CN101714466A - Preparation method of double electric layers supercapacitor - Google Patents
Preparation method of double electric layers supercapacitor Download PDFInfo
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Abstract
The invention relates to a preparation method of a double electric layers supercapacitor. The method comprises the following steps: preparing electrode paste, coating, rolling, dividing and cutting to obtain electrode plates, drying, dividing and cutting to obtain diaphragms, winding, welding, channeling, performing vacuum drying and injecting fluid under vacuum. The invention adopts high precision coating method to ensure the thickness of the electrode and the uniformity of electrical property, a special rolling technology is adopted to repeatedly roll the coated electrode so as to increase the adhesion strength of the electrode material and reduce the equivalent series resistance of the electrode; and reduce the equivalent series resistance of the electrode; the electrode has high mechanical strength and good thermal conductivity; the energy storage density of the prepared supercapacitor is up to 5.6Wh/kg, the power density is up to 13kW/kg; continuous coating of a plurality of carbon layers is realized and the carbon layers are cut to obtain a plurality of electrode plates, thus the production efficiency is greatly increased; and the preparation method of the invention has simple operation, the forming of the electrode is convenient to control, and the method is applicable to mass production.
Description
Technical field
The present invention relates to a kind of preparation method of double electric layers supercapacitor.
Background technology
A complete ultracapacitor comprises bipolar electrode, electrolyte, collector, spacer and five parts of package casing.Wherein electrode is the core part of ultracapacitor, and its structure, character play decisive influence to the performance of ultracapacitor.The technology of preparing of electrode material directly influences the performance of electrode material in the ultracapacitor, and then influences the performance of ultracapacitor.Therefore, research and development specific capacity electrode material big, that resistivity is little is the task of top priority.
Publication number is that the Chinese patent application of 101404210A discloses a kind of high-power super capacitor, and its pole piece is the single or double coating, and adopts the mode with the pole piece thinning to reduce the capacitor internal resistance, reaches the effect that improves its power; The patent No. is that 200410009700.3 Chinese patent discloses a kind of ultracapacitor, it adopts metal oxide nanotubes composite carbon sill as electrode, utilized the nanometer cooperative effect on nano carbon-base material surface and metal oxide nanotubes surface, increased the utilance of active material surface area, adopt organic electrolyte simultaneously, the energy density of ultracapacitor and power density are largely increased; The patent No. is the manufacture method that 200610047458.8 Chinese patent discloses a kind of electrode of super capacitor, it adopts composite caking agent and curtain coating rubbing method to make activated carbon electrodes, gained electrode softness, mechanical strength be big, be easy to serialization production, and the thinnest doing to 20 microns.
For the large-scale production that makes electrode material for super capacitor becomes a reality, the preparation of electrode material and technology should break through and innovate to some extent.The electrode material for super capacitor manufacturing technology should be towards Heat stability is good, bonding strength height, corrosion resistance is strong, technology is simple and the direction that is suitable for large-scale production develops.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of double electric layers supercapacitor.
Technical program of the present invention lies in adopting a kind of preparation method of double electric layers supercapacitor, this method may further comprise the steps
A) preparing electrode paste: with carbonaceous active material, conductive agent, binding agent according to 70～85: 6～11: 5～15 weight proportion mixes, with 500～1500 rev/mins of high-speed stirred 3～10 hours, make uniform electrode slurry, the three-dimensional dimension of described its particulate of carbonaceous active material should be 20～350 microns, and specific area is 250～3800 meters squared per gram; The carbonaceous active material is lower as the conductance of electrode material, adds conductive agent and can increase its conductivity; Binding ability extreme difference between the particulate of carbonaceous active material adds an amount of binding agent and can make it be easy to moulding; The slurry that uses this manner of formulation to make has certain viscosity, density, conductivity and flowability;
B) coating: the slurry that step a) is made uses the axial clearance coating method to be coated in continuous aluminium foil strip two sides uniformly, and heating, drying, wherein used aluminum foil thickness is 0.01～0.08mm, coating thickness is 10～200 μ m, middle coating clearance is 2 times that electrode is reserved lug, and it is that the width of lug adds 2～15mm that both sides remain not utter misery aluminium foil width; This coating method both can make pole piece reach higher quality, can guarantee the needs of large-scale production again;
C) the cutting of roll-in and pole piece, drying: the electrode that step b) is made divides three phases to carry out roll-in, cut then and obtain single electrode plates, under 60～80 ℃ with pole piece drying 10～72 hours; This method can make the pole piece pliability that makes good, apply firmly, and made ultracapacitor internal resistance is less;
D) barrier film is cut: cut porous septum;
E) reel: step c) and d) pole piece and the porous septum that obtain respectively, obtain pole core according to the overlapping coiling of order of pole piece, outer barrier film, pole piece, inner septum; Pole core will roll and closely make its structural strength big;
F) welding: the pole core two ends compacting that step e) is made earlier, the last lower cushion block that will have welding groove and dipping hole is again riveted or is welded on the lug of pole core two ends compacting;
G) slot rolling: step f) gained pole core is packed in the aluminum electric capacity housing, wherein between lower cushion block and the housing bottom, go up between cushion block and the end cap and be connected, and be furnished with sealing ring and insulating washer, the slot rolling that a week has certain depth and thickness is rolled in pairing housing section office, space between last cushion block and end cap, make the slot rolling inwall compress sealing ring and insulating washer, end cap that is connected with last lower cushion block and housing are respectively draws both positive and negative polarity; This fit system had both guaranteed effective sealing of housing, guaranteed effective insulation of both positive and negative polarity again;
H) vacuumize: the ultracapacitor monomer that formed end cap in the step g) is left liquid injection hole carried out vacuumize, 90～160 ℃ of following vacuumizes of temperature 10～96 hours;
I) vacuum fluid injection: filling electrolyte 20～400ml under vacuum state, adopt screw or welding or riveted joint sealing liquid injection port at last.
The described conductive agent of step a) is a kind of or its combination in any in conductive carbon black, acetylene black, graphite and the wire; Described binding agent is a kind of or its combination in any in polytetrafluoroethylene, Kynoar, phenolic resins, polyester, polyamide and the butadiene rubber, these binding agents both can be Powdered also can be emulsion form.
The described roll-in concrete steps of step c) are as follows: [1] is under the 30-40% condition at room temperature, ambient humidity, adjust the hydraulic pressure roll-in and carry out the roll-in of phase I by force for 7-16MPa, the total compression amount is 35-40%, and the decrement of single is 5-10%, determines the compression number of times according to the total compression amount; [2] under 120-140 ℃, drying condition, to adjust the hydraulic pressure roll-in and carry out the roll-in of second stage by force for 4-10MPa, the total compression amount is 20-30%, the single decrement is 4-7%, determines the compression number of times according to the total compression amount; [3] under room temperature, drying condition, adjusting the hydraulic pressure roll-in is by force 2-6MPa, and the total compression amount is 10-15%, and the single decrement is 2-5%, determines the compression number of times according to the total compression amount; Roller process through three phases can be cut.
The described barrier film of step d) is a kind of or its combination in any in papery porous capacitor diaphragm, polypropylene non-woven fabric layer barrier film, polycthylene grafted mould layer barrier film, the asbestos fibre.
Described end cap of step g) and housing, its part of exposing super capacitor can be processed into binding post or screw thread.
Step I) described electrolyte is non-aqueous organic electrolyte, by solute and solvent composition, wherein solute is the tetrafluoro boric acid amine salt, comprise tetrafluoro boric acid tetraethyl amine, tetrafluoro boric acid methyl triethylamine, tetrafluoro boric acid dimethyl diethylamide, tetrafluoro boric acid trimethyl one ethylamine or the combination of above-mentioned two or more solute; Solvent is the mixed liquor of acetonitrile, propene carbonate, gamma-butyrolacton or sulfolane organic solvent or above-mentioned two or more solvents; Concentration of electrolyte is 0.7mol/L～1.7mol/L.
Step I) described vacuum fluid injection, the vacuum environment water content is controlled at below the 23PPM, and Control for Oxygen Content is below 5PPM.
The invention has the beneficial effects as follows and adopted high-precision coating method, electrode slurry is coated in uniformly the two sides of continuous aluminium foil strip, guarantee the uniformity of thickness of electrode and electrical property, and adopt special rolling process that coated electrode is carried out rolling repeatedly, improve the electrode material adhesion strength, reduce the electrode equivalent series resistance simultaneously; Adopt the broad-area electrode terminal, improved the heavy-current discharge characteristic of capacitor greatly, farthest eliminated the phenomenon of the inner local pyrexia of capacitor simultaneously; The energy storage density of prepared ultracapacitor reaches 5.6Wh/kg, and power density is up to 13kW/kg; Owing to realized many carbon-coatings of continuously coating, divided again to be cut to several electrode plates, so production efficiency is greatly improved; Preparation method of the present invention is simple to operate, and electrode moulding control is convenient, is convenient to large-scale production.
Description of drawings
Fig. 1 is a pole piece coating method schematic diagram; Wherein black region is the utter misery zone, and white portion is coating clearance (a not utter misery aluminium foil part);
Fig. 2 is the pole piece schematic diagram after cutting; Wherein black part is divided into the utter misery part, and white portion is lug (a not utter misery aluminium foil part);
Fig. 3 is a pole piece barrier film overlap mode schematic diagram;
Fig. 4 is the supercapacitor structures schematic diagram.
Embodiment
The structural representation of the prepared double electric layers supercapacitor of the present invention such as Fig. 4, wherein end cap 1 is connected with last cushion block 7 as the exit of electric capacity one utmost point, Φ 2～8mm screwed hole is arranged as liquid injection hole on the end cap 1; Screw 2 and compound gasket 4 cooperate with liquid injection hole, and seal; Insulating washer 3 and 6 prevents that cushion block 7 and end cap 1 are communicated with housing 10, plays insulating effect; Leave the electrolyte pod apertures above the last cushion block 7, and welding groove or riveted joint zone are arranged; Fuse 8 two ends behind the coiling and last cushion block 7 and lower cushion block 9 weld or are riveted together; Lower cushion block 9 bottoms and housing 10 are connected, and housing is as another extraction pole.
The preparation method of double electric layers supercapacitor
A) preparing electrode paste: carbonaceous active material, conductive black, polytetrafluoroethylene are mixed according to 70: 6: 5 weight proportion, with 500 rev/mins of high-speed stirred 10 hours, make uniform electrode slurry, the three-dimensional dimension of described its particulate of carbonaceous active material should be 20～350 microns, and specific area is 250～3800 meters squared per gram;
B) coating: the slurry that step a) is made is coated in continuous aluminium foil strip two sides uniformly according to Fig. 1 mode, and heating, drying, guarantee the uniformity of thickness of electrode and electrical property, wherein used aluminum foil thickness is 0.01mm, coating thickness is 10 μ m, middle coating clearance is 2 times that electrode is reserved lug, and it is that the width of lug adds 2mm that both sides remain not utter misery aluminium foil width;
C) roll-in and pole piece cut drying: the electrode that step b) is made carries out roll-in, concrete roll-in step is as follows: [1] is under 30% condition at room temperature, ambient humidity, adjust the hydraulic pressure roll-in and carry out the roll-in of phase I by force for 7MPa, the total compression amount is 35%, the decrement of single is 5%, determines the compression number of times according to the total compression amount; [2] under 120 ℃, drying condition, to adjust the hydraulic pressure roll-in and carry out the roll-in of second stage by force for 4MPa, the total compression amount is 20%, the single decrement is 4%, determines the compression number of times according to the total compression amount; [3] under room temperature, drying condition, adjusting the hydraulic pressure roll-in is by force 2MPa, and the total compression amount is 10%, and the single decrement is 2%, determines the compression number of times according to the total compression amount; Cut then and obtain single electrode plates as shown in Figure 2, under 60 ℃ with dry 10 hours of pole piece;
D) barrier film is cut: cut papery porous capacitor diaphragm;
E) pole piece and the porous septum that obtains respectively coiling: with step c) and d), according to the overlapping coiling of order of pole piece 14, outer barrier film 13, pole piece 12, inner septum 11, electrode cores will roll closely, and the mode that stacks of pole piece and barrier film is as shown in Figure 3;
F) welding: the fuse two ends compacting that step e) is made earlier, the last lower cushion block that will have welding groove and dipping hole is again riveted or is welded on the lug of fuse two ends compacting;
G) slot rolling: step f) gained electrode cores is packed in the aluminum electric capacity housing, wherein between lower cushion block and the housing bottom, go up between cushion block and the end cap and be connected, and be furnished with sealing ring and insulating washer, the slot rolling that a week has certain depth and thickness is rolled in pairing housing section office, space between last cushion block and end cap, make the slot rolling inwall compress sealing ring and insulating washer, end cap that is connected with last lower cushion block and housing are respectively draws both positive and negative polarity, and the part that end cap and housing expose super capacitor is processed into binding post;
H) vacuumize: the ultracapacitor monomer that formed end cap in the step g) is left liquid injection hole carried out vacuumize, 90 ℃ of following vacuumizes of temperature 96 hours;
I) vacuum fluid injection: the electrolyte of under vacuum state, annotating (electrolyte is the acetonitrile solution of tetrafluoro boric acid four hexyl amines) 20ml, wherein the vacuum environment water content is controlled at 23PPM, and Control for Oxygen Content adopts screw or welding or riveted joint sealing liquid injection port at last at 5PPM.
The preparation method of double electric layers supercapacitor
A) preparing electrode paste: carbonaceous active material, acetylene black, Kynoar are mixed according to 78: 8: 10 weight proportion, with 1000 rev/mins of high-speed stirred 7 hours, make uniform electrode slurry, the three-dimensional dimension of described its particulate of carbonaceous active material should be 20～350 microns, and specific area is 250～3800 meters squared per gram;
B) coating: the slurry that step a) is made is coated in continuous aluminium foil strip two sides uniformly according to Fig. 1 mode, and heating, drying, guarantee the uniformity of thickness of electrode and electrical property, wherein used aluminum foil thickness is 0.05mm, coating thickness is 100 μ m, middle coating clearance is 2 times that electrode is reserved lug, and it is that the width of lug adds 5mm that both sides remain not utter misery aluminium foil width;
C) roll-in and pole piece cut drying: the electrode that step b) is made carries out roll-in, concrete roll-in step is as follows: [1] is under 35% condition at room temperature, ambient humidity, adjust the hydraulic pressure roll-in and carry out the roll-in of phase I by force for 12MPa, the total compression amount is 38%, the decrement of single is 7%, determines the compression number of times according to the total compression amount; [2] under 130 ℃, drying condition, to adjust the hydraulic pressure roll-in and carry out the roll-in of second stage by force for 7MPa, the total compression amount is 25%, the single decrement is 5%, determines the compression number of times according to the total compression amount; [3] under room temperature, drying condition, adjusting the hydraulic pressure roll-in is by force 4MPa, and the total compression amount is 12%, and the single decrement is 4%, determines the compression number of times according to the total compression amount; Cut then and obtain single electrode plates as shown in Figure 2, under 70 ℃ with dry 40 hours of pole piece;
D) barrier film is cut: cut polypropylene non-woven fabric layer barrier film;
E) pole piece and the barrier film that obtains respectively coiling: with step c) and d), according to the overlapping coiling of order of pole piece 14, outer barrier film 13, pole piece 12, inner septum 11, electrode cores will roll closely, and the mode that stacks of pole piece and barrier film is as shown in Figure 3;
F) welding: the fuse two ends compacting that step e) is made earlier, the last lower cushion block that will have welding groove and dipping hole is again riveted or is welded on the lug of fuse two ends compacting;
G) slot rolling: step f) gained electrode cores is packed in the aluminum electric capacity housing, wherein between lower cushion block and the housing bottom, go up between cushion block and the end cap and be connected, and be furnished with sealing ring and insulating washer, the slot rolling that a week has certain depth and thickness is rolled in the pairing housing section in space office between last cushion block and end cap, make the slot rolling inwall compress sealing ring and insulating washer, end cap that is connected with last lower cushion block and housing are respectively draws both positive and negative polarity, and the part that end cap and housing expose super capacitor is processed into binding post;
H) vacuumize: the ultracapacitor monomer that formed end cap in the step g) is left liquid injection hole carried out vacuumize, 125 ℃ of following vacuumizes of temperature 55 hours;
I) vacuum fluid injection: the electrolyte of under vacuum state, annotating (electrolyte is the carbonic allyl ester solution of tetrafluoro boric acid methyl triethylamine) 200ml, wherein the vacuum environment water content is controlled at 15PPM, Control for Oxygen Content adopts screw or welding or riveted joint sealing liquid injection port at last at 3PPM.
Embodiment 3
The preparation method of double electric layers supercapacitor
A) preparing electrode paste: carbonaceous active material, graphite, phenolic resins are mixed according to 85: 11: 15 weight proportion, with 1500 rev/mins of high-speed stirred 3 hours, make uniform electrode slurry, the three-dimensional dimension of described its particulate of carbonaceous active material should be 20～350 microns, and specific area is 250～3800 meters squared per gram;
B) coating: the slurry that step a) is made is coated in continuous aluminium foil strip two sides uniformly according to Fig. 1 mode, and heating, drying, guarantee the uniformity of thickness of electrode and electrical property, wherein used aluminum foil thickness is 0.08mm, coating thickness is 200 μ m, middle coating clearance is 2 times that electrode is reserved lug, and it is that the width of lug adds 10mm that both sides remain not utter misery aluminium foil width;
C) roll-in and pole piece cut drying: the electrode that step b) is made carries out roll-in, concrete roll-in step is as follows: [1] is under 40% condition at room temperature, ambient humidity, adjust the hydraulic pressure roll-in and carry out the roll-in of phase I by force for 16MPa, the total compression amount is 40%, the decrement of single is 10%, determines the compression number of times according to the total compression amount; [2] under 140 ℃, drying condition, to adjust the hydraulic pressure roll-in and carry out the roll-in of second stage by force for 10MPa, the total compression amount is 30%, the single decrement is 7%, determines the compression number of times according to the total compression amount; [3] under room temperature, drying condition, adjusting the hydraulic pressure roll-in is by force 6MPa, and the total compression amount is 15%, and the single decrement is 5%, determines the compression number of times according to the total compression amount.Cut then and obtain single electrode plates as shown in Figure 2, under 80 ℃ with dry 72 hours of pole piece;
D) barrier film is cut: cut porous septum, the barrier film that uses is asbestos fibre;
E) pole piece and the porous septum that obtains respectively coiling: with step c) and d), according to the overlapping coiling of order of pole piece 14, outer barrier film 13, pole piece 12, inner septum 11, electrode cores will roll closely, and the mode that stacks of pole piece and barrier film is as shown in Figure 3;
F) welding: the fuse two ends compacting that step e) is made earlier, the last lower cushion block that will have welding groove and dipping hole is again riveted or is welded on the lug of fuse two ends compacting;
G) slot rolling: step f) gained electrode cores is packed in the aluminum electric capacity housing, wherein between lower cushion block and the housing bottom, go up between cushion block and the end cap and be connected, and be furnished with sealing ring and insulating washer, the slot rolling that a week has certain depth and thickness is rolled in the pairing housing section in space office between last cushion block and end cap, make the slot rolling inwall compress sealing ring and insulating washer, end cap that is connected with last lower cushion block and housing are respectively draws both positive and negative polarity, and the part that end cap and housing expose super capacitor is processed into screw thread;
H) vacuumize: the ultracapacitor monomer that formed end cap in the step g) is left liquid injection hole carried out vacuumize, 160 ℃ of following vacuumizes of temperature 10 hours;
I) vacuum fluid injection: the electrolyte of under vacuum state, annotating (electrolyte is the sulfolane solution of tetrafluoro boric acid dimethyl diethylamide) 400ml, wherein the vacuum environment water content is controlled at 10PPM, Control for Oxygen Content adopts screw or welding or riveted joint sealing liquid injection port at last at 1PPM.
Claims (7)
1. the preparation method of a double electric layers supercapacitor, it is characterized in that: described preparation method may further comprise the steps
A) preparing electrode paste: with carbonaceous active material, conductive agent, binding agent according to 70～85: 6～11: 5～15 weight proportion mixes, with 500～1500 rev/mins of high-speed stirred 3～10 hours, make uniform electrode slurry, the three-dimensional dimension of described its particulate of carbonaceous active material should be 20～350 microns, and specific area is 250～3800 meters squared per gram;
B) coating: the slurry that step a) is made uses the axial clearance coating method to be coated in continuous aluminium foil strip two sides uniformly, and heating, drying, wherein used aluminum foil thickness is 0.01～0.08mm, coating thickness is 10～200 μ m, middle coating clearance is 2 times that electrode is reserved lug, and it is that the width of lug adds 2～15mm that both sides remain not utter misery aluminium foil width;
C) the cutting of roll-in and pole piece, drying: the electrode that step b) is made divides three phases to carry out roll-in, cut then and obtain single electrode plates, under 60～80 ℃ with pole piece drying 10～72 hours;
D) barrier film is cut: cut porous septum;
E) reel: step c) and d) pole piece and the porous septum that obtain respectively, obtain pole core according to the overlapping coiling of order of pole piece, outer barrier film, pole piece, inner septum;
F) welding: the pole core two ends compacting that step e) is made earlier, the last lower cushion block that will have welding groove and dipping hole is again riveted or is welded on the lug of pole core two ends compacting;
G) slot rolling: step f) gained pole core is packed in the aluminum electric capacity housing, wherein between lower cushion block and the housing bottom, go up between cushion block and the end cap and be connected, and be furnished with sealing ring and insulating washer, the slot rolling that a week has certain depth and thickness is rolled in pairing housing section office, space between last cushion block and end cap, make the slot rolling inwall compress sealing ring and insulating washer, end cap that is connected with last lower cushion block and housing are respectively draws both positive and negative polarity;
H) vacuumize: the ultracapacitor monomer that formed end cap in the step g) is left liquid injection hole carried out vacuumize, 90～160 ℃ of following vacuumizes of temperature 10～96 hours;
I) vacuum fluid injection: filling electrolyte 20～400ml under vacuum state, adopt screw or welding or riveted joint sealing liquid injection port at last.
2. the preparation method of a kind of double electric layers supercapacitor according to claim 1, it is characterized in that: the described conductive agent of step a) is a kind of or its combination in any in conductive carbon black, acetylene black, graphite and the wire; Described binding agent is a kind of or its combination in any in polytetrafluoroethylene, Kynoar, phenolic resins, polyester, polyamide and the butadiene rubber, these binding agents both can be Powdered also can be emulsion form.
3. the preparation method of a kind of double electric layers supercapacitor according to claim 1, it is characterized in that: the described roll-in concrete steps of step c) are as follows: [1] is under the 30-40% condition at room temperature, ambient humidity, adjust the hydraulic pressure roll-in and carry out the roll-in of phase I by force for 7-16MPa, the total compression amount is 35-40%, the decrement of single is 5-10%, determines the compression number of times according to the total compression amount; [2] under 120-140 ℃, drying condition, to adjust the hydraulic pressure roll-in and carry out the roll-in of second stage by force for 4-10MPa, the total compression amount is 20-30%, the single decrement is 4-7%, determines the compression number of times according to the total compression amount; [3] under room temperature, drying condition, adjusting the hydraulic pressure roll-in is by force 2-6MPa, and the total compression amount is 10-15%, and the single decrement is 2-5%, determines the compression number of times according to the total compression amount; Roller process through three phases can be cut.
4. the preparation method of a kind of double electric layers supercapacitor according to claim 1, it is characterized in that: the described barrier film of step d) is a kind of or its combination in any in papery porous capacitor diaphragm, polypropylene non-woven fabric layer barrier film, polycthylene grafted mould layer barrier film, the asbestos fibre.
5. the preparation method of a kind of double electric layers supercapacitor according to claim 1, it is characterized in that: described end cap of step g) and housing, its part of exposing super capacitor can be processed into binding post or screw thread.
6. the preparation method of a kind of double electric layers supercapacitor according to claim 1, it is characterized in that: step I) described electrolyte is non-aqueous organic electrolyte, by solute and solvent composition, wherein solute is the tetrafluoro boric acid amine salt, comprise tetrafluoro boric acid tetraethyl amine, tetrafluoro boric acid methyl triethylamine, tetrafluoro boric acid dimethyl diethylamide, tetrafluoro boric acid trimethyl one ethylamine or the combination of above-mentioned two or more solute; Solvent is the mixed liquor of acetonitrile, propene carbonate, gamma-butyrolacton or sulfolane organic solvent or above-mentioned two or more solvents; Concentration of electrolyte is 0.7mol/L～1.7mol/L.
7. the preparation method of a kind of double electric layers supercapacitor according to claim 1 is characterized in that: step I) described vacuum fluid injection, and the vacuum environment water content is controlled at below the 23PPM, and Control for Oxygen Content is below 5PPM.
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