CN102874884A - Preparation method of super capacitor electrode material (nickel oxide) - Google Patents
Preparation method of super capacitor electrode material (nickel oxide) Download PDFInfo
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- CN102874884A CN102874884A CN2012104389359A CN201210438935A CN102874884A CN 102874884 A CN102874884 A CN 102874884A CN 2012104389359 A CN2012104389359 A CN 2012104389359A CN 201210438935 A CN201210438935 A CN 201210438935A CN 102874884 A CN102874884 A CN 102874884A
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Abstract
The invention relates to a preparation method of a super capacitor electrode material (nickel oxide). The preparation method comprises the steps as follows: nickel nitrate hexahydrate (Ni(NO3)2.6H2O) and polyvinylpyrrolidone (PVP) are dissolved in methanol and water and stirred to prepare a mixed solution; the mixed solution is poured into a polytetrafluoroethylene hydrothermal reaction kettle to react for 3-24 hours under the hydrothermal condition of 150-200 DEG C, and then the reaction kettle is cooled to the room temperature; a product obtained through centrifugation is washed and dried; a dried sample is calcined; and the obtained sample is the super capacitor electrode material. The invention has the advantages that the method is simple and environment-friendly and is low in cost and suitable for mass production; and the prepared porous floriform electrode material (nickel oxide) not only has higher specific capacitance, but also has favorable electrochemical stability, and is a superior super capacitor electrode material.
Description
Technical field
The invention belongs to the preparation field of electrode materials, specifically relate to a kind of preparation method of electrode material for super capacitor nickel oxide.
Background technology
Day by day serious along with the continuous consumption of the fast development of global economy, fossil energy, environmental pollution studied a kind of efficient, low cost, environmental friendliness, high performance Energy conversion and stocking system and seemed more and more important.Electrochemical capacitor also claims ultracapacitor, it is a kind of electrical condenser more excellent than traditional capacitor on performance, because large one more than the order of magnitude of this novel energy device energy Ratios traditional physical capacitor that can store, have again simultaneously the advantages such as power density is high, the duration of charging is short, long service life, be widely used in electromobile, military affairs, the fields such as mobile communication equipment, thus caused the extensive concern of researcher.
Electrochemical capacitor can be divided into two classes according to Charge Storage mechanism: a class is electrochemical capacitor in double electrode layer, and the electrode materials of such electrical condenser mainly is carbon material; Another kind of is the Faraday pseudo-capacitance device, and the electrode materials of such electrical condenser mainly is transition metal oxide.Carbon material has that high-specific surface area, cost are low, the advantage such as have extended cycle life, but it is than the low business development that seriously limits the carbon-based electrode material of electric capacity; Therefore transition metal oxide is considered to optimal electrode materials owing to having high ratio electric capacity and excellent cyclic reversibility.In the transition metal oxide electrode materials, ruthenium oxide receives general concern owing to having very high ratio electric capacity, but it is expensive, low hole, the drawbacks limit such as poisonous its large-scale practical application.
In other transition metal oxide, nickel oxide (NiO) is owing to having environmental friendliness, low-cost, controlled surface and structure properties, the most important thing is, NiO has very high theory than electric capacity (2584F/g), and these advantages make NiO become a kind of ideal electrode material that can satisfy practical application.Till research in front, prepared the NiO electrode materials of multiple different-shape and structure, but the actual specific electric capacity that obtains compares electric capacity far below theory.Development porous electrode material is that at present research the most also is most possibly to improve one of method than electric capacity.Report porous Ni is arranged recently, and then Au deposits MnO thereon as collector
2, can improve than electric capacity (H.G.Zhang, et.al, Nat.Nanotechnol.2011,6,277; X.Y.Lang, et.al, Nat.Nanotechnol.2011,6,232.), but preparation process is complicated, and cost is high, has therefore limited its large-scale practical application.
Summary of the invention
The object of the present invention is to provide a kind of preparation method of electrode material for super capacitor nickel oxide, the method can significantly improve ratio electric capacity and the cyclical stability of NiO electrode materials, simultaneously can be simple, and fast, prepare on a large scale this material and satisfy practical application.
The preparation method of a kind of electrode material for super capacitor nickel oxide of the present invention, step comprises as follows:
(1) takes by weighing Nickelous nitrate hexahydrate Ni (NO
3)
26H
2O and polyvinylpyrrolidone PVP are dissolved in the mixing solutions of methyl alcohol and water, and stir, and make mixing solutions, Ni (NO
3)
26H
2O, PVP proportioning are 2-4mmol:0.05-1g;
(2) above-mentioned mixing solutions is poured in the hydrothermal reaction kettle, reaction is 3-24 hour under the 150-200 ℃ of hydrothermal condition, and rear cooling reactor is to room temperature;
(3) centrifugal resulting product NiO, washing, drying is with dried sample calcining; Namely get electrode material for super capacitor.
The volume ratio of methyl alcohol and water is 47-4 in methyl alcohol in the described step (1) and the mixing solutions of water: 1.
Polyvinylpyrrolidone PVP in the described step (1) is PVP-K25, PVP-K30 or PVP-K90.
Reactor compactedness in the described step (2) is 80%.
Centrifugal resulting product color in the described step (3) is green.
Calcining temperature in the described step (3) is 300-500 ℃.
Calcination time in the described step (3) is 20-200 minute.
Washing in the described step (3) is for using respectively deionized water and washing with alcohol.
Product NiO in the described step (3) is self-assembled into flower-like structure by ultra-thin porous nanometer sheet.
Beneficial effect
(1) the NiO electrode materials for preparing with method of the present invention is the porous flower-like structure, not only has than high specific capacitance, has simultaneously good electrochemical stability, is a kind of good electrode material for super capacitor.
(2) simple, the environmental protection of the preparation method of NiO of the present invention, cost are low, have solved the problem of the large-scale application difficulty of NiO in the ultracapacitor industry.
Description of drawings
Fig. 1 is the NiO electrode materials low power SEM picture of embodiment 1 preparation;
Fig. 2 is the NiO electrode materials high power SEM picture of embodiment 1 preparation;
Fig. 3 is the NiO electrode materials cyclical stability test picture of embodiment 1 preparation.
Embodiment
Embodiment 1
(1) takes by weighing raw material Nickelous nitrate hexahydrate (Ni (NO
3)
26H
2O) 3.4mmol and polyvinylpyrrolidone (PVP) 0.5g is dissolved in the first alcohol and water, and stirs, and makes mixing solutions; Wherein, the volume of described methyl alcohol and water is respectively 43ml, 5ml;
(2) above-mentioned mixing solutions is poured in the tetrafluoroethylene hydrothermal reaction kettle, kept 80% compactedness, described hydrothermal reaction kettle is put into air dry oven, reaction is 6 hours under 180 ℃ of conditions, and rear cooling reactor is to room temperature.
(3) centrifugal resulting product, respectively with deionized water and alcohol solvent washing, and dry; Dried sample is put into retort furnace 450 ℃ of calcinings 40 minutes; Resulting final black sample is ultracapacitor nickel oxide electrode material.
Embodiment 2
(1) takes by weighing raw material Nickelous nitrate hexahydrate (Ni (NO
3)
26H
2O) 2mmol and polyvinylpyrrolidone (PVP) 0.05g is dissolved in the first alcohol and water, and stirs, and makes mixing solutions; Wherein, the volume of described methyl alcohol and water is respectively 41ml, 7ml;
(2) above-mentioned mixing solutions is poured in the tetrafluoroethylene hydrothermal reaction kettle, kept 80% compactedness, described hydrothermal reaction kettle is put into air dry oven, reaction is 24 hours under 150 ℃ of conditions, and rear cooling reactor is to room temperature.
(3) centrifugal resulting product, respectively with deionized water and alcohol solvent washing, and dry; Dried sample is put into retort furnace 450 ℃ of calcinings 40 minutes; Resulting final black sample is ultracapacitor nickel oxide electrode material.
Embodiment 3
(1) takes by weighing raw material Nickelous nitrate hexahydrate (Ni (NO
3)
26H
2O) 4mmol and polyvinylpyrrolidone (PVP) 1g is dissolved in the first alcohol and water, and stirs, and makes mixing solutions; Wherein, the volume of described methyl alcohol and water is respectively 40ml, 8ml;
(2) above-mentioned mixing solutions is poured in the tetrafluoroethylene hydrothermal reaction kettle, kept 80% compactedness, described hydrothermal reaction kettle is put into air dry oven, reaction is 3 hours under 180 ℃ of conditions, and rear cooling reactor is to room temperature.
(3) centrifugal resulting product, respectively with deionized water and alcohol solvent washing, and dry; Dried sample is put into retort furnace 450 ℃ of calcinings 40 minutes; Resulting final black sample is ultracapacitor nickel oxide electrode material.
Embodiment 4
(1) takes by weighing raw material Nickelous nitrate hexahydrate (Ni (NO
3)
26H
2O) 3.4mmol and polyvinylpyrrolidone (PVP) 0.5g is dissolved in the first alcohol and water, and stirs, and makes mixing solutions; Wherein, the volume of described methyl alcohol and water is respectively 40ml, 8ml;
(2) above-mentioned mixing solutions is poured in the tetrafluoroethylene hydrothermal reaction kettle, kept 80% compactedness, described hydrothermal reaction kettle is put into air dry oven, reaction is 24 hours under 180 ℃ of conditions, and rear cooling reactor is to room temperature.
(3) centrifugal resulting product, respectively with deionized water and alcohol solvent washing, and dry; Dried sample is put into retort furnace 450 ℃ of calcinings 40 minutes; Resulting final black sample is ultracapacitor nickel oxide electrode material.
Claims (8)
1. the preparation method of an electrode material for super capacitor nickel oxide comprises:
(1) takes by weighing Nickelous nitrate hexahydrate Ni (NO
3)
26H
2O and polyvinylpyrrolidone PVP are dissolved in the mixing solutions of methyl alcohol and water, and stir, and make mixing solutions, Ni (NO
3)
26H
2O, PVP proportioning are 2-4mmol:0.05-1g;
(2) above-mentioned mixing solutions is poured in the hydrothermal reaction kettle, reaction is 3-24 hour under the 150-200 ℃ of hydrothermal condition, and rear cooling reactor is to room temperature;
(3) centrifugal resulting product NiO, washing, drying is with dried sample calcining; Namely get electrode material for super capacitor.
2. the preparation method of described a kind of electrode material for super capacitor nickel oxide according to claim 1, it is characterized in that: the volume ratio of methyl alcohol and water is 47-4 in the methyl alcohol in the described step (1) and the mixing solutions of water: 1.
3. the preparation method of described a kind of electrode material for super capacitor nickel oxide according to claim 1, it is characterized in that: the polyvinylpyrrolidone PVP in the described step (1) is PVP-K25, PVP-K30 or PVP-K90.
4. the preparation method of described a kind of electrode material for super capacitor nickel oxide according to claim 1, it is characterized in that: the reactor compactedness in the described step (2) is 80%.
5. the preparation method of described a kind of electrode material for super capacitor nickel oxide according to claim 1, it is characterized in that: the calcining temperature in the described step (3) is 300-500 ℃.
6. the preparation method of described a kind of electrode material for super capacitor nickel oxide according to claim 1, it is characterized in that: the calcination time in the described step (3) is 20-200 minute.
7. the preparation method of described a kind of electrode material for super capacitor nickel oxide according to claim 1, it is characterized in that: the washing in the described step (3) is for using respectively deionized water and washing with alcohol.
8. the preparation method of described a kind of electrode material for super capacitor nickel oxide according to claim 1, it is characterized in that: the product NiO in the described step (3) is self-assembled into flower-like structure by ultra-thin porous nanometer sheet.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104098147A (en) * | 2014-07-16 | 2014-10-15 | 兰州大学 | Preparation of rose-shaped NiO nanometer particles through electrochemical method |
| CN105469901A (en) * | 2015-11-20 | 2016-04-06 | 燕山大学 | In-situ-growth-based method for preparing nickel hydroxide-nickel oxide film electrode |
| CN112062170A (en) * | 2020-09-09 | 2020-12-11 | 中国海洋大学 | Hydrothermal preparation method of nickel oxide electrochromic film with graded porous morphology and structure |
| CN113184925A (en) * | 2021-04-25 | 2021-07-30 | 沈阳大学 | MnO with core-shell structure2Preparation method of/NiO binary composite material |
-
2012
- 2012-11-06 CN CN2012104389359A patent/CN102874884A/en active Pending
Non-Patent Citations (2)
| Title |
|---|
| 《CrystEngComm》 20110609 Yinfang Cui et al. "Lotus-root-like NiO nanosheets and flower-like NiO microspheres: synthesis and magnetic properties" 第4930-4934页 1-10 , * |
| YINFANG CUI ET AL.: ""Lotus-root-like NiO nanosheets and flower-like NiO microspheres: synthesis and magnetic properties"", 《CRYSTENGCOMM》 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104098147A (en) * | 2014-07-16 | 2014-10-15 | 兰州大学 | Preparation of rose-shaped NiO nanometer particles through electrochemical method |
| CN104098147B (en) * | 2014-07-16 | 2016-05-11 | 兰州大学 | There is the NiO nano particle of rose-shaped shape characteristic with electrochemical method preparation |
| CN105469901A (en) * | 2015-11-20 | 2016-04-06 | 燕山大学 | In-situ-growth-based method for preparing nickel hydroxide-nickel oxide film electrode |
| CN112062170A (en) * | 2020-09-09 | 2020-12-11 | 中国海洋大学 | Hydrothermal preparation method of nickel oxide electrochromic film with graded porous morphology and structure |
| CN113184925A (en) * | 2021-04-25 | 2021-07-30 | 沈阳大学 | MnO with core-shell structure2Preparation method of/NiO binary composite material |
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Application publication date: 20130116 |