CN1971786A - An electrochemical capacitor electrode material and its preparing method - Google Patents
An electrochemical capacitor electrode material and its preparing method Download PDFInfo
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- CN1971786A CN1971786A CNA2005100478033A CN200510047803A CN1971786A CN 1971786 A CN1971786 A CN 1971786A CN A2005100478033 A CNA2005100478033 A CN A2005100478033A CN 200510047803 A CN200510047803 A CN 200510047803A CN 1971786 A CN1971786 A CN 1971786A
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- 239000007772 electrode material Substances 0.000 title claims abstract description 46
- 239000003990 capacitor Substances 0.000 title claims abstract description 42
- 238000000034 method Methods 0.000 title claims abstract description 16
- 239000000463 material Substances 0.000 claims abstract description 20
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 15
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims abstract description 14
- 239000000203 mixture Substances 0.000 claims abstract description 14
- 230000007062 hydrolysis Effects 0.000 claims abstract description 13
- 238000006460 hydrolysis reaction Methods 0.000 claims abstract description 13
- 150000001875 compounds Chemical class 0.000 claims abstract description 9
- 238000001035 drying Methods 0.000 claims abstract description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-M hydroxide Chemical compound [OH-] XLYOFNOQVPJJNP-UHFFFAOYSA-M 0.000 claims abstract description 8
- 229910052759 nickel Inorganic materials 0.000 claims abstract description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 17
- 238000001556 precipitation Methods 0.000 claims description 16
- 239000011148 porous material Substances 0.000 claims description 13
- 229910052799 carbon Inorganic materials 0.000 claims description 11
- 238000002360 preparation method Methods 0.000 claims description 10
- 239000003153 chemical reaction reagent Substances 0.000 claims description 9
- 230000000694 effects Effects 0.000 claims description 8
- 229910052723 transition metal Inorganic materials 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 7
- 238000011175 product filtration Methods 0.000 claims description 7
- 150000003839 salts Chemical class 0.000 claims description 7
- 229910021393 carbon nanotube Inorganic materials 0.000 claims description 6
- 239000002041 carbon nanotube Substances 0.000 claims description 6
- 229910017052 cobalt Inorganic materials 0.000 claims description 6
- 239000010941 cobalt Substances 0.000 claims description 6
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 claims description 6
- 238000011065 in-situ storage Methods 0.000 claims description 6
- 239000002244 precipitate Substances 0.000 claims description 6
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims description 5
- 239000004202 carbamide Substances 0.000 claims description 5
- 239000003610 charcoal Substances 0.000 claims description 5
- 239000002994 raw material Substances 0.000 claims description 5
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 4
- KBJMLQFLOWQJNF-UHFFFAOYSA-N nickel(ii) nitrate Chemical compound [Ni+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O KBJMLQFLOWQJNF-UHFFFAOYSA-N 0.000 claims description 4
- ATRRKUHOCOJYRX-UHFFFAOYSA-N Ammonium bicarbonate Chemical compound [NH4+].OC([O-])=O ATRRKUHOCOJYRX-UHFFFAOYSA-N 0.000 claims description 3
- MQRWBMAEBQOWAF-UHFFFAOYSA-N acetic acid;nickel Chemical compound [Ni].CC(O)=O.CC(O)=O MQRWBMAEBQOWAF-UHFFFAOYSA-N 0.000 claims description 3
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 3
- 239000003575 carbonaceous material Substances 0.000 claims description 3
- UFMZWBIQTDUYBN-UHFFFAOYSA-N cobalt dinitrate Chemical compound [Co+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O UFMZWBIQTDUYBN-UHFFFAOYSA-N 0.000 claims description 3
- 229910001981 cobalt nitrate Inorganic materials 0.000 claims description 3
- 239000002131 composite material Substances 0.000 claims description 3
- 229910021392 nanocarbon Inorganic materials 0.000 claims description 3
- 229940078494 nickel acetate Drugs 0.000 claims description 3
- 239000012286 potassium permanganate Substances 0.000 claims description 3
- XMWRBQBLMFGWIX-UHFFFAOYSA-N C60 fullerene Chemical class C12=C3C(C4=C56)=C7C8=C5C5=C9C%10=C6C6=C4C1=C1C4=C6C6=C%10C%10=C9C9=C%11C5=C8C5=C8C7=C3C3=C7C2=C1C1=C2C4=C6C4=C%10C6=C9C9=C%11C5=C5C8=C3C3=C7C1=C1C2=C4C6=C2C9=C5C3=C12 XMWRBQBLMFGWIX-UHFFFAOYSA-N 0.000 claims description 2
- 229910021586 Nickel(II) chloride Inorganic materials 0.000 claims description 2
- RCEAADKTGXTDOA-UHFFFAOYSA-N OS(O)(=O)=O.CCCCCCCCCCCC[Na] Chemical compound OS(O)(=O)=O.CCCCCCCCCCCC[Na] RCEAADKTGXTDOA-UHFFFAOYSA-N 0.000 claims description 2
- 229920003171 Poly (ethylene oxide) Polymers 0.000 claims description 2
- 150000001450 anions Chemical class 0.000 claims description 2
- 229920001400 block copolymer Polymers 0.000 claims description 2
- 239000002134 carbon nanofiber Substances 0.000 claims description 2
- 150000001768 cations Chemical class 0.000 claims description 2
- PHFQLYPOURZARY-UHFFFAOYSA-N chromium trinitrate Chemical compound [Cr+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O PHFQLYPOURZARY-UHFFFAOYSA-N 0.000 claims description 2
- 229940011182 cobalt acetate Drugs 0.000 claims description 2
- QAHREYKOYSIQPH-UHFFFAOYSA-L cobalt(II) acetate Chemical compound [Co+2].CC([O-])=O.CC([O-])=O QAHREYKOYSIQPH-UHFFFAOYSA-L 0.000 claims description 2
- LQZZUXJYWNFBMV-UHFFFAOYSA-N dodecan-1-ol Chemical class CCCCCCCCCCCCO LQZZUXJYWNFBMV-UHFFFAOYSA-N 0.000 claims description 2
- 229910003472 fullerene Inorganic materials 0.000 claims description 2
- 239000007788 liquid Substances 0.000 claims description 2
- 229910021645 metal ion Inorganic materials 0.000 claims description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 2
- QMMRZOWCJAIUJA-UHFFFAOYSA-L nickel dichloride Chemical compound Cl[Ni]Cl QMMRZOWCJAIUJA-UHFFFAOYSA-L 0.000 claims description 2
- LGQLOGILCSXPEA-UHFFFAOYSA-L nickel sulfate Chemical compound [Ni+2].[O-]S([O-])(=O)=O LGQLOGILCSXPEA-UHFFFAOYSA-L 0.000 claims description 2
- 229910000363 nickel(II) sulfate Inorganic materials 0.000 claims description 2
- -1 polyoxyethylene Polymers 0.000 claims description 2
- 238000009938 salting Methods 0.000 claims description 2
- 239000002086 nanomaterial Substances 0.000 claims 1
- 239000002736 nonionic surfactant Substances 0.000 claims 1
- 230000005540 biological transmission Effects 0.000 abstract description 3
- 239000007795 chemical reaction product Substances 0.000 abstract description 2
- 239000003795 chemical substances by application Substances 0.000 abstract 3
- 230000008021 deposition Effects 0.000 abstract 3
- 230000003647 oxidation Effects 0.000 abstract 2
- 238000007254 oxidation reaction Methods 0.000 abstract 2
- 150000001868 cobalt Chemical class 0.000 abstract 1
- 238000001816 cooling Methods 0.000 abstract 1
- 239000002184 metal Substances 0.000 abstract 1
- 229910052751 metal Inorganic materials 0.000 abstract 1
- 229910052705 radium Inorganic materials 0.000 abstract 1
- HCWPIIXVSYCSAN-UHFFFAOYSA-N radium atom Chemical compound [Ra] HCWPIIXVSYCSAN-UHFFFAOYSA-N 0.000 abstract 1
- 229910000480 nickel oxide Inorganic materials 0.000 description 8
- GNRSAWUEBMWBQH-UHFFFAOYSA-N oxonickel Chemical compound [Ni]=O GNRSAWUEBMWBQH-UHFFFAOYSA-N 0.000 description 8
- 238000009826 distribution Methods 0.000 description 5
- 239000003792 electrolyte Substances 0.000 description 5
- 150000002500 ions Chemical class 0.000 description 5
- 150000002815 nickel Chemical class 0.000 description 5
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 description 4
- 238000004146 energy storage Methods 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- 238000011282 treatment Methods 0.000 description 3
- IEQAICDLOKRSRL-UHFFFAOYSA-N 2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-[2-(2-dodecoxyethoxy)ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethoxy]ethanol Chemical compound CCCCCCCCCCCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCOCCO IEQAICDLOKRSRL-UHFFFAOYSA-N 0.000 description 2
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 230000005611 electricity Effects 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 2
- 229910052757 nitrogen Inorganic materials 0.000 description 2
- LZZYPRNAOMGNLH-UHFFFAOYSA-M Cetrimonium bromide Chemical compound [Br-].CCCCCCCCCCCCCCCC[N+](C)(C)C LZZYPRNAOMGNLH-UHFFFAOYSA-M 0.000 description 1
- VYZAMTAEIAYCRO-UHFFFAOYSA-N Chromium Chemical compound [Cr] VYZAMTAEIAYCRO-UHFFFAOYSA-N 0.000 description 1
- DGAQECJNVWCQMB-PUAWFVPOSA-M Ilexoside XXIX Chemical compound C[C@@H]1CC[C@@]2(CC[C@@]3(C(=CC[C@H]4[C@]3(CC[C@@H]5[C@@]4(CC[C@@H](C5(C)C)OS(=O)(=O)[O-])C)C)[C@@H]2[C@]1(C)O)C)C(=O)O[C@H]6[C@@H]([C@H]([C@@H]([C@H](O6)CO)O)O)O.[Na+] DGAQECJNVWCQMB-PUAWFVPOSA-M 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- PMZURENOXWZQFD-UHFFFAOYSA-L Sodium Sulfate Chemical compound [Na+].[Na+].[O-]S([O-])(=O)=O PMZURENOXWZQFD-UHFFFAOYSA-L 0.000 description 1
- 238000009825 accumulation Methods 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 238000013019 agitation Methods 0.000 description 1
- 239000003125 aqueous solvent Substances 0.000 description 1
- 238000000498 ball milling Methods 0.000 description 1
- 229910052804 chromium Inorganic materials 0.000 description 1
- 239000011651 chromium Substances 0.000 description 1
- 238000004140 cleaning Methods 0.000 description 1
- 229910000428 cobalt oxide Inorganic materials 0.000 description 1
- IVMYJDGYRUAWML-UHFFFAOYSA-N cobalt(ii) oxide Chemical compound [Co]=O IVMYJDGYRUAWML-UHFFFAOYSA-N 0.000 description 1
- 238000000748 compression moulding Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 239000006185 dispersion Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910052742 iron Inorganic materials 0.000 description 1
- 229910052748 manganese Inorganic materials 0.000 description 1
- 239000011572 manganese Substances 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000001338 self-assembly Methods 0.000 description 1
- 238000005245 sintering Methods 0.000 description 1
- 229910052708 sodium Inorganic materials 0.000 description 1
- 239000011734 sodium Substances 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- HFQQZARZPUDIFP-UHFFFAOYSA-M sodium;2-dodecylbenzenesulfonate Chemical compound [Na+].CCCCCCCCCCCCC1=CC=CC=C1S([O-])(=O)=O HFQQZARZPUDIFP-UHFFFAOYSA-M 0.000 description 1
- 238000003860 storage Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 239000004094 surface-active agent Substances 0.000 description 1
Images
Classifications
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- 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
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- Electric Double-Layer Capacitors Or The Like (AREA)
Abstract
This invention relates to electrochemical capacitor electrode materials and process method, wherein, the compound materials comprises nickel or cobalt salt or other transmission compound, deposition agent, hole process agent, water with quality proportion as 1:1-20: 0.1-5:1-100; Through water solution to combine original deposition and self combination method to directly grow hole oxidation materials to get capacitor electrode materials; the materials pass mixture hydrolysis, deposition agent under 100 to 300 degrees to make transmission metal icon to form hydroxide for cooling and drying reaction product to process middle hole structure oxidation with hole radium as 5 to 10 nm and surface area as 100 to 300 m2/g.
Description
Technical field
The present invention relates to electrochemical capacitor electrode material improvement technology, a kind of novel electrochemical capacitor electrode material and preparation method thereof is provided especially.
Background technology
Along with a large amount of uses of the mankind to fossil energy, the fossil energy deposit is day by day short, environmental pollution is serious day by day, a kind of cleaning of an urgent demand and the reproducible energy.Electrochemical capacitor has the capacitor of microfarad or pico farad order of magnitude capacity and a kind of energy-storage travelling wave tube between the high energy density cells between tradition and receives very big concern as a kind of, it can provide bigger energy density and power density, can be used as free of contamination small-sized back-up source and be used for multiple electric equipment, also be expected to form electric power system and in electric automobile, back-up source and accumulation power supply, play a great role in high energy density cells.Electrochemical capacitor comes storage of electrical energy by forming electric double layer process or accurate Faradic electricity chemical reaction, and environmentally safe is the energy-storage travelling wave tube of green energy resource.Therefore, develop a kind of larger capacity, to have a good electrochemical capacitor of excellent instantaneous charge-discharge performance, cyclicity very urgent.
Because the pore structure and the specific area utilization ratio of electrochemical capacitor have very big influence to its power density and energy density, therefore having proper pore structure can make ion transfer unobstructed, having very the high electrochemical activity surface can effective charge assemble and transmission course, helps improving power density, the energy density of electrochemical capacitor.Therefore how improving the pore structure distribution of electrochemical capacitor electrode material and the utilization ratio of increasing specific surface area is to improve the key factor of electrochemical capacitor performance.At present, the electrode material of electrochemical capacitor adopts the active carbon of high-specific surface area more, is unfavorable for ion transfer but the active carbon hole is the micropore of molecular level, and its effective ratio area is lower, thereby influences the further raising of power density; Active carbon electrode material is by electric double layer principle store electrical energy simultaneously, and energy density is far below the energy storage mode of accurate Faradic electricity chemical reaction.Thereby limited the raising of electrochemical capacitor power density and energy density.
Summary of the invention
In order further to improve electrochemical power density and energy density, the object of the present invention is to provide a kind of novel electrochemical capacitor electrode material and preparation method thereof, electrochemical capacitor electrode material has very high power density and energy density; The present invention by in water solution system in conjunction with orifice oxide in in-situ precipitate and the self-assembling method direct growth, with middle orifice oxide and with the compound capacitor electrode material that obtains of electrode material such as active carbon.The electrochemical capacitor of this electrode material preparation has very high specific area and suitable ion transfer passage, has obtained high electrochemical power density and energy density.
Technical scheme of the present invention is:
A kind of electrochemical capacitor electrode material, the raw material of this composite material comprises the salt of nickel or cobalt or compound, precipitation reagent, pore creating material, the water of other magnesium-yttrium-transition metals, mass ratio is 1: (1-20): (0.1-5): (1-100), by in water solution system, obtaining capacitor electrode material in conjunction with orifice oxide material in in-situ precipitate and the self-assembling method direct growth, its aperture is 5～10nm, and specific area is 100～300m
2/ g; Orifice oxide and methods such as other electrode material ball millings or mechanical agitation are evenly disperseed in maybe will obtaining, and the mass ratio of middle orifice oxide and other electrode materials is 1: (0.1-10), obtain the recombiner condenser electrode material.
Described other electrode materials are active carbon, zero dimension (referring to that various fullerenes and diameter are at 1-50 nanometer charcoal ball) or nano carbon material in one dimension (refer to the fibrous raw material of wood-charcoal material of diameter below 500 nanometers, comprise CNT (carbon nano-tube) and carbon nano-fiber).
The preparation method of described electrochemical capacitor electrode material, by in water solution system, obtaining capacitor electrode material in conjunction with orifice oxide material in in-situ precipitate and the self-assembling method direct growth, in maybe will obtaining orifice oxide and with the compound capacitor electrode material that obtains of electrode material such as active carbon.Concrete process is:
With the suitable combination thing of the salt of nickel or cobalt and other magnesium-yttrium-transition metals (as iron, chromium, manganese etc., as nickel nitrate, nickel acetate, nickel chloride, nickelous sulfate, cobalt acetate, cobalt nitrate, ferric nitrate, chromic nitrate, potassium permanganate etc.), precipitation reagent (ammoniacal liquor, urea, weak base such as carbonic acid ammonia or material) with reproducibility, pore creating material (block copolymer, as polyoxyethylene (P123) etc., the anion/cation surfacant, as sour sodium, neopelex (SDBS), lauryl sodium sulfate (SDS), softex kw (CTMAB) etc., nonionic is given birth to surfactant, as ethoxylated dodecyl alcohol (Brij30) etc.), evenly mix (the suitable combination thing of the salt of nickel or cobalt and other magnesium-yttrium-transition metals wherein of dissolving fully according to a certain percentage, precipitation reagent, the mass ratio range of pore creating material and aqueous solvent is 1: 1-20: 0.1-5: 1-100), then under 100-300 ℃ of airtight condition with the mixture hydrolysis, under the precipitation reagent effect, make the metal ion in the magnesium-yttrium-transition metal salting liquid form its hydroxide or oxide precipitation, cool to room temperature with the product filtration drying after, at 100-500 ℃ of heat treatment 1-10 hour, just can obtain the central hole structure oxide.Wherein can control specific area and the pore-size distribution that obtains end product by the ratio of regulating salt and pore creating material.
By top in-situ precipitate and self-assembling method process, can obtain the aperture is 5～10nm, and specific area is 100～300m
2/ g metal oxide, this oxide has good electrochemical properties, can be directly used in the electrode material of electrochemical capacitor, or evenly disperse to obtain recombiner condenser electrode material, the specific area that electrode material is high and suitable ion transfer passage with middle orifice oxide and with active carbon, zero dimension or nano carbon material in one dimension simultaneously.
Advantage of the present invention is:
The invention relates to a kind of preparation method who improves electrochemical capacitor electrode electrochemically active specific surface area electrode material and composite material thereof, this electrochemical capacitor by on collector electrode directly the middle orifice oxide of compression moulding high-specific surface area as electrochemical capacitor electrode material.Main feature of the present invention is by orifice oxide material in water solution system in-situ precipitate and the self assembly associated methods direct growth, this oxide has very high electrode electro Chemical active area and suitable ion transfer passage, with it is electrode material or compound with other electrode material (as active carbon, CNT (carbon nano-tube) etc.), can obtain high electrochemical energy metric density and power density electrochemical capacitor, the aperture is 5～10nm, and specific area is 100～300m
2/ g.
Description of drawings
Fig. 1 is the XRD curve of the primary sample and the mesopore nickel oxide sample of different sintering temperatures processing.
Fig. 2 is the SEM photo of mesopore nickel oxide.
Fig. 3 is the nitrogen adsorption isotherm (a) and the pore structure distribution curve (b) of mesopore nickel oxide after the treatment of different temperature.
Embodiment
Below in conjunction with embodiment the present invention is further described.
Embodiment 1
Nickel nitrate, urea, P123, water were according to mass ratio 1: 2: 3: 10 mix dissolving fully, mixture hydrolysis under 200 ℃ of airtight conditions then, under the weak base effect, make the nickel salt hydrolysis form its precipitation of hydroxide, cool to room temperature with the product filtration drying after, 100 ℃ of heat treatments 1.5 hours, just can obtain the nickel oxide of central hole structure, its aperture is 4nm, and specific area is 260m
2/ g.Treatment of different temperature obtains the XRD result such as the accompanying drawing 1 of sample, morphology observation such as accompanying drawing 2, and adsorption curve and pore-size distribution are electrode material with it, are electrolyte with 6M KOH, are assembled into electrochemical capacitor then, specific capacity can reach 120F/g.
Embodiment 2
Nickel nitrate, urea, P123, water were according to mass ratio 1: 2: 3: 10 mix dissolving fully, mixture hydrolysis under 200 ℃ of airtight conditions then, under the weak base effect, make the nickel salt hydrolysis form its precipitation of hydroxide, cool to room temperature with the product filtration drying after, 250 ℃ of heat treatments 5 hours, just can obtain the nickel oxide of central hole structure, its aperture is 6nm, and specific area is 190m
2/ g.(the BET specific area is 2000m with mesopore nickel oxide+active carbon
2/ g) be active material, with its even dispersion, the two mass ratio is 1: 1, obtains the recombiner condenser electrode material, is electrolyte with 6M KOH, is assembled into electrochemical capacitor then, specific capacity can reach 290F/g.
Embodiment 3
Cobalt nitrate, urea, P123 and water were according to mass ratio 1: 5: 1: 20 mix dissolving fully, mixture hydrolysis under 100 ℃ of airtight conditions then, under the weak base effect, make the nickel salt hydrolysis form its precipitation of hydroxide, cool to room temperature with the product filtration drying after, 450 ℃ of heat treatments 7 hours, just can obtain the cobalt oxide of central hole structure, its aperture is 8nm, and specific area is 245m
2/ g.With it is electrode material, is electrolyte with 6M KOH, is assembled into electrochemical capacitor then, and specific capacity can reach 180F/g.
Embodiment 4
Nickel acetate, ammoniacal liquor, neopelex, water were according to mass ratio 1: 9: 0.5: 90 mix dissolving fully, mixture hydrolysis under 270 ℃ of airtight conditions then, under the weak base effect, make the nickel salt hydrolysis form its precipitation of hydroxide, cool to room temperature with the product filtration drying after, 200 ℃ of heat treatments 9 hours, just can obtain the nickel oxide of central hole structure, its aperture is 5nm, and specific area is 270m
2/ g.With it is electrode material, is electrolyte with 6M KOH, is assembled into electrochemical capacitor then, and specific capacity can reach 200F/g.
Embodiment 5
Potassium permanganate, carbonic acid ammonia, Brij30, water were according to mass ratio 1: 15: 1: 10 mix dissolving fully, mixture hydrolysis under 200 ℃ of airtight conditions then, under the weak base effect, make the nickel salt hydrolysis form its precipitation of hydroxide, cool to room temperature with the product filtration drying after, 200 ℃ of heat treatments 5 hours, just can obtain the manganese oxide of central hole structure, its aperture is 5.5nm, and specific area is 150m
2/ g.With it is electrode material, is electrolyte with 6M KOH, is assembled into electrochemical capacitor then, and specific capacity can reach 135F/g.
Fig. 3 is the nitrogen adsorption isotherm (a) and the pore structure distribution curve (b) of mesopore nickel oxide after the treatment of different temperature.
Claims (6)
1, a kind of electrochemical capacitor electrode material, it is characterized in that: the raw material of this composite material comprises the salt of nickel or cobalt or compound, precipitation reagent, pore creating material, the water of other magnesium-yttrium-transition metals, mass ratio is 1: 1-20: 0.1-5: 1-100, by in water solution system, obtaining capacitor electrode material in conjunction with orifice oxide material in in-situ precipitate and the self-assembling method direct growth, its aperture is 5～10nm, and specific area is 100～300m
2/ g; Orifice oxide and other electrode materials evenly disperse in maybe will obtaining, and mass ratio is 1: 0.1-10 obtains the recombiner condenser electrode material.
2, according to the described electrochemical capacitor electrode material of claim 1, it is characterized in that: described other electrode materials are active carbon, zero dimension or an awl carbon nano-material; Zero-dimension nano raw material of wood-charcoal material refers to various fullerenes and diameter at 1-50 nanometer charcoal ball, and nano carbon material in one dimension refers to the fibrous raw material of wood-charcoal material of diameter below 500 nanometers, comprises CNT (carbon nano-tube) and carbon nano-fiber.
3, preparation method according to the described electrochemical capacitor electrode material of claim 1, it is characterized in that: with the salt of nickel or cobalt or the compound of other magnesium-yttrium-transition metals, precipitation reagent, pore creating material, water evenly mixes dissolving fully according to mass ratio 1: 1-10: 0.1-5: 1-100, then under 100-300 ℃ of airtight condition with the mixture hydrolysis, under the precipitation reagent effect, make the metal ion in the magnesium-yttrium-transition metal salting liquid form its hydroxide or oxide precipitation, cool to room temperature with the product filtration drying after, at 100-500 ℃ of heat treatment 1-10 hour, obtaining the aperture was 5～10nm, specific area is 100～300m
2The central hole structure oxide of/g; Described precipitation reagent is weak base or material with reproducibility, and described pore creating material is block copolymer, anion/cation surfacant or nonionic surfactant.
4, according to the preparation method of the described electrochemical capacitor electrode material of claim 3, it is characterized in that: the salt of described nickel or cobalt or the compound of other magnesium-yttrium-transition metals are nickel nitrate, nickel acetate, nickel chloride, nickelous sulfate, cobalt acetate, cobalt nitrate, ferric nitrate, chromic nitrate or potassium permanganate.
5, according to the preparation method of the described electrochemical capacitor electrode material of claim 3, it is characterized in that: described precipitation reagent is ammoniacal liquor, urea or carbonic acid ammonia.
6, according to the preparation method of the described electrochemical capacitor electrode material of claim 3, it is characterized in that: described pore creating material is polyoxyethylene, neopelex, lauryl sodium sulfate, softex kw or ethoxylated dodecyl alcohol.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100478033A CN100533618C (en) | 2005-11-25 | 2005-11-25 | An electrochemical capacitor electrode material and its preparing method |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100478033A CN100533618C (en) | 2005-11-25 | 2005-11-25 | An electrochemical capacitor electrode material and its preparing method |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1971786A true CN1971786A (en) | 2007-05-30 |
| CN100533618C CN100533618C (en) | 2009-08-26 |
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| Application Number | Title | Priority Date | Filing Date |
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| CNB2005100478033A Expired - Fee Related CN100533618C (en) | 2005-11-25 | 2005-11-25 | An electrochemical capacitor electrode material and its preparing method |
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Cited By (6)
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| CN104882291A (en) * | 2015-04-14 | 2015-09-02 | 西北师范大学 | Super capacitor electrode material, preparation method and application thereof |
| CN105754560A (en) * | 2016-02-03 | 2016-07-13 | 易达（福建）旅游集团有限公司 | Self-heating hot compress material and preparation method thereof |
| CN106057486A (en) * | 2016-05-11 | 2016-10-26 | 温州大学 | Carbon sphere-Fe oxide composite material and preparation method and use thereof |
| CN106531466A (en) * | 2016-11-18 | 2017-03-22 | 桂林电子科技大学 | Preparation method for three-element oxide composite material and application |
| CN107331878A (en) * | 2017-05-31 | 2017-11-07 | 惠州亿纬锂能股份有限公司 | Lithium manganese dioxide cell positive pole pore creating material, the porous anode using its preparation |
| CN111153448A (en) * | 2019-12-27 | 2020-05-15 | 中南林业科技大学 | Preparation method and application of bamboo/wood-based nano-cellulose limited transition metal oxide electrode material |
Family Cites Families (2)
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| US20040047798A1 (en) * | 2000-05-24 | 2004-03-11 | Oh Seung Mo | Mesoporous carbon material, carbon/metal oxide composite materials, and electrochemical capacitors using them |
| CN100359613C (en) * | 2003-11-18 | 2008-01-02 | 哈尔滨工程大学三金高新技术有限责任公司 | Method for making metal oxide/carbon electrochemical capacitor and electrode |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104882291A (en) * | 2015-04-14 | 2015-09-02 | 西北师范大学 | Super capacitor electrode material, preparation method and application thereof |
| CN104882291B (en) * | 2015-04-14 | 2018-04-06 | 西北师范大学 | A kind of electrode material for super capacitor and its preparation method and application |
| CN105754560A (en) * | 2016-02-03 | 2016-07-13 | 易达（福建）旅游集团有限公司 | Self-heating hot compress material and preparation method thereof |
| CN106057486A (en) * | 2016-05-11 | 2016-10-26 | 温州大学 | Carbon sphere-Fe oxide composite material and preparation method and use thereof |
| CN106531466A (en) * | 2016-11-18 | 2017-03-22 | 桂林电子科技大学 | Preparation method for three-element oxide composite material and application |
| CN106531466B (en) * | 2016-11-18 | 2018-10-19 | 桂林电子科技大学 | A kind of preparation and application of ternary oxide composite material |
| CN107331878A (en) * | 2017-05-31 | 2017-11-07 | 惠州亿纬锂能股份有限公司 | Lithium manganese dioxide cell positive pole pore creating material, the porous anode using its preparation |
| CN111153448A (en) * | 2019-12-27 | 2020-05-15 | 中南林业科技大学 | Preparation method and application of bamboo/wood-based nano-cellulose limited transition metal oxide electrode material |
| CN111153448B (en) * | 2019-12-27 | 2022-07-15 | 中南林业科技大学 | Preparation method and application of bamboo/wood-based nano-cellulose limited transition metal oxide electrode material |
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