CN102568856A - Method for assembling supercapacitor based on hollow carbon nano cage - Google Patents
Method for assembling supercapacitor based on hollow carbon nano cage Download PDFInfo
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- CN102568856A CN102568856A CN2012100657480A CN201210065748A CN102568856A CN 102568856 A CN102568856 A CN 102568856A CN 2012100657480 A CN2012100657480 A CN 2012100657480A CN 201210065748 A CN201210065748 A CN 201210065748A CN 102568856 A CN102568856 A CN 102568856A
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- 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 a method for assembling a supercapacitor based on a hollow carbon nano cage. The method comprises the following steps of: 1) mixing water, an organic solvent and Nafion according to a volume ratio of 4:0.8:0.2, obtaining a Nafion mixed solution at the concentration of 5 percent, performing ultrasonic dispersion on the hollow carbon nano cage synthesized at the temperature of between 670 and 1,100 DEG C, and forming hollow carbon nano cage slurry; 2) uniformly smearing the hollow carbon nano cage slurry on a current collector, naturally drying the hollow carbon nano cage slurry to obtain hollow carbon nano cage electrodes, and immersing the electrodes in an electrolyte for later use; and 3) separating the two identical electrodes obtained in the step 2) by an ionic permeation membrane immersed by the electrolyte, compacting and sealing the two electrodes, and assembling the supercapacitor. The supercapacitor assembled by the method has relatively high stability; as for the electrodes at the concentration of 0.255 mg/cm<2>, the maximum specific capacitance at low charging and discharging rates is 260 F/g; and high performance can still be kept at relatively high charging and discharging rates.
Description
Technical field
The present invention relates to a kind of assemble method of the ultracapacitor based on hollow nano cages.
Background technology
Ultracapacitor has received extensive concern and big quantity research (Nat.Mater.2008 as a kind of novel energy-storing device; 7; 845-854), this is that is: its energy density and power density are all between between the two because ultracapacitor has been filled up the blank between battery and the traditional capacitor.The ultracapacitor high energy density, the power density of super large and it is gained great popularity is applied to: crane, elevator, electric automobile, numerous areas such as energy management system.(Nat.Mater.2008,7,845; Adv.Mater.2011, DOI:10.1002/adma.201100984; Chem.Rev.2004,104,4245; J.Power Sources 2006,157,11; Energy Environ.Sci.2010,3,1294; Angew.Chem.Int.Ed.2011,50,1683; Science 2008,321, and 651; The material that Science 2010,329,1637) can be applied to ultracapacitor has many, comprises metal oxide, conducting polymer and material with carbon element etc.What wherein material with carbon element was studied is maximum; This is to be close to infinite many microstructures because it has; And the specific surface that possibly obtain having superelevation thus, the pore passage structure of rule and the material of stable skeleton, and these characteristics are the favorable factor that improves the ultracapacitor performance.So far, there is the material with carbon element of many types to be studied, comprises active carbon (Electrochem.Comm.2008,10,1809 as electrode material for super capacitor; Electrochem.Comm.2008,10,868; Electrochem.Comm.2008,10,795), CNT (Nat.Mater.2006,5,987; Adv.Funct.Mater.2001,11,387; PNAS 2009,106,21491), and template carbon (Adv.Mater.2011, DOI:10.1002/adma.201100984) and Graphene (Adv.Mater.2011,23,2833; Science 2011,332, and 1537).This wherein active carbon when more high-power discharging and recharging, perform poor, the carbon pipe is not higher than electric capacity, and the height of template carbon and Graphene preparation and activating cost have limited their application.
Summary of the invention
The purpose of this invention is to provide a kind of assemble method of the ultracapacitor based on hollow nano cages, this ultracapacitor has high-performance and lower cost.
The assemble method of the ultracapacitor based on hollow nano cages according to the invention comprises the steps:
1) configuration hollow nano cages slurries:
Water, organic solvent and Nafion 4: 0.8: 0.2 are by volume mixed, obtain concentration and be 5% Nafion mixed solution; To form the hollow nano cages slurries 670-1100 ℃ of synthetic down ultrasonic being scattered in the aforementioned mixed solution of hollow nano cages again;
2) get the hollow nano cages slurries that dispose in the step 1) and evenly be applied on the collector, treat its air dry, promptly make the hollow nano cages electrode, be soaked in the following used electrolyte this electrode subsequent use.
3) assembling is based on the ultracapacitor of hollow nano cages electrode:
Will be according to step 2) two identical electrodes obtaining use the ion that soaks into through electrolyte to see through film to separate, compress and seal two electrodes, i.e. and assembling becomes ultracapacitor.
Above-mentioned steps 1) in, organic solvent is an ethanol, the mixture of any one or more than one arbitrary proportion in propyl alcohol or the acetone, and specifically the needs according to dispersiveness adopt single or mixed solvent.
Above-mentioned steps 1) in, because the too rare or too dense film forming that all is unfavorable for of hollow nano cages slurries, so its concentration is preferably 2～5mg/mL.
Above-mentioned steps 1) in, be unfavorable for disperseing because ultrasonic time is too short, oversize also is unnecessary, and therefore the time of ultrasonic dispersion preferably is not less than and was no more than 60 minutes in 30 minutes.
Above-mentioned steps 2) in, for guaranteeing collector stable in properties in condenser dielectric, collector is selected from copper sheet, stainless steel substrates, platinized platinum or aluminium flake.
Above-mentioned steps 2) in, the hollow nano cages slurries are applied on the collector through dry back formed coat thickly is preferred 2-200 μ m, and its reason is that coat is too thin, and the utilance of collector is low, and the interior electric capacity of unit are is low; Coat is too thick, and resistance can increase, and coat also comes off easily.
Above-mentioned steps 2) in; For preventing that the hollow nano cages slurries are applied on the collector that formed coat comes off from flow collection sheet after dry; Thereby ultracapacitor was lost efficacy, can before or after the coat drying, on coat, apply 1-20kg/cm
2Pressure is to form uniform coat and to keep firm.After the compacting electrochemical capacitor performance is reduced not quite, still can keep more than 95%.
Above-mentioned steps 2) and in the step 3), said electrolyte is selected sulfuric acid, alkali metal hydroxide (like potassium hydroxide, NaOH), sulfate (like sodium sulphate) or perchlorate (like lithium perchlorate) for use, and concentration is 0.1-5mol/mL.
The present invention has following advantage:
Adopting ultracapacitor operating potential scope that the present invention obtains is 0.9V for sulfuric acid solution during as electrolyte; Is 1.3V for alkali metal hydroxide (like potassium hydroxide or NaOH) during as electrolyte, is 1.8V for sulfate or perchlorate (like sodium sulphate or lithium perchlorate) during as electrolyte.
The ultracapacitor that employing the present invention obtains is for 0.255mg/cm
2The electrode of thickness is 260F/g at the maximum down ratio electric capacity of low charge-discharge velocity, under higher charge-discharge velocity, still can keep high-performance, and for example the 10A/g charge-discharge velocity is down～180F/g, under the 100A/g still greater than 110F/g.
The ultracapacitor that adopts the present invention to obtain has stability preferably, and when for example discharging and recharging with 10A/g, electric capacity keeps almost constant in 1000 a week decline about 10% in ensuing 9000 weeks.
Embodiment
Embodiment 1 is that the 0.1mg/mL hollow nano cages suspension-turbid liquid that dispersion liquid disposes is the electrode that collector is processed with the vitreous carbon with water-ethanol-5%Nafion solution.
Take by weighing the hollow nano cages of 670 ℃ of preparations of 10mg; Ultrasonic dispersion is 30 minutes in 100mL water-ethanol-5%Nafion mixed liquor (ratio is 4: 0.8: 0.2); Forming concentration is the outstanding turbid slurries of 0.1mg/mL hollow nano cages slurries, measures 15 μ L and should hang turbid slurries, drops on the vitreous carbon collector of diameter 5mm; To form the homogeneous film of thickness 2 μ m; Treat its air dry, promptly obtain electrode of super capacitor, be soaked in the 0.1mol/mL sulfuric acid electrolyte this electrode subsequent use based on hollow nano cages.Use the ion that soaks into through the 0.1mol/mL sulfuric acid electrolyte to see through film at two electrodes of processing according to said method and separate, compress and seal two electrodes, i.e. assembling becomes ultracapacitor.Have the operating voltage of 0.9V according to the ultracapacitor that obtains accordingly, have the ratio electric capacity of 210F/g during for 0.1A/g in discharge rate, 10A/g has～150F/g, and 100A/g has 100F/g.Its stability is discharged and recharged experiment confirm at a high speed by 10000 weeks.
Embodiment 2 is that 700 ℃ of synthetic hollow nano cages suspension-turbid liquids of 2mg/mL that dispersion liquid disposes are the electrode that collector is processed with the vitreous carbon with water-ethanol-5%Nafion solution.
Take by weighing 700 ℃ of synthetic hollow nano cages of 10mg; Ultrasonic dispersion is 40 minutes in 5mL water-ethanol-5%Nafion mixed liquor (ratio is 4: 0.8: 0.2); Forming concentration is the outstanding turbid slurries of 2mg/mL hollow nano cages slurries, measures 20 μ L and should hang turbid slurries, drops on the vitreous carbon collector of diameter 5mm; To form the homogeneous film of thickness 10 μ m; Treat its air dry, promptly obtain electrode of super capacitor, be soaked in the 1mol/mL sulfuric acid electrolyte this electrode subsequent use based on hollow nano cages.Use the ion that soaks into through the 1mol/mL sulfuric acid electrolyte to see through film at two electrodes of processing according to said method and separate, compress and seal two electrodes, i.e. assembling becomes ultracapacitor.Have the operating voltage of 0.9V according to the ultracapacitor that obtains accordingly, have the ratio electric capacity of 240F/g during for 0.1A/g in discharge rate, 10A/g has～170F/g, and 100A/g has 110F/g.Its stability is discharged and recharged experiment confirm at a high speed by 10000 weeks.
Embodiment 3 is that 700 ℃ of synthetic hollow nano cages suspension-turbid liquids of 2.5mg/mL that dispersion liquid disposes are the electrode that collector is processed with the platinized platinum with water-ethanol-5%Nafion solution.
Take by weighing 700 ℃ of synthetic hollow nano cages of 10mg; Ultrasonic dispersion is 50 minutes in 4mL water-ethanol-5%Nafion mixed liquor (ratio is 4: 0.8: 0.2); Forming concentration is the outstanding turbid slurries of 2.5mg/mL hollow nano cages slurries; Measure 25 μ L and should hang turbid slurries, drop on the platinized platinum collector of diameter 5mm, 20kg/cm exerted pressure on film before pole drying
2The pressure compacting to form the homogeneous film of thickness 15 μ m, is treated its air dry, promptly obtains the electrode of super capacitor based on hollow nano cages, is soaked in the 5mol/mL sulfuric acid electrolyte this electrode subsequent use.Use the ion that soaks into through the 5mol/mL sulfuric acid electrolyte to see through film at two electrodes of processing according to said method and separate, compress and seal two electrodes, i.e. assembling becomes ultracapacitor.Have the operating voltage of 0.9V according to the ultracapacitor that obtains accordingly, have the ratio electric capacity of 240F/g during for 0.1A/g in discharge rate, 10A/g has～170F/g, and 100A/g has 105F/g.Its stability is discharged and recharged experiment confirm at a high speed by 10000 weeks.
Embodiment 4 is that 750 ℃ of synthetic hollow nano cages suspension-turbid liquids of 5mg/mL that dispersion liquid disposes are the electrode that collector is processed with the platinized platinum with water-ethanol-5%Nafion solution.
Take by weighing 750 ℃ of synthetic hollow nano cages of 10mg; Ultrasonic dispersion is 40 minutes in 2mL water-ethanol-5%Nafion mixed liquor (ratio is 4: 0.8: 0.2); Forming concentration is the outstanding turbid slurries of 5mg/mL hollow nano cages slurries; Measure 40 μ L and should hang turbid slurries, drop on the platinized platinum collector of diameter 10mm, 10kg/cm exerts pressure on film after pole drying
2The pressure compacting to form the homogeneous film of thickness 30 μ m, is treated its air dry, promptly obtains the electrode of super capacitor based on hollow nano cages, is soaked in the 0.1mol/mL potassium hydroxide electrolyte this electrode subsequent use.Use the ion that soaks into through the 0.1mol/mL potassium hydroxide electrolyte to see through film at two electrodes of processing according to said method and separate, compress and seal two electrodes, i.e. assembling becomes ultracapacitor.Have the operating voltage of 0.9V according to the ultracapacitor that obtains accordingly, have the ratio electric capacity of 220F/g during for 0.1A/g in discharge rate, 10A/g has～170F/g, and 100A/g has 100F/g.Its stability is discharged and recharged experiment confirm at a high speed by 10000 weeks.
Embodiment 5 is that the 10mg/mL hollow nano cages suspension-turbid liquid that dispersion liquid disposes is the electrode that collector is processed with the vitreous carbon with water-propyl alcohol-5%Nafion solution.
Take by weighing the hollow nano cages of 700 ℃ of preparations of 10mg; Ultrasonic dispersion is 45 minutes in 1mL water-propyl alcohol-5%Nafion mixed liquor (ratio is 4: 0.8: 0.2); Forming concentration is the outstanding turbid slurries of 10mg/mL hollow nano cages slurries; Measure 60 μ L and should hang turbid slurries, drop on the vitreous carbon collector of diameter 5mm, 1kg/cm exerted pressure on film before pole drying
2The pressure compacting to form the homogeneous film of thickness 50 μ m, is treated its air dry, promptly obtains the electrode of super capacitor based on hollow nano cages, is soaked in the 0.1mol/mL NaOH electrolyte this electrode subsequent use.Use the ion that soaks into through 0.1mol/mL NaOH electrolyte to see through film at two electrodes of processing according to said method and separate, compress and seal two electrodes, i.e. assembling becomes ultracapacitor.Have the operating voltage of 0.9V according to the ultracapacitor that obtains accordingly, have the ratio electric capacity of 240F/g during for 0.1A/g in discharge rate, 10A/g has～200F/g, and 100A/g has 105F/g.Its stability is discharged and recharged experiment confirm at a high speed by 10000 weeks.
Embodiment 6 is that the 2mg/mL hollow nano cages suspension-turbid liquid that dispersion liquid disposes is the electrode that collector is processed with the vitreous carbon with water-acetone-5%Nafion solution.
Take by weighing 750 ℃ of preparations of 10mg hollow nano cages; Ultrasonic dispersion is 45 minutes in 5mL water-acetone-5%Nafion mixed liquor (ratio is 4: 0.8: 0.2); Forming concentration is the outstanding turbid slurries of 2mg/mL hollow nano cages slurries; Measure 80 μ L and should hang turbid slurries, drop on the vitreous carbon collector of diameter 5mm, 15kg/cm exerts pressure on film after pole drying
2The pressure compacting to form the homogeneous film of thickness 70 μ m, is treated its air dry, promptly obtains the electrode of super capacitor based on hollow nano cages, is soaked in the 1mol/mL NaOH electrolyte this electrode subsequent use.Use the ion that soaks into through 1mol/mL NaOH electrolyte to see through film at two electrodes of processing according to said method and separate, compress and seal two electrodes, i.e. assembling becomes ultracapacitor.Have the operating voltage of 0.9V according to the ultracapacitor that obtains accordingly, have the ratio electric capacity of 260F/g during for 0.1A/g in discharge rate, 10A/g has～180F/g, and 100A/g has 110F/g.Its stability is discharged and recharged experiment confirm at a high speed by 10000 weeks.
Embodiment 7 is that the 10mg/mL hollow nano cages suspension-turbid liquid that dispersion liquid disposes is the electrode that collector is processed with the platinized platinum with water-ethanol-5%Nafion solution.
Take by weighing 800 ℃ of preparations of 10mg hollow nano cages; Ultrasonic dispersion is 45 minutes in 1mL water-ethanol-5%Nafion mixed liquor (ratio is 4: 0.8: 0.2); Forming concentration is the outstanding turbid slurries of 10mg/mL hollow nano cages slurries; Measure 100 μ L and should hang turbid slurries, drop on the platinized platinum collector of diameter 5mm, 10kg/cm exerts pressure on film after pole drying
2The pressure compacting to form the homogeneous film of thickness 95 μ m, is treated its air dry, promptly obtains the electrode of super capacitor based on hollow nano cages, is soaked in the 0.1mol/mL sodium sulphate electrolyte this electrode subsequent use.Use the ion that soaks into through 0.1mol/mL sodium sulphate electrolyte to see through film at two electrodes of processing according to said method and separate, compress and seal two electrodes, i.e. assembling becomes ultracapacitor.Have the operating voltage of 0.9V according to the ultracapacitor that obtains accordingly, have the ratio electric capacity of 245F/g during for 0.1A/g in discharge rate, 10A/g has～170F/g, and 100A/g has 102F/g.Its stability is discharged and recharged experiment confirm at a high speed by 10000 weeks.
Embodiment 8 is that the 5mg/mL hollow nano cages suspension-turbid liquid that dispersion liquid disposes is the electrode that collector is processed with the platinized platinum with water-ethanol-5%Nafion solution.
Take by weighing 850 ℃ of preparations of 10mg hollow nano cages; Ultrasonic dispersion is 45 minutes in 2mL water-ethanol-5%Nafion mixed liquor (ratio is 4: 0.8: 0.2), and forming concentration is the outstanding turbid slurries of 5mg/mL hollow nano cages slurries, measures 125 μ L and should hang turbid slurries; Drop on the platinized platinum collector of diameter 5mm; The 20kg/cm2 pressure compacting of on film, exerting pressure before the pole drying to form the homogeneous film of thickness 120 μ m, is treated its air dry; Promptly obtain electrode of super capacitor, be soaked in the 1mol/mL sodium sulphate electrolyte this electrode subsequent use based on hollow nano cages.Use the ion that soaks into through 1mol/mL sodium sulphate electrolyte to see through film at two electrodes of processing according to said method and separate, compress and seal two electrodes, i.e. assembling becomes ultracapacitor.Have the operating voltage of 1.8V according to the ultracapacitor that obtains accordingly, have the ratio electric capacity of 210F/g during for 0.1A/g in discharge rate, 10A/g has～150F/g, and 100A/g has 90F/g.Its stability is discharged and recharged experiment confirm at a high speed by 10000 weeks.
Embodiment 9 is that the 2mg/mL hollow nano cages suspension-turbid liquid that dispersion liquid disposes is the electrode that collector is processed with the vitreous carbon with water-ethanol-5%Nafion solution.
Take by weighing 900 ℃ of preparations of 10mg hollow nano cages; Ultrasonic dispersion is 30 minutes in 5mL water-ethanol-5%Nafion mixed liquor (ratio is 4: 0.8: 0.2); Forming concentration is the outstanding turbid slurries of 2mg/mL hollow nano cages slurries; Measure 150 these suspension-turbid liquids of μ L, drop on the vitreous carbon collector of diameter 5mm, 10kg/cm exerted pressure on film before pole drying
2The pressure compacting to form the homogeneous film of thickness 130 μ m, is treated its air dry, promptly obtains the electrode of super capacitor based on hollow nano cages, is soaked in the 5mol/mL sodium sulphate electrolyte this electrode subsequent use.Use the ion that soaks into through 5mol/mL sodium sulphate electrolyte to see through film at two electrodes of processing according to said method and separate, compress and seal two electrodes, i.e. assembling becomes ultracapacitor.Have the operating voltage of 1.3V according to the ultracapacitor that obtains accordingly, have the ratio electric capacity of about 210F/g during for 1A/g in discharge rate, 10A/g has～180F/g, and 100A/g has 110F/g.
Embodiment 10 is that 670 ℃ of synthetic hollow nano cages suspension-turbid liquids of 2.5mg/mL that dispersion liquid disposes are the electrode that collector is processed with the vitreous carbon with water-ethanol-5%Nafion solution.
Take by weighing 670 ℃ of synthetic hollow nano cages of 10mg; Ultrasonic dispersion is 40 minutes in 4mL water-ethanol-5%Nafion mixed liquor (ratio is 4: 0.8: 0.2); Forming concentration is the outstanding turbid slurries of 2.5mg/mL hollow nano cages slurries; Measure 175 these suspension-turbid liquids of μ L, drop on the vitreous carbon collector of diameter 5mm, 10kg/cm exerts pressure on film after pole drying
2The pressure compacting to form the homogeneous film of thickness 160 μ m, is treated its air dry, promptly obtains the electrode of super capacitor based on hollow nano cages, is soaked in the 1mol/mL lithium perchlorate electrolyte this electrode subsequent use.Use the ion that soaks into through 1mol/mL lithium perchlorate electrolyte to see through film at two electrodes of processing according to said method and separate, compress and seal two electrodes, i.e. assembling becomes ultracapacitor.Have the operating voltage of 1.8V according to the ultracapacitor that obtains accordingly, have the ratio electric capacity of 220F/g during for 0.1A/g in discharge rate, 10A/g has～160F/g, and 100A/g has 100F/g.Its stability is discharged and recharged experiment confirm at a high speed by 10000 weeks.
Embodiment 11 is that 750 ℃ of synthetic hollow nano cages suspension-turbid liquids of 0.1mg/mL that dispersion liquid disposes are the electrode that collector is processed with the vitreous carbon with water-ethanol-5%Nafion solution.
Take by weighing 750 ℃ of synthetic hollow nano cages of 10mg; Ultrasonic dispersion is 45 minutes in 100mL water-ethanol-5%Nafion mixed liquor (ratio is 4: 0.8: 0.2); Forming concentration is the outstanding turbid slurries of 0.1mg/mL hollow nano cages slurries; Measure 200 μ L and should hang turbid slurries, drop on the vitreous carbon collector of diameter 5mm, 10kg/cm exerted pressure on film before pole drying
2The pressure compacting to form the homogeneous film of thickness 180 μ m, is treated its air dry, promptly obtains the electrode of super capacitor based on hollow nano cages, is soaked in the 5mol/mL lithium perchlorate electrolyte this electrode subsequent use.Use the ion that soaks into through 5mol/mL lithium perchlorate electrolyte to see through film at two electrodes of processing according to said method and separate, compress and seal two electrodes, i.e. assembling becomes ultracapacitor.Have the operating voltage of 0.9V according to the ultracapacitor that obtains accordingly, have the ratio electric capacity of 260F/g during for 0.1A/g in discharge rate, 10A/g has～170F/g, and 100A/g has 100F/g.Its stability is discharged and recharged experiment confirm at a high speed by 10000 weeks.
Embodiment 12 is that 800 ℃ of synthetic hollow nano cages suspension-turbid liquids of 5mg/mL that dispersion liquid disposes are the electrode that collector is processed with the vitreous carbon with water-ethanol-5%Nafion solution.
Take by weighing 800 ℃ of synthetic hollow nano cages of 10mg; Ultrasonic dispersion is 35 minutes in 2mL water-ethanol-5%Nafion mixed liquor (ratio is 4: 0.8: 0.2); Forming concentration is the outstanding turbid slurries of 5mg/mL hollow nano cages slurries; Measure 220 μ L and should hang turbid slurries, drop on the vitreous carbon afflux of diameter 5mm, 20kg/cm exerted pressure on film before pole drying
2The pressure compacting to form the homogeneous film of thickness 200 μ m, is treated its air dry, promptly obtains the electrode of super capacitor based on hollow nano cages, is soaked in the 2mol/mL sulfuric acid electrolyte this electrode subsequent use.Use the ion that soaks into through the 2mol/mL sulfuric acid electrolyte to see through film at two electrodes of processing according to said method and separate, compress and seal two electrodes, i.e. assembling becomes ultracapacitor.Have the operating voltage of 0.9V according to the ultracapacitor that obtains accordingly, have the ratio electric capacity of 240F/g during for 0.1A/g in discharge rate, 10A/g has～170F/g, and 100A/g has 110F/g.Its stability is discharged and recharged experiment confirm at a high speed by 10000 weeks.
Embodiment 13 is that 850 ℃ of synthetic hollow nano cages suspension-turbid liquids of 5mg/mL that dispersion liquid disposes are the electrode that collector is processed with the vitreous carbon with water-ethanol-5%Nafion solution.
Take by weighing 850 ℃ of synthetic hollow nano cages of 10mg; Ultrasonic dispersion is 35 minutes in 2mL water-ethanol-5%Nafion mixed liquor (ratio is 4: 0.8: 0.2); Forming concentration is the outstanding turbid slurries of 5mg/mL hollow nano cages slurries; Measure 25 μ L and should hang turbid slurries, drop on the vitreous carbon collector of diameter 5mm, 10kg/cm exerted pressure on film before pole drying
2The pressure compacting to form the homogeneous film of thickness 15 μ m, is treated its air dry, promptly obtains the electrode of super capacitor based on hollow nano cages, is soaked in the 4mol/mL sulfuric acid electrolyte this electrode subsequent use.Use the ion that soaks into through the 4mol/mL sulfuric acid electrolyte to see through film at two electrodes of processing according to said method and separate, compress and seal two electrodes, i.e. assembling becomes ultracapacitor.Have the operating voltage of 0.9V according to the ultracapacitor that obtains accordingly, have the ratio electric capacity of 230F/g during for 0.1A/g in discharge rate, 10A/g has～165F/g, and 100A/g has 100F/g.Its stability is discharged and recharged experiment confirm at a high speed by 10000 weeks.
Embodiment 14 is that 900 ℃ of synthetic hollow nano cages suspension-turbid liquids of 5mg/mL that dispersion liquid disposes are the electrode that collector is processed with the vitreous carbon with water-ethanol-5%Nafion solution.
Take by weighing 900 ℃ of synthetic hollow nano cages of 10mg; Ultrasonic dispersion is 45 minutes in 2mL water-ethanol-5%Nafion mixed liquor (ratio is 4: 0.8: 0.2); Forming concentration is the outstanding turbid slurries of 5mg/mL hollow nano cages slurries; Measure 25 μ L and should hang turbid slurries, drop on the vitreous carbon collector of diameter 5mm, 10kg/cm exerted pressure on film before pole drying
2The pressure compacting to form the homogeneous film of thickness 15 μ m, is treated its air dry, promptly obtains the electrode of super capacitor based on hollow nano cages, is soaked in the 0.1mol/mL sulfuric acid electrolyte this electrode subsequent use.Use the ion that soaks into through the 0.1mol/mL sulfuric acid electrolyte to see through film at two electrodes of processing according to said method and separate, compress and seal two electrodes, i.e. assembling becomes ultracapacitor.Have the operating voltage of 1.3V according to the ultracapacitor that obtains accordingly, have the ratio electric capacity of 220F/g during for 0.1A/g in discharge rate, 10A/g has～155F/g, and 100A/g has 98F/g.Its stability is discharged and recharged experiment confirm at a high speed by 10000 weeks.
Embodiment 15 is that 950 ℃ of synthetic hollow nano cages suspension-turbid liquids of 5mg/mL that dispersion liquid disposes are the electrode that collector is processed with the vitreous carbon with water-ethanol-5%Nafion solution.
Take by weighing 950 ℃ of synthetic hollow nano cages of 10mg; Ultrasonic dispersion is 45 minutes in 2mL water-ethanol-5%Nafion mixed liquor (ratio is 4: 0.8: 0.2); Forming concentration is the outstanding turbid slurries of 5mg/mL hollow nano cages slurries; Measure 25 μ L and should hang turbid slurries, drop on the vitreous carbon collector of diameter 5mm, 20kg/cm exerts pressure on film after pole drying
2The pressure compacting to form the homogeneous film of thickness 15 μ m, is treated its air dry, promptly obtains the electrode of super capacitor based on hollow nano cages, is soaked in the 0.1mol/mL sulfuric acid electrolyte this electrode subsequent use.Use the ion that soaks into through the 0.1mol/mL sulfuric acid electrolyte to see through film at two electrodes of processing according to said method and separate, compress and seal two electrodes, i.e. assembling becomes ultracapacitor.Have the operating voltage of 0.9V according to the ultracapacitor that obtains accordingly, have the ratio electric capacity of 200F/g during for 0.1A/g in discharge rate, 10A/g has～140F/g, and 100A/g has 90F/g.Its stability is discharged and recharged experiment confirm at a high speed by 10000 weeks.
Embodiment 16 is that 1000 ℃ of synthetic hollow nano cages suspension-turbid liquids of 5mg/mL that dispersion liquid disposes are the electrode that collector is processed with the vitreous carbon with water-ethanol-5%Nafion solution.
Take by weighing 1000 ℃ of synthetic hollow nano cages of 10mg; Ultrasonic dispersion is 45 minutes in 2mL water-ethanol-5%Nafion mixed liquor (ratio is 4: 0.8: 0.2); Forming concentration is the outstanding turbid slurries of 5mg/mL hollow nano cages slurries; Measure 25 μ L and should hang turbid slurries, drop on the vitreous carbon collector of diameter 5mm, 10kg/cm exerted pressure on film before pole drying
2The pressure compacting to form the homogeneous film of thickness 15 μ m, is treated its air dry, promptly obtains the electrode of super capacitor based on hollow nano cages, is soaked in the 5mol/mL sulfuric acid electrolyte this electrode subsequent use.Use the ion that soaks into through the 5mol/mL sulfuric acid electrolyte to see through film at two electrodes of processing according to said method and separate, compress and seal two electrodes, i.e. assembling becomes ultracapacitor.Have the operating voltage of 0.9V according to the ultracapacitor that obtains accordingly, have the ratio electric capacity of 170F/g during for 0.1A/g in discharge rate, 10A/g has～110F/g, and 100A/g has 80F/g.Its stability is discharged and recharged experiment confirm at a high speed by 10000 weeks.
Embodiment 17 is that 1050 ℃ of synthetic hollow nano cages suspension-turbid liquids of 2.5mg/mL that dispersion liquid disposes are the electrode that collector is processed with the vitreous carbon with water-ethanol-5%Nafion solution.
Take by weighing 1050 ℃ of synthetic hollow nano cages of 10mg; Ultrasonic dispersion is 45 minutes in 4mL water-ethanol-5%Nafion mixed liquor (ratio is 4: 0.8: 0.2); Forming concentration is the outstanding turbid slurries of 2.5mg/mL hollow nano cages slurries; Measure 25 μ L and should hang turbid slurries, drop on the vitreous carbon collector of diameter 5mm, 10kg/cm exerted pressure on film before pole drying
2The pressure compacting to form the homogeneous film of thickness 15 μ m, is treated its air dry, promptly obtains the electrode of super capacitor based on hollow nano cages, is soaked in the 0.1mol/mL sulfuric acid electrolyte this electrode subsequent use.Use the ion that soaks into through the 0.1mol/mL sulfuric acid electrolyte to see through film at two electrodes of processing according to said method and separate, compress and seal two electrodes, i.e. assembling becomes ultracapacitor.Have the operating voltage of 0.9V according to the ultracapacitor that obtains accordingly, have the ratio electric capacity of 150F/g during for 0.1A/g in discharge rate, 10A/g has～110F/g, and 100A/g has 75F/g.Its stability is discharged and recharged experiment confirm at a high speed by 10000 weeks.
Embodiment 18 is that 1100 ℃ of synthetic hollow nano cages suspension-turbid liquids of 5mg/mL that dispersion liquid disposes are the electrode that collector is processed with the vitreous carbon with water-ethanol-5%Nafion solution.
Take by weighing 1100 ℃ of synthetic hollow nano cages of 10mg; Ultrasonic dispersion is 45 minutes in 2mL water-ethanol-5%Nafion mixed liquor (ratio is 4: 0.8: 0.2); Forming concentration is the outstanding turbid slurries of 5mg/mL hollow nano cages slurries; Measure 25 μ L and should hang turbid slurries, drop on the vitreous carbon collector of diameter 5mm, 10kg/cm exerted pressure on film before pole drying
2The pressure compacting to form the homogeneous film of thickness 15 μ m, is treated its air dry, promptly obtains the electrode of super capacitor based on hollow nano cages, is soaked in the 0.1mol/mL sulfuric acid electrolyte this electrode subsequent use.Use the ion that soaks into through the 0.1mol/mL sulfuric acid electrolyte to see through film at two electrodes of processing according to said method and separate, compress and seal two electrodes, i.e. assembling becomes ultracapacitor.Have the operating voltage of 0.9V according to the ultracapacitor that obtains accordingly, have the ratio electric capacity of 130F/g during for 0.1A/g in discharge rate, 10A/g has～90F/g, and 100A/g has 70F/g.Its stability is discharged and recharged experiment confirm at a high speed by 10000 weeks.
Claims (9)
1. the assemble method based on the ultracapacitor of hollow nano cages is characterized in that comprising the steps:
1) configuration hollow nano cages slurries:
Water, organic solvent and Nafion 4: 0.8: 0.2 are by volume mixed, obtain concentration and be 5% Nafion mixed solution; To form the hollow nano cages slurries 670-1100 ℃ of synthetic down ultrasonic being scattered in the aforementioned mixed solution of hollow nano cages again;
2) get the hollow nano cages slurries that dispose in the step 1) and evenly be applied on the collector, treat its air dry, promptly make the hollow nano cages electrode, be soaked in the following used electrolyte this electrode subsequent use.
3) assembling is based on the ultracapacitor of hollow nano cages electrode
Will be according to step 2) two identical electrodes obtaining use the ion that soaks into through electrolyte to see through film to separate, compress and seal two electrodes, i.e. and assembling becomes ultracapacitor.
2. the method for claim 1 is characterized in that it is characterized in that in the step 1), organic solvent is an ethanol, the mixture of any one or more than one arbitrary proportion in propyl alcohol or the acetone.
3. the method for claim 1 is characterized in that it is characterized in that in the step 1), the concentration of hollow nano cages slurries can be 0.1～10mg/mL.
4. the method for claim 1 is characterized in that it is characterized in that it is characterized in that in the step 1) in the step 1), and ultrasonic jitter time is not less than and was no more than 60 minutes in 30 minutes.
5. the method for claim 1 is characterized in that it is characterized in that step 2) in, collector is selected from vitreous carbon, copper sheet, stainless steel substrates, platinized platinum or aluminium flake.
6. the method for claim 1 is characterized in that step 2) in, the hollow nano cages slurries are applied on the collector the thick 2-200 μ m hollow nano cages electrode film of formed coat after dry.
7. the method for claim 1 is characterized in that step 2) in, on coat, exerting pressure before or after the pole drying, to form even coat.
8. method as claimed in claim 7 is characterized in that step 2) in, before or after the pole drying on coat applied pressure be 1-20kg/cm
2
9. the method for claim 1 is characterized in that in the step 3), and said electrolyte is selected from sulfuric acid, alkali metal hydroxide, sulfate or perchlorate, and concentration is 0.1-5mol/mL.
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| CN114914102A (en) * | 2022-06-07 | 2022-08-16 | 南京大学 | Preparation process of collapsed carbon-based nano cage electrode material |
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