CN105321727A - Preparation method for net-laminated porous carbon/graphene composite electrode material for supercapacitor - Google Patents
Preparation method for net-laminated porous carbon/graphene composite electrode material for supercapacitor Download PDFInfo
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Abstract
The invention relates to a preparation method for a net-laminated porous carbon/graphene composite electrode material for a supercapacitor. The preparation method comprises the following steps: (1) ultrasonically dispersing graphite oxide into different solvents to obtain a graphite oxide suspension liquid, adding a formaldehyde solution and phloroglucinol, mechanically stirring to dissolve the mixture, and adding a hydrochloric acid solution, then moving to a drying oven, performing a polymerization reaction, then performing suction filtration, washing and drying to obtain a phenolic resin/graphite oxide composite material precursor; and (2), mixing the precursor obtained in the step (1) with potassium hydroxide by a dry method, putting the mixture into a corundum porcelain boat, putting the corundum porcelain boat into a tubular furnace, performing constant temperature carbonization, and naturally cooling to the room temperature, taking the obtained product out, grinding the product and putting the grinded product to a beaker, then acid washing, distilled water washing and drying the product to obtain the target product. The preparation method is simple in preparation equipment and technology, and suitable for the rapid and industrial large-scale production; when the net-laminated porous carbon/graphene composite electrode material is used for the supercapacitor, the prepared supercapacitor is higher in specific capacitance and rate, and longer in cycle life.
Description
Technical field
The present invention relates to a kind of preparation method of ultracapacitor stratum reticulare shape porous charcoal/graphene combination electrode material, belong to electrode material for super capacitor preparation method technical field.
Background technology
Along with the quick increase of portable electronic equipment, electric automobile, hybrid power electric car use amount, the demand of the energy storage device of high power density, high-energy-density is increased day by day.Ultracapacitor causes research boom widely owing to having the feature such as the power density higher than battery and the energy density higher than traditional capacitor.Choice and design electrode material is most important for the performance of ultracapacitor.Good electrode material should have larger effective ratio area for electrolyte ion provides the interface of absorption; Also need to have ion transfer passage fast, to reduce the diffusional resistance of electrolyte ion simultaneously.But for electrode material, these two vital features are often conflicted to a certain extent mutually, can not meet simultaneously.Therefore design suitable nanostructure and electrode material for super capacitor is become more and more important.Carbon Materials is widely used in ultracapacitor owing to having the advantages such as high conductance, low cost, structure easy-regulating, stable chemical nature.Wherein Graphene is because himself splendid electronic conductivity, good machinery and thermal stability and high-specific surface area, is studied widely especially.But, strong π-π active force is there is between graphene sheet layer, serious stacking phenomenon can be there is in preparation process, thus the effective ratio of large losses surface and increase electrolyte ion transmission resistance, seriously constrain the application of Graphene in ultracapacitor field.Graphene composite material then can overcome the stacking difficult problem of Graphene effectively, because other composition in composite material can stop the reunion of Graphene effectively, thus improves the ratio capacitance of grapheme material.Wherein the compound of Graphene and porous charcoal not only can improve the effective ratio area of grapheme material, and can not reduce the chemical stability of material, is a kind of method that very feasible preparation has excellent capacitive property electrode material.
ZhibinLei has prepared a kind of mesoporous carbon microballoon/graphene combination electrode material, its preparation process is: utilize amidized mesoporous silicon oxide microballoons and graphite oxide compound to obtain preparing the template of target material, then be that carbon source carries out chemical vapour deposition (CVD) with ferrocene, recycling hf etching falls silicon oxide microsphere, obtains mesoporous carbon microballoon/graphene combination electrode material.Its preparation technology is loaded down with trivial details, high to equipment requirement, and the hydrofluoric acid needing to use hard template and there is severe corrosive, cause cost to raise, and cannot large-scale production.MengLi utilizes phenolic resins to do carbon source to have prepared the composite material of mesoporous carbon/Graphene, using triblock copolymer (EO106PO70EO106) as soft template, novolak resin/graphite oxide predecessor under the condition of high temperature hydro-thermal, then carbonization obtain target product after removing template, but the application of template improves its preparation cost, and lower specific area limits its capacitive property.Chinese patent CN102167308B discloses a kind of preparation method of mesoporous carbon/graphene composite material.Its preparation technology utilizes hydroxy compounds and aldehyde compound to form the presoma of composite material with graphite oxide under the help of surfactant, then carries out the composite material that pre-carbonization and carbonization treatment obtain mesoporous carbon and Graphene.Chinese patent CN103824701A discloses a kind of Activated Graphite alkene combination electrode material, utilizes the method for physical mixed to be mixed with active carbon by Graphene, carries out pre-activate and activation process obtains target product under the help of activator.Its Activated Graphite alkene composite material prepared can as the electrode of ultracapacitor, fuel cell etc., but the composite structure that this preparation technology obtains is wayward, causes very bigger serface not to be utilized effectively.Chinese patent CN104319116A discloses the preparation method of a kind of ultracapacitor Microporous Carbon/graphene combination electrode material.Coal tar pitch and graphite oxide is utilized to be carbon source, take potassium hydroxide as activator, Microporous Carbon/the graphene composite material of preparation has high specific surface area, average pore size is between 1.85-2.04nm, it has higher ratio capacitance as electrode material for super capacitor, but more micropore limits its multiplying power property.
As can be seen from above public technology, the technology of preparing of above-mentioned porous charcoal/Graphene electrodes material uses surfactant or template mostly, needs to remove in follow-up processing procedure, adds the cost of technique, reduce the efficiency of technique.In addition the pattern of material and structure wayward, cause the skewness of micropore, mesoporous, macropore, thus limit its capacitive property as electrode material or multiplying power property.Literature search result shows, utilize phenolic resins, graphite oxide for carbon source, do not adopt any template or surfactant, utilize the guide effect of graphene oxide, by the polymerization changing solvent control line type phenolic resins directly prepare have grade pore structure, high specific capacitance value, high rate capability stratum reticulare shape porous charcoal/graphene combination electrode material rarely have report.
Summary of the invention
The object of the invention is to overcome above-mentioned deficiency, provide a kind of preparation method of novel ultracapacitor stratum reticulare shape porous charcoal/graphene combination electrode material.
To achieve these goals, technical scheme of the present invention is as follows.
A preparation method for ultracapacitor stratum reticulare shape porous charcoal/graphene combination electrode material, is characterized in that: its step is as follows:
(1) preparation of predecessor: graphite oxide ultrasonic disperse is obtained graphite oxide suspension in different solvents, then 37% formalin and phloroglucin is added, mechanical agitation adds 37% hydrochloric acid solution as catalyst after dissolving, then be transferred in baking oven, after polymerization reaction 3-6 hour, obtain phenolic resins/graphene oxide composite material predecessor by suction filtration, washing, drying.
(2) preparation of porous charcoal/graphene combination electrode material: the predecessor obtain step (1) and potassium hydroxide pass through dry mixed, be placed in corundum porcelain boat, described porcelain boat is put in tube furnace, argon gas 10min is passed into by after the air emptying in described tube furnace with the flow of 80ml/min, design temperature is heated to the heating rate of 5 DEG C/min, after 600-800 DEG C of constant temperature carbonization 1-3h, Temperature fall is to room temperature, finally the product obtained is taken out, beaker is put into after grinding, through pickling, target product ultracapacitor stratum reticulare shape porous charcoal/graphene combination electrode material is obtained after distilled water washing and drying.
Further, in step (1), solvent used is water mixed alkoxide solution.
Further, the concentration of the graphite oxide suspension in step (1) is 1-5mg/ml.
Further, the water alcohol volume ratio in water mixed alkoxide solution is 40: 3.
Further, in water mixed alkoxide solution, alcohol used is the one in ethanol, propyl alcohol, ethylene glycol, normal propyl alcohol or n-butanol.
Further, the mass ratio of the graphite oxide added in step (1), formaldehyde, phloroglucin, hydrochloric acid is 4-20: 78.2: 150: 119.
Further, the polymeric reaction temperature of the phenolic resins/graphene oxide composite material in step (1) is 25-80 DEG C.
Further, the potassium hydroxide consumption in step (2) is 0-5 times of phenolic resins/graphene oxide predecessor.
This beneficial effect of the invention is: Preparation equipment of the present invention and technique simply, are applicable to quick, industrialization large-scale production, not by any surfactant or template in the process of preparation.Utilize the guide effect of graphene oxide, the linear polymerization process of phenolic resins in surface of graphene oxide is controlled by changing solvent, make prepared porous charcoal/graphene composite material have uniform net slice Rotating fields, there is flourishing mesoporous and large pore size distribution.Linear phenol-aldehyde resin is as primary carbon source simultaneously, has the micropore that a large amount of duct is shorter, can provide higher specific area, do not limit again the fast transport of ion after activation.Have benefited from this net layer structure with grade pore size distribution, it is applied to ultracapacitor and has higher ratio capacitance value and the speed characteristic of superelevation, and has longer cycle life.
Accompanying drawing explanation
The electron scanning micrograph of Fig. 1, stratum reticulare shape porous charcoal/graphene combination electrode material prepared by the embodiment of the present invention 2.
The electron scanning micrograph of Fig. 2, stratum reticulare shape porous charcoal/graphene combination electrode material prepared by the embodiment of the present invention 3.
The electron scanning micrograph of Fig. 3, stratum reticulare shape porous charcoal/graphene combination electrode material prepared by the embodiment of the present invention 4.
The constant current charge-discharge curve of Fig. 4, stratum reticulare shape porous charcoal/graphene combination electrode material prepared by the embodiment of the present invention 4.
The multiplying power property curve of Fig. 5, stratum reticulare shape porous charcoal/graphene combination electrode material prepared by the embodiment of the present invention 4.
Embodiment
Below in conjunction with embodiment, the specific embodiment of the present invention is described, better to understand the present invention.
Embodiment 1:
Taking 40mg graphite oxide powder ultrasonic is scattered in 40ml water/ethanol (volume ratio is 40: 3) mixed solution, obtain graphite oxide suspension, then in suspension, 0.782g phloroglucin, 1.5g37% formalin is added, after stirring half an hour, add 1.19g37% hydrochloric acid solution, be transferred in 80 DEG C of baking ovens after continuing to stir half an hour and react 4h.Phenolic resins/graphite oxide predecessor is obtained by suction filtration, washing, drying.The phenolic resins obtained/graphite oxide predecessor is put into tube furnace, under the protection of 80ml/min argon gas atmosphere, is raised to 800 DEG C of carbonization 2h with 5 DEG C/min, then naturally cools to room temperature, after grinding, pickling, distilled water washing and drying, obtain product.Below can carry out routinely, using obtained product as electrode of super capacitor active component, polytetrafluoroethylene (PTFE) is binding agent, is scattered in 1ml absolute ethyl alcohol, then in 100 DEG C of dry 12h.The proportioning (mass ratio) of electrode material is: active material (composite material of above-mentioned preparation): binding agent=95: 5.Be coated in by dried mixture in 1 × 1cm2 nickel foam, at 100Kg/cm2 pressure in flakes as work electrode, wherein the quality of active material is 2mg.Using platinum plate electrode as to electrode, saturated calomel electrode as reference electrode, at the capacitive property of 6MKOH solution testing electrode material.In the voltage range of-1-0V, carry out constant current charge-discharge test with different current densities.Under the current density of 1A/g, its ratio capacitance value is 132.3F/g, and when current density brings up to 50A/g, its ratio capacitance value is 111.4F/g, and ratio capacitance conservation rate is 84.2%.
Embodiment 2
Taking 40mg graphite oxide powder ultrasonic is scattered in 40ml deionized water, obtain graphite oxide suspension, then in suspension, 0.782g phloroglucin, 1.5g37% formalin is added, after stirring half an hour, add 1.19g37% hydrochloric acid solution, be transferred in 80 DEG C of baking ovens after continuing to stir half an hour and react 4h.Phenolic resins/graphite oxide predecessor is obtained by suction filtration, washing, drying.The phenolic resins obtained/graphite oxide predecessor is put into tube furnace, under the protection of 80ml/min argon gas atmosphere, is raised to 800 DEG C of charing 2h with 5 DEG C/min, then naturally cools to room temperature, after grinding, pickling, distilled water washing and drying, obtain product.Make electrode by the conventional method described in embodiment 1 below and test its capacitive property.Under the current density of 1A/g, its ratio capacitance value is 122.2F/g, and when current density brings up to 50A/g, its ratio capacitance value is 100.6F/g, and ratio capacitance conservation rate is 82.3%.
Embodiment 3
Taking 40mg graphite oxide powder ultrasonic is scattered in 40ml deionized water/n-butanol (volume ratio is 40: 3), obtain graphite oxide suspension, then in suspension, 0.782g phloroglucin, 1.5g37% formalin is added, after stirring half an hour, add 1.19g37% hydrochloric acid solution, be transferred in 80 DEG C of baking ovens after continuing to stir half an hour and react 4h.Phenolic resins/graphite oxide predecessor is obtained by suction filtration, washing, drying.The phenolic resins obtained/graphite oxide predecessor is put into tube furnace, under the protection of 80ml/min argon gas atmosphere, is raised to 800 DEG C of carbonization 2h with 5 DEG C/min, then naturally cools to room temperature, after grinding, pickling, distilled water washing and drying, obtain product.Make electrode by the conventional method described in embodiment 1 below and test its capacitive property.Under the current density of 1A/g, its ratio capacitance value is 114.3F/g, and when current density brings up to 50A/g, its ratio capacitance value is 89.5F/g, and ratio capacitance conservation rate is 78.3%.
Embodiment 4
Taking 40mg graphite oxide powder ultrasonic is scattered in 40ml deionized water/ethanol (volume ratio is 40: 3), obtain graphite oxide suspension, then in suspension, 0.782g phloroglucin, 1.5g37% formalin is added, after stirring half an hour, add 1.19g37% hydrochloric acid solution, be transferred in 80 DEG C of baking ovens after continuing to stir half an hour and react 4h.Phenolic resins/graphite oxide predecessor is obtained by suction filtration, washing, drying.By the phenolic resins obtained/graphite oxide predecessor and potassium hydroxide with 1: 5 mass ratio pass through dry mixed; mixture is put into tube furnace; under the protection of 80ml/min argon gas atmosphere; 800 DEG C of carbonization 2h are raised to 5 DEG C/min; then naturally cool to room temperature, after grinding, pickling, distilled water washing and drying, obtain product.Make electrode by the conventional method described in embodiment 1 below and test its capacitive property.Under the current density of 1A/g, its ratio capacitance value is 269.8F/g, and when current density brings up to 50A/g, its ratio capacitance value is 236.5F/g, and ratio capacitance conservation rate is 87.8%.
Embodiment 5
Taking 40mg graphite oxide powder ultrasonic is scattered in 40ml deionized water/ethanol (volume ratio is 40: 3), obtain graphite oxide suspension, then in suspension, 0.782g phloroglucin, 1.5g37% formalin is added, after stirring half an hour, add 1.19g37% hydrochloric acid solution, be transferred in 80 DEG C of baking ovens after continuing to stir half an hour and react 4h.Phenolic resins/graphite oxide predecessor is obtained by suction filtration, washing, drying.By the phenolic resins obtained/graphite oxide predecessor and potassium hydroxide with 1: 3 mass ratio pass through dry mixed; mixture is put into tube furnace; under the protection of 80ml/min argon gas atmosphere; 800 DEG C of carbonization 2h are raised to 5 DEG C/min; then naturally cool to room temperature, after grinding, pickling, distilled water washing and drying, obtain product.Make electrode by the conventional method described in embodiment 1 below and test its capacitive property.Under the current density of 1A/g, its ratio capacitance value is 194.0F/g, and when current density brings up to 50A/g, its ratio capacitance value is 154.3F/g, and ratio capacitance conservation rate is 79.5%.
The electron scanning micrograph of the porous charcoal/graphene combination electrode material synthesized for embodiment 2 and embodiment 3 is showed in Fig. 1 and Fig. 2 respectively, as can be seen from the figure, although it is also lamellar structure, but compared with embodiment 4, its lamella inside is significantly large pore size distribution not, illustrates that the suitable preparation of solvent to stratum reticulare shape porous charcoal/graphene combination electrode material of selection is most important.
Constant current charge-discharge curve during electron scanning micrograph, the 10A/g of porous charcoal/graphene combination electrode material synthesized for example 4, high rate performance curve are shown in Fig. 3, Fig. 4, Fig. 5.As can be seen from electron scanning micrograph, porous charcoal/the graphene composite material of preparation has net layer structure, its lamellar spacing is less than 500nm, and pore size distribution is flourishing, there is abundant mesoporous and macropore, be conducive to the specific surface that electrolyte ion arrives electrode material fast, make porous charcoal/graphene composite material have excellent high rate performance.Its constant current charge-discharge curve and the display of high rate performance curve, material has excellent electric double layer capacitance performance, and under the superhigh-current-density of 50A/g, still has the ratio capacitance value of 236.5F/g, conservation rate, up to 87.8%, is better than the numerical value of open report in the past.
The above is the preferred embodiment of the present invention; it should be pointed out that for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications are also considered as protection scope of the present invention.
Claims (8)
1. a ultracapacitor preparation method for stratum reticulare shape porous charcoal/graphene combination electrode material, is characterized in that: its step is as follows:
(1) preparation of predecessor: graphite oxide ultrasonic disperse is obtained graphite oxide suspension in different solvents, then 37% formalin and phloroglucin is added, mechanical agitation adds 37% hydrochloric acid solution as catalyst after dissolving, then be transferred in baking oven, after polymerization reaction 3-6 hour, obtain phenolic resins/graphene oxide composite material predecessor by suction filtration, washing, drying.
(2) preparation of porous charcoal/graphene combination electrode material: the predecessor obtain step (1) and potassium hydroxide pass through dry mixed, be placed in corundum porcelain boat, described porcelain boat is put in tube furnace, argon gas 10min is passed into by after the air emptying in described tube furnace with the flow of 80ml/min, design temperature is heated to the heating rate of 5 DEG C/min, after 600-800 DEG C of constant temperature carbonization 1-3h, Temperature fall is to room temperature, finally the product obtained is taken out, beaker is put into after grinding, through pickling, target product ultracapacitor stratum reticulare shape porous charcoal/graphene combination electrode material is obtained after distilled water washing and drying.
2. according to the preparation method of ultracapacitor described in claim 1 with stratum reticulare shape porous charcoal/graphene combination electrode material, it is characterized in that: solvent used in described step (1) is water mixed alkoxide solution.
3. according to the preparation method of ultracapacitor described in claim 1 with stratum reticulare shape porous charcoal/graphene combination electrode material, it is characterized in that: the concentration of the graphite oxide suspension in described step (1) is 1-5mg/ml.
4. according to the preparation method of ultracapacitor described in claim 2 with stratum reticulare shape porous charcoal/graphene combination electrode material, it is characterized in that: the water alcohol volume ratio in described water mixed alkoxide solution is 40: 3.
5. according to the preparation method of ultracapacitor described in claim 2 with stratum reticulare shape porous charcoal/graphene combination electrode material, it is characterized in that: in described water mixed alkoxide solution, alcohol used is the one in ethanol, propyl alcohol, ethylene glycol, normal propyl alcohol or n-butanol.
6. according to the preparation method of ultracapacitor described in claim 1 with stratum reticulare shape porous charcoal/graphene combination electrode material, it is characterized in that: the mass ratio of the graphite oxide added in described step (1), formaldehyde, phloroglucin, hydrochloric acid is 4-20: 78.2: 150: 119.
7. according to the preparation method of ultracapacitor described in claim 1 with stratum reticulare shape porous charcoal/graphene combination electrode material, it is characterized in that: the polymeric reaction temperature of the phenolic resins/graphene oxide composite material in described step (1) is 25-80 DEG C.
8. according to the preparation method of ultracapacitor described in claim 1 with stratum reticulare shape porous charcoal/graphene combination electrode material, it is characterized in that: the potassium hydroxide consumption in described step (2) is 0-5 times of phenolic resins/graphene oxide predecessor.
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| CN107170590A (en) * | 2017-05-18 | 2017-09-15 | 齐鲁工业大学 | A kind of electrode material for super capacitor and preparation method thereof |
| CN107902651A (en) * | 2017-10-18 | 2018-04-13 | 中国科学院山西煤炭化学研究所 | A kind of graphene-based capacitance carbon large-scale preparation method |
| CN115849377A (en) * | 2023-01-10 | 2023-03-28 | 哈密市美好活性炭有限公司 | Active carbon composite material and preparation method and application thereof |
| CN116197184A (en) * | 2023-03-29 | 2023-06-02 | 通威太阳能(眉山)有限公司 | Cleaning method of Poly boat |
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