CN103214043A - Method for preparing graded NiO micro-spherical electrode material by nickel mesh deposition - Google Patents
Method for preparing graded NiO micro-spherical electrode material by nickel mesh deposition Download PDFInfo
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- CN103214043A CN103214043A CN2013101659581A CN201310165958A CN103214043A CN 103214043 A CN103214043 A CN 103214043A CN 2013101659581 A CN2013101659581 A CN 2013101659581A CN 201310165958 A CN201310165958 A CN 201310165958A CN 103214043 A CN103214043 A CN 103214043A
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Abstract
The invention provides a method for preparing a graded NiO micro-spherical electrode material by nickel mesh deposition. The method comprises the following steps of: dissolving 2-6mmol of nickel sulfate (NiSO4.6H2O) in 10ml of distilled water; then adding 1-3mmol of ammonium sulfate ((NH4)2SO4) for ultrasonic dissolving; slowly dropping 3-9mL of ammonia water (25wt%.); magnetically stirring and reacting for 10 minutes; reacting in an oven at 90 DEG C for 3 hours; suspending the nickel mesh in the liquid; continuously reacting for 2-10 hours; naturally cooling to room temperature; washing the product by stilled water; drying for 4-12 hours at 60-90 DEG C to obtain a nickel mesh deposition nickel oxide precursor; and roasting the product at 300-400 DEG C to obtain the product. The technical scheme adopted by the invention is as follows: the NiO graded microspheres grow on a nickel mesh porous support body, so that the material is novel in shape and uniform in grain size. The utilization ratio of active substances and the conducting capacity of electrolyte are greatly improved while the nickel mesh porous structure is maintained. The method is simple in process, high in production efficiency, low in cost and easy to obtain raw materials, mild in reaction condition and low in energy consumption, so that the material has wide application prospect in electrode materials of supercapacitors.
Description
Technical field
The invention belongs to nickel screen and deposit the method for preparing graduation NiO microballoon electrode materials.
Background technology
NiO is very high in the nature abundance, cheap, environmental sound and electrochemical properties are good, has higher specific surface area, oxidation-reduction quality and charge storage characteristic preferably, characteristics such as controlled size, pattern and structural performance make it become one of comparatively ideal electrode materials in the electrochemical capacitor.At present, the investigator adopts prepared in various methods to go out nano particle, nanometer rod, nano wire, nano belt, nano-rings, nanometer sheet, nanotube of nickel oxide etc.Be coated on collection liquid surface as the normal employing of electrode materials and carbon, tetrafluoroethylene sizing agent blended mode, but this method often exists the electrode active material utilization ratio low, shortcomings such as electrode vesicular structure retentivity difference.
Provided by the invention based on nickel screen porous supporting body growth NiO hierarchy microballoon, the pattern novelty, the grain size homogeneous when keeping the nickel screen vesicular structure, can improve the utilization ratio of active substance and the transmissibility of electrolytic solution greatly.This method technology is simple, production efficiency is high, and raw material is cheap and easy to get, and the gentle energy consumption of reaction conditions is low, has a extensive future aspect electrode material for super capacitor.
Summary of the invention
The objective of the invention is nickel screen deposition preparation graduation NiO microballoon electrode materials.
Technical scheme of the present invention is as follows:
(1) pre-treatment of nickel screen: with nickel screen (10mm * 10mm * 1.1mm) respectively at supersound washing in acetone and the ethanol solution, and at 6moldm
-3HCl and 0.1mmoldm
-3NiCl
2Soak 15min and 4h in the solution respectively, last, standby with distilled water wash oven dry back.
(2) with the single nickel salt (NiSO of 2-6mmol
46H
2O) be dissolved in the 10mL distilled water, add the ammonium sulfate ((NH of 1-3 mmol again
4)
2SO
4) ultrasonic dissolution, slow dropping ammonia (25%wt.) 3-9mL, behind the magnetic agitation reaction 10min, in baking oven, behind 90 ℃ of reaction 3h, nickel screen is suspended from the above-mentioned solution, continue reaction 2-10h after, naturally cool to room temperature, behind the product distilled water wash, 60-90 ℃ of dry 4-12h obtains nickel screen deposition nickel oxide precursor.
(3) products therefrom roasting under 300-400 ℃ of condition is promptly obtained product.
Description of drawings
The raw-material SEM photo of Fig. 1 nickel screen.
The SEM photo of the sedimentary hierarchy NiO of Fig. 2 nickel screen microballoon.
Embodiment
Below in conjunction with embodiment technical scheme of the present invention and effect are further described.But employed concrete grammar, prescription and explanation are not limitation of the present invention.
Embodiment 1: with the single nickel salt (NiSO of 3 mmol
46H
2O) be dissolved in the 10mL distilled water, add the ammonium sulfate ((NH of 1.5 mmol again
4)
2SO
4) ultrasonic dissolution, slow dropping ammonia (25%wt.) 4.5mL, behind the magnetic agitation reaction 10min, in baking oven, behind 90 ℃ of reaction 3h, nickel screen is suspended from the above-mentioned solution, after continuing reaction 5h, naturally cool to room temperature, behind the distilled water wash, 60-90 ℃ of dry 4-12h, obtain sedimentary nickel oxide precursor on the nickel screen, roasting in the products therefrom air atmosphere is obtained product.
Embodiment 2: it is 2-6 mmol that the single nickel salt among the embodiment 1 takes by weighing molar weight; The ammonium sulfate molar weight that adds is 1-3mmol; The volume of dropping ammonia is 3-9mL.
Embodiment 3: the reaction times behind the adding nickel screen is 2-10h, and dried powder is heated to 300-400 ℃ with the temperature rise rate of 5-10 ℃/min, roasting 30min-2h under the air conditions.
Embodiment 4: the product that is obtained electron microscope observation, its pattern are the hierarchy microballoons that diameter is about 10-20 μ m.
Claims (4)
1. prepare the method for the NiO microballoon electrode materials of classifying as follows for nickel screen deposition: with the single nickel salt (NiSO of 2-6mmol
46H
2O) be dissolved in the 10mL distilled water, add the ammonium sulfate ((NH of 1-3 mmol again
4)
2SO
4) ultrasonic dissolution, slow dropping ammonia (25%wt.) 3-9mL, behind the magnetic agitation reaction 10min, in baking oven, behind 90 ℃ of reaction 3h, nickel screen is suspended from the above-mentioned solution, after continuing reaction 2-10h, naturally cool to room temperature, behind the product distilled water wash, 60-90 ℃ of dry 4-12h, obtain nickel screen deposition nickel oxide precursor, products therefrom roasting under 300-400 ℃ of condition is promptly obtained product.
2. nickel screen deposition according to claim 1 prepares the method for graduation NiO microballoon electrode materials, it is characterized in that it is 2-6 mmol that described single nickel salt takes by weighing molar weight; The ammonium sulfate molar weight that adds is 1-3mmol; The volume of dropping ammonia is 3-9mL.
3. nickel screen deposition according to claim 1 prepares the method for graduation NiO microballoon electrode materials, the reaction times that it is characterized in that adding behind the nickel screen is 2-10h, dried powder is heated to 300-400 ℃ with the temperature rise rate of 5-10 ℃/min, roasting 30min-2h under the air conditions.
4. nickel screen deposition according to claim 1 prepares the method for graduation NiO microballoon electrode materials, it is characterized in that the product that is obtained electron microscope observation, and its pattern is the hierarchy microballoon that diameter is about 10-20 μ m.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310165958.1A CN103214043B (en) | 2013-05-08 | 2013-05-08 | Nickel screen deposition prepares the method for graduation NiO microballoon electrode materials |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310165958.1A CN103214043B (en) | 2013-05-08 | 2013-05-08 | Nickel screen deposition prepares the method for graduation NiO microballoon electrode materials |
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| Publication Number | Publication Date |
|---|---|
| CN103214043A true CN103214043A (en) | 2013-07-24 |
| CN103214043B CN103214043B (en) | 2015-10-28 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103898549A (en) * | 2013-12-20 | 2014-07-02 | 吉林化工学院 | Method for preparing graded hollow structure NiO/Ni electrode material by microwave process |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110108116A1 (en) * | 2009-11-11 | 2011-05-12 | Korea Institute Of Machinery And Materials | P-type NiO conducting film for organic solar cell, a method for preparation of NiO conducting film, and an organic solar cell with enhanced light-to-electric energy conversion using the same |
| CN102842435A (en) * | 2012-09-14 | 2012-12-26 | 东华大学 | Preparation of three-dimensional NiO-MnOOH core-shell hybrid hierarchical structure material |
| CN102849805A (en) * | 2012-09-14 | 2013-01-02 | 东华大学 | Three-dimensional porous nickel oxide hierarchical material preparation method |
-
2013
- 2013-05-08 CN CN201310165958.1A patent/CN103214043B/en not_active Expired - Fee Related
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20110108116A1 (en) * | 2009-11-11 | 2011-05-12 | Korea Institute Of Machinery And Materials | P-type NiO conducting film for organic solar cell, a method for preparation of NiO conducting film, and an organic solar cell with enhanced light-to-electric energy conversion using the same |
| CN102842435A (en) * | 2012-09-14 | 2012-12-26 | 东华大学 | Preparation of three-dimensional NiO-MnOOH core-shell hybrid hierarchical structure material |
| CN102849805A (en) * | 2012-09-14 | 2013-01-02 | 东华大学 | Three-dimensional porous nickel oxide hierarchical material preparation method |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103898549A (en) * | 2013-12-20 | 2014-07-02 | 吉林化工学院 | Method for preparing graded hollow structure NiO/Ni electrode material by microwave process |
| CN103898549B (en) * | 2013-12-20 | 2017-02-15 | 吉林化工学院 | Method for preparing graded hollow structure NiO/Ni electrode material by microwave process |
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