CN102543459B - Basic cobalt nitrate/ordered mesopore carbon combination electrode material and preparation method thereof - Google Patents
Basic cobalt nitrate/ordered mesopore carbon combination electrode material and preparation method thereof Download PDFInfo
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Abstract
The invention provides a basic cobalt nitrate/ordered mesopore carbon combination electrode material and a preparation method thereof. The combination electrode material comprises the following components by weight percent: 0-50% of metal oxide, 10-50% of basic cobalt nitrate, and 1-90% of ordered mesopore carbon; the metal oxide is one or more than one of NiO, SnO2 or Fe3O4, and the structure general formula of the basic cobalt nitrate is Co(OxHy)NO3; and x is 0.1-9, and y is 0.1-12. According to the invention, a one-step method is utilized for preparation, the process is simple, the cost is low, and the combination electrode material is suitable for industrialization production. The specific capacitance of a single electrode is 660-1200F/g, the energy density of the single electrode is 1000-3000 Wh/kg; and the preparation of the combination electrode material can be carried out in inorganic water system electrolyte KOH, and is pollution-free and high in security, and the combination electrode material is utilized as an electrode material of a super capacitor, and can be used for greatly improving the energy density of the capacitor.
Description
Technical field
The present invention relates to a kind of preparation method for composite electrode material for super capacitor.
Technical background
The energy is the power of the national economic development, is also the important indicator of weighing national overall national strength, Civilization development degree and living standard.Follow the sharp increase of population and economic developing rapidly, the energy is shortage day by day, and environment comes into one's own day by day, carries out the exploitation of the energy and rationally utilizes the sustainable development that is directly connected to human society, the emphasis of Ye Shi various countries research.Electric energy is being played the part of very important role as a kind of important energy in modern production and life.Energy-storage travelling wave tube is applied to the various aspects of productive life, also more and more higher to the performance requirement of energy-storage travelling wave tube.Although traditional capacitor can provide very large power, its energy density is limited, can not meet actual needs.Along with science and technology and social development, many occasions (as electric automobile) are more and more higher to the requirement of power, also far beyond the ability to bear of current battery simultaneously.Under this background, a kind of novel energy-storage travelling wave tube-" ultracapacitor " is developed rapidly.
Ultracapacitor (Supercapacitor), is also electrochemical capacitor (Electrochemicalacitor), is a kind of energy density and the power density novel energy-storing element between traditional capacitor and battery.It has the features such as the long and serviceability temperature wide ranges of the ratio electric capacity larger than traditional capacitor, the power density larger than storage battery, service life cycle.Ultracapacitor 20th century six the seventies first occur in the U.S., and move towards gradually market in the eighties, because the potential prospect on electric automobile causes concern, and develop rapidly along with the development of electric automobile, become the focus of domestic and international research.Since 1957 (USP, 2800616) Becker has delivered one piece of patent about ultracapacitor, the development of ultracapacitor is constantly weeded out the old and bring forth the new.Nowadays, ultracapacitor oneself be widely used in the power set of memory protect, portable electric appts and oligosaprobic hybrid automobile of Circuits System.It has wide application prospects in the various fields such as hybrid-electric car, mobile phone, microcomputer.
Since 1992, USDOE and United States advanced battery association just started to organize National Laboratory, university and industrial quarters (Maxwell, GE etc.) to release the feasibility study plan of ultracapacitor used for electric vehicle; 2009, the U.S.'s " next generation " battery and electric motor car plan: national energy portion subsidizes 2,400,000,000 dollars, and wherein 1,500,000,000 dollars subsidize battery and the accessory manufacture thereof of the U.S., to improve the circulation volume of battery.2000, Germany formulated " Renewable Energy Law " regulation new forms of energy account for Germany all energy consumptions 50%, German electric automobile is planned at the year two thousand twenty, reaches 1,000,000 electric automobiles and becomes the leader of electric automobile market.1996, European Union started the project of ultracapacitor, and target is development specific energy 6Wh/kg, 8Wh/L, and specific power 1.5kW/kg, 2kW/L, cycle life exceedes the ultracapacitor of 100,000 times.
Electrode material is ultracapacitor core component, and its properity has conclusive effect to the performance of ultracapacitor.Electrode material is divided into four classes: Carbon Materials, metal oxide, high molecular polymer and composite material.
Carbon Materials (active carbon, carbon nano-tube, carbon nanocoils, carbon gel, carbon fiber etc.) is the electrode material that ultracapacitor is conventional, and according to electric double layer theory, the electric double layer capacitance on carbon resistance rod surface is about 20 μ Fcm
-2if specific area is 1000m
2g
-1, be 200F/g than electric capacity.
In various Carbon Materials, Mesoporous Carbon Materials is owing to having the suitable electrode material as ultracapacitor in larger aperture.Wherein ordered mesoporous Carbon Materials is because its special duct order is conducive to embedding therein of electrolyte ion and deviates to be subject to extensive concern.Take the material with pore structure as template, first carbon precursor is injected in the duct of template, after charing, remove template, a kind of porosu solid material of the structure of pallet repeatedly is just preserved, mesoporous melecular sieves can be controlled pore passage structure and skeleton simultaneously, and the si molecular sieves preparation that can have different pore passage structures by selection has the Mesoporous Carbon Materials of various pore passage structures.There is sucrose in the charcoal source of preparing ordered mesoporous carbon, phenol, formaldehyde resin and furfuryl alcohol.
Due to the electric double layer capacitance that faraday's electric capacity of metal oxide and hydroxides generation produces much larger than active carbon material surface, therefore pseudo capacitance device just progressively replaces double electric layer capacitor becomes the focus of research and development.As RuO
2be subject to common concern owing to thering is very high ratio electric capacity.Although RuO
2specific capacity is up to 760F/g, function admirable aspect capacity and conductivity, but expensive.Because they generally have strong toxicity, environmental pollution is serious again, and the electrode material that people are devoted to find functional, cheap and environmentally safe for this reason substitutes precious metal material.Many achievements in research both domestic and external show: transition metal oxide material can be used as the substitute of metal oxide containing precious metals electrode material.As Conway once pointed out, some transition metal oxides are as MnO
x, NiO
xand CoO
xdeng the chemical property also with metal oxide containing precious metals, all become studied compared with being hopeful to substitute the electrode material of ruthenium.
Research shows, adopt the capacitor of metal oxide/charcoal combination electrode material can bring into play electric double layer and pseudo-capacitance simultaneously, can make full use of electric double layer principle and fake capacitance principle mutually acts synergistically and carries out charge storage, realize the Performance and Cost Modeling of material and coordinate, and there is the new electrode materials of the not available premium properties of unitary electrode material.But, the preparation method based on metal oxide/charcoal combination electrode material capacitor at present, condition is loaded down with trivial details mostly, and metal oxide/charcoal combination electrode material is than electric capacity not high (300F/g left and right) merely, and its performance has much room for improvement.
Recently, some scholar's research metal hydroxides/charcoal combination electrode material, the energy-storage property of finding material has had great breakthrough, trace it to its cause, because fake capacitance or pseudo capacitance are that chemisorbed/desorption that height of formation is reversible or oxidation/reduction reaction produce the electric capacity relevant with electrode charge current potential by electrode surface or the underpotential deposition of active material occurs on the two dimension of body in mutually or accurate two-dimensional space.But owing to lacking free OH in pure metal oxides electrode
-so, OH in reaction
-migration be restricted, can only electrode/electrolyte interface occur redox, show surface reaction mechanism.In course of reaction, only have a part of metallic atom on oxide grain surface that redox reaction can occur.And contain OH in metal hydroxides/charcoal combination electrode
-so, OH in electrochemical reaction
-migration unrestricted, can occur in electrode/electrolyte interface and electrode interior, show surface reaction and internal-response mechanism simultaneously.
Due to the architectural characteristic of electrode material for super capacitor, as closely related with preparation technology in granular size, particle diameter distribution and pattern etc., therefore exploring combination electrode material new preparation process has important meaning.At present, the method for preparing electrode material mainly contains coprecipitation, sol-gel process, electrodeposition process and solvent-thermal method etc.
Under solvent heat condition, the character (density, viscosity, peptizaiton) of solvent influences each other, alter a great deal, and differ greatly under its character and usual conditions, accordingly, the dissolving of reactant, disperseed and chemical reactivity improves greatly or strengthens, this just makes reaction at lower temperature, to occur.Material prepared by solvent-thermal method have active good, purity is high, pattern and the advantage such as granular size is controlled, without through high-temperature calcination, can directly synthesize that particle diameter is little, pattern is regular and the electrochemical active material of good dispersion, is conducive to improve its chemical property.
From the above analysis, the ratio electric capacity of Carbon Materials is lower, and the cost of metal oxide containing precious metals is higher, and business application is more difficult, therefore develops synthesis technique simple, and combination electrode material cheaply, is the problem that people extremely pay close attention to.
Summary of the invention
The object of this invention is to provide a kind of alkali formula cobalt nitrate/ordered mesoporous carbon combination electrode material and preparation method thereof, the above-mentioned defect existing to overcome prior art, meets the needs that relevant field is developed.
Alkali formula cobalt nitrate/ordered mesoporous carbon combination electrode material of the present invention, is made up of the component of following percentage by weight:
Alkali formula cobalt nitrate 10～50%
Ordered mesoporous carbon 1～90%
Described metal oxide is NiO, SnO
2or Fe
3o
4in one or more;
The general structure of described alkali formula cobalt nitrate is Co (O
xh
y) NO
3;
Wherein: x is that 0.1～9, y is 0.1～12; Preferably, x is that 2, y is 3;
The specific area of described ordered mesoporous carbon is 50m
2/ g～3000m
2/ g, total hole volume is 0.5～2cm
3/ g;
The specific area of described combination electrode material is 300m
2/ g～2000m
2/ g, total hole volume is 0.5～2cm
3/ g, pore diameter range is 2nm～10nm;
Preferably, described alkali formula cobalt nitrate/ordered mesoporous carbon combination electrode material, is made up of the component of following percentage by weight:
Nano-metal-oxide 0～10%
Nanometer alkali formula cobalt nitrate 15～20%,
Ordered mesoporous carbon 80～85%
The preparation method of described alkali formula cobalt nitrate/ordered mesoporous carbon combination electrode material, comprises the steps:
React 2～8h by 125～200 ℃ of cabaltous nitrate hexahydrate, ethanol and ordered mesoporous carbons, collect product, 70～80 ℃ dry 1～4 hour, obtain product: i.e. described alkali formula cobalt nitrate/ordered mesoporous carbon combination electrode material;
Nitrate, acetate, sulfate or chloride that described metal soluble-salt is nickel, tin or iron;
The weight content of cabaltous nitrate hexahydrate in ethanol is 10%～50%;
Alkali formula cobalt nitrate/ordered mesoporous carbon combination electrode material of the present invention, can adopt method well known in the art, and preparation becomes electrode slice, is then assembled into capacitor with electrode slice.
Alkali formula cobalt nitrate/ordered mesoporous carbon combination electrode material of the present invention, can adopt the method for Q/CLY 001-2010 standard regulation to detect evaluation.
Ultracapacitor of the present invention is by the advantage of combination electrode material:
Electrode for super capacitor material of the present invention is take cabaltous nitrate hexahydrate, ordered mesoporous carbon as raw material, employing one-step method is prepared from, simple, with low cost, the applicable suitability for industrialized production of this preparation method's technique, by alkali formula cobalt nitrate/ordered mesoporous carbon combination electrode material of the present invention, unipolar is 800～1200F/g than electric capacity, and energy density is 1000～3000Wh/kg; And carry out in water based inorganic electrolyte KOH, pollution-free, safe, adopt the electrode material of alkali formula cobalt nitrate/ordered mesoporous carbon combination electrode material of the present invention as ultracapacitor, can greatly improve the energy density of capacitor.
Accompanying drawing explanation
The X-ray diffractogram of alkali formula cobalt nitrate/ordered mesoporous carbon electrode material for super capacitor in Fig. 1 embodiment 1;
The transmission electron microscope picture of alkali formula cobalt nitrate/ordered mesoporous carbon electrode material for super capacitor in Fig. 2 embodiment 1;
The N of alkali formula cobalt nitrate/ordered mesoporous carbon electrode material for super capacitor in Fig. 3 embodiment 1
2adsorption-desorption thermoisopleth;
The graph of pore diameter distribution of alkali formula cobalt nitrate/ordered mesoporous carbon electrode material for super capacitor in Fig. 4 embodiment 1;
The cyclic voltammogram of alkali formula cobalt nitrate/ordered mesoporous carbon electrode material for super capacitor under different scanning rates in Fig. 5 embodiment 1;
In Fig. 6 embodiment 1 alkali formula cobalt nitrate/ordered mesoporous carbon electrode material for super capacitor under different scanning rates than electric capacity figure;
The constant current charge-discharge figure of alkali formula cobalt nitrate/ordered mesoporous carbon electrode material for super capacitor in Fig. 7 embodiment 1;
The cyclic voltammogram of alkali formula cobalt nitrate/ordered mesoporous carbon electrode material for super capacitor under different scanning rates in Fig. 8 embodiment 2;
The cyclic voltammogram of alkali formula cobalt nitrate/ordered mesoporous carbon electrode material for super capacitor under different scanning rates in Fig. 9 embodiment 3;
The cyclic voltammogram of alkali formula cobalt nitrate-tin oxide/ordered mesoporous carbon electrode material for super capacitor under different scanning rates in Figure 10 embodiment 4;
Embodiment
Below in conjunction with embodiment and accompanying drawing, the invention will be further described, but the present invention is not limited to example below, and the technical scheme that every modification, replacement or change of making based on technology basic thought of the present invention realizes all belongs to scope of the present invention.
Embodiment 1
In embodiment 1, the specific area of ordered mesoporous carbon is 1258m
2/ g, total hole volume is 1.19cm
3/ g, mesopore aperture is 3.78nm;
The specific area of composite material is 711.5m
2/ g, total hole volume is 0.7192cm
3/ g, mesopore aperture is 3.98nm;
Take 0.9058g cabaltous nitrate hexahydrate and be placed in beaker, add 8g ethanol, add 1g ordered mesoporous carbon, reactant is stirred to 2h, pack in 50ml polytetrafluoro reactor, stainless steel sealing is incubated 4h at 175 ℃ of reaction temperatures, collect product and be dried at 80 ℃, obtain described alkali formula cobalt nitrate/ordered mesoporous carbon combination electrode material.In the alkali formula cobalt nitrate/ordered mesoporous carbon combination electrode material being made by said method, alkali formula cobalt nitrate accounts for 20% of combination electrode material total weight.
The XRD figure of the composite material making is as shown in Fig. 1 No. 1.
The structural formula of alkali formula cobalt nitrate is Co (O
2h
3) NO
3;
Transmission electron microscope as shown in Figure 2; N
2adsorption-desorption thermoisopleth as shown in Figure 3; Graph of pore diameter distribution is as Fig. 4; The specific area of product is 778.7m
2g
-1; By the alkali formula cobalt nitrate/ordered mesoporous carbon combination electrode material, conductive carbon black (model BP200) and the adhesive polytetrafluoroethylene (PTFE) that obtain 75: 20: 5 batchings in mass ratio, on magnetic stirring apparatus, make after slurry, be coated in the hydraulic press compacting through 10MPa in nickel foam and make electrode slice.
Conductive carbon black BP200 adopts the product of Cabot Co.,Ltd of the U.S.; Adhesive PTFE adopts the product of Shanghai Sanaifu New Material Co., Ltd;
Adopt three-electrode system, respectively take combination electrode as work electrode, platinized platinum makes auxiliary electrode, saturated calomel electrode (SCE) is reference electrode, carries out cyclic voltammetry at-0.2～0.7V potential region.Take the 6mol/L KOH aqueous solution as electrolyte, the ratio electric capacity that records composite material is 1170F/g under sweep speed 5mV/s.
Fig. 5 is shown in the cyclic voltammetry curve test of the alkali formula cobalt nitrate/ordered mesoporous carbon combination electrode material obtaining under different scanning rates; Than capacitance values as shown in Figure 6; Constant current charge-discharge figure as shown in Figure 7.
Embodiment 2
In embodiment 2, the specific area of ordered mesoporous carbon is 1538m
2/ g, total hole volume is 1.32cm
3/ g, mesopore aperture is 3.95nm;
The specific area of composite material is 778.7m
2/ g, total hole volume is 0.92cm
3/ g, mesopore aperture is 4.70nm;
Take 0.7500g cabaltous nitrate hexahydrate and be placed in beaker, add 8g ethanol, add 1g ordered mesoporous carbon, reactant is stirred to 4h, pack in 50ml polytetrafluoro reactor, stainless steel sealing, at 125 ℃ of reaction temperatures, be incubated 6h, collect product and be dried at 80 ℃, obtain alkali formula cobalt nitrate/ordered mesoporous carbon combination electrode material, alkali formula cobalt nitrate accounts for 17% of combination electrode material total weight.
The general structure of alkali formula cobalt nitrate is Co (O
2h
3) NO
3;
The XRD figure of the combination electrode material making is as shown in Fig. 1 No. 2.
The test of combination electrode material is with embodiment 1, and the ratio electric capacity that records combination electrode material is 1079F/g under sweep speed 5mV/s.Fig. 8 is shown in the cyclic voltammetry curve test of combination electrode material under different scanning rates.
Embodiment 3
In embodiment 3, the specific area of ordered mesoporous carbon is 1258m
2/ g, total hole volume is 1.19cm
3/ g, mesopore aperture is 3.78nm;
The specific area of composite material is 682.3m
2/ g, total hole volume is 0.8cm
3/ g, mesopore aperture is 4.73nm;
Take 0.6391g cabaltous nitrate hexahydrate and be placed in beaker, add 8g ethanol, add 1g ordered mesoporous carbon, reactant is stirred to 2h, pack in 50ml polytetrafluoro reactor, stainless steel sealing, at 150 ℃ of reaction temperatures, be incubated 2h, collect product and be dried at 80 ℃, obtain alkali formula cobalt nitrate/ordered mesoporous carbon combination electrode material, alkali formula cobalt nitrate accounts for 15% of combination electrode material total weight.
The general structure of alkali formula cobalt nitrate is Co (O
2h
3) NO
3;
The XRD figure of the composite material making is as shown in Fig. 1 No. 3.The test of combination electrode is with embodiment 1, and the ratio electric capacity that records composite material is 661F/g under sweep speed 5mV/s.Fig. 9 is shown in the cyclic voltammetry curve test of combination electrode material under different scanning rates.
Embodiment 4
In embodiment 3, the specific area 1258m of ordered mesoporous carbon
2/ g, total hole volume is 1.19cm
3/ g, mesopore aperture is 3.78nm;
The specific area of composite material is 614.2m
2/ g, total hole volume is 0.56cm
3/ g, mesopore aperture is 3.67nm;
Take 0.4529g cabaltous nitrate hexahydrate and 0.5455g five hydration stannic chlorides are placed in beaker, add 8g absolute ethyl alcohol, add 1g ordered mesoporous carbon, reactant is stirred to 2h, pack in 50ml polytetrafluoro reactor, stainless steel sealing is incubated 4h at 200 ℃ of reaction temperatures, collect product and be dried at 80 ℃, obtain product alkali formula cobalt nitrate-tin ash/ordered mesoporous carbon combination electrode material.
Alkali formula cobalt nitrate accounts for 10% of combination electrode material total weight, SnO
2account for 10% of combination electrode material total weight, surplus is ordered mesoporous carbon.
The general structure of alkali formula cobalt nitrate is Co (O
2h
3) NO
3;
The XRD figure of the composite material making is as shown in Fig. 1 No. 4.The test of combination electrode is with embodiment 1, and the ratio electric capacity that records composite material is 1105F/g under sweep speed 5mV/s.Figure 10 is shown in the cyclic voltammetry curve test of combination electrode material under different scanning rates.
Claims (5)
1. alkali formula cobalt nitrate/ordered mesoporous carbon combination electrode material, is characterized in that, is made up of the component of following percentage by weight:
Metal oxide 0～50%
Alkali formula cobalt nitrate 10～50%
Ordered mesoporous carbon 1～90%
Described metal oxide is NiO, SnO
2or Fe
3o
4in one or more;
The general structure of described alkali formula cobalt nitrate is Co (O
xh
y) NO
3;
Wherein: x is that 2, y is 3.
2. alkali formula cobalt nitrate/ordered mesoporous carbon combination electrode material according to claim 1, is characterized in that, described alkali formula cobalt nitrate/ordered mesoporous carbon combination electrode material, is made up of the component of following percentage by weight:
Nano-metal-oxide 0～10%
Nanometer alkali formula cobalt nitrate 15～20%,
Ordered mesoporous carbon 80～85%.
3. according to the alkali formula cobalt nitrate/ordered mesoporous carbon combination electrode material described in claim 1～2 any one, it is characterized in that, the specific area of described ordered mesoporous carbon is 50m
2/ g～3000m
2/ g, total hole volume is 0.5～2cm
3/ g;
The specific area of described combination electrode material is 300m
2/ g～2000m
2/ g, total hole volume is 0.5～2cm
3/ g, pore diameter range is 2nm～10nm.
4. the preparation method of alkali formula cobalt nitrate/ordered mesoporous carbon combination electrode material according to claim 1, it is characterized in that, comprise the steps: cabaltous nitrate hexahydrate, ethanol and ordered mesoporous carbon reaction, collect product, dry, obtain described alkali formula cobalt nitrate/ordered mesoporous carbon combination electrode material.
5. method according to claim 4, is characterized in that, reacts 2～8h by 125～200 ℃ of cabaltous nitrate hexahydrate, ethanol and ordered mesoporous carbons, collects product, 70～80 ℃ dry 1～4 hour.
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| EP1052017A2 (en) * | 1999-05-13 | 2000-11-15 | Nippon Shokubai Co., Ltd | Catalyst containing Mo, Bi, Fe, Ce and Zr; its use in the production of unsaturated aldehyde and unsaturated carboxylic acid |
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| CN101801850A (en) * | 2007-07-17 | 2010-08-11 | 格雷斯公司 | Basic aluminum nitrate |
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