CN102709517A - Flexible integrated precious-metal-contained particle-carbon electrode and preparation method thereof - Google Patents
Flexible integrated precious-metal-contained particle-carbon electrode and preparation method thereof Download PDFInfo
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- CN102709517A CN102709517A CN2012101938458A CN201210193845A CN102709517A CN 102709517 A CN102709517 A CN 102709517A CN 2012101938458 A CN2012101938458 A CN 2012101938458A CN 201210193845 A CN201210193845 A CN 201210193845A CN 102709517 A CN102709517 A CN 102709517A
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Abstract
The invention relates to a flexible integrated precious-metal-contained particle-carbon electrode and a preparation method thereof. The method is characterized in that graphite oxide is used for reducing a graphene microchip, and the graphene microchip is self-assembled and combined with active substance metal particles to form the integrated electrode. The preparation method of the integrated electrode comprises the steps of step 1, dispersion of graphite oxide and precious metal precursors: the graphite oxide and the precious metal precursor particles are placed into polarity solvent to be dispersed, and uniformly-dispersed sol or solution is formed; and step 2, preparation of the electrode: a reducing agent is added into the sol or the solution to be stirred and reacted under the temperature of 0 to 200 DEG C, and after a period of time, the sol or the solution is made into the electrode after being filtered and dried. The precious-metal/carbon flexible electrode has large active substance load and good flexibility, is bendable and has large specific capacity; and when in use, the electrode has advantages of large power, low cost and no environmental pollution, and a novel method for preparing the integrated precious metal-carbon flexible electrode without conductive agent and bond is developed.
Description
Technical field
The invention belongs to the electrochemical energy storage technical field, particularly, relate to a kind of novel electrode, the flexible integrated preparation method who contains noble metal granule-carbon electrode.
Background technology
Because the scarcity day by day of non-renewable energy resources such as global oil, natural gas, coal and the increasingly serious problem of environmental pollution that utilizes these energy to bring; People begin to seek other alternative cleaning, safety and regenerative resource, for example wind energy, solar energy, tidal energy, geothermal energy etc.And these energy will conveniently use, and need be converted into electric energy, promptly need utilize the electrochemical power source of high power capacity to carry out the energy storage.
Electrochemical cell is a kind of important energy, is used for civilian consumption, industry and military field in a large number.This mainly is because the exploitation of progress, more lower powered requirement and the portable set of electronic technology, and power consumption equipment growth that battery capacity and power characteristic are required is also to the universal facilitation that played of chemical power source in addition.Lithium battery comprises that lithium primary battery and lithium secondary battery and lithium ion battery are compared with other traditional electrical chemical power source such as zinc/manganese dioxide battery etc. and has great advantage; Not only in specific capacity; Aspect such as energy density and power density is with the obvious advantage; And because the raw materials used low pollution to environment of its preparation impels the application of lithium battery more and more wider.Particularly be applied to the research and development upsurge of electric motor car, make that the Application Research prospect of lithium battery is very good along with present electrokinetic cell.Noble metal can form certain alloy with lithium, has high energy density, can be used as negative pole and in film lithium cell, uses.Simultaneously, noble metal has advantages of high catalytic activity, can be used as positive pole and in the air electrode of lithium-air battery or fuel, uses.
Yet in the traditional electrode preparation, need to add a large amount of conductive agents, thereby cause electrode integral energy density to reduce to a great extent.Moreover, the dispersion that also needs will be good with conductive agent is coated on the metal collector again.So both need loaded down with trivial details technology, again equipment had been proposed higher requirement.Moreover being coated in can influence the flexible of electrode and reduce the electrode flexible on traditional metal forming, limited the scope of application of electrode largely.
Therefore, more wide space is arranged, must carry out necessary improvement electrode preparation method in order to make electrode.
Summary of the invention
The purpose of this invention is to provide the integrated noble metal granule-carbon electrode and preparation method thereof that contains of a kind of flexibility, this method is reduced into the Graphene microplate with graphite oxide under the effect of suction filtration; And self assembly combines the method for active material noble metal granule; Prepared the electrode that does not contain conductive agent, binding agent, it is big that this electrode has the active material carrying capacity, flexible good; Flexible, the advantage of big specific capacity.
In order to realize above purpose; The invention provides the integrated preparation method who contains noble metal granule-carbon electrode of a kind of flexibility; This method adopts graphite oxide reduction Graphene microplate; This Graphene microplate self assembly and the integrated electrode that combines the active material noble metal granule to form comprise following concrete steps:
Step 1, the dispersion of graphite oxide and noble metal precursor body: graphite oxide and noble metal precursor body particle are joined in the polar solvent, disperse, form homodisperse colloidal sol body or solution;
Step 2, the preparation of electrode: add reducing agent, under 0 ~ 200 ℃, stirring reaction after 0.5-24 hour, filters, and after the drying, makes electrode.
The said filtration of the present invention can be Direct Filtration, vacuum filtration, press filtration or other laboratory, industrial filter method.Filter medium can be all filter mediums such as filter paper, plastics filter membrane, ceramic membrane.Further, this filtration is preferably vacuum filtration, is beneficial to the self assembly of Graphene microplate and combines noble metal granule.
The dispersing apparatus that described dispersion is adopted comprises that ultrasonic dispersion, mechanical agitation, ball mill five equilibrium are casually arranged with fully.Drying condition is a natural air drying, the oven dry of heating, freezing all drying means such as air-dry.
The above-mentioned flexible integrated preparation method who contains noble metal granule-carbon electrode, wherein, the noble metal described in the step 1 is meant one or several of metals such as Ag, Au, Pt, Pd, Ru, Cu.
The above-mentioned flexible integrated preparation method who contains noble metal granule-carbon electrode; Wherein, Polar solvent described in the step 1 is selected in water, ethanol, acetonitrile, N-methyl-pyrrolidones, the carrene any one, perhaps two or more mixed solvent arbitrarily between them.
The above-mentioned flexible integrated preparation method who contains noble metal granule-carbon electrode, wherein, the reducing agent described in the step 2 is N
2H
4, NaBH
4, in the formaldehyde, ascorbic acid any one, perhaps two or more mixture arbitrarily between them.
The electrode that the present invention also provides a kind of above-mentioned flexible integrated preparation method who contains noble metal granule-carbon electrode to make; This electrodes use graphite oxide reduction Graphene microplate self assembly; Flexible integrated noble metal carbon electrode in conjunction with the method for active material noble metal granule forms does not comprise conductive agent and binding agent in this integrated electrode.
Under the reduction of electrode preparation method dependence of the present invention own; Graphite oxide (being the Graphene microplate) and noble metal granule self assembly effect through reduction; Perhaps directly combine the method for active material noble metal granule to prepare the electrode that does not contain the binding agent of conductive agent, preparation technology is simple.And; Like this preparation that noble metal-the carbon flexible electrode has the active material carrying capacity is big, flexible good, flexible; Energy density is high; Big specific capacity has the characteristics of more high-power, low cost and non-environmental-pollution during use, opened up the novel preparation method of the integrated noble metal flexible electrode that does not contain conductive agent.
Description of drawings
Fig. 1 prepares gained electrode SEM Electronic Speculum figure for adopting silver acetate presoma and the self assembly of reduction-oxidation graphite.
Fig. 2 is the charging and discharging curve of integrated electrode of the present invention in 2016 little button batteries, and capacity is based on the electrode total weight.
Embodiment
Specify embodiment of the present invention below in conjunction with accompanying drawing and embodiment.
Adopt noble metal precursor body (preferred silver acetate) and graphite oxide under the effect of reducing agent; It is as shown in Figure 1 that self assembly prepares gained electrode SEM Electronic Speculum figure; Can find out the integrated electrode of preparation, argent simple substance uniform particles ground embeds in the Graphene lamella, and self assembly is integrally formed polarizing electrode.The preparation of this integrated electrode comprises following concrete steps:
Step 1; The dispersion of graphite oxide and noble metal precursor body: graphite oxide and noble metal precursor body particle are joined in the polar solvent; Disperse (dispersing apparatus can be all dispersing apparatus such as ultrasonic dispersion, mechanical agitation, ball mill), form homodisperse colloidal sol body or solution; Described noble metal is meant one or several of metals such as Ag, Au, Pt, Pd, Ru, Cu.This noble metal precursor body is meant the precious metal salt presoma, like acetate, and nitrate etc.Described polar solvent is selected in water, ethanol, acetonitrile, N-methyl-pyrrolidones, the carrene any one, perhaps two or more mixed solvent arbitrarily between them.
Step 2, the preparation of electrode: add reducing agent, under 0 ~ 200 ℃, stirring reaction behind the certain hour (as 0.5-24 hour), filters, and after the drying, makes electrode.
Described reducing agent is reduced to the Graphene microplate with graphite oxide, and precious metal ion is reduced to precious metal simple substance, and this reducing agent is selected N
2H
4, NaBH
4, in the formaldehyde, ascorbic acid any one, perhaps two or more mixture arbitrarily between them.
Filtration of the present invention is meant all laboratories, industrial filter methods such as Direct Filtration, suction filtration press filtration or other filtration, and filter medium is all filter mediums such as filter paper, plastics filter membrane, ceramic membrane.Filtration of the present invention is preferably vacuum filtration, under the effect of vacuum filtration, help the Graphene microplate self assembly and with the combining of noble metal granule, thereby be integrally formed polarizing electrode.
Embodiment 1
The concrete preparation method of integrated electrode of the present invention is:
Step 1 is disperseed 1mg/ml graphite oxide aqueous solution 100ml and 0.1g silver acetate 24 hours under ultrasonic disperser vibration.
Step 2 adds the 1g ascorbic acid down at 100 ℃, under the mechanical agitation, and reaction 20h, then, as filter medium, suction filtration is 10 hours under vacuum with filter paper, and drying is 20 hours in 200 ℃ of baking ovens, peels off filter paper, makes electrode.
The sequin that preparation gained combination electrode is washed into diameter 14mm is as positive pole, with metal lithium sheet as negative pole, with 1M LiPF
6/ EC (ethylene carbonate)-DEC (diethyl carbonate) (volume ratio 3:7) is as electrolyte, and being assemblied in battery configuration is in 2016 button cells.Between 3-0V, discharge, discharge platform is about 0.05V, and under the 20mA current discharge, discharge capacity is about 1170mAh/g first, and the initial charge capacity is 686mAh/g, and is as shown in Figure 2.
Embodiment 2
The concrete preparation method of integrated electrode of the present invention is:
Step 1 is disperseed 1mg/ml graphite oxide aqueous solution 100ml and 0.2g silver acetate 24 hours under ultrasonic disperser vibration.
Step 2 adds down the 1g formaldehyde at 100 ℃, under the mechanical agitation, reaction 20h, then with filter paper as filter medium, suction filtration is 10 hours under vacuum, in 200 ℃ of baking ovens dry 20 hours, peel off filter paper, make electrode.
The sequin that preparation gained combination electrode is washed into diameter 14mm is as positive pole, with metal lithium sheet as negative pole, with 1M LiPF
6/ EC-DEC (volume ratio 3:7) is as electrolyte, and being assemblied in battery configuration is in 2016 button cells.Between 3-0V, discharge, discharge platform is about 0.1V, and under the 500mA current discharge, discharge capacity is still about 500mAh/g.
Below only be preferred embodiment of the present invention, according to above-mentioned design of the present invention, those skilled in the art can also make various modifications and conversion according to actual conditions to this.For example, variation of the selection of above-mentioned material and composition proportioning and battery structure or the like.Yet similar this conversion all belongs to scope of the present invention with revising.
Although content of the present invention has been done detailed introduction through above-mentioned preferred embodiment, will be appreciated that above-mentioned description should not be considered to limitation of the present invention.After those skilled in the art have read foregoing, for multiple modification of the present invention with to substitute all will be conspicuous.Therefore, protection scope of the present invention should be limited appended claim.
Claims (6)
1. integrated preparation method who contains noble metal granule-carbon electrode of flexibility; It is characterized in that; This method is reduced into the Graphene microplate with graphite oxide, and this Graphene microplate self assembly and the integrated electrode that combines the active material noble metal granule to form comprise following concrete steps:
Step 1, the dispersion of graphite oxide and noble metal precursor body: graphite oxide and noble metal precursor body particle are joined in the polar solvent, disperse, form homodisperse colloidal sol body or solution;
Step 2, the preparation of electrode: add reducing agent, under 0 ~ 200 ℃, stirring reaction after 0.5-24 hour, filters, and after the drying, makes electrode.
2. the integrated preparation method who contains noble metal granule-carbon electrode of flexibility as claimed in claim 1 is characterized in that the noble metal described in the step 1 is meant one or several of metals such as Ag, Au, Pt, Pd, Ru, Cu.
3. the integrated preparation method who contains noble metal granule-carbon electrode of flexibility as claimed in claim 1; It is characterized in that; Polar solvent described in the step 1 is selected in water, ethanol, acetonitrile, N-methyl-pyrrolidones, the carrene any one, perhaps two or more mixed solvent arbitrarily between them.
4. the integrated preparation method who contains noble metal granule-carbon electrode of flexibility as claimed in claim 1 is characterized in that the reducing agent described in the step 2 is N
2H
4, NaBH
4, in the formaldehyde, ascorbic acid any one, perhaps two or more mixture arbitrarily between them.
5. the integrated preparation method who contains noble metal granule-carbon electrode of flexibility as claimed in claim 1 is characterized in that, is filtered into vacuum filtration described in the step 2.
6. the electrode that makes like the integrated preparation method who contains noble metal granule-carbon electrode of any described flexibility among the claim 1-5; It is characterized in that; This electrodes use graphite oxide reduction Graphene microplate self assembly; Flexible integrated noble metal carbon electrode in conjunction with the method for active material noble metal granule forms does not comprise conductive agent and binding agent in this electrode.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108824086A (en) * | 2018-07-06 | 2018-11-16 | 江西克莱威纳米碳材料有限公司 | Carbon nanotube-aramid far-infrared paper and preparation method thereof, and carbon nanotube far-infrared physiotherapy shoe sole lining |
| CN111948263A (en) * | 2020-07-15 | 2020-11-17 | 武汉大学 | Low-cost batch preparation method and application of noble metal electrode array |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101814607A (en) * | 2010-04-17 | 2010-08-25 | 上海交通大学 | Preparation method of platinum/graphen catalyst for proton exchange membrane fuel cell |
| CN102387984A (en) * | 2008-09-08 | 2012-03-21 | 新加坡南洋理工大学 | Nanoparticle decorated nanostructured material as electrode material and method for obtaining the same |
| CN102426868A (en) * | 2011-09-05 | 2012-04-25 | 湖南大学 | Water-soluble graphene-noble-metal nano-composite and preparation method and application thereof |
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Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102387984A (en) * | 2008-09-08 | 2012-03-21 | 新加坡南洋理工大学 | Nanoparticle decorated nanostructured material as electrode material and method for obtaining the same |
| CN101814607A (en) * | 2010-04-17 | 2010-08-25 | 上海交通大学 | Preparation method of platinum/graphen catalyst for proton exchange membrane fuel cell |
| CN102426868A (en) * | 2011-09-05 | 2012-04-25 | 湖南大学 | Water-soluble graphene-noble-metal nano-composite and preparation method and application thereof |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108824086A (en) * | 2018-07-06 | 2018-11-16 | 江西克莱威纳米碳材料有限公司 | Carbon nanotube-aramid far-infrared paper and preparation method thereof, and carbon nanotube far-infrared physiotherapy shoe sole lining |
| CN108824086B (en) * | 2018-07-06 | 2020-10-02 | 江西克莱威纳米碳材料有限公司 | Carbon nanotube-aramid far-infrared paper and preparation method thereof, and carbon nanotube far-infrared physiotherapy shoe sole lining |
| CN111948263A (en) * | 2020-07-15 | 2020-11-17 | 武汉大学 | Low-cost batch preparation method and application of noble metal electrode array |
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Application publication date: 20121003 |