CN105895388A - Preparation method for three-dimensional porous sheet-shaped zinc cobaltate nanomaterial - Google Patents
Preparation method for three-dimensional porous sheet-shaped zinc cobaltate nanomaterial Download PDFInfo
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- CN105895388A CN105895388A CN201610433812.4A CN201610433812A CN105895388A CN 105895388 A CN105895388 A CN 105895388A CN 201610433812 A CN201610433812 A CN 201610433812A CN 105895388 A CN105895388 A CN 105895388A
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- porous sheet
- dimensional porous
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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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- 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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- 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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- 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 provides a preparation method for a three-dimensional porous sheet-shaped zinc cobaltate nanomaterial. The preparation method is characterized in that the zinc cobaltate nanomaterial structure is grown in a tiled manner, and adopts the porous sheet-shaped three-dimensional structure. Compared with the prior art, the product obtained by the preparation method has high purity and dispersity, good and controllable crystalline form, low production cost, and high reproducibility; the prepared three-dimensional porous sheet-shaped zinc cobaltate nanomaterial is grown on foamed nick, which can be directly used as the electrode material of a supercapacitor; and therefore, high cycling stability and high capacity are realized, so that the zinc cobaltate nanomaterial has a potential application value in energy storage.
Description
Technical field
The invention belongs to technical field of nano material, relate to the preparation method of a kind of three-dimensional porous sheet cobalt acid zinc nano material.
Background technology
The development advanced by leaps and bounds along with science and technology and the update of electronic 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 has following a few class: material with carbon element class electrode material, conducting polymer species electrode material, metal oxide-type electrode material.But, in actual applications, it is found that, the most all there is respective defect in these traditional electrode materials, such as: active area is little, poorly conductive, capacitance are low, circulation timei is short, energy density and power density are little, due to the existence of these defects, are difficult to meet higher application demand in reality.
Summary of the invention
For solving above-mentioned technical problem, the present invention provides the preparation method of a kind of three-dimensional porous sheet cobalt acid zinc nano material, and prepared material can be directly as the electrode material of ultracapacitor.
Present invention also offers the application of a kind of three-dimensional porous sheet cobalt acid zinc nano material.
The present invention provide three-dimensional porous sheet cobalt acid zinc nano material, this structure tiling growth, in porous flake, the three-dimensional structure having.
The preparation method of a kind of three-dimensional porous sheet cobalt acid zinc nano material that the present invention provides, comprises the following steps:
A, surface have the nickel foam of impurity clean up；
B, redistilled water, zinc chloride, CoCL2 6H2O, urea and ammonium fluoride are mixed, obtain mixed liquor, add in reactor, nickel foam after cleaning immerses in mixed liquor, and reactor is airtight, reacts 7-12 h at 100-160 DEG C, it is cooled to room temperature, clean, drying at room temperature, i.e. prepare the nickel foam growing three-dimensional porous sheet cobalt acid zinc nano material.
The cleaning method of step a is: surface has the nickel foam of impurity be sequentially placed in ethanol, acetone, watery hydrochloric acid, redistilled water and carries out ultrasonic cleaning, and the ultrasonic cleaning time is respectively 10-20 min.
In mixed solution obtained by step b, chlorination zinc concentration >=0.008 mol/L, concentration >=0.016 mol/L of CoCL2 6H2O, concentration >=0.040 mol/L of urea, concentration >=0.008 mol/L of ammonium fluoride, volume >=25 mL of redistilled water.In step c, potassium permanganate concentration in mixed liquor is 0.009-0.04 mol/L, and the concentration of the concentrated hydrochloric acid added is 12 mol/L.The volume of concentrated hydrochloric acid is: 0.1-0.3
ML, concentrated hydrochloric acid is about 1:260 with the volume ratio of distilled water)
The application of a kind of three-dimensional porous sheet cobalt acid zinc nano material that the present invention provides, as the electrode material of ultracapacitor.
A kind of method preparing three-dimensional porous sheet cobalt acid zinc nano material that the present invention provides, it is in airtight high-temperature high-pressure reaction kettle, use redistilled water as reaction dissolvent, add zinc chloride, CoCL2 6H2O, urea and ammonium fluoride to mix, by heating reaction system, produce a hyperbaric environment and prepare three-dimensional porous sheet cobalt acid zinc nano material.With prior art is compared, preparation method product purity height that the present invention provides, good dispersion, good crystalline and can controlling, production cost is low, favorable reproducibility.Prepared three-dimensional porous sheet cobalt acid zinc nano material is grown in nickel foam, can be directly as the electrode material of ultracapacitor, achieve long cyclical stability, big concrete electric capacity, high energy density and power density, there is in terms of energy storage potential using value.
Detailed description of the invention
Embodiment 1
The preparation method of a kind of three-dimensional porous sheet cobalt acid zinc nano material, comprises the following steps:
A, surface has the nickel sheet of impurity be sequentially placed in ethanol, acetone, watery hydrochloric acid, redistilled water carry out ultrasonic cleaning 15 min；
B, 25 mL redistilled waters, 0.2 mmol zinc chloride, 0.4 mmol CoCL2 6H2O, 1 mmol urea and 0.4 mmol ammonium fluoride are mixed after add in 60 mL reactors, the nickel foam processed is immersed in mixed liquor, tighten kettle cover, 9 h are reacted at 120 DEG C, take out reactor and naturally cool to room temperature, rinse well with ethanol, redistilled water successively, drying at room temperature, i.e. prepare the nickel foam growing three-dimensional porous sheet cobalt acid zinc nano material.
The application of a kind of three-dimensional porous sheet cobalt acid zinc nano material, as the electrode material of ultracapacitor.
Made three-dimensional porous sheet cobalt acid zinc nano material pattern for tiling growth, in porous flake, the three-dimensional structure having.
Take 10 mL 0.1 M NaOH solution and put in electrolytic cell as electrolyte solution, as working electrode, be 5 mV ss sweeping speed using the three-dimensional porous sheet cobalt acid zinc nano material of preparation in embodiment 1-1Time survey cyclic voltammetry curve, be then 10 mV s sweeping speed-1Time survey cyclic voltammetry curve, the like to obtain sweeping speed be 20 mV s-1、50 mV s-1、100 mV s-1, from obtain CV figure it can be seen that along with sweep speed increase voltage linear relation.
Take 10 mL 0.1 M NaOH solution and put in electrolytic cell as electrolyte solution, using the three-dimensional porous sheet cobalt acid zinc nano material of preparation is as working electrode in embodiment 1, at 5A g-1Time obtain charging and discharging curve, at 10A g-1Time obtain charging and discharging curve, at 20 A g-1Time obtain charging and discharging curve, at 30A g-1Time obtain charging and discharging curve, at 40 A g-1Time obtain charging and discharging curve, can show that three-dimensional porous sheet cobalt acid zinc nano material is compared other material as electrode and had higher capacitance from charging and discharging curve.
Embodiment 2
The preparation method of a kind of three-dimensional porous sheet cobalt acid zinc nano material, comprises the following steps:
A, surface has the nickel sheet of impurity be sequentially placed in ethanol, acetone, watery hydrochloric acid, redistilled water carry out ultrasonic cleaning 15 min；
B, 30 mL redistilled waters, 0.3 mmol zinc chloride, 0.4 mmol CoCL2 6H2O, 2 mmol urea and 0.5 mmol ammonium fluoride are mixed after add in 60 mL reactors, the nickel foam processed is immersed in mixed liquor, tighten kettle cover, 9 h are reacted at 100 DEG C, take out reactor and naturally cool to room temperature, rinse well with ethanol, redistilled water successively, drying at room temperature, i.e. prepare the nickel foam of three-dimensional porous sheet cobalt acid zinc nano material.
The application of a kind of three-dimensional porous sheet cobalt acid zinc nano material, as the electrode material of ultracapacitor.
Embodiment 3
The preparation method of a kind of three-dimensional porous sheet cobalt acid zinc nano material, comprises the following steps:
A, surface has the nickel sheet of impurity be sequentially placed in ethanol, acetone, hydrochloric acid, redistilled water carry out ultrasonic cleaning 15 min；
B, 25 mL redistilled waters, 0.3 mmol zinc chloride, 0.6 mmol CoCL2 6H2O, 1 mmol urea and 0.4 mmol ammonium fluoride are mixed after add in 60 mL reactors, the nickel foam processed is immersed in mixed liquor, tighten kettle cover, 5 h are reacted at 160 DEG C, take out reactor and naturally cool to room temperature, rinse well with ethanol, redistilled water successively, drying at room temperature, i.e. prepare the nickel foam growing cobalt acid zinc nano-wire array.
The application of a kind of three-dimensional porous sheet cobalt acid zinc nano material, as the electrode material of ultracapacitor.
Embodiment 4
The preparation method of a kind of three-dimensional porous sheet cobalt acid zinc nano material, comprises the following steps:
A, surface has the nickel sheet of impurity be sequentially placed in ethanol, acetone, watery hydrochloric acid, redistilled water carry out ultrasonic cleaning 20 min；
B, 25 mL redistilled waters, 0.4 mmol zinc chloride, 0.6 mmol CoCL2 6H2O, 2 mmol urea and 0.6mmol ammonium fluoride are mixed after add in 60 mL reactors, the nickel foam processed is immersed in mixed liquor, tighten kettle cover, 5 h are reacted at 150 DEG C, take out reactor and naturally cool to room temperature, rinse well with ethanol, redistilled water successively, drying at room temperature, i.e. prepare the nickel foam growing cobalt acid zinc nano-wire array.
The application of a kind of three-dimensional porous sheet cobalt acid zinc nano material, as the electrode material of ultracapacitor.
Embodiment 5
The preparation method of a kind of three-dimensional porous sheet cobalt acid zinc nano material, comprises the following steps:
A, surface has the nickel sheet of impurity be sequentially placed in ethanol, acetone, watery hydrochloric acid, redistilled water carry out ultrasonic cleaning 10 min；
B, 25 mL redistilled waters, 0.2 mmol zinc chloride, 0.6 mmol CoCL2 6H2O, 3 mmol urea and 0.4 mmol ammonium fluoride are mixed after add in 60 mL reactors, the nickel foam processed is immersed in mixed liquor, tighten kettle cover, 7 h are reacted at 110 DEG C, take out reactor and naturally cool to room temperature, rinse well with ethanol, redistilled water successively, drying at room temperature, i.e. prepare the nickel foam growing cobalt acid zinc nano-wire array.
The application of a kind of three-dimensional porous sheet cobalt acid zinc nano material, as the electrode material of ultracapacitor.
Claims (3)
1. the preparation method of a three-dimensional porous sheet cobalt acid zinc nano material, it is characterised in that comprise the following steps:
A, surface have the nickel foam of impurity clean up；
B, redistilled water, zinc chloride, CoCL2 6H2O, urea and ammonium fluoride are mixed, obtain mixed liquor, add in reactor, nickel foam after cleaning immerses in mixed liquor, and reactor is airtight, reacts 7-12 h at 100-160 DEG C, it is cooled to room temperature, clean, drying at room temperature, i.e. prepare the nickel foam growing three-dimensional porous sheet cobalt acid zinc nano material.
The preparation method of the most three-dimensional porous sheet cobalt acid zinc nano material, it is characterized in that, the cleaning method of step a is: surface has the nickel foam of impurity be sequentially placed in ethanol, acetone, watery hydrochloric acid, redistilled water and carries out ultrasonic cleaning, and the ultrasonic cleaning time is respectively 10-20 min.
The preparation method of the most three-dimensional porous sheet cobalt acid zinc nano material, it is characterized in that, in mixed solution obtained by step b, chlorination zinc concentration >=0.008 mol/L, concentration >=0.016 mol/L of CoCL2 6H2O, concentration >=0.040 mol/L of urea, concentration >=0.008 mol/L of ammonium fluoride, volume >=25 mL of redistilled water.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106356198A (en) * | 2016-09-23 | 2017-01-25 | 安徽师范大学 | Mesoporous ZnCo2O4 nanosheet and NiCo2O4 nanowire composite material and preparation method and application thereof |
| CN109273283A (en) * | 2018-09-28 | 2019-01-25 | 哈尔滨商业大学 | A kind of preparation method of nickel foam/molybdic acid nickel cobalt acid zinc laminated film |
| CN109637824A (en) * | 2018-11-27 | 2019-04-16 | 山东大学 | A kind of New Co Fe for supercapacitor2S4Nanometer sheet/nickel foam composite material and preparation method |
| CN111593346A (en) * | 2019-02-20 | 2020-08-28 | 天津理工大学 | Inorganic super-hydrophobic anti-ice structure with hierarchical pore structure and preparation method and application thereof |
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| CN102664103A (en) * | 2012-03-31 | 2012-09-12 | 华中科技大学 | Zinc cobaltate nanorod/foam nickel composite electrode, preparation method thereof and application thereof |
| CN103440998A (en) * | 2013-08-21 | 2013-12-11 | 吉林大学 | Zinc cobaltate nanosheet array/foamed nickel combined electrode, preparation method and application thereof |
| CN104465117A (en) * | 2014-11-08 | 2015-03-25 | 安徽师范大学 | ZnCo2O4@MnO core-shell heterostructure nanotube array material, and preparation method and application thereof |
-
2016
- 2016-06-18 CN CN201610433812.4A patent/CN105895388A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102664103A (en) * | 2012-03-31 | 2012-09-12 | 华中科技大学 | Zinc cobaltate nanorod/foam nickel composite electrode, preparation method thereof and application thereof |
| CN103440998A (en) * | 2013-08-21 | 2013-12-11 | 吉林大学 | Zinc cobaltate nanosheet array/foamed nickel combined electrode, preparation method and application thereof |
| CN104465117A (en) * | 2014-11-08 | 2015-03-25 | 安徽师范大学 | ZnCo2O4@MnO core-shell heterostructure nanotube array material, and preparation method and application thereof |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106356198A (en) * | 2016-09-23 | 2017-01-25 | 安徽师范大学 | Mesoporous ZnCo2O4 nanosheet and NiCo2O4 nanowire composite material and preparation method and application thereof |
| CN106356198B (en) * | 2016-09-23 | 2018-08-17 | 安徽师范大学 | A kind of mesoporous ZnCo2O4Nanometer sheet@NiCo2O4Nanowire composite, preparation method and applications |
| CN109273283A (en) * | 2018-09-28 | 2019-01-25 | 哈尔滨商业大学 | A kind of preparation method of nickel foam/molybdic acid nickel cobalt acid zinc laminated film |
| CN109637824A (en) * | 2018-11-27 | 2019-04-16 | 山东大学 | A kind of New Co Fe for supercapacitor2S4Nanometer sheet/nickel foam composite material and preparation method |
| CN111593346A (en) * | 2019-02-20 | 2020-08-28 | 天津理工大学 | Inorganic super-hydrophobic anti-ice structure with hierarchical pore structure and preparation method and application thereof |
| CN111593346B (en) * | 2019-02-20 | 2022-10-18 | 天津理工大学 | Inorganic super-hydrophobic anti-ice structure with hierarchical pore structure and preparation method and application thereof |
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