CN105869913B - A kind of ultracapacitor and preparation method thereof - Google Patents
A kind of ultracapacitor and preparation method thereof Download PDFInfo
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- CN105869913B CN105869913B CN201610211110.1A CN201610211110A CN105869913B CN 105869913 B CN105869913 B CN 105869913B CN 201610211110 A CN201610211110 A CN 201610211110A CN 105869913 B CN105869913 B CN 105869913B
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- 238000002360 preparation method Methods 0.000 title abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical group [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 75
- 229910052799 carbon Inorganic materials 0.000 claims abstract description 63
- 239000003792 electrolyte Substances 0.000 claims abstract description 40
- 239000002131 composite material Substances 0.000 claims abstract description 34
- 238000010276 construction Methods 0.000 claims abstract description 33
- 239000007772 electrode material Substances 0.000 claims abstract description 30
- 239000002086 nanomaterial Substances 0.000 claims abstract description 28
- 229910052751 metal Inorganic materials 0.000 claims abstract description 25
- 239000002184 metal Substances 0.000 claims abstract description 25
- 239000002002 slurry Substances 0.000 claims abstract description 18
- 238000000034 method Methods 0.000 claims abstract description 13
- 238000000465 moulding Methods 0.000 claims abstract description 11
- 239000003990 capacitor Substances 0.000 claims description 28
- 239000007788 liquid Substances 0.000 claims description 27
- 238000002347 injection Methods 0.000 claims description 17
- 239000007924 injection Substances 0.000 claims description 17
- 239000006260 foam Substances 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims description 8
- 230000032683 aging Effects 0.000 claims description 8
- 239000004411 aluminium Substances 0.000 claims description 8
- 229910052782 aluminium Inorganic materials 0.000 claims description 8
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 8
- 239000002041 carbon nanotube Substances 0.000 claims description 8
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 8
- 238000007872 degassing Methods 0.000 claims description 8
- 238000007493 shaping process Methods 0.000 claims description 8
- 229910052709 silver Inorganic materials 0.000 claims description 8
- 239000004332 silver Substances 0.000 claims description 8
- 238000002604 ultrasonography Methods 0.000 claims description 8
- 229910021389 graphene Inorganic materials 0.000 claims description 7
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 6
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 6
- 229910052802 copper Inorganic materials 0.000 claims description 6
- 239000010949 copper Substances 0.000 claims description 6
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 claims description 6
- 241000446313 Lamella Species 0.000 claims description 5
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims description 4
- 229910052759 nickel Inorganic materials 0.000 claims description 3
- 229910052697 platinum Inorganic materials 0.000 claims description 3
- 238000005868 electrolysis reaction Methods 0.000 claims description 2
- 239000003292 glue Substances 0.000 claims description 2
- 229910052742 iron Inorganic materials 0.000 claims description 2
- 238000005086 pumping Methods 0.000 claims 1
- 150000002739 metals Chemical class 0.000 abstract description 4
- 239000008151 electrolyte solution Substances 0.000 abstract description 3
- 239000005486 organic electrolyte Substances 0.000 abstract description 2
- 239000000470 constituent Substances 0.000 abstract 1
- 239000006185 dispersion Substances 0.000 abstract 1
- 238000004806 packaging method and process Methods 0.000 abstract 1
- 239000003575 carbonaceous material Substances 0.000 description 6
- -1 ethyl ammonium tetrafluoroborate Chemical compound 0.000 description 4
- WEVYAHXRMPXWCK-UHFFFAOYSA-N Acetonitrile Chemical compound CC#N WEVYAHXRMPXWCK-UHFFFAOYSA-N 0.000 description 3
- 239000000853 adhesive Substances 0.000 description 3
- 230000001070 adhesive effect Effects 0.000 description 3
- 210000005069 ears Anatomy 0.000 description 3
- 239000012530 fluid Substances 0.000 description 3
- 238000010521 absorption reaction Methods 0.000 description 2
- 230000018044 dehydration Effects 0.000 description 2
- 238000006297 dehydration reaction Methods 0.000 description 2
- 239000000203 mixture Substances 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229940124530 sulfonamide Drugs 0.000 description 2
- 238000003466 welding Methods 0.000 description 2
- IBZJNLWLRUHZIX-UHFFFAOYSA-N 1-ethyl-3-methyl-2h-imidazole Chemical class CCN1CN(C)C=C1 IBZJNLWLRUHZIX-UHFFFAOYSA-N 0.000 description 1
- 240000007594 Oryza sativa Species 0.000 description 1
- 235000007164 Oryza sativa Nutrition 0.000 description 1
- 235000010338 boric acid Nutrition 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 230000007423 decrease Effects 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 235000009566 rice Nutrition 0.000 description 1
- 238000005096 rolling process Methods 0.000 description 1
Classifications
-
- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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 electrode material of a kind of ultracapacitor and preparation method thereof, the ultracapacitor is carbon nano-electrode material, and collector is carbon-coated porous metals, and mass fraction of the carbon nanomaterial in ultracapacitor is 20 35%；Preparation method is also disclosed in the present invention, including in the electrolytic solution by the dispersion of carbon nano-electrode material, constitutes slurry；By slurry vacuumize or pressurized conditions under squeeze into porous current collector, formed electrode and collector composite construction；Finally collector and metal tabs are welded, the composite construction diaphragm of electrode and collector is separated, packaging molding；Ultracapacitor product obtained by this method has active constituent content high, and the high advantage of volume energy density can be operated suitable for aqueous electrolyte, organic electrolyte and il electrolyte in 1 5V.
Description
Technical field
The invention belongs to ultracapacitor preparing technical fields, and in particular to a kind of carbon nano-electrode and carbon nanometer collector
Ultracapacitor and preparation method thereof.
Background technology
Double electric layers supercapacitor has charging soon, long lifespan, the big advantage of power density, in heavy-duty engine, mainframe
In terms of the startup of tool recovers energy with brake, there is irreplaceable role.Recent development trend is to use carbon nanomaterial
Electrode material is done, to substitute active carbon electrode material, and is operated under higher voltage (3V), to obtain higher energy
Density, to expand the application field of ultracapacitor.
Most traditional capacitor arrangement is that electrode material is attached on metal plate collector, and lug of then burn-oning is used in combination
Diaphragm is separated by, and injects electrolyte, forms capacitor system.For carbon nanomaterial since density is light, liquid absorption amount is big, processing difficulties.Simultaneously
Active force between plate type metal collector is weak, needs to use adhesive, results in voltage window decline, and internal resistance increases.Institute
To have the report using porous metals collector, after electrode material is refined, porous metals collection is injected in slurrying in the electrolytic solution
In fluid, play the role of fixed electrode material, also avoids using adhesive, improve the mass fraction of electrode material.So
And the shortcomings that metal collector has weight big, and mechanical strength increases with porosity and declines rapidly, cause Continuous maching difficult
And it is with high costs.Also have and carbon nanomaterial is directly prepared into pad, while playing electrode material and collector.But
The hole of such collector is still too big, and liquid absorption amount is big, and volume energy is not high, and expansive disadvantage, while many big specific surfaces
Long-pending carbon nanomaterial filming performance is bad, limits its use.
Invention content
In order to solve the above-mentioned problems of the prior art, the purpose of the present invention is to provide a kind of ultracapacitor and its
Preparation method, carbon-coated foam-metal current collector body wherein by the injection of carbon nano-electrode form composite construction, are received with improving carbon
Mass fraction of the rice material in ultracapacitor, and improve the volume energy density of capacitor.
To achieve the above objectives, the present invention adopts the following technical scheme that：
The electrode material of a kind of ultracapacitor, the ultracapacitor is carbon nanomaterial, and collector is carbon-coated
Foam metal, mass fraction of the carbon nanomaterial in ultracapacitor are 20-35%.
The carbon nanomaterial, including carbon nanotube and graphene or the two are mixed with arbitrary proportion；Wherein carbon
A diameter of 0.6-200nm, the draw ratio 1-1000 of nanotube；Wherein the thickness of graphene is 0.35-5nm, and lamella area is
0.001-25μm2。
The mass fraction of carbon is 0.1-5%, structure Sp in the carbon-coated foam metal2Hydridization；The sky of collector
Gap rate is 70-96%, and thickness is 50-500 μm.
Metal is aluminium, copper, nickel, silver or platinum in the foam metal.
The method of ultracapacitor described above, includes the following steps：
Step 1：The carbon nanomaterial is added in electrolyte, ultrasound 1-30 minutes at 20-60 DEG C, 1-3kW,
Form the slurry that viscosity is 15000-500000 centipoises；
Step 2：The mode that above-mentioned slurry is squeezed or vacuumized, makes it into the hole of collector, forms electrode
The composite construction of material and collector；
Step 3：By roll-in, the partial electrolyte liquid in above-mentioned composite construction is squeezed out, it is 20- to make the thickness of composite construction
400μm；
Step 4：Step 3 gained composite construction is fixed with metal tabs with conductive silver glue, and is welded；Again with diaphragm point
Every then multi-disc assembling is packaged molding, only stays a liquid injection port, obtain shaping capacitor；
Step 5：By above-mentioned shaping capacitor by being dehydrated, degassing and Aging Step add electrolyte, make institute in capacitor
There is the mass ratio of carbon material and electrolyte to be：1:1.2~1:3.
Step 6：Liquid injection port is closed, capacitor product is formed, the wherein mass fraction of carbon nanomaterial is 20-35%.
The pressure squeezed described in step 2 is 0.2-1MPa；The vacuum degree vacuumized is 10-1-10-2Pa。
The material of metal tabs described in step 4 is aluminium, silver, copper or iron.
Electrolyte described in step 1 be aqueous electrolyte, organic electrolyte or il electrolyte, can 1-5V operation.
Compared to the prior art the present invention, has the following advantages that：
1) carbon-coated foam-metal current collector body, is compared, high mechanical strength than simple metal collector used in, is not afraid of crowded
Pressure, can be molded under high rolling pressure, be conducive to improve the compactness of electrode material, reduce internal resistance, reduce cost.
2) since the carbon itself in collector also contributes to capacitance, so its porosity ranges can be than porous metals collector
Width it is very much, broaden for the granularity requirements of carbon nano-electrode material, improve the available types of electrode material, advantageously reduce
Processing cost improves volume energy density.
3) carbon nano electrode material is filled in carbon-coated foam-metal current collector body, forms composite construction, can both reduces carbon
The swellability of nano material in the electrolytic solution, and with good interface compatibility and small contact resistance.
4) compared with the process for using flat metal collector, due to not having adhesive, which uses week
Phase is longer, is more conducive to the performance for playing electrode material.
Specific implementation mode
Below in conjunction with specific embodiment, the present invention is described in further detail.
Embodiment 1
The carbon nanotube for being 1000 using a diameter of 0.6nm, draw ratio is electrode material, in aqueous electrolyte (such as 6mol/L
KOH solution) in, at 20 DEG C, 1kW ultrasound 30 minutes, is formed viscosity for 15000 centipoises slurry.Above-mentioned slurry is taken out
Vacuum (10-1Pa mode), making it into carbon-coated Foam silver collector, (mass fraction of carbon is 0.1%, structure Sp2
Hydridization.The voidage of collector be 96%, thickness be 500 μm) hole in, formed electrode material and collector composite junction
Structure.By roll-in, the partial electrolyte liquid in above-mentioned composite construction is squeezed out, it is 400 μm to make the thickness of composite construction.It will be above-mentioned multiple
Structure is closed to be welded with aluminium pole ears.Separated again with diaphragm, multi-disc assembling, encapsulated moulding only stays a liquid injection port.By above-mentioned molding
Capacitor adds electrolyte, makes the quality of all carbon materials and electrolyte in capacitor by the conventional procedures such as degassing and aging
Than for：1:1.2.Liquid injection port is closed, capacitor product is formed, the wherein mass fraction of carbon nanomaterial is 35%.It can be
It is operated under 1V, the capacitance based on carbon nanomaterial is 250F/g.
Embodiment 2
It is 0.35nm with thickness, lamella area is 0.001 μm2Graphene be electrode material, in organic liquor electrolyte (four
The acetonitrile solution of ethyl ammonium tetrafluoroborate) in, ultrasound 10 minutes at 50 DEG C, 1kW form the slurry that viscosity is 20000 centipoises
Material.By above-mentioned slurry with vacuumizing (10-1Pa mode) makes it into the carbon-coated foamed nickel current collector (mass fraction of carbon
It is 5%, structure is Sp2 hydridization.The voidage of collector be 70%, thickness be 300 μm) hole in, formed electrode material with
The composite construction of collector.By roll-in, the partial electrolyte liquid in above-mentioned composite construction is squeezed out, makes the thickness of composite construction be
250μm.By above-mentioned composite construction and silver-colored tab welding.Separated again with diaphragm, multi-disc assembling, encapsulated moulding only stays a liquid injection port.
By above-mentioned shaping capacitor by being dehydrated, the conventional procedures such as degassing and aging add electrolyte, make all carbon materials in capacitor
Mass ratio with electrolyte is：1:2.2.Liquid injection port is closed, capacitor product, the wherein mass fraction of carbon nanomaterial are formed
It is 27.5%.It can be operated at 3V, the capacitance based on carbon nanomaterial is 150F/g.
Embodiment 3
It is 2nm with thickness, lamella area is 25 μm2Graphene and a diameter of 200nm, draw ratio be 1 carbon nanotube
Mixture be electrode material, the mass ratio of the two is 1:1. in il electrolyte (the double trifluoros of 1- ethyl-3-methylimidazoles
Sulfonamide) in, ultrasound 20 minutes at 60 DEG C, 0.8kW form the slurry that viscosity is 340000 centipoises.By above-mentioned slurry
Material squeeze mode (1MPa) mode, make it into carbon-coated foam copper current collector (mass fraction of carbon be 1.5%,
Structure is Sp2 hydridization.The voidage of collector is 90%, and thickness is 300 μm) hole in, form electrode material and collector
Composite construction.By roll-in, the partial electrolyte liquid in above-mentioned composite construction is squeezed out, it is 220 μm to make the thickness of composite construction.
Above-mentioned composite construction and copper polar ear are welded.Separated again with diaphragm, multi-disc assembling, encapsulated moulding only stays a liquid injection port.It will be above-mentioned
Shaping capacitor adds electrolyte by dehydration, the conventional procedures such as degassing and aging, makes all carbon materials and electrolysis in capacitor
The mass ratio of liquid is：1:3.Liquid injection port is closed, capacitor product is formed, the wherein mass fraction of carbon nanomaterial is 20%.
It can be operated at 4V, the capacitance based on carbon nanomaterial is 105F/g.
Embodiment 4
It is 0.7nm with thickness, lamella area is 1 μm2Graphene and a diameter of 1nm, draw ratio be 30 carbon nanotube
Mixture be electrode material, the mass ratio of the two is 1:1. in il electrolyte (the double trifluoros of N- methyl butyls pyrrolidines
Sulfonamide) in, ultrasound 1 minute at 60 DEG C, 1kW forms the slurry that viscosity is 100000 centipoises.Above-mentioned slurry is used
The mode of the mode (0.2MPa) of extruding, making it into carbon-coated foam platinum collector, (mass fraction of carbon is 3%, structure
For Sp2 hydridization.The voidage of collector is 70%, and thickness is 50 μm) hole in, form the compound of electrode material and collector
Structure.By roll-in, the partial electrolyte liquid in above-mentioned composite construction is squeezed out, it is 40 μm to make the thickness of composite construction.It will be above-mentioned
Composite construction is welded with aluminium pole ears.Separated again with diaphragm, multi-disc assembling, encapsulated moulding only stays a liquid injection port.By above-mentioned molding electricity
Container adds electrolyte, makes the matter of all carbon materials and electrolyte in capacitor by dehydration, the conventional procedures such as degassing and aging
Measuring ratio is：1:2.5.Liquid injection port is closed, capacitor product is formed, the wherein mass fraction of carbon nanomaterial is 24%.It can be with
It is operated at 5V, the capacitance based on carbon nanomaterial is 200F/g.
Embodiment 5
The carbon nanotube for being 600 using a diameter of 1.2nm, draw ratio is electrode material, in il electrolyte (1- second
Base -3- methyl tetrafluoro boric acids imidazoles) in, ultrasound 20 minutes at 30 DEG C, 2kW form the slurry that viscosity is 35000 centipoises.It will
The mode for the mode (1MPa) that above-mentioned slurry squeezes, making it into carbon-coated Foam silver collector, (mass fraction of carbon is
2%, structure is Sp2 hydridization.The voidage of collector be 85%, thickness be 200 μm) hole in, formed electrode material with collection
The composite construction of fluid.By roll-in, the partial electrolyte liquid in above-mentioned composite construction is squeezed out, makes the thickness of composite construction be
120μm.By above-mentioned composite construction and silver-colored tab welding.Separated again with diaphragm, multi-disc assembling, encapsulated moulding only stays a liquid injection port.
By above-mentioned shaping capacitor by being dehydrated, the conventional procedures such as degassing and aging add electrolyte, make all carbon materials in capacitor
Mass ratio with electrolyte is：1:2.Liquid injection port is closed, capacitor product is formed, the mass fraction of wherein carbon nanomaterial is
28%.It can be operated at 4V, the capacitance based on carbon nanomaterial is 200F/g.
Embodiment 6
The carbon nanotube for being 1 using a diameter of 200nm, draw ratio is electrode material, in il electrolyte (two (trifluoros
Sulfonyloxy methyl) 1- ethyl-3-methylimidazoles) in, ultrasound 30 minutes at 40 DEG C, 3kW form the slurry that viscosity is 500000 centipoises
Material.The mode for the mode (2MPa) that above-mentioned slurry is squeezed makes it into the carbon-coated foamed aluminium collector (quality of carbon point
Number is 1%, and structure is Sp2 hydridization.The voidage of collector be 96%, thickness be 400 μm) hole in, formed electrode material
With the composite construction of collector.By roll-in, the partial electrolyte liquid in above-mentioned composite construction is squeezed out, the thickness of composite construction is made
It is 280 μm.Above-mentioned composite construction and aluminium pole ears are welded.Separated again with diaphragm, multi-disc assembling, encapsulated moulding only stays a fluid injection
Mouthful.By above-mentioned shaping capacitor by being dehydrated, the conventional procedures such as degassing and aging add electrolyte, make all carbon in capacitor
The mass ratio of material and electrolyte is 1:2.Liquid injection port is closed, capacitor product, the wherein quality of carbon nanomaterial point are formed
Number is 25%.It can be operated at 3.5V, the capacitance based on carbon nanomaterial is 130F/g.
Claims (7)
1. a kind of ultracapacitor, which is characterized in that the electrode material of the ultracapacitor is carbon nanomaterial, and collector is
Carbon-coated foam metal, mass fraction of the carbon nanomaterial in ultracapacitor are 20-35%；The carbon-coated foam
The mass fraction of carbon is 0.1-5%, structure Sp in metal2Hydridization；The voidage of collector is 70-96%, thickness 50-
500μm。
2. ultracapacitor according to claim 1, which is characterized in that the carbon nanomaterial, including carbon nanotube
With graphene, the two is mixed with arbitrary proportion；The wherein a diameter of 0.6-200nm, draw ratio 1-1000 of carbon nanotube；
Wherein the thickness of graphene is 0.35-5nm, and lamella area is 0.001-25 μm2。
3. ultracapacitor according to claim 1, which is characterized in that in the foam metal metal be aluminium, copper, nickel,
Silver or platinum.
4. a kind of method preparing any one of claims 1 to 3 ultracapacitor, it is characterised in that：Include the following steps：
Step 1：The carbon nanomaterial is added in electrolyte, ultrasound 1-30 minutes at 20-60 DEG C, 1-3kW, is formed
Viscosity is the slurry of 15000-500000 centipoises；
Step 2：The mode that above-mentioned slurry is squeezed or vacuumized, makes it into the hole of collector, forms electrode material
With the composite construction of collector；
Step 3：By roll-in, the partial electrolyte liquid in above-mentioned composite construction is squeezed out, it is 20-400 μ to make the thickness of composite construction
m；
Step 4：Step 3 gained composite construction is fixed with metal tabs with conductive silver glue, and is welded；Separated again with diaphragm, it is more
Piece assembles, and is then packaged molding, only stays a liquid injection port, obtain shaping capacitor；
Step 5：By above-mentioned shaping capacitor by being dehydrated, degassing and Aging Step add electrolyte, make all carbon in capacitor
The mass ratio of material and electrolyte is：1:1.2~1:3；
Step 6：Liquid injection port is closed, capacitor product, wherein mass fraction of the carbon nanomaterial in ultracapacitor are formed
For 20-35%.
5. according to the method described in claim 4, it is characterized in that：The pressure squeezed described in step 2 is 0.2-1MPa；The pumping
The vacuum degree of vacuum is 10-1-10-2Pa。
6. according to the method described in claim 4, it is characterized in that：The material of metal tabs described in step 4 be aluminium, silver, copper or
Iron.
7. according to the method described in claim 4, it is characterized in that, electrolyte described in step 1 is aqueous electrolyte, organic electrolysis
Liquid or il electrolyte, being capable of 1-5V operations.
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