CN103151182A - Nano nickel oxide electrode material and application thereof - Google Patents
Nano nickel oxide electrode material and application thereof Download PDFInfo
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- CN103151182A CN103151182A CN2013100496163A CN201310049616A CN103151182A CN 103151182 A CN103151182 A CN 103151182A CN 2013100496163 A CN2013100496163 A CN 2013100496163A CN 201310049616 A CN201310049616 A CN 201310049616A CN 103151182 A CN103151182 A CN 103151182A
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Abstract
The invention discloses a nano nickel oxide electrode material which is characterized in that a method for preparing the nano nickel oxide electrode material comprises the following steps of: taking lignosulfonate as a template, introducing a nickel ion under a solution state, precipitating and separating the nickel ion after combined reaction, then removing the template and finally obtaining the nano nickel oxide electrode material. The nano nickel oxide electrode material has the beneficial effects that a template agent required by the method is environmentally-friendly and is easy to obtain, and the preparation method is simple. The prepared nano nickel oxide electrode material has the advantages of high specific surface area, good circulation and large-current charging and discharging stability, high specific capacitance and the like and is very suitable for a super capacitor.
Description
Technical field
The invention belongs to electrochemistry and new energy materials field, particularly provide a kind of nano nickel oxide electrode material preparation method and as the application of electrode material for super capacitor.
Background technology
In recent years, development along with electric automobile and various electronic equipments, electrochemical capacitor becomes study hotspot gradually. compares with traditional capacitor, the electrochemical capacitor energy density is higher, operating temperature range is wider. and simultaneously, it has again the incomparable high power density of traditional chemical power supply, long circulation life and superior pulse charge-discharge performance.
Well-known unformed ruthenium oxide hydration is the most promising electrode material of high power high-energy-density ultracapacitor, but expensive scarcity of resources, electrolyte pollution environment used has limited its business development greatly.The oxide electrode materials such as nickel oxide have the function similar to ruthenium oxide hydration, and low price, are subjected to very much researcher's concern.Although explored in recent years the method for multiple synthesis of nano nickel oxide, still exist following problem to need to solve: (1) complicated process of preparation, long flow path; (2) a large amount of organic solvents of the many employings of nano NiO solid that obtain with sol-gel process, in the formation gel process, solvent evaporates is harmful, not environmental protection.(3) in template synthesis nano NiO process, the template cost is higher, is unfavorable for large-scale production.
In addition, studies show that in a large number, the factors such as the chemical property of NiO and pattern, specific area, pore structure are closely related.Usually has the chemical property that the NiO material of high-specific surface area and flourishing pore structure shows more excellent.
Therefore, how to make NiO preparation process technique simple, flow process shortens, the raw material environmental sound of employing, and low grade of cost seems most important.And seek a kind of new preparation method, the NiO material that makes has high-specific surface area, high porosity, long service life, good cycling stability, higher than electric capacity, chemical property is excellent is the important key that realizes modern production.
Summary of the invention
The object of the present invention is to provide a kind of nano nickel oxide electrode material that can be used for ultracapacitor and preparation method thereof.
The technical solution used in the present invention is:
A kind of nano nickel oxide electrode material, described nano nickel oxide electrode material prepares by the following method: lignosulfonates and nickel source are soluble in water, add alkaline matter to obtain reactant liquor, be heated to react 2-3 hour at 70-95 ℃ of (preferred 80 ~ 90 ℃) temperature, generate precipitation, with the centrifugal rear filtration of reaction mixture, Washing of Filter Cake, oven dry, then in 300-600 ℃ of temperature lower calcination 3 ~ 5 hours, to remove template,, make described nano nickel oxide electrode material; Described nickel source is one or more the mixing in nickel nitrate, nickelous sulfate, nickel chloride, preferably sulfuric acid nickel or nickel nitrate; The mass ratio of described nickel source, lignosulfonates is 1:0.6～1, and the quality amount ratio of described alkaline matter and water is 20～40:100.
Described lignosulfonates are one or both in sodium lignin sulfonate, calcium lignosulfonate, preferred sodium lignin sulfonate.
Described alkaline matter is preferably one or more the mixing in the ammoniacal liquor, triethanolamine, triethylamine, potassium hydroxide, hexamethylenetetramine of mass percentage concentration 25%-28%, is preferably hexamethylenetetramine or triethylamine.
Described nickel source is preferably nickel nitrate or nickelous sulfate.
The volumetric usage of described water is counted 20～50mL/g, preferred 20～40mL/g with the quality in nickel source usually.
The temperature of described calcining is preferably 350～450 ℃.
Described Washing of Filter Cake, oven dry with the distilled water washing, are dried 12h-48h usually at 80 ℃ of temperature.
Nano nickel oxide electrode material provided by the invention can be used as electrode material for super capacitor.The method for preparing electrode of super capacitor can adopt and well known to a person skilled in the art the whole bag of tricks.The nano nickel oxide electrode material needs milled processed as last making electrode.
Beneficial effect of the present invention is: nano oxidized method for preparing nickel is simple, and lignosulfonates are cheap and easy to get as the template raw material, does not have the high pollution additives to produce.And the nano oxidized nickel material of preparation has high-specific surface area, and (Fig. 2, specific area reaches 238m
2G
-1), good circulation (Fig. 3) and high current charge-discharge (Fig. 5) stability, the advantages such as high specific capacitance (Fig. 4) are suitable as the electrode material of ultracapacitor very much.The present invention utilizes the biological template lignin of environmental protection cheapness to prepare the New Type of Mesoporous nickel oxide, has the advantages such as high-specific surface area, high specific capacitance, low cost, has a extensive future.
Description of drawings
The TEM figure of the nano nickel oxide electrode material that Fig. 1 embodiment 1 makes.
The desorption absorption figure of the nitrogen of the nano nickel oxide electrode material that Fig. 2 embodiment 1 makes, wherein the little figure in the upper left corner is graph of pore diameter distribution, average pore size is between 5-20nm as can be seen from Figure.
The cyclic voltammetry curve of the nano nickel oxide electrode material that Fig. 3 embodiment 1 makes, in Fig. 3, curve a, b, c are respectively the cyclic voltammetry curve of circulation 10 times, 500 times, 1000 times the time.
The nano nickel oxide electrode material that Fig. 4 embodiment 1 and embodiment 2 make is than the relative cycle-index curve chart of electric capacity, in Fig. 4, curve N a-NiO represents the nano nickel oxide electrode material that embodiment 1 makes, and curve C a-NiO represents the nano nickel oxide electrode material that embodiment 2 makes;
Fig. 5 is the constant current charge-discharge figure of the nano nickel oxide electrode material that makes of embodiment 1
Embodiment
Below in conjunction with specific embodiment, the present invention is conducted further description, but protection scope of the present invention is not limited to this.Embodiment 1
Sample preparation: first 3g sodium lignin sulfonate and 3g nickelous sulfate are dissolved in the 100ml deionized water, after mixing fully, then add the 30g hexamethylenetetramine, heating is stirred to 80 ℃, reacts 3 hours, produces the yellowish-brown precipitation.Centrifugal rear filtration, filter cake washs with distilled water, then puts into 80 ℃ of temperature oven dry 12h of vacuum drying chamber, obtains the yellowish-brown solid.The yellowish-brown solid is sent into Muffle furnace, at 350 ℃, under air atmosphere, calcined 3 hours, make nano nickel oxide electrode material 1g after cooling.The TEM figure of products therefrom as shown in Figure 1.Record through BET specific area method of testing, the specific area of material is 238m
2G
-1, average pore size is distributed between 5-20nm, as shown in Figure 2.
Electrode fabrication: the nano-nickel oxide that makes is ground to form powder, with conductive agent acetylene black, polytetrafluoroethylene PTFE (binding agent) in mass ratio the ratio of 8:1:1 mix, be coated in equably on the nickel foam of accurate weighing, dry post-drying at 10MP pressure lower sheeting, is made work electrode, make reference electrode with the Ag/AgCl electrode, platinized platinum is as auxiliary electrode, and the KOH solution of 6mol/L is that electrolyte consists of three-electrode system, is used for testing chemical property.
Cyclic voltammetry curve as shown in Figure 3, setting parameter is: initial potential 0V, stop current potential 0.7V, sweep speed is 0.02V/s.In Fig. 3, curve a, b, c are respectively circulation 10 times, the cyclic voltammetry curve when 500 times and 1000 times.As can be seen from the figure curvilinear motion is little, and good cycling stability is described.
The cyclic voltammetry curve that obtains according to cyclic voltammetry is by formula
The curve of the relative cycle-index of ratio electric capacity that calculates is as shown in Na-NiO curve in Fig. 4.As can be seen from the figure material circulates through 1000 times, and is from 255F/g to 201F/g, more little than capacitance fade than electric capacity.
Carry out constant current charge-discharge experiment, charging and discharging currents is respectively 1A/g, 2A/g, 4A/g and 10A/g, and voltage range is 0-0.7V, discharge voltage with discharge time change curve as shown in Figure 5, according to formula C
s=I Δ t/m Δ V calculates than electric capacity, can obtain becoming 201F/g than electric capacity from 231F/g when the curent change from 1A/g to 10A/g, and be 87% than electric capacity conservation rate.Illustrative material has reasonable stability under high current charge-discharge, capacitance fade is little.
Embodiment 2
Other operations and reaction condition are with embodiment 1, difference is that sodium lignin sulfonate wherein replaces with the 3g calcium lignosulfonate, hexamethylenetetramine replaces with the 40g triethylamine, and the nano nickel oxide electrode material that makes carries out performance test according to the method for embodiment 1.Record through BET, the specific area of material is 203m
2G
-1, average pore size is distributed between 5-20nm.In cyclic voltammetry, than the curve of the relative cycle-index of electric capacity as shown in Ca-NiO curve in Fig. 4.
Embodiment 3
With embodiment 1, difference is that nickelous sulfate wherein replaces with the 3g nickel nitrate, makes the nano nickel oxide electrode material, carries out performance test according to the method for embodiment 1 with reaction condition in other operations.
In the constant current charge-discharge experiment, material becomes 247F/g than electric capacity from 275F/g when the curent change from 1A/g to 10A/g, be 90% than electric capacity conservation rate.
Embodiment 4
With embodiment 2, difference is that reaction temperature wherein becomes 90 ℃ by 80 ℃ with reaction condition in other operations, and the calcining heat of Muffle furnace becomes 450 ℃ by 350 ℃, makes the nano nickel oxide electrode material, carries out performance test according to the method for embodiment 1.
In the constant current charge-discharge experiment, material becomes 157F/g than electric capacity from 181F/g when the curent change from 1A/g to 10A/g, be 87% than electric capacity conservation rate.
Embodiment 5
With embodiment 1, difference is the 3g nickelous sulfate is become the 5g nickelous sulfate, makes the nano nickel oxide electrode material, carries out performance test according to the method for embodiment 1 with reaction condition in other operations.
In the constant current charge-discharge experiment, material becomes 254F/g than electric capacity from 281F/g when the curent change from 1A/g to 10A/g, be 90% than electric capacity conservation rate.
Claims (6)
1. nano nickel oxide electrode material, it is characterized in that described nano nickel oxide electrode material prepares by the following method: lignosulfonates and nickel source are soluble in water, add alkaline matter to obtain reactant liquor, be heated to react 2-3 hour at 70-95 ℃ of temperature, generate precipitation, with the centrifugal rear filtration of reaction mixture, Washing of Filter Cake, oven dry, in 300-600 ℃ of temperature lower calcination 3 ~ 5 hours, make described nano nickel oxide electrode material again; Described nickel source is one or more the mixing in nickel nitrate, nickelous sulfate, nickel chloride; The mass ratio of described nickel source, lignosulfonates is 1:0.6 ~ 1, and the quality amount ratio of described alkaline matter and water is 20 ~ 40:100.
2. nano nickel oxide electrode material as claimed in claim 1, is characterized in that described lignosulfonates are one or both in sodium lignin sulfonate, calcium lignosulfonate.
3. nano nickel oxide electrode material as claimed in claim 1 is characterized in that described alkaline matter is one or more the mixing in the ammoniacal liquor, triethanolamine, triethylamine, potassium hydroxide, hexamethylenetetramine of mass percentage concentration 25 ~ 28%.
4. nano nickel oxide electrode material as claimed in claim 3, is characterized in that described alkaline matter is hexamethylenetetramine or triethylamine.
5. nano nickel oxide electrode material as claimed in claim 1, the volumetric usage that it is characterized in that described water is counted 20 ~ 50mL/g with the quality in nickel source.
6. nano nickel oxide electrode material as claimed in claim 1 is as the application of electrode material for super capacitor.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103956469A (en) * | 2014-04-28 | 2014-07-30 | 云南大学 | Hollow nanometer pipe-shaped NiO@C compound material and preparation method thereof |
| CN108975307A (en) * | 2018-08-06 | 2018-12-11 | 浙江工业大学 | A kind of preparation method being classified mesoporous carbon nano composite oxides nickel material |
| CN109148829A (en) * | 2018-08-06 | 2019-01-04 | 浙江工业大学 | A kind of biomass derived Nano Carbon nickel oxide electrode and its application |
| CN109166735A (en) * | 2018-08-06 | 2019-01-08 | 浙江工业大学 | A kind of lignin is the preparation method of the combined oxidation nickel capacitor of carbon source |
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| US20070095657A1 (en) * | 2005-11-02 | 2007-05-03 | Kim Dong-Young | Metal oxide supercapacitor having metal oxide electrode coated onto titanium dioxide ultrafine fiber and method for preparing the same |
| CN102385998A (en) * | 2011-12-08 | 2012-03-21 | 南开大学 | NiO electrode material with high specific capacitance and preparation method thereof |
| CN102887550A (en) * | 2012-10-09 | 2013-01-23 | 四川大学 | Method for producing mesoporous nickel oxide |
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2013
- 2013-02-07 CN CN201310049616.3A patent/CN103151182B/en active Active
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| CN1609007A (en) * | 2004-10-21 | 2005-04-27 | 上海交通大学 | Process of preparing porous nickel oxide with plant structure |
| US20070095657A1 (en) * | 2005-11-02 | 2007-05-03 | Kim Dong-Young | Metal oxide supercapacitor having metal oxide electrode coated onto titanium dioxide ultrafine fiber and method for preparing the same |
| CN102385998A (en) * | 2011-12-08 | 2012-03-21 | 南开大学 | NiO electrode material with high specific capacitance and preparation method thereof |
| CN102887550A (en) * | 2012-10-09 | 2013-01-23 | 四川大学 | Method for producing mesoporous nickel oxide |
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| 武拥建等: "胶质碳球为模板制备NiO空心球", 《无机化学学报》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103956469A (en) * | 2014-04-28 | 2014-07-30 | 云南大学 | Hollow nanometer pipe-shaped NiO@C compound material and preparation method thereof |
| CN108975307A (en) * | 2018-08-06 | 2018-12-11 | 浙江工业大学 | A kind of preparation method being classified mesoporous carbon nano composite oxides nickel material |
| CN109148829A (en) * | 2018-08-06 | 2019-01-04 | 浙江工业大学 | A kind of biomass derived Nano Carbon nickel oxide electrode and its application |
| CN109166735A (en) * | 2018-08-06 | 2019-01-08 | 浙江工业大学 | A kind of lignin is the preparation method of the combined oxidation nickel capacitor of carbon source |
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