elastic capacitor or a wearable capacitor comprising the above-described rGO-L iOH micro-spring/wood composite electrode material.
An electronic device driven by the capacitor.
Compared with the prior art, the invention has the following beneficial technical effects:
according to the preparation method of the rGO-L iOH micro-spring/wood composite electrode material, lithium carbonate is selected as a lithium source, and a mixed aqueous solution of the lithium carbonate and graphene oxide is subjected to ultrasonic crushing treatment to obtain L iCO3And GO, dewatering and then carrying out high-temperature treatment, wherein lithium carbonate is converted into lithium hydroxide and grows between reduced graphene oxide sheet layers to form a lithium hydroxide supported reduced graphene oxide micro-spring structure, simultaneously removing lignin in wood and carbonizing, and expanding an rGO-L iOH micro-spring into a pore channel of carbonized delignified wood to obtain an electrode material with three-dimensional high specific capacitance, high elasticity, high porosity and high specific surface areaThe three-dimensional composite elastic material is formed, the process is simple, the loading capacity of electrons is improved, and the transmission rate of charges is improved, so that the internal resistance of the material is reduced, and the energy storage characteristic of the material is improved.
The rGO-L iOH micro-spring/wood composite electrode material has the advantages that L iOH grows between graphene oxide sheet layers to obtain reduced graphene oxide supported by lithium hydroxide, so that the aim of separating graphene can be achieved, and the reduced graphene oxide can be endowed with a certain elastic action, the reduced graphene oxide is used as a contributor of pseudo capacitance, the pseudo capacitance characteristic is built together with the lithium hydroxide, so that a reduced graphene oxide loaded lithium hydroxide composite material with a large specific surface area is built, the material and double electric layer characteristics of carbonized wood form a synergistic action, an obtained super capacitor has the peak clipping and valley filling effects, a small spring model formed by L iOH growing between the reduced graphene oxide sheet layers has a certain elastic action, and forms a composite 3D electrode material together with the wood when the material enters arched structural pore channels of the wood, so that the material has the characteristics of high specific capacitance, high elasticity, high porosity and high specific surface area, and has an excellent damping effect, when the composite material is subjected to an external force, the arched 3D electrode material and the wood form a composite electrode material, so that the wood has a certain mechanical effect of protecting the arched structural pore channels of the wood, the wood is capable of preventing the wood from being damaged by the electrochemical load of the wood, and capable of preventing the wood from being damaged by the wood, and capable of reducing graphene oxide, so that the wood, the wood can not only can be completely damaged by the wood, and can be discharged in a certain amount of the wood, so that the wood, and the wood, the wood can be discharged, and the wood.
Drawings
FIG. 1 is a scanning electron microscope image of a cross section of wood in the rGO-L iOH micro-spring/wood composite electrode material prepared in example 1 of the present invention.
FIG. 2 is a scanning electron micrograph of the rGO-L iOH micro-spring/wood composite electrode material prepared in example 1 of the present invention along the length direction of the wood.
FIG. 3 is a comparison graph of specific capacitance of high temperature reduced pure wood and rGO-L iOH micro-spring/wood composite electrode material prepared in example 1 of the present invention under 1000 cyclic voltammetry.
FIG. 4 is a graph of capacitance retention curves for different scan rates for high temperature reduced pure wood and the rGO-L iOH micro-spring/wood composite electrode material prepared in example 1 of the present invention.
FIG. 5 is a graph of the effect of the rGO-L iOH micro-spring/wood composite electrode material prepared in example 1 of the present invention when subjected to external force.
FIG. 6 is a plot of cyclic voltammetry for different compression and recovery times for the rGO-L iOH micro-spring/wood composite electrode material prepared in example 1 of the present invention.
FIG. 7 is a graph of the relationship between the number of compression and recovery times and the retention and capacitance of the rGO-L iOH micro-spring/wood composite electrode material prepared in example 1 of the present invention.
Detailed Description
The present invention will now be described in further detail with reference to specific examples, which are intended to be illustrative, but not limiting, of the invention.
Graphene is the thinnest two-dimensional carbon structure material, and graphene and its derivatives are widely used in many fields such as composite materials, electronic devices, energy storage, and adsorptive separation. Graphene has light weight, high SSA (single-layer oxidation), high conductivity and excellent mechanical, optical, electronic and thermal properties, but the agglomeration phenomenon of graphene greatly limits the application of graphene, so that an oxygen-containing functional group is introduced to modify graphene to meet special requirements, but the method is influenced by chemical reaction temperature, pH, oxidation degree and the like and still has a certain agglomeration phenomenon; the other method is to grow metal oxide among graphene sheet layers to achieve the purpose of separating and reducing the graphene oxide sheet layers, so that the practical application rate of the graphene is improved.
The invention relates to a preparation method of a 3D rGO-L iOH micro spring and wood composite elastic electrode material, which is characterized in that L iOH grows between graphene oxide sheet layers to obtain reduced graphene oxide supported by lithium hydroxide, so that the aim of separating graphene can be achieved, and the reduced graphene oxide can be endowed with a certain elastic action.
Specifically, graphene oxide is prepared by a Hummers method, and aims to further utilize graphene oxide, lithium carbonate is used as a lithium source, and the graphene oxide and the lithium carbonate are uniformly dispersed by ultrasound; performing high-temperature treatment by using a CVD (chemical vapor deposition) method, wherein lithium carbonate is converted into lithium hydroxide at 1000-1200 ℃ in an argon atmosphere and grows between reduced graphene oxide sheet layers to form a micro spring structure of the reduced graphene oxide supported by the lithium hydroxide, the micro structure means that the size of the structure is micron-sized, and lithium carbonate and the graphene oxide are blown into wood pore channels by a vacuumizing and nitrogen blowing method; the structure and the arched structure of wood jointly form a 3D composite structure material with high specific capacitance and high elasticity.
The invention discloses a preparation method of a 3D rGO-L iOH micro spring and wood compounded elastic electrode material, which comprises the following steps:
fully mixing graphene oxide with lithium carbonate by using an ultrasonic cell crusher, and crushing large graphene oxide blocks to enable the graphene oxide blocks to enter wood pore channels; the operating frequency is 20 ~ 24KHz, and the supersound power is 200 ~ 600W, and the temperature: 25-40 ℃;
step 2, L iCO3Placing the aerogel with GO into a tubular furnace for temperature programming, heating to 130-300 ℃ in air at a heating rate of 2-15 ℃/min at room temperature, and keeping the temperature for 2-4 h to remove water;
heating to 1000-1200 ℃ in nitrogen or inert gas at a heating rate of 5-15 ℃/min, preserving heat for 2-5 h, taking out the material after the temperature is reduced to room temperature, and placing the material in a dryer for keeping to obtain the L iOH supported rGO micro spring;
step 3, cutting a wood chip with the length of 2cm, the width of 3cm and the thickness of 5mm, weighing 1.8g of sodium chlorite and 3ml of glacial acetic acid, putting the sodium chlorite and the glacial acetic acid into a 500ml beaker, dissolving the sodium chlorite and the glacial acetic acid into 200ml of deionized water, putting the prepared wood into the beaker, and taking out the wood after 3 hours at the temperature of 70 ℃ and the rotating speed of 50 rpm;
freezing in liquid nitrogen for 3 min, and freeze drying at-3 deg.C for 5 hr to obtain dried delignified wood;
heating the dried delignified wood to 650-800 ℃ in nitrogen or inert gas at the heating rate of 3-15 ℃/min at room temperature, and preserving the heat for 3-6 h to obtain carbonized delignified wood;
and 4, ultrasonically dispersing 0.02-0.05 g of L iOH supported rGO micro-spring in 80-200 ml of ethanol solution with the mass concentration of 90% -100%, blowing the micro-spring into the pore channel of the carbonized delignified wood by using a double-row pipe air pumping and blowing method, and obtaining the L iOH supported rGO micro-spring and wood composite elastic electrode material after ethanol is volatilized.
The 3D rGO-L iOH micro-spring/wood composite electrode material can be further assembled into an elastic capacitor or a flexible wearable capacitor, and the specific assembly process is that any porous membrane is taken as a diaphragm, the material is placed on one surface of the diaphragm, the same material or other electrode materials are placed on the other surface of the diaphragm, the materials on the two sides represent positive and negative electrodes, the whole assembly is formed into a capacitor, and the test results are respectively described later.
The capacitor can drive any electronic equipment within the charging range of the assembled capacitor, is a portable electronic equipment, such as a watch, a display screen or an L ED lamp, can be used as a mobile phone battery or a mobile charging power supply, and also can be used as a compressible power supply which is used for power supplies of different models, namely, the power supplies of different models before and after compression.
Example 1
The invention relates to a preparation method of a 3D rGO-L iOH micro spring and wood compounded elastic electrode material, which comprises the following steps,
the working frequency of the ultrasonic cell crusher is 20KHz, the ultrasonic power is 300W, and the temperature is 30 ℃;
step 2, L iCO3Placing the aerogel with GO into a tubular furnace, raising the temperature by a program, keeping the temperature at the room temperature of 5 ℃/min to 150 ℃ for 2h, keeping the temperature at the room temperature of 10 ℃/min to 1000 ℃ for 2h, taking out the material after the temperature is reduced to the room temperature, and placing the material in a dryer to obtain an L iOH supported rGO micro-spring;
step 3, cutting a wood chip with the length of 2cm, the width of 3cm and the thickness of 5mm, weighing 1.8g of sodium chlorite and 3ml of glacial acetic acid, putting the weighed sodium chlorite and the glacial acetic acid into a 500ml beaker, dissolving the weighed sodium chlorite and the glacial acetic acid into 200ml of deionized water, and putting the prepared wood into the beaker; obtaining delignified wood after 3 hours at 70 ℃ under the condition that the rotating speed is 50rpm, freezing the delignified wood in liquid nitrogen for 3 minutes, and freeze-drying the delignified wood for 5 hours at-3 ℃ to obtain dried delignified wood;
heating the dried delignified wood to 650 ℃ in nitrogen gas at the heating rate of 5 ℃/min at room temperature, and preserving the heat for 3h to obtain carbonized delignified wood;
and 4, ultrasonically dispersing 0.02g of L iOH-supported rGO micro-spring in 100ml of 90% ethanol solution, blowing the micro-spring into a pore channel of wood by using a double-row pipe air pumping and blowing method, and obtaining the L iOH-supported rGO micro-spring and wood composite elastic electrode material after ethanol is volatilized.
Example 2
The invention relates to a preparation method of a 3D rGO-L iOH micro spring and wood compounded elastic electrode material, which comprises the following steps,
the working frequency of the ultrasonic cell crusher is 22KHz, the ultrasonic power is 250W, and the temperature is 32 ℃;
step 2, L iCO3Placing the aerogel with GO into a tubular furnace, raising the temperature by a program, keeping the temperature at room temperature of 7 ℃/min to 180 ℃ for 4h, keeping the temperature at 15 ℃/min to 1100 ℃ for 2.5h, taking out the material after the temperature is reduced to room temperature, and placing the material in a dryer to obtain an L iOH supported rGO micro spring;
step 3, cutting a wood chip with the length of 5cm, the width of 4cm and the thickness of 8mm, weighing 2g of sodium chlorite and 4ml of glacial acetic acid, putting the sodium chlorite and the glacial acetic acid into a 500ml beaker, dissolving the sodium chlorite and the glacial acetic acid in 300ml of deionized water, and putting the prepared wood into the beaker; obtaining delignified wood after 4 hours at 75 ℃ under the condition that the rotating speed is 60rpm, freezing the delignified wood in liquid nitrogen for 2 minutes, and then freezing and drying the delignified wood for 4 hours at-6 ℃ to obtain dried delignified wood;
heating the dried delignified wood to 700 ℃ in argon gas at the heating rate of 8 ℃/min at room temperature, and preserving the heat for 3h to obtain carbonized delignified wood;
and 4, ultrasonically dispersing 0.03g of L iOH supported rGO micro spring in 130ml of 95% ethanol solution, blowing the micro spring into a pore channel of wood by using a double-row pipe air pumping and blowing method, and obtaining the L iOH supported rGO micro spring and wood composite elastic electrode material after ethanol is volatilized.
Example 3
The invention relates to a preparation method of a 3D rGO-L iOH micro spring and wood compounded elastic electrode material, which comprises the following steps,
the working frequency of the ultrasonic cell crusher is 23KHz, the ultrasonic power is 400W, and the temperature is 37 ℃;
step 2, L iCO3Placing the aerogel and GO into a tubular furnace, raising the temperature by a program, keeping the temperature at the room temperature of 10 ℃/min to 250 ℃ for 2.5h, keeping the temperature at the room temperature of 10 ℃/min to 1150 ℃ for 4h, taking out the material after the temperature is reduced to the room temperature, and placing the material in a dryer to obtain an L iOH supported rGO micro spring;
step 3, cutting a wood chip with the length of 7cm, the width of 3cm and the thickness of 6mm, weighing 4g of sodium chlorite and 9ml of glacial acetic acid, putting the weighed sodium chlorite and the glacial acetic acid into a 1000ml beaker, dissolving the weighed sodium chlorite and the glacial acetic acid into 500ml of deionized water, and putting the prepared wood into the beaker; obtaining delignified wood after 2 hours at 75 ℃ and the rotating speed of 80rpm, freezing the delignified wood in liquid nitrogen for 5 minutes, and freeze-drying the delignified wood for 3.5 hours at-12 ℃ to obtain dried delignified wood;
heating the dried delignified wood to 750 ℃ in nitrogen gas at the heating rate of 10 ℃/min at room temperature, and preserving heat for 3h to obtain carbonized delignified wood;
and 4, ultrasonically dispersing 0.04g of L iOH-supported rGO micro spring in 150ml of 90% ethanol solution, blowing the micro spring into a pore channel of wood by using a double-row pipe air pumping and blowing method, and obtaining the L iOH-supported rGO micro spring and wood composite elastic electrode material after ethanol is volatilized.
Example 4
The invention relates to a preparation method of a 3D rGO-L iOH micro spring and wood compounded elastic electrode material, which comprises the following steps,
the working frequency of the ultrasonic cell crusher is 24KHz, the ultrasonic power is 600W, and the temperature is 40 ℃;
step 2, L iCO3Placing the aerogel with GO into a tubular furnace, raising the temperature by a program, keeping the temperature at room temperature of 15 ℃/min to 300 ℃ for 3h, keeping the temperature at 15 ℃/min to 1200 ℃ for 5h, taking out the material after the temperature is reduced to the room temperature, and placing the material in a dryer to obtain an L iOH supported rGO micro spring;
step 3, cutting a wood chip with the length of 10cm, the width of 3cm and the thickness of 9mm, weighing 8g of sodium chlorite and 15ml of glacial acetic acid, putting the weighed sodium chlorite and glacial acetic acid into a 1000ml beaker, dissolving the weighed sodium chlorite and glacial acetic acid in 700ml of deionized water, and putting the prepared wood into the beaker; obtaining delignified wood after 3 hours at 80 ℃ under the condition that the rotating speed is 95rpm, freezing the delignified wood in liquid nitrogen for 12 minutes, and then freezing and drying the delignified wood for 4 hours at-20 ℃ to obtain dried delignified wood;
heating the dried delignified wood to 800 ℃ in nitrogen or inert gas at the heating rate of 15 ℃/min at room temperature, and preserving heat for 4h to obtain carbonized delignified wood;
and 4, ultrasonically dispersing 0.05g of L iOH supported rGO micro spring in 140ml of ethanol, blowing the micro spring into a pore channel of the wood by using a double-row pipe air pumping and blowing method, and obtaining the L iOH supported rGO micro spring and wood composite elastic electrode material after the ethanol is volatilized.
Example 5
The invention relates to a preparation method of a 3D rGO-L iOH micro spring and wood compounded elastic electrode material, which comprises the following steps,
the working frequency of the ultrasonic cell crusher is 21KHz, the ultrasonic power is 500W, and the temperature is 25 ℃;
step 2, L iCO3Placing the aerogel with GO into a tubular furnace, raising the temperature by program, keeping the temperature at room temperature from 2 ℃/min to 130 ℃ for 4h, then keeping the temperature at 5 ℃/min to 1050 ℃ for 3h, taking out the material after the temperature is reduced to room temperature, and placing the material in a dryer to obtain L iOHA supported rGO micro spring;
step 3, cutting a wood chip with the length of 10cm, the width of 3cm and the thickness of 9mm, weighing 8g of sodium chlorite and 15ml of glacial acetic acid, putting the weighed sodium chlorite and glacial acetic acid into a 1000ml beaker, dissolving the weighed sodium chlorite and glacial acetic acid in 700ml of deionized water, and putting the prepared wood into the beaker; obtaining delignified wood after 3 hours at 80 ℃ under the condition that the rotating speed is 95rpm, freezing the delignified wood in liquid nitrogen for 12 minutes, and then freezing and drying the delignified wood for 4 hours at-20 ℃ to obtain dried delignified wood;
heating the dried delignified wood to 700 ℃ in nitrogen or inert gas at the heating rate of 3 ℃/min at room temperature, and preserving heat for 6h to obtain carbonized delignified wood;
and 4, ultrasonically dispersing 0.05g of L iOH-supported rGO micro spring in 120ml of ethanol, blowing the micro spring into a pore channel of the wood by using a double-row pipe air pumping and blowing method, and obtaining the L iOH-supported rGO micro spring and wood composite elastic electrode material after the ethanol is volatilized.
Fig. 1 is a cross-sectional direction of a wood pipeline structure in which graphene oxide and L iOH compounds are grown, and it can be seen that a graphene oxide lamellar structure enters a pore channel of wood, which increases a specific surface area of rGO-L iOH/wood, and introduces a pseudocapacitance characteristic of a lithium ion battery, and it is worth mentioning that L iOH not only brings the pseudocapacitance characteristic, but also has an effect of stratifying graphene oxide, that is, L iOH acts between graphene oxide lamellar layers, which increases an energy storage density and a power density of the material, and a second major functional characteristic brought by this is that the graphene oxide lamellar structure provides a considerable damping effect for the composite material, and when the composite material is subjected to an external force, the pipeline structure of the wood resists most of the acting force, and at the same time, the graphene oxide lamellar structure inside the pipeline further decomposes the acting force, and the two synergistic effects bring a significant elastic function to the material.
Fig. 2 can see that the graphene oxide surface is attached with L iOH compound and grows at the defect of carbonized wood.
FIG. 3 shows the high temperature reduction of pure wood and rGO-L iOH micro-spring/wood composite electrode prepared in example 1 of the present invention when KOH electrolyte of 1.5M/L is testedThe specific capacitance of the material under 1000 times of cyclic voltammetry is compared, and the result shows that the scanning rate is 200mV s-1In time, the 3D rGO-L iOH micro-spring/wood composite electrode material has high specific capacitance of 351.7Fg-1And still maintain 346.7F g after 1000 cycles-1133.2F g much higher than pure carbonized wood-1126.6F g remaining after 1000 cycles-1The results show that the composite material is an electrode material for a high-performance supercapacitor, which is benefited from the fact that L i supported lamellar reduced graphene oxide and a wood substrate have larger electrical conductivity, and provide a fast channel and a larger specific surface area for electron transmission and a proper pore structure.
FIG. 4 is a graph showing the capacitance retention curves of high temperature reduced pure wood and the rGO-L iOH micro-spring/wood composite electrode material prepared in example 1 of the present invention at different scan rates when testing 1.5M/L KOH electrolyte, where the 3D rGO-L iOH micro-spring/wood composite electrode material is higher than pure carbonized wood at the same scan rate, and the capacitance retention of the 3D rGO-L iOH micro-spring/wood composite electrode material is slowly reduced with the increase of the scan rate, and at 500mv s-1The capacitance retention of 3D rGO-L iOH micro-spring/wood composite electrode material still reached 98% at scan rates higher than 92% of pure carbonized wood, therefore, the superior rate capability of 3D rGO-L iOH micro-spring/wood composite electrode material can be attributed to the short diffusion path reduction of ions, high surface activity, increased conductivity.
Fig. 5 is an effect diagram of the 3D rGO-L iOH micro-spring/wood composite electrode material before compression, during compression and after removal of external force when subjected to external force, firstly, the wood arched pipeline firstly plays an elastic role of F2, and when reaching a certain degree, L i in the pipeline supports graphene to play an elastic role of F3 again, thereby playing an overall obvious elastic effect.
Figure 6 shows that as the number of compressions and recoveries increases,at 100mv s-1The cyclic voltammetry curve of the composite material under the scanning rate is slowly converted into an arc from a regular rectangular shape because the internal pipeline structure of the composite material is continuously damaged due to multiple compression and recovery of the material, and the growth damage of L iOH is inevitably generated after multiple charge/discharge, so that more obstacles are generated, and the transmission path of electrons becomes more and more difficult, but the curve is still in a symmetrical arc shape, which is benefited by the fact that the composite material has nearly one hundred percent of carbon content, namely excellent structural design.
FIG. 7 is a graph of the relationship between the number of compression and recovery times of rGO-L iOH micro-spring/wood composite electrode material and the retention rate and capacitance of the capacitor when testing 1.5M/L KOH electrolyte, and the results show that under 5000 compression and recovery times, the rGO-L iOH micro-spring/wood composite electrode material still has 275F g-1The specific capacitance and the capacitance retention rate of 77 percent indicate that the material has quite good electrochemical characteristics and elastic characteristics.
Claims (10)
- A preparation method of an rGO-L iOH micro-spring/wood composite electrode material is characterized by comprising the following steps,step 1, ultrasonically crushing a mixed system of lithium carbonate, graphene oxide and deionized water, and freeze-drying, wherein the ratio of the lithium carbonate to the graphene oxide is (0.1-0.3) mol, (0.1-0.5) g, so as to obtain L iCO3And an aerogel of GO;step 2, L iCO3Removing water in the aerogel with GO, and then preserving heat for 2-5 hours at 1000-1200 ℃ in nitrogen or inert gas to obtain an rGO-L iOH micro spring;and 3, inflating the rGO-L iOH micro spring into a pore channel of the carbonized delignified wood to obtain the rGO-L iOH micro spring/wood composite electrode material.
- 2. The method for preparing the rGO-L iOH micro-spring/wood composite electrode material according to claim 1, wherein in the step 1, the ratio of lithium carbonate to deionized water is (0.1-0.3) mol (150-400) ml.
- 3. The preparation method of the rGO-L iOH micro-spring/wood composite electrode material as claimed in claim 1, wherein the mixed system in the step 1 is subjected to ultrasonic pulverization by using an ultrasonic cell pulverizer, and the required time is 10-30 min;the working frequency of the ultrasonic cell crusher is 20-24 KHz, the ultrasonic power is 200-600W, and the temperature is 25-40 ℃.
- 4. The preparation method of the rGO-L iOH micro-spring/wood composite electrode material as claimed in claim 1, wherein the mixed system in the step 1 is freeze-dried at-50 to-5 ℃ for 2 to 4 hours.
- 5. The method of preparing the rGO-L iOH micro-spring/wood composite electrode material of claim 1, wherein in step 2, L iCO is added3And keeping the temperature of the aerogel and GO at 130-300 ℃ for 2-4 h, and then keeping the temperature at 1000-1200 ℃.
- 6. The preparation method of the rGO-L iOH micro-spring/wood composite electrode material as claimed in claim 1, wherein in the step 2, wood chips are soaked in a mixed system composed of sodium chlorite, glacial acetic acid and deionized water, stirred, then sequentially frozen and freeze-dried, and finally, the temperature is kept for 3-6 h at 650-800 ℃ in nitrogen or inert gas at a heating rate of 3-15 ℃/min to obtain the carbonized delignified wood.
- 7. The method for preparing the rGO-L iOH micro-spring/wood composite electrode material as claimed in claim 1, wherein in step 3, the rGO-L iOH micro-spring is ultrasonically dispersed in ethanol or ethanol solution with volume fraction greater than or equal to 90%, the micro-spring is blown into the pore channel of the carbonized delignified wood by a double-row pipe air pumping and blowing method, and the rGO-L iOH micro-spring/wood composite electrode material is obtained after the ethanol is volatilized.
- 8. An rGO-L iOH micro-spring/wood composite electrode material obtained by the preparation method of the rGO-L iOH micro-spring/wood composite electrode material of any one of claims 1-7.
- 9. An elastic capacitor or wearable capacitor comprising the rGO-L iOH microspring/wood composite electrode material of claim 8.
- 10. An electronic device driven by the capacitor of claim 9.
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