CN105845461A - Carbon-filled foamed nickel, preparation method and application of carbon-filled foamed nickel - Google Patents
Carbon-filled foamed nickel, preparation method and application of carbon-filled foamed nickel Download PDFInfo
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- CN105845461A CN105845461A CN201610163874.8A CN201610163874A CN105845461A CN 105845461 A CN105845461 A CN 105845461A CN 201610163874 A CN201610163874 A CN 201610163874A CN 105845461 A CN105845461 A CN 105845461A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
- H01G11/44—Raw materials therefor, e.g. resins or coal
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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
Abstract
The invention belongs to the electrode material field and relates to a carbon-filled foamed nickel, a preparation method and application of the carbon-filled foamed nickel. The preparation method of the carbon-filled foamed nickel provided by the invention includes the following steps that: foamed nickel is impregnated in a carbon source aqueous solution, wherein the carbon source aqueous solution contains glucose and ethylene diamine; and heating is carried out to realize carbonization, so that the carbon-filled foamed nickel can be obtained. According to the preparation method provided by the invention, the glucose is adopted as a carbon source for impregnating the foamed nickel, and the ethylene diamine is introduced when the foamed nickel is impregnated, and therefore, the carbon filling degree of the obtained carbon-filled foamed nickel can be significantly improved, and thus, the electrical properties of the carbon-filled foamed nickel can be improved. As indicated by experimental results, the carbon-filled foamed nickel obtained by adopting the preparation method is so compact that light cannot be transmitted through the carbon-filled foamed nickel nearly, and the carbon-filled foamed nickel does not have any large gaps to allow light to pass through; after 75 times of circulation, the capacity of a supercapacitor made of the carbon-filled foamed nickel can still maintain 60% of the original capacity, and the supercapacitor has good electrochemical stability.
Description
Technical field
The invention belongs to electrode material field, particularly relate to a kind of carbon filled and process nickel and its preparation method and application.
Background technology
Ultracapacitor as a new generation's energy-storage travelling wave tube, with its high-rate charge-discharge capability, high power density, permanent cycle life and by extensive concern, in fields such as information, traffic, electronics, there is the biggest potential and using value.The performance of ultracapacitor depends on activity and the dynamics of electrode material, therefore, in order to improve the chemical property of ultracapacitor, select suitable electrode material, optimize its structure, improve activity and the dynamics of electrode material, be just particularly important.
The electrode of the ultracapacitor of current preparation is many using nickel foam as collector, loose structure yet with nickel foam, leave substantial amounts of unemployed space on it, thus cause the electric property of the ultracapacitor using nickel foam as current collector material unsatisfactory.For solving this problem, existing research worker carries out the research improving nickel foam space utilization degree.Such as, by the way of using and filling the carbon source materials such as glucose, cellulose or nano-carbon material in nickel foam, nickel foam is made carbon filled and process nickel, to improve the space utilization degree of nickel foam.But the carbon compactedness of existing carbon filled and process nickel is relatively low, cause the electric property of ultracapacitor being made from poor.
Summary of the invention
In view of this, it is an object of the invention to provide a kind of carbon filled and process nickel and its preparation method and application, the carbon filled and process nickel that the method using the present invention to provide prepares has higher carbon compactedness, and electric property is excellent.
The invention provides the preparation method of a kind of carbon filled and process nickel, comprise the following steps:
Nickel foam is immersed in carbon source aqueous solution, heats carbonization, obtain carbon filled and process nickel；
Containing glucose and ethylenediamine in described carbon source aqueous solution.
Preferably, described glucose content in carbon source aqueous solution is 0.1～0.5g/mL.
Preferably, described ethylenediamine content in carbon source aqueous solution is 0.01～0.1mL/mL.
Preferably, possibly together with carbon materials in described carbon source aqueous solution；Described carbon materials includes Graphene and/or CNT.
Preferably, described carbon materials content in carbon source aqueous solution is 1～2mg/mL.
Preferably, the temperature of described heating carbonization is 160～190 DEG C；The time of described heating carbonization is 12～24h.
Preferably, the aperture of described nickel foam is 50～200 μm；The specific surface area of described nickel foam is 0.5～2.0m2/g。
Preferably, the product that heating carbonization obtains carries out washing and being dried successively, obtains carbon filled and process nickel.
The carbon filled and process nickel that a kind of method described in technique scheme that the invention provides prepares.
The invention provides a kind of ultracapacitor, the electrode material of described ultracapacitor includes the carbon filled and process nickel described in technique scheme.
Compared with prior art, the invention provides a kind of carbon filled and process nickel and its preparation method and application.The carbon filled and process method for preparing nickel that the present invention provides comprises the following steps: nickel foam be immersed in carbon source aqueous solution, heats carbonization, obtains carbon filled and process nickel；Containing glucose and ethylenediamine in described carbon source aqueous solution.The method that the present invention provides is using glucose as the carbon source of impregnated foam nickel, and introduces ethylenediamine when impregnated foam nickel, thus significantly improves the carbon compactedness of prepared carbon filled and process nickel, and then improves the electric property of carbon filled and process nickel.Test result indicate that, the carbon filled and process nickel that the method using the present invention to provide prepares is the closeest light tight, no longer has big space printing opacity；After the ultracapacitor using this carbon filled and process nickel to prepare circulates for 75 times, capacity remains at more than the 60% of raw capacity, has preferable electrochemical stability.
Accompanying drawing explanation
In order to be illustrated more clearly that the embodiment of the present invention or technical scheme of the prior art, the accompanying drawing used required in embodiment or description of the prior art will be briefly described below, apparently, accompanying drawing in describing below is only embodiments of the invention, for those of ordinary skill in the art, on the premise of not paying creative work, it is also possible to obtain other accompanying drawing according to the accompanying drawing provided.
Fig. 1 is the carbon filled and process nickel digital photograph figure that the embodiment of the present invention 1 provides；
Fig. 2 is the carbon filled and process nickel scanning electron microscope (SEM) photograph that the embodiment of the present invention 1 provides；
Fig. 3 is carbon filled and process nickel × 300 scanning electron microscope (SEM) photograph that the embodiment of the present invention 2 provides；
Fig. 4 is carbon filled and process nickel × 10,000 scanning electron microscope (SEM) photograph that the embodiment of the present invention 2 provides；
Fig. 5 is the ultracapacitor charge-discharge performance cyclic curve figure under different multiplying being assembled into by embodiment 1 carbon filled and process nickel that the embodiment of the present invention 3 provides；
Fig. 6 is the ultracapacitor charging and discharging curve figure under different multiplying being assembled into by embodiment 1 carbon filled and process nickel that the embodiment of the present invention 3 provides；
Fig. 7 is the ultracapacitor charge-discharge performance cyclic curve figure under different multiplying being assembled into by embodiment 2 carbon filled and process nickel that the embodiment of the present invention 3 provides.
Detailed description of the invention
Below the technical scheme in the embodiment of the present invention is clearly and completely described, it is clear that described embodiment is only a part of embodiment of the present invention rather than whole embodiments.Based on the embodiment in the present invention, the every other embodiment that those of ordinary skill in the art are obtained under not making creative work premise, broadly fall into the scope of protection of the invention.
The invention provides the preparation method of a kind of carbon filled and process nickel, comprise the following steps:
Nickel foam is immersed in carbon source aqueous solution, heats carbonization, obtain carbon filled and process nickel；
Containing glucose and ethylenediamine in described carbon source aqueous solution.
In the preparation method that the present invention provides, first nickel foam is immersed in carbon source aqueous solution.Wherein, the aperture of described nickel foam is preferably 50～200 μm；The specific surface area of described nickel foam is preferably 0.5～2.0m2/g.In the present invention, containing glucose and ethylenediamine in described carbon source aqueous solution；Described glucose content in carbon source aqueous solution of stating is preferably 0.1～0.5g/mL, more preferably 0.2～0.4g/mL, most preferably 0.32～0.33g/mL；Described ethylenediamine content in carbon source aqueous solution is preferably 0.01～0.1mL/mL, more preferably 0.03～0.07mL/mL, most preferably 0.054mL/mL.In the present invention, preferably possibly together with carbon materials in described carbon source aqueous solution；Described carbon materials preferably includes Graphene and/or CNT；Described carbon materials content in carbon source aqueous solution is preferably 1～2mg/mL, more preferably 1.2～1.5mg/mL, most preferably 1.35～1.36mg/mL.
In the present invention, it is preferred to described nickel foam washed successively before nickel foam is immersed in carbon source aqueous solution and be dried.In the present invention, the mode of described washing, particularly as follows: first described nickel foam be immersed in hydrochloric acid, uses acetone supersound washing afterwards, finally uses the alternately washing of deionized water and absolute alcohol.Wherein, the concentration of described hydrochloric acid is preferably 0.2～0.8mol/L, more preferably 0.5～0.6mol/L；The time that described nickel foam impregnates in hydrochloric acid is preferably 10～30min, more preferably 20～25min；The time of described supersound washing is preferably 5～20min, more preferably 10～15min.
After nickel foam being immersed in carbon source aqueous solution, carry out heating carbonization.Wherein, the temperature of described heating carbonization is preferably 160～190 DEG C, more preferably 180～190 DEG C；The time of described heating carbonization is preferably 12～24h.After heating carbonization terminates, obtain heating carbonized product.In the present invention, it is preferred to the product obtaining heating carbonization washs successively and is dried.Wherein, the mode of described washing is alternately cleaned preferably with ethanol and deionized water；Described dry mode preferably room temperature dries or lyophilization；The described dry time is preferably 48～96h, more preferably 60～72h.After Gan Zaoing, obtain carbon filled and process nickel.
The method that the present invention provides is using glucose as the carbon source of impregnated foam nickel, and introduces ethylenediamine when impregnated foam nickel, thus significantly improves the carbon compactedness of prepared carbon filled and process nickel, and then improves the electric property of carbon filled and process nickel.Test result indicate that, the carbon filled and process nickel that the method using the present invention to provide prepares is the closeest light tight, no longer has big space printing opacity；After the ultracapacitor using this carbon filled and process nickel to prepare circulates for 75 times, capacity remains at more than the 60% of raw capacity, has preferable electrochemical stability.
The carbon filled and process nickel that a kind of method described in technique scheme that present invention also offers prepares.
Present invention also offers a kind of ultracapacitor, the electrode material of described ultracapacitor includes the carbon filled and process nickel described in technique scheme.
The ultracapacitor that the present invention provides includes positive pole, negative pole, electrolyte and the isolating membrane between positive pole and negative pole.Wherein, the material of described positive pole and negative pole includes described carbon filled and process nickel；Described electrolyte is preferably the organic solution of lithium salts；Electrolyte in described electrolyte is preferably lithium hexafluoro phosphate；Solvent in described electrolyte is preferably one or more in polyvinylpyrrolidone, ethylene carbonate and Allyl carbonate, more preferably diethyl carbonate；In described electrolyte, the molar concentration of electrolyte is preferably 0.1～3mol/L, more preferably 0.5～1.5mol/L, most preferably 1mol/L；Described isolating membrane preferably peels off fiber.In the present invention, according to the technical scheme of assembling ultracapacitor well known to those skilled in the art, directly positive pole, negative pole, isolating membrane and electrolyte that technique scheme provides are assembled, i.e. can get the ultracapacitor that the present invention provides.
For the sake of becoming apparent from, it is described in detail below by following example.
Embodiment 1
Cut arbitrary shape nickel foam (aperture 50～200 μm, specific surface area 0.5～2.0m2/ g), dilute hydrochloric acid (0.5M) takes out after soaking 20min.Oxide layer with the nickel surface that defoams.Nickel foam after above-mentioned immersion is placed and in acetone, supersound washing 10min.By the nickel foam deionized water after washing with acetone and absolute alcohol alternately washing.With other residual impurities of nickel surface that defoam.The most standby.Accurately weigh glucose 12g to be dissolved in 35ml deionized water, add 2mL ethylenediamine, after being uniformly dissolved, proceed in 50ml reactor, above-mentioned dried nickel foam is vertically put in reactor.Being maintained in course of reaction, nickel foam is constantly in standing structure.Reactor is positioned over 190 DEG C of baking ovens.Take out after reaction 12.With medicine spoon, reactant is dug out.Alternately cleaning with ethanol and deionized water, defoam the mesoporous carbon outside nickel volume.Product is positioned under normal temperature condition and is dried 72h, obtain carbon filled and process nickel.
To above-mentioned prepared carbon filled and process nickel shooting digital photograph, result is as shown in Figure 1.Fig. 1 is the carbon filled and process nickel digital photograph figure that the embodiment of the present invention 1 provides, and three black disks of the most numbered 1,2,3 are to repeat according to the method described above to prepare three the carbon filled and process nickel obtained 3 times respectively.As seen in Figure 1, the carbon filled and process nickel that the present embodiment prepares does not has big space, the closeest light tight.
Above-mentioned prepared carbon filled and process nickel is scanned electron microscopic observation, and result is as shown in Figure 2.Fig. 2 is the carbon filled and process nickel scanning electron microscope (SEM) photograph that the embodiment of the present invention 1 provides.As seen in Figure 2, the intact nickel foam skeletal internal that is filled in of glucose after carbonization, substantially can be filled up completely with, take full advantage of the inner space of nickel foam skeleton.
Embodiment 2
Cut arbitrary shape nickel foam (aperture 50～200 μm, specific surface area 0.5～2.0m2/ g), dilute hydrochloric acid (0.5M) takes out after soaking 20min.Oxide layer with the nickel surface that defoams.Nickel foam after above-mentioned immersion is placed and in acetone, supersound washing 10min.By the nickel foam deionized water after washing with acetone and absolute alcohol alternately washing.With other residual impurities of nickel surface that defoam.The most standby.Accurately weighing glucose 12g to be dissolved in 35ml deionized water, adding a certain amount of is Graphene (50mg), adds 2mL ethylenediamine, after being uniformly dissolved, proceeds in 50ml reactor, above-mentioned dried nickel foam vertically put in reactor.Being maintained in course of reaction, nickel foam is constantly in standing structure.Reactor is positioned over 180 DEG C of baking ovens.Take out after reaction 24h.With medicine spoon, reactant is dug out.Alternately cleaning with ethanol and deionized water, defoam the mesoporous carbon outside nickel volume.Product is positioned over lyophilization 72h, obtains carbon filled and process nickel.
Above-mentioned prepared carbon filled and process nickel is scanned electron microscopic observation, and result is as shown in Figure 3 and Figure 4.Fig. 3 is carbon filled and process nickel × 300 scanning electron microscope (SEM) photograph that the embodiment of the present invention 2 provides；Fig. 4 is carbon filled and process nickel × 10,000 scanning electron microscope (SEM) photograph that the embodiment of the present invention 2 provides.As seen in Figure 3, the intact nickel foam skeletal internal that is filled in of glucose after carbonization, substantially can be filled up completely with, take full advantage of the inner space of nickel foam skeleton, the glucose caking property after carbonization is preferable, does not haves the situation coming off or departing from bonding.Glucose after carbonization keeps loose structure as seen in Figure 4, and the transmission for ion provides necessary passage, and the carbon filled and process nickel that therefore the present embodiment provides can use as electrode material.
Embodiment 3
The electric property evaluation of carbon filled and process nickel
The carbon filled and process nickel that embodiment 1 and embodiment 2 prepare is assembled into ultracapacitor, by carrying out repeatedly charge-discharge test, evaluates the electric property of ultracapacitor.
Capacitor specifications is as follows: positive pole and negative material: the carbon filled and process nickel that embodiment 1 or embodiment 2 prepare；Barrier film: polyolefin porous membrane；Electrolyte: 3mol/L lithium hexafluoro phosphate/Allyl carbonate organic solution；Capacitor specifications: positive pole: radius 0.5cm disk, negative pole: radius 0.5cm disk, barrier film: radius 0.5cm disc-shaped polyolefin porous membrane.
Testing result is as shown in Fig. 5～Fig. 7, wherein, Fig. 5 is the ultracapacitor charge-discharge performance cyclic curve figure under different multiplying being assembled into by embodiment 1 carbon filled and process nickel that the embodiment of the present invention 3 provides, Fig. 6 is the ultracapacitor charging and discharging curve figure under different multiplying being assembled into by embodiment 1 carbon filled and process nickel that the embodiment of the present invention 3 provides, and Fig. 7 is the ultracapacitor charge-discharge performance cyclic curve figure under different multiplying being assembled into by embodiment 2 carbon filled and process nickel that the embodiment of the present invention 3 provides.In Fig. 5～Fig. 7,0.1C, 0.2C ... 30C represents that discharge current is 0.1C, 0.2C, 30C respectively, and wherein C represents the capacity of battery.
By Fig. 5 and Fig. 6 it can be seen that the ultracapacitor electricity excellent performance that is assembled into of the carbon filled and process nickel prepared by embodiment 1, capacitance is respectively up to 1000mA h/g, and after 75 circulations, capacity remains at the 70～90% of raw capacity；As seen in Figure 7, embodiment 2 the ultracapacitor electricity excellent performance that the carbon filled and process nickel prepared is assembled into, capacitance is respectively up to 2600mA h/g, and after 75 circulations, capacity remains at the 65～85% of raw capacity；
The above is only the preferred embodiment of the present invention; it should be pointed out that, for those skilled in the art, under the premise without departing from the principles of the invention; can also make some improvements and modifications, these improvements and modifications also should be regarded as protection scope of the present invention.
Claims (10)
1. a preparation method for carbon filled and process nickel, comprises the following steps:
Nickel foam is immersed in carbon source aqueous solution, heats carbonization, obtain carbon filled and process nickel；
Containing glucose and ethylenediamine in described carbon source aqueous solution.
Preparation method the most according to claim 1, it is characterised in that described glucose is at carbon source water
Content in solution is 0.1～0.5g/mL.
Preparation method the most according to claim 1, it is characterised in that described ethylenediamine is at carbon source water
Content in solution is 0.01～0.1mL/mL.
Preparation method the most according to claim 1, it is characterised in that in described carbon source aqueous solution also
Containing carbon materials；Described carbon materials includes Graphene and/or CNT.
Preparation method the most according to claim 4, it is characterised in that described carbon materials is in carbon source
Content in aqueous solution is 1～2mg/mL.
Preparation method the most according to claim 1, it is characterised in that the temperature of described heating carbonization
It it is 160～190 DEG C；The time of described heating carbonization is 12～24h.
Preparation method the most according to claim 1, it is characterised in that the aperture of described nickel foam is
50～200 μm；The specific surface area of described nickel foam is 0.5～2.0m2/g。
Preparation method the most according to claim 1, it is characterised in that the product that heating carbonization obtains
Carry out successively washing and being dried, obtain carbon filled and process nickel.
9. the carbon filled and process nickel that method described in an any one of claim 1～8 prepares.
10. a ultracapacitor, the electrode material of described ultracapacitor includes described in claim 9
Carbon filled and process nickel.
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Application publication date: 20160810 |