CN102543459A - 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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- CN102543459A CN102543459A CN2010106047662A CN201010604766A CN102543459A CN 102543459 A CN102543459 A CN 102543459A CN 2010106047662 A CN2010106047662 A CN 2010106047662A CN 201010604766 A CN201010604766 A CN 201010604766A CN 102543459 A CN102543459 A CN 102543459A
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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 who is used for composite electrode material for super capacitor.
Technical background
The energy is the power of the national economic development, also is the important indicator of weighing national overall national strength, national civilized development degree and living standard.Follow the sharp increase and the rapid economic development of population, the energy is shortage day by day, and environment comes into one's own day by day, and carry out the exploitation of the energy and rationally utilize the sustainable development that is directly connected to human society, also be the emphasis of various countries' research.Electric energy as a kind of important energy change in modern times production and the life in playing the part of very important role.Energy-storage travelling wave tube is applied to the various aspects of productive life, and is also increasingly high to the performance requirement of energy-storage travelling wave tube.Though traditional capacitor can provide very large power, its energy density is limited, can not satisfy actual needs.Simultaneously along with the development of science and technology with society, many occasions (like electric automobile) to power require increasingly high, also head and shoulders above the ability to bear of current battery.A kind of novel energy-storage travelling wave tube-" ultracapacitor " obtained fast development under this background.
Ultracapacitor (Supercapacitor) also is 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 ratio electric capacity bigger than traditional capacitor, the power density bigger than storage battery, recycle characteristics such as long and serviceability temperature wide ranges of life-span.Ultracapacitor 20th century six the seventies at first occur in the U.S., and move towards market gradually in the eighties, owing to 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 had delivered one piece of patent about ultracapacitor, the development of ultracapacitor was 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 various fields such as hybrid-electric car, mobile phone, microcomputer.
Since 1992, USDOE and United States advanced battery association just began to organize National Laboratory, university and industrial quarters (Maxwell, GE etc.) to release the feasibility study plan of used for electric vehicle ultracapacitor; 2009, the U.S.'s " next generation " battery and electric motor car plan: national energy portion subsidized 2,400,000,000 dollars, and wherein 1,500,000,000 dollars of battery and accessory manufacturings thereof that subsidize the U.S. are to improve the circulation volume of battery.2000, Germany formulated " regenerative resource method " 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 in electric automobile market.1996, European Union began the project of ultracapacitor, and target is development specific energy 6Wh/kg, 8Wh/L, and specific power 1.5kW/kg, 2kW/L, cycle life surpasses 100,000 times ultracapacitor.
Electrode material is a ultracapacitor core part, and its structure, performance have conclusive effect to the performance of ultracapacitor.Electrode material is divided into four types: raw material of wood-charcoal material, metal oxide, high molecular polymer and composite material.
Raw material of wood-charcoal material (active carbon, CNT, carbon nanocoils, carbon gel, carbon fiber etc.) is ultracapacitor electrode material commonly used, and is theoretical according to electric double layer, and the electric double layer capacitance on carbon resistance rod surface is about 20 μ Fcm
-2, if specific area is 1000m
2g
-1, be 200F/g then than electric capacity.
In various raw material of wood-charcoal material, mesopore raw material of wood-charcoal material is owing to have the suitable electrode material as ultracapacitor in bigger aperture.Wherein in order mesopore raw material of wood-charcoal material owing to its special duct order help electrolyte ion therein embedding and deviate to receive extensive concern.With the material that has pore structure is template; At first the carbon precursor is injected in the duct of template; Remove template after the charing; A kind of porosu solid material of the structure of pallet repeatedly just is able to preserve, and the mesoporous silicon molecular sieve then can control pore passage structure and skeleton simultaneously, and can prepare the mesopore raw material of wood-charcoal material with various pore passage structures through the si molecular sieves of selecting to have different pore passage structures.There is sucrose in the charcoal source for preparing orderly mesopore charcoal, phenol, formaldehyde resin and furfuryl alcohol.
Because the electric double layer capacitance that faraday's electric capacity that metal oxide and hydroxides produce produces much larger than the active carbon material surface, so the pseudo capacitance device just progressively replaces the focus that double electric layer capacitor becomes research and development.Like RuO
2Receive common concern owing to having very high ratio electric capacity.Although RuO
2Specific capacity is up to 760F/g, function admirable aspect capacity and conductivity, but cost an arm and a leg.Because they generally have strong toxicity, environmental pollution is serious again, and people's electrode material of being devoted to seek functional, cheap and environmentally safe substitutes precious metal material for this reason.Many achievements in research both domestic and external show: the transition metal oxide material can be used as the substitute of metal oxide containing precious metals electrode material.Once pointed out some transition metal oxides such as MnO like Conway
x, NiO
xAnd CoO
xDeng the chemical property that also has metal oxide containing precious metals, all become and be hopeful to substitute the electrode material of ruthenium and be studied.
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 acts synergistically each other and carries out charge storage; Realize the performance and the cost coordination of material, and have the novel electrode material of the not available premium properties of unitary electrode material.Yet based on the preparation method of metal oxide/charcoal combination electrode material capacitor, condition is loaded down with trivial details mostly at present, and metal oxide/the charcoal combination electrode material is than electric capacity not high (about 300F/g) 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; Tracing it to its cause, is because fake capacitance or pseudo capacitance are by the underpotential deposition that active material takes place on the electrode surface or on two dimension or the accurate two-dimensional space of body in mutually, forms highly reversible chemisorbed/desorption or the oxidation/reduction reaction generation electric capacity relevant with the electrode charging potential.But owing to lack free OH in the pure metal oxides electrode
-So, OH in the reaction
-Migration be restricted, can only redox take place at the electrode/electrolyte interface, show surface reaction mechanism.Have only a part of metallic atom on oxide grain surface that redox reaction can take place in the course of reaction.And contain OH in metal hydroxides/charcoal combination electrode
-So, OH in the electrochemical reaction
-Migration unrestricted, can take place in electrode/electrolyte interface and electrode interior, show surface reaction and internal-response mechanism simultaneously.
Because the architectural characteristic of electrode material for super capacitor is closely related with preparation technology like granular size, particle size distribution and pattern etc., therefore exploring the 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 the solvent thermal condition; The character of solvent (density, viscosity, peptizaiton) influences each other; Alter a great deal, and differ greatly under its character and the usual conditions, corresponding; The dissolving of reactant, disperseed and chemical reactivity improves greatly or strengthens, this just makes reaction under lower temperature, to take place.The material of solvent-thermal method preparation has active good, advantage such as purity is high, pattern and granular size are controlled, need not through high-temperature calcination, can synthesize directly that particle diameter is little, pattern is regular and the electrochemical active material of good dispersion, helps improving its chemical property.
Therefore can know that from above analysis the ratio electric capacity of raw material of wood-charcoal material is lower, the cost of metal oxide containing precious metals is higher, and commercial application is difficulty, and it is simple to develop synthesis technique, and combination electrode material is the very problem of concern of people institute cheaply.
Summary of the invention
The purpose of this invention is to provide a kind of alkali formula cobalt nitrate/orderly mesopore charcoal combination electrode material and preparation method thereof,, satisfy the needs of relevant field development to overcome the above-mentioned defective that prior art exists.
Alkali formula cobalt nitrate of the present invention/orderly mesopore charcoal combination electrode material, form by following components in weight percentage:
Alkali formula cobalt nitrate 10～50%
Orderly mesopore charcoal 1～90%
Said metal oxide is NiO, SnO
2Or Fe
3O
4In one or more;
The general structure of said alkali formula cobalt nitrate is Co (O
xH
y) NO
3
Wherein: x is 0.1～9, and y is 0.1～12; Preferably, x is 2, and y is 3;
The specific area of said orderly mesopore charcoal is 50m
2/ g～3000m
2/ g, total hole volume are 0.5～2cm
3/ g;
The specific area of said combination electrode material is 300m
2/ g～2000m
2/ g, total hole volume are 0.5～2cm
3/ g, pore diameter range are 2nm～10nm;
Preferably, described alkali formula cobalt nitrate/orderly mesopore charcoal combination electrode material, form by following components in weight percentage:
Nano-metal-oxide 0～10%
Nanometer alkali formula cobalt nitrate 15～20%,
The preparation method of described alkali formula cobalt nitrate/orderly mesopore charcoal combination electrode material comprises the steps:
With cabaltous nitrate hexahydrate, ethanol and 125～200 ℃ of mesopore charcoals reaction 2～8h down in order, collect product, 70～80 ℃ of dryings 1～4 hour, promptly get product: promptly described alkali formula cobalt nitrate/orderly mesopore charcoal combination electrode material;
Nitrate, acetate, sulfate or chloride that said metal soluble-salt is nickel, tin or iron;
The weight content of cabaltous nitrate hexahydrate in ethanol is 10%～50%;
Alkali formula cobalt nitrate of the present invention/orderly mesopore charcoal combination electrode material can adopt method well known in the art, and preparation becomes electrode slice, is assembled into capacitor with electrode slice then.
Alkali formula cobalt nitrate of the present invention/orderly mesopore charcoal combination electrode material can adopt the method for Q/CLY 001-2010 standard code to detect evaluation.
Ultracapacitor of the present invention is with the advantage of combination electrode material:
Electrode for super capacitor material of the present invention is with cabaltous nitrate hexahydrate, in order the mesopore charcoal is a raw material; The employing one-step method is prepared from; Simple, with low cost, the suitable suitability for industrialized production of this preparation method's technology; By alkali formula cobalt nitrate of the present invention/orderly mesopore charcoal combination electrode material, unipolar is 800～1200F/g than electric capacity, and energy density is 1000～3000Wh/kg; And in water based inorganic electrolyte KOH, carry out, pollution-free, safe, adopt the electrode material of alkali formula cobalt nitrate of the present invention/orderly mesopore charcoal combination electrode material as ultracapacitor, can improve the energy density of capacitor greatly.
Description of drawings
The X-ray diffractogram of alkali formula cobalt nitrate among Fig. 1 embodiment 1/orderly mesopore charcoal super capacitor electrode material;
The transmission electron microscope picture of alkali formula cobalt nitrate among Fig. 2 embodiment 1/orderly mesopore charcoal super capacitor electrode material;
The N of alkali formula cobalt nitrate among Fig. 3 embodiment 1/orderly mesopore charcoal super capacitor electrode material
2The adsorption-desorption thermoisopleth;
The graph of pore diameter distribution of alkali formula cobalt nitrate among Fig. 4 embodiment 1/orderly mesopore charcoal super capacitor electrode material;
Alkali formula cobalt nitrate among Fig. 5 embodiment 1/orderly cyclic voltammogram of mesopore charcoal super capacitor electrode material under different scanning rates;
The mesopore charcoal super capacitor electrode material of alkali formula cobalt nitrate among Fig. 6 embodiment 1/in order under different scanning rates than electric capacity figure;
The constant current charge-discharge figure of alkali formula cobalt nitrate among Fig. 7 embodiment 1/orderly mesopore charcoal super capacitor electrode material;
Alkali formula cobalt nitrate among Fig. 8 embodiment 2/orderly cyclic voltammogram of mesopore charcoal super capacitor electrode material under different scanning rates;
Alkali formula cobalt nitrate among Fig. 9 embodiment 3/orderly cyclic voltammogram of mesopore charcoal super capacitor electrode material under different scanning rates;
Alkali formula cobalt nitrate-tin oxide among Figure 10 embodiment 4/orderly cyclic voltammogram of mesopore charcoal super capacitor electrode material under different scanning rates;
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is described further, but the present invention is not limited to following example, every technical scheme of making based on technological basic thought of the present invention that modification, replacement or change realized all belongs to scope of the present invention.
Embodiment 1
Among the embodiment 1, the specific area of mesopore charcoal is 1258m in order
2/ g, total hole volume are 1.19cm
3/ g, the mesopore aperture is 3.78nm;
The specific area of composite material is 711.5m
2/ g, total hole volume are 0.7192cm
3/ g, the mesopore aperture is 3.98nm;
Take by weighing the 0.9058g cabaltous nitrate hexahydrate and place beaker, add 8g ethanol, add the orderly mesopore charcoal of 1g; Reactant is stirred 2h; The 50ml that packs into gathers in the tetrafluoro reactor, and the stainless steel sealing is incubated 4h down for 175 ℃ in reaction temperature; Collect product 80 ℃ of dryings, promptly get described alkali formula cobalt nitrate/orderly mesopore charcoal combination electrode material.In the mesopore charcoal combination electrode material of the alkali formula cobalt nitrate that is made by said method/in order, alkali formula cobalt nitrate accounts for 20% of combination electrode material total weight.
The XRD figure of the composite material that makes is shown among Fig. 1 No. 1.
The structural formula of alkali formula cobalt nitrate is Co (O
2H
3) NO
3
Transmission electron microscope is as shown in Figure 2; N
2The adsorption-desorption thermoisopleth is as shown in Figure 3; Graph of pore diameter distribution such as Fig. 4; The specific area of product is 778.7m
2g
-1With the alkali formula cobalt nitrate that obtains/mesopore charcoal combination electrode material, conductive carbon black (model BP200) and adhesive polytetrafluoroethylene (PTFE) are pressed 75: 20: 5 batchings of mass ratio in order; After processing slurry on the magnetic stirring apparatus, the hydraulic press compacting that is coated on the nickel foam through 10MPa promptly makes electrode slice.
Conductive carbon black BP200 adopts the product of U.S. Cabot Co.,Ltd; Adhesive PTFE adopts the product of Shanghai Sanaifu New Material Co., Ltd;
Adopt three-electrode system, promptly respectively with combination electrode as work electrode, platinized platinum make auxiliary electrode, saturated calomel electrode (SCE) be a reference electrode, carry out cyclic voltammetric at-0.2～0.7V potential region and test.With the 6mol/L KOH aqueous solution is electrolyte, and the ratio electric capacity that records composite material is 1170F/g under sweep speed 5mV/s.
The alkali formula cobalt nitrate that obtains/Fig. 5 is seen in the cyclic voltammetry curve test of mesopore charcoal combination electrode material under different scanning rates in order; More as shown in Figure 6 than capacitance values; Constant current charge-discharge figure is as shown in Figure 7.
Embodiment 2
Among the embodiment 2, the specific area of mesopore charcoal is 1538m in order
2/ g, total hole volume are 1.32cm
3/ g, the mesopore aperture is 3.95nm;
The specific area of composite material is 778.7m
2/ g, total hole volume are 0.92cm
3/ g, the mesopore aperture is 4.70nm;
Take by weighing the 0.7500g cabaltous nitrate hexahydrate and place beaker, add 8g ethanol, add the orderly mesopore charcoal of 1g; Reactant is stirred 4h, and the 50ml that packs into gathers in the tetrafluoro reactor, the stainless steel sealing; Be incubated 6h down for 125 ℃ in reaction temperature; Collect product 80 ℃ of dryings, promptly get alkali formula cobalt nitrate/orderly mesopore charcoal 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 that makes is shown among 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 seen in the cyclic voltammetry curve test of combination electrode material under different scanning rates.
Embodiment 3
Among the embodiment 3, the specific area of mesopore charcoal is 1258m in order
2/ g, total hole volume are 1.19cm
3/ g, the mesopore aperture is 3.78nm;
The specific area of composite material is 682.3m
2/ g, total hole volume are 0.8cm
3/ g, the mesopore aperture is 4.73nm;
Take by weighing the 0.6391g cabaltous nitrate hexahydrate and place beaker, add 8g ethanol, add the orderly mesopore charcoal of 1g; Reactant is stirred 2h, and the 50ml that packs into gathers in the tetrafluoro reactor, the stainless steel sealing; Be incubated 2h down for 150 ℃ in reaction temperature; Collect product 80 ℃ of dryings, promptly get alkali formula cobalt nitrate/orderly mesopore charcoal 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 that makes is shown among 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 seen in the cyclic voltammetry curve test of combination electrode material under different scanning rates.
Embodiment 4
Among the embodiment 3, the specific area 1258m of orderly mesopore charcoal
2/ g, total hole volume are 1.19cm
3/ g, the mesopore aperture is 3.78nm;
The specific area of composite material is 614.2m
2/ g, total hole volume are 0.56cm
3/ g, the mesopore aperture is 3.67nm;
Take by weighing the 0.4529g cabaltous nitrate hexahydrate and 0.5455g five hydration stannic chlorides place beaker, add the 8g absolute ethyl alcohol, add the orderly mesopore charcoal of 1g; Reactant is stirred 2h; The 50ml that packs into gathers in the tetrafluoro reactor, and the stainless steel sealing is incubated 4h down for 200 ℃ in reaction temperature; Collect product 80 ℃ of dryings, promptly get product alkali formula cobalt nitrate-tin ash/orderly mesopore charcoal 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 orderly mesopore charcoal.
The general structure of alkali formula cobalt nitrate is Co (O
2H
3) NO
3
The XRD figure of the composite material that makes is shown among 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 seen in the cyclic voltammetry curve test of combination electrode material under different scanning rates.
Claims (8)
1. alkali formula cobalt nitrate/orderly mesopore charcoal combination electrode material is characterized in that, is made up of following components in weight percentage:
Metal oxide 0～50%
Alkali formula cobalt nitrate 10～50%
Orderly mesopore charcoal 1～90%
Said metal oxide is NiO, SnO
2Or Fe
3O
4In one or more;
The general structure of said alkali formula cobalt nitrate is Co (O
xH
y) NO
3
Wherein: x is 0.1～9, and y is 0.1～12.
2. alkali formula cobalt nitrate according to claim 1/orderly mesopore charcoal combination electrode material is characterized in that x is 2, and y is 3.
3. alkali formula cobalt nitrate according to claim 1/orderly mesopore charcoal combination electrode material is characterized in that, described alkali formula cobalt nitrate/orderly mesopore charcoal combination electrode material is made up of following components in weight percentage:
Nano-metal-oxide 0～10%
Nanometer alkali formula cobalt nitrate 15～20%,
Orderly mesopore charcoal 80～85%.
4. alkali formula cobalt nitrate according to claim 2/orderly mesopore charcoal combination electrode material is characterized in that, described alkali formula cobalt nitrate/orderly mesopore charcoal combination electrode material is made up of following components in weight percentage:
Nano-metal-oxide 0～10%
Nanometer alkali formula cobalt nitrate 15～20%,
Orderly mesopore charcoal 80～85%.
5. according to each described alkali formula cobalt nitrate of claim 1～4/orderly mesopore charcoal combination electrode material, it is characterized in that the specific area of said orderly mesopore charcoal is 50m
2/ g～3000m
2/ g, total hole volume are 0.5～2cm
3/ g;
The specific area of said combination electrode material is 300m
2/ g～2000m
2/ g, total hole volume are 0.5～2cm
3/ g, pore diameter range are 2nm～10nm.
According to claim the preparation method of mesopore charcoal combination electrode material of 1～5 each alkali formula cobalt nitrate of stating/in order; It is characterized in that; Comprise the steps: cabaltous nitrate hexahydrate, ethanol and mesopore charcoal reaction in order; Collect product, drying promptly gets described alkali formula cobalt nitrate/orderly mesopore charcoal combination electrode material.
7. method according to claim 6 is characterized in that, nitrate, acetate, sulfate or chloride that said metal soluble-salt is nickel, tin or iron.
8. according to claim 6 or 7 described methods, it is characterized in that,, collect product, 70～80 ℃ of dryings 1～4 hour with cabaltous nitrate hexahydrate, ethanol and 125～200 ℃ of mesopore charcoals reaction 2～8h down in order.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112165986A (en) * | 2018-03-22 | 2021-01-01 | 英国石油有限公司 | Supported cobalt-containing fischer-tropsch catalysts, process for their preparation and their use |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112165986A (en) * | 2018-03-22 | 2021-01-01 | 英国石油有限公司 | Supported cobalt-containing fischer-tropsch catalysts, process for their preparation and their use |
| CN112165986B (en) * | 2018-03-22 | 2023-08-08 | 英国石油有限公司 | Supported cobalt-containing Fischer-Tropsch catalyst, preparation method and application thereof |
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