CN104810160A - Alkali carbonate nickel copper nanowires array and preparation method and use thereof - Google Patents
Alkali carbonate nickel copper nanowires array and preparation method and use thereof Download PDFInfo
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- CN104810160A CN104810160A CN201510145464.6A CN201510145464A CN104810160A CN 104810160 A CN104810160 A CN 104810160A CN 201510145464 A CN201510145464 A CN 201510145464A CN 104810160 A CN104810160 A CN 104810160A
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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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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y30/00—Nanotechnology for materials or surface science, e.g. nanocomposites
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
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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
- H01G11/26—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features
- H01G11/28—Electrodes characterised by their structure, e.g. multi-layered, porosity or surface features arranged or disposed on a current collector; Layers or phases between electrodes and current collectors, e.g. adhesives
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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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- 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 relates to an alkali carbonate nickel copper nanowires array and a preparation method and use thereof. The alkali carbonate nickel copper nanowires array uses foamy coppers as a base, wherein the alkali carbonate nickel copper nanowires are uniformity grown on the foamy coppers, and structural alignment is orderly and regular. Compared with existing technology, the alkali carbonate nickel copper nanowires array has strict requirements on reaction temperature and reaction time of a reactant. The alkali carbonate nickel copper nanowires array is simple and convenient to operate, low in energy consumption and cost of preparation, high in repeatability, high in purity of obtained products, and good in crystalline form and easy to control. Obtained alkali carbonate nickel copper nanowires array can be used as a super capacitor electrode material directly. The alkali carbonate nickel copper nanowires array and the preparation method and the use thereof not only enhance electrical conductivity, but also achieve long stability, and have potential application values on energy storages.
Description
Technical field
The present invention relates to nano material synthesis field, be specifically related to a kind of ambrose alloy subcarbonate nano-wire array, its preparation method and application.
Background technology
Ultracapacitor has the advantages such as power density is high, the charging interval is short, good temp characteristic, long service life.The update of the development of advancing by leaps and bounds along with science and technology and electron stored energy product, the research of electrode material for super capacitor has caused the great interest of researchers.At present, traditional electrode material for super capacitor mainly contains following a few class: material with carbon element class electrode material, conducting polymer class electrode material, metal oxide containing precious metals class electrode material.High performance electrode material for super capacitor need meet following 2 requirements: good conductivity and the specific area of electrode material are large.But, in actual applications, it is found that, more or less all there is respective defect in these traditional electrode materials, as: active area is little, and poorly conductive, capacitance are low, circulation timei is short, energy density and power density little, due to the existence of these defects, be difficult to meet application demand higher in reality.
Summary of the invention
The object of the invention is to the deficiency for conventional electrode materials, the invention provides a kind of ambrose alloy subcarbonate nano-wire array.Present invention also offers a kind of preparation method of ambrose alloy subcarbonate nano-wire array, and application, the ambrose alloy subcarbonate nano-wire array obtained, directly can be used as electrode material for super capacitor.A kind of ambrose alloy subcarbonate nano-wire array material provided by the invention take foam copper as substrate, and ambrose alloy subcarbonate nano wire homoepitaxial is on foam copper, and this structural arrangement is neatly regular.Concrete technical scheme is as follows:
A kind of ambrose alloy subcarbonate nano-wire array, is formed by foam copper and at its epontic ambrose alloy subcarbonate nano-wire array.
A preparation method for ambrose alloy subcarbonate nano-wire array, comprises the following steps:
(1) redistilled water, divalent nickel salt, cupric salt and urea are mixed;
(2) stirring makes its Homogeneous phase mixing, obtains mixed liquor;
(3) mixed liquor is poured in reactor;
(4) foam copper is immersed;
(5) react;
(6) cool;
(7) dry, namely obtain ambrose alloy subcarbonate nano-wire array.
Further, in step (4), foam copper is the foam copper of cleaning rear surface cleaning, and/or, also comprise step before step (1): had on surface the foam copper of impurity to clean up.
Further, step is cooled to room temperature in (6), and/or, drying at room temperature in step (7).
Further, also cleaning step is comprised between step (6) and (7): described cleaning step adopts redistilled water, washes of absolute alcohol.
Further, by reactor confined reaction in step (5), and/or described reaction for react 2-10h at 120-180 DEG C.
Further, described cleaning step is: had on surface the foam copper of impurity to carry out ultrasonic cleaning with acetone, ethanol, redistilled water successively, the ultrasonic cleaning time is 10-20min.
Further, the concentration>=0.1mol L of Nickelous nitrate hexahydrate
-1, the concentration>=0.1mol L of Gerhardite
-1, the concentration>=0.4mol L of urea
-1, the volume>=20mL of redistilled water.
The purposes of above-mentioned ambrose alloy subcarbonate nano-wire array, as the electrode material of ultracapacitor.
Compared with currently available technology, ambrose alloy subcarbonate nano-wire array prepared by the present invention is grown directly upon on foam copper, can directly as the electrode material of ultracapacitor, not only increase conductivity, and achieve long stability, in addition binary composite improves energy density and the power density of material, has potential using value in stored energy.The preparation method of a kind of ambrose alloy subcarbonate nano-wire array provided by the invention, in airtight high-temperature high-pressure reaction kettle, adopt redistilled water as reaction dissolvent, add Nickelous nitrate hexahydrate, Gerhardite, urea mixing, stirring is uniformly mixed liquid, by heating reaction system, produce a hyperbaric environment and prepare a kind of effective ways of ambrose alloy subcarbonate nano-wire array material.The present invention is easy and simple to handle, consumes energy low, and synthesis cost is low, and reappearance is high, and products therefrom purity is high, good crystalline and can controlling.
Accompanying drawing explanation
Fig. 1 is the electron scanning micrograph (SEM) of the low enlargement ratio of ambrose alloy subcarbonate nano-wire array prepared by embodiment 1;
Fig. 2 is the electron scanning micrograph (SEM) of the high magnification of ambrose alloy subcarbonate nano-wire array prepared by embodiment 1;
Fig. 3 is the powder x-ray diffraction figure (XRD) of ambrose alloy subcarbonate nano-wire array prepared by embodiment 1;
Fig. 4 is the transmission electron microscope photo (TEM) of ambrose alloy subcarbonate nano-wire array prepared by embodiment 1
Fig. 5 is the electron scanning micrograph (SEM) of ambrose alloy subcarbonate nano-wire array prepared by embodiment 2;
Fig. 6 is the electron scanning micrograph (SEM) of ambrose alloy subcarbonate nano-wire array prepared by embodiment 3;
Fig. 7 is the electron scanning micrograph (SEM) of ambrose alloy subcarbonate nano-wire array prepared by embodiment 4;
Fig. 8 is the electron scanning micrograph (SEM) of ambrose alloy subcarbonate nano-wire array prepared by embodiment 5;
Fig. 9 is the cyclic voltammetry curve figure (CV) of ambrose alloy subcarbonate nano-wire array prepared by embodiment 1;
Figure 10 is the charging and discharging curve figure of ambrose alloy subcarbonate nano-wire array prepared by embodiment 1;
Figure 11 is the concrete electric capacity-current density correlation curve figure of ambrose alloy subcarbonate nano-wire array prepared by embodiment 1.
Embodiment
Describe the present invention with reference to the accompanying drawings below, it is a kind of preferred embodiment in numerous embodiments of the present invention.
A preparation method for ambrose alloy subcarbonate nano-wire array, comprises the following steps:
A, the foam copper of impurity is had to clean up on surface: had on surface the foam copper of impurity to carry out ultrasonic cleaning with acetone, ethanol, redistilled water successively, the ultrasonic cleaning time is 10-20min;
B, ambrose alloy subcarbonate nano-wire array preparation section:
Redistilled water, divalent nickel salt, cupric salt and urea are mixed, after continuous stirring makes its Homogeneous phase mixing, obtain mixed liquor, pour in reactor, the foam copper of cleaning rear surface cleaning is immersed, reactor is airtight, reaction, is cooled to room temperature, with redistilled water, washes of absolute alcohol, drying at room temperature, namely obtains ambrose alloy subcarbonate nano-wire array.Concentration>=0.1mol the L of Nickelous nitrate hexahydrate used
-1, the concentration>=0.1mol L of Gerhardite
-1, the concentration>=0.4mol L of urea
-1, the volume>=20mL of redistilled water.Described reaction for react 2-10h at 120-180 DEG C.
Prepared ambrose alloy subcarbonate nanowire array growth, can directly as the electrode material of ultracapacitor on foam copper.
Embodiment 1
The clean operation of a, foam copper:
Had on surface the foam copper of impurity to carry out ultrasonic cleaning with acetone, ethanol, redistilled water successively, the ultrasonic cleaning time is 15min;
B, ambrose alloy subcarbonate nano-wire array preparation section:
At normal temperatures, 2mmol Nickelous nitrate hexahydrate, 2mmol Gerhardite and 8mmol urea are dissolved in 20mL redistilled water, continuous stirring makes it be uniformly mixed to form settled solution, pours in 60mL reactor, immerses in mixed liquor by the foam copper handled well, tighten kettle cover, at 160 DEG C, react 6h, take out reactor and naturally cool to room temperature, use redistilled water, washes of absolute alcohol clean successively, naturally dry, namely obtain ambrose alloy subcarbonate nano-wire array.
An application for ambrose alloy subcarbonate nano-wire array, as the application of the electrode material of ultracapacitor.
As shown in Figure 1, the uniform sequential growth of ambrose alloy subcarbonate nano-wire array is on foam copper for the pattern of made ambrose alloy subcarbonate nano-wire array.
Embodiment 2
The clean operation of a, foam copper: identical with embodiment 1;
B, ambrose alloy subcarbonate nano-wire array preparation section:
At normal temperatures, 2mmol Nickelous nitrate hexahydrate, 2mmol Gerhardite and 8mmol urea are dissolved in 20mL redistilled water, continuous stirring makes it be uniformly mixed to form settled solution, pours in 60mL reactor, immerses in mixed liquor by the foam copper handled well, tighten kettle cover, at 160 DEG C, react 2h, take out reactor and naturally cool to room temperature, use redistilled water, washes of absolute alcohol clean successively, naturally dry, namely obtain ambrose alloy subcarbonate nano-wire array.
An application for ambrose alloy subcarbonate nano-wire array, as the application of the electrode material of ultracapacitor.
The pattern of made ambrose alloy subcarbonate nano-wire array as shown in Figure 5.
Embodiment 3
The clean operation of a, foam copper: identical with embodiment 1;
B, ambrose alloy subcarbonate nano-wire array preparation section:
At normal temperatures, 2mmol Nickelous nitrate hexahydrate, 2mmol Gerhardite and 8mmol urea are dissolved in 20mL redistilled water, continuous stirring makes it be uniformly mixed to form settled solution, pours in 60mL reactor, immerses in mixed liquor by the foam copper handled well, tighten kettle cover, at 160 DEG C, react 10h, take out reactor and naturally cool to room temperature, use redistilled water, washes of absolute alcohol clean successively, naturally dry, namely obtain ambrose alloy subcarbonate nano-wire array.
An application for ambrose alloy subcarbonate nano-wire array, as the application of the electrode material of ultracapacitor.
The pattern of made ambrose alloy subcarbonate nano-wire array as shown in Figure 6.
Embodiment 4
The clean operation of a, foam copper: identical with embodiment 1;
B, ambrose alloy subcarbonate nano-wire array preparation section:
At normal temperatures, 2mmol Nickelous nitrate hexahydrate, 2mmol Gerhardite and 8mmol urea are dissolved in 20mL redistilled water, continuous stirring makes it be uniformly mixed to form settled solution, pours in 60mL reactor, immerses in mixed liquor by the foam copper handled well, tighten kettle cover, at 120 DEG C, react 6h, take out reactor and naturally cool to room temperature, use redistilled water, washes of absolute alcohol clean successively, naturally dry, namely obtain ambrose alloy subcarbonate nano-wire array.
An application for ambrose alloy subcarbonate nano-wire array, as the application of the electrode material of ultracapacitor.
The pattern of made ambrose alloy subcarbonate nano-wire array as shown in Figure 7.
Embodiment 5
The clean operation of a, foam copper: identical with embodiment 1;
B, ambrose alloy subcarbonate nano-wire array preparation section:
At normal temperatures, 2mmol Nickelous nitrate hexahydrate, 2mmol Gerhardite and 8mmol urea are dissolved in 20mL redistilled water, continuous stirring makes it be uniformly mixed to form settled solution, pours in 60mL reactor, immerses in mixed liquor by the foam copper handled well, tighten kettle cover, at 180 DEG C, react 6h, take out reactor and naturally cool to room temperature, use redistilled water, washes of absolute alcohol clean successively, naturally dry, namely obtain ambrose alloy subcarbonate nano-wire array.
An application for ambrose alloy subcarbonate nano-wire array, as the application of the electrode material of ultracapacitor.
The pattern of made ambrose alloy subcarbonate nano-wire array as shown in Figure 8.
Embodiment 6 (electrochemical applications)
A kind of ambrose alloy subcarbonate nano-wire array embodiment 1 prepared, is directly used for doing electrode, using KOH solution as electrolyte, does electrochemical properties test.
Get 10mL 6.0M KOH solution and put into electrolysis tank as electrolyte solution, using the electrode of preparation in embodiment 1 as work electrode, connect three-electrode system, open electrochemical workstation.Set relevant parameter, sweep speed for 5mVs
-1time survey cyclic voltammetry curve (in Fig. 9 curve 1), then sweeping speed for 10mV s
-1time survey cyclic voltammetry curve (in Fig. 9 curve 2), the like obtain sweeping speed for 20mV s
-1(in Fig. 9 curve 3), 30mV s
-1(in Fig. 9 curve 4), 50mV s
-1(in Fig. 9 curve 5), 70mV s
-1(in Fig. 9 curve 6), 100mV s
-1(in Fig. 9 curve 7), as can be seen from the CV figure obtained, along with the increase electromotive force sweeping speed is linear.
Get 10mL 6.0M KOH solution and put into electrolysis tank as electrolyte solution, using the electrode of preparation in embodiment 1 as work electrode, connect three-electrode system, open electrochemical workstation.Set relevant parameter, at 1A g
-1time obtain charging and discharging curve (in Figure 10 curve 1), at 2A g
-1time obtain charging and discharging curve (in Figure 10 curve 2), at 3A g
-1time obtain charging and discharging curve (in Figure 10 curve 3), at 5A g
-1time obtain charging and discharging curve (in Figure 10 curve 4), at 10A g
-1time obtain charging and discharging curve (in Figure 10 curve 5), can show that ambrose alloy subcarbonate nano-material compares other material capacity as electrode from charging and discharging curve large, be 1A g by calculating in current density
-1time, maximum concrete electric capacity is 971F g
-1.
Above by reference to the accompanying drawings to invention has been exemplary description; obvious specific implementation of the present invention is not subject to the restrictions described above; as long as have employed the various improvement that method of the present invention is conceived and technical scheme is carried out; or directly apply to other occasion, all within protection scope of the present invention without improving.
Claims (9)
1. an ambrose alloy subcarbonate nano-wire array, is characterized in that, forms by foam copper and at its epontic ambrose alloy subcarbonate nano-wire array.
2. a preparation method for ambrose alloy subcarbonate nano-wire array, is characterized in that, comprises the following steps:
(1) redistilled water, divalent nickel salt, cupric salt and urea are mixed;
(2) stirring makes its Homogeneous phase mixing, obtains mixed liquor;
(3) mixed liquor is poured in reactor;
(4) foam copper is immersed;
(5) react;
(6) cool;
(7) dry, namely obtain ambrose alloy subcarbonate nano-wire array.
3. the preparation method of ambrose alloy subcarbonate nano-wire array as claimed in claim 2, it is characterized in that, in step (4), foam copper is the foam copper of cleaning rear surface cleaning, and/or, also comprise step before step (1): had on surface the foam copper of impurity to clean up.
4. the preparation method of ambrose alloy subcarbonate nano-wire array as claimed in claim 2 or claim 3, it is characterized in that, step is cooled to room temperature in (6), and/or, drying at room temperature in step (7).
5. the preparation method of the ambrose alloy subcarbonate nano-wire array according to any one of claim 2-4, it is characterized in that, between step (6) and (7), also comprise cleaning step: described cleaning step adopts redistilled water, washes of absolute alcohol.
6. the preparation method of the ambrose alloy subcarbonate nano-wire array according to any one of claim 2-5, is characterized in that, by reactor confined reaction in step (5), and/or described reaction for react 2-10h at 120-180 DEG C.
7. the preparation method of ambrose alloy subcarbonate nano-wire array as claimed in claim 5, it is characterized in that, described cleaning step is: had on surface the foam copper of impurity to carry out ultrasonic cleaning with acetone, ethanol, redistilled water successively, the ultrasonic cleaning time is 10-20min.
8. the preparation method of the ambrose alloy subcarbonate nano-wire array according to any one of claim 2-7, is characterized in that, the concentration>=0.1mol L of Nickelous nitrate hexahydrate
-1, the concentration>=0.1mol L of Gerhardite
-1, the concentration>=0.4mol L of urea
-1, the volume>=20mL of redistilled water.
9. the purposes of ambrose alloy subcarbonate nano-wire array as claimed in claim 1, is characterized in that, as the electrode material of ultracapacitor.
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Cited By (3)
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| CN106206049A (en) * | 2016-08-12 | 2016-12-07 | 浙江美都墨烯科技有限公司 | A kind of graphene combination electrode material and preparation method |
| CN113213554A (en) * | 2021-04-28 | 2021-08-06 | 合肥工业大学 | Sea urchin flower shape Ni0.3Co0.6Cu0.1(CO3)0.5Preparation method of (OH) electrode material |
| CN113930782A (en) * | 2021-09-24 | 2022-01-14 | 南京信息工程大学 | Preparation method and application of self-supporting electrode |
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Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106206049A (en) * | 2016-08-12 | 2016-12-07 | 浙江美都墨烯科技有限公司 | A kind of graphene combination electrode material and preparation method |
| CN106206049B (en) * | 2016-08-12 | 2018-02-06 | 浙江美都墨烯科技有限公司 | A kind of graphene combination electrode material and preparation method |
| CN113213554A (en) * | 2021-04-28 | 2021-08-06 | 合肥工业大学 | Sea urchin flower shape Ni0.3Co0.6Cu0.1(CO3)0.5Preparation method of (OH) electrode material |
| CN113213554B (en) * | 2021-04-28 | 2023-09-22 | 合肥工业大学 | Sea urchin flower-like Ni 0.3 Co 0.6 Cu 0.1 (CO 3 ) 0.5 Preparation method of (OH) electrode material |
| CN113930782A (en) * | 2021-09-24 | 2022-01-14 | 南京信息工程大学 | Preparation method and application of self-supporting electrode |
| CN113930782B (en) * | 2021-09-24 | 2023-06-20 | 南京信息工程大学 | Preparation method and application of self-supporting electrode |
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