CN105314688B - A kind of preparation method and applications of nickel oxide nano piece - Google Patents
A kind of preparation method and applications of nickel oxide nano piece Download PDFInfo
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- CN105314688B CN105314688B CN201510924207.2A CN201510924207A CN105314688B CN 105314688 B CN105314688 B CN 105314688B CN 201510924207 A CN201510924207 A CN 201510924207A CN 105314688 B CN105314688 B CN 105314688B
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- 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 present invention provides a kind of preparation method and applications of nickel oxide nano piece, and preparation method is comprised the following steps：A, by soluble nickel salt, sodium citrate is sufficiently stirred for after mixing in being proportionally added into water, obtain uniform solution, b, four cyano nickel (II) of solubility acid potassium is added to the water after mixing and is sufficiently stirred for, obtain uniform solution, c, the solution solution that step a is obtained being added in step b, then in standing, obtaining growth has light green to precipitate, d, then the light green pelleting centrifugation obtained in step c is collected, deionized water and ethanol are fully washed, products therefrom heat preservation and dryness, subsequently heat treatment is carried out at different temperatures, roasting, both light green nickel oxide nano piece powder body had been obtained.The nickel oxide nano piece can be used for super capacitor electrode.The invention has the beneficial effects as follows the nickel oxide nano piece has larger specific surface area, there is good specific capacity and cycle performance for constructing electrode of super capacitor.
Description
Technical field
The invention belongs to inorganic advanced material technical field and electrochemical energy storage technical field, more particularly, to a kind of oxidation
The preparation method and applications of nickel nano film.
Background technology
Due to larger capacitance amount, power density, energy density and long-life the features such as, in recent years ultracapacitor
Research enjoy people concern (Nanoscale, 2013,5 (10):4378-4387), it is expected to become 21 century new green energy
Source.It is well known that the renewal of electrode material has very important effect to the performance of ultracapacitor.Traditional high-ratio surface
Absorbent charcoal material is used as the electric double layer capacitance that electrode is for increasing capacitor.However, there are the more than ten years centre due to electrode material
Carbon Materials are continued to use always so that the development of ultracapacitor once stayed cool.At the end of last century, along with nanotechnology
Develop rapidly, people have gradually deepened the understanding of the importance in the aperture to the Carbon Materials with high surface, meanwhile, to tool
There are the exploitation of the transition metal oxide of " pseudo capacitance (or oxidoreduction electric capacity) " behavior, be greatly facilitated super
The development of capacitor, most metals oxide belong to Redox interface storing up electricity as storing up electricity mechanism during electrode.In view of mesh
In the research of front ultracapacitor, the specific capacitance of carbon based material is less and the defect such as expensive of ruthenium-based material, and people attempt synthesis
The substituting oxide electrode material (such as nickel oxide, cobalt oxide, manganese oxide etc.) of low price, function admirable.In these replacements
In material, because the advantages of nickel oxide possesses the price of excellent electro-chemical properties and relative moderate, lead in ultracapacitor in the recent period
Domain causes widely studied and concern.Document shows：The energy storage of oxidoreduction electric capacity mainly by electrode material (such as metal oxygen
Compound) surface or near surface redox reaction (Electrochim.Acta, 2005,50,5641-5646).According to this
Energy storage mechnism understands that it is to increase one of effective ways of metal-oxide pseudo capacitance to prepare nano material.By changing
The pattern of metal oxide nano-material, increases the specific surface area of material, improves the aspects such as the pore structure of material, prepared gold
Category oxide-based nanomaterial all shows excellent chemical property.
At present, prepare method that nickel oxide nano piece mainly adopts for：Template, Radiation Synthesis Method, microemulsion method, chemistry
Gas-phase reaction method and hydro-thermal method etc..It should be noted that solwution method and hydro-thermal method are the good methods for preparing nickel oxide nano piece, but
Its most preparation process needs to adjust pH value, and yield is relatively low, it is difficult to large-scale promotion (J.Mater.Chem., 2011,21,
18792-18798；《University of Anhui's journal (natural science edition)》, 03 phase in 2013).Template with nickel salt as raw material is former because of which
Material is expensive, and step is more, unsuitable for industrialized production (J.Mater.Chem., 2011,21,6602-6606).Additionally,
Chemical gas-phase reaction method and Radiation Synthesis Method are special because of the equipment that its preparation needs, and increased production cost.At present, from simplified behaviour
Make to consider with save energy angle, metal organic compound thermal decomposition method is increasingly becoming the main research of synthesis nano-oxide
Method (J.Phys.Chem.C, 2012,116,7227-7235), product prepared by the method have homogeneous structure, soilless sticking, phase
The features such as, duct larger to area is abundant is by many worker's extensive concerns.So far, using metal organic compound heat
Decomposition method prepares the report with two dimension, porous, the nickel oxide material of flaky nanometer structure and its related application and not yet reports.
Therefore, a kind of simple to operate, efficiency high, low cost, eco-friendly preparation method are developed, acquisition structure is homogeneous, duct is rich
The nickel oxide nano sheet material of the features such as rich, surface area is high, controllability is strong, tool are of great significance.
The content of the invention
It is an object of the invention to provide a kind of preparation cost is relatively low, it is easy to accomplish industrialization, implements effective, feasible, be situated between
See the preparation method and applications of the nickel oxide nano piece that structure is remained intact.
The technical scheme is that：The preparation method of the nickel oxide nano piece of the present invention, comprises the following steps：
A, soluble nickel salt, sodium citrate are proportionally added into into in water mixing after be sufficiently stirred for, obtain uniform solution,
It is sufficiently stirred for after b, mixing that four cyano nickel (II) of solubility acid potassium is added to the water, obtains uniform solution,
C, the solution being added to the solution that step a is obtained in step b, then in standing, obtaining growth has light green to sink
Form sediment；
D and then the light green pelleting centrifugation obtained in step c is collected, deionized water and ethanol are fully washed, gained
Product is placed in heat preservation and dryness in vacuum drying oven, subsequently carries out heat treatment at different temperatures, and roasting had both obtained light green oxidation
Nickel nano film powder body.
Further, in step a the soluble nickel salt, the mol ratio of sodium citrate are 1: 2, in step a
The amount of water is 200mL.
Further, in step b, the amount of water is 200mL.
Further, in step a, soluble nickel salt is Nickel dichloride., nickel acetate, nickel nitrate or nickel sulfate.
Further, the time of repose in step c isDwell temperature in step c is
Further, in step d in vacuum drying oven heat preservation and dryness process beTemperature environment in enter
It is capable, when a length of 12 hours.
Further, in step d, heat treatment preferably existsTemperature environment in carry out, ramp isAnd the time is preferably
The nickel oxide nano piece, for electrochemical energy storage field, particularly useful as electrode material for super capacitor.
By countless nano-particle monomer compositions, the nano-particle is nickel oxide to the nickel oxide nano piece, described to receive
Rice piece is two-dimentional porous hexagon or pentagon, and the size of the nanometer blade unit is aboutThickness is about
27nm。
The present invention has the advantages and positive effects that：The method of the invention preparation process is simple, it is easy to operate, do not have
Environmental pollution, low energy consumption, it is reproducible, be appropriate to large-scale industrial production, by the method for the invention obtain oxygen
Change nickel nano film and there is larger specific surface area, there is good specific capacity and cycle performance for constructing electrode of super capacitor
The advantages of.
Description of the drawings
Fig. 1 is the X-ray diffraction spectra figure of sample in embodiment 1 and 2；
Fig. 2 is the low power scanning electron microscope (SEM) photograph of sample in embodiment 1；
Fig. 3 is the high power transmission electron microscope picture of sample in embodiment 2；
Fig. 4 is the specific surface area experiment curv of sample in embodiment 1；
Fig. 5 is the low power scanning electron microscope (SEM) photograph of sample in embodiment 3；
Fig. 6 is cyclic voltammogram of the sample preparation the electrode obtained in the case where difference sweeps speed in embodiment 1；
Fig. 7 is the cyclical stability figure of sample preparation the electrode obtained in embodiment 1.
Specific embodiment
Below in conjunction with the accompanying drawings the present invention is elaborated.
Embodiment 1
Prepare nickel oxide nano piece：
A, Nickel dichloride hexahydrate, sodium citrate are sufficiently stirred for after example 1: 2 is added in 200mL water mixing in molar ratio
2min, obtains uniform solution,
B, four cyano nickel (II) of solubility acid potassium is added in 200mL water mixing after be sufficiently stirred for 2min, obtain homogeneous
Solution,
C, the solution being added to the solution that step a is obtained in step b, then in 20 DEG C of standing 24h of temperature, are grown
There is light green to precipitate；
D then by the light green pelleting centrifugation obtained in step c, washing after, collect and simultaneously dry 12h in temperature 50 C, most
Afterwards in 300 DEG C of roastings, heating rate is 1 DEG C/min, roasting 1h, has both obtained light green nickel oxide nano piece powder body.
As shown in figure 1, the nickel oxide nano piece x-ray powder diffraction instrument for obtaining embodiment 1 is characterized, sample is as a result shown
Product peak is matched with the standard spectrogram of nickel oxide (JCPDS file no.4-835, space group:Fm3m), this explanation experiment
It is successfully prepared nickel oxide nano piece；Fig. 2 is that the low power scanning electron microscope (SEM) photograph result of embodiment 1 shows that sample is received for porous nickel oxide
Rice piece.
As shown in figure 4, being calculated according to experiment curv, the specific surface area of 1 gained nickel oxide nano piece of embodiment is
118.2m2/g。
Nickel oxide nano piece electrochemical property test：
By gained nickel oxide nano sheet material in the embodiment of the present invention 1 and acetylene black and PVDF in mass ratio 75:15:10 mix
Close, then a little N-Methyl pyrrolidone of Deca (NMP) is mixed evenly which, under the pressure of 15MPa is pressed against what is processed
Working electrode is made in nickel foam, electrode area is about 1cm2, thickness about 0.2mm.Electrochemical experimental device adopts three electrodes
System, respectively with saturated calomel electrode as reference electrode, platinum electrode (1cm × 1cm) is that, to electrode, 1M KOH solutions are electric to support
Xie Zhi, is circulated the electro-chemical tests such as volt-ampere and discharge and recharge respectively with CHI760D electrochemical workstations.
Fig. 6 obtains cyclic voltammetry curve under different scanning rates of the product in 1M KOH solutions by embodiment 1.By scheming
It can be seen that, the cyclic voltammetry curve significant difference of material is close to rectangular shape with typical double layer capacitor, and this shows this
The electric capacity of material mostlys come from the fake capacitance based on oxidation-reduction process.
Charge and discharge circulation life curves of the Fig. 7 for 1 nickel oxide active electrode of embodiment.From figure it has also been discovered that, electrode
Specific capacitance gradually decay with the increase of cycle-index, circulation 500 circle after specific capacitance still maintain the 75% of first circle specific capacitance
Left and right, shows preferable cycle performance.
Embodiment 2
Prepare nickel oxide nano piece：
A, Nickel dichloride hexahydrate, sodium citrate are sufficiently stirred for after example 1: 2 is added in 200mL water mixing in molar ratio
2min, obtains uniform solution,
B, four cyano nickel (II) of solubility acid potassium is added in 200mL water mixing after be sufficiently stirred for 2min, obtain homogeneous
Solution,
C, the solution being added to the solution that step a is obtained in step b, then in 20 DEG C of standing 0.5h of temperature, are given birth to
Length has light green to precipitate；
D then by the light green pelleting centrifugation obtained in step c, washing after, collect and simultaneously dry 12h in temperature 60 C, most
Afterwards in 300 DEG C of roastings, heating rate is 1 DEG C/min, roasting 1h, has both obtained light green nickel oxide nano piece powder body.
Fig. 3 is the high power transmission electron microscope picture of gained nickel oxide nano piece in embodiment 2.
Embodiment 3
Prepare nickel oxide nano piece：
A, Nickel dichloride hexahydrate, sodium citrate are sufficiently stirred for after example 1: 2 is added in 200mL water mixing in molar ratio
2min, obtains uniform solution,
B, four cyano nickel (II) of solubility acid potassium is added in 200mL water mixing after be sufficiently stirred for 2min, obtain homogeneous
Solution,
C, the solution being added to the solution that step a is obtained in step b, then in 20 DEG C of standing 24h of temperature, are grown
There is light green to precipitate；
D then by the light green pelleting centrifugation obtained in step c, washing after, collect and simultaneously dry 12h in temperature 50 C, most
Afterwards in 350 DEG C of roastings, heating rate is 1 DEG C/min, roasting 0.5h, has both obtained light green nickel oxide nano piece powder body.
Fig. 5 is the low power scanning electron microscope (SEM) photograph of the nickel oxide nano piece obtained in embodiment 3, as a result shows that sample is porous oxygen
Change nickel nano film.
Embodiment 4
Prepare nickel oxide nano piece：
A, Nickel dichloride hexahydrate, sodium citrate are sufficiently stirred for after example 1: 2 is added in 200mL water mixing in molar ratio
2min, obtains uniform solution,
B, four cyano nickel (II) of solubility acid potassium is added in 200mL water mixing after be sufficiently stirred for 2min, obtain homogeneous
Solution,
C, the solution being added to the solution that step a is obtained in step b, then in 80 DEG C of standing 24h of temperature, are grown
There is light green to precipitate；
D then by the light green pelleting centrifugation obtained in step c, washing after, collect and in 80 DEG C of temperature drying 12h, most
Afterwards in 300 DEG C of roastings, heating rate is 1 DEG C/min, roasting 1h, has both obtained light green nickel oxide nano piece powder body.
Embodiment 5
Prepare nickel oxide nano piece：
A, six hydration nickel sulfate, sodium citrate are sufficiently stirred for after example 1: 2 is added in 200mL water mixing in molar ratio
2min, obtains uniform solution,
B, four cyano nickel (II) of solubility acid potassium is added in 200mL water mixing after be sufficiently stirred for 2min, obtain homogeneous
Solution,
C, the solution being added to the solution that step a is obtained in step b, then in 40 DEG C of standing 24h of temperature, are grown
There is light green to precipitate；
D then by the light green pelleting centrifugation obtained in step c, washing after, collect and simultaneously dry 12h in temperature 70 C, most
Afterwards in 300 DEG C of roastings, heating rate is 2 DEG C/min, roasting 1h, has both obtained light green nickel oxide nano piece powder body.
Embodiment 6
Prepare nickel oxide nano piece：
A, six are hydrated nickel acetates, sodium citrate and are sufficiently stirred for after example 1: 2 is added in 200mL water mixing in molar ratio
2min, obtains uniform solution,
B, four cyano nickel (II) of solubility acid potassium is added in 200mL water mixing after be sufficiently stirred for 2min, obtain homogeneous
Solution,
C, the solution being added to the solution that step a is obtained in step b, then in 30 DEG C of standing 12h of temperature, are grown
There is light green to precipitate；
D then by the light green pelleting centrifugation obtained in step c, washing after, collect and simultaneously dry 12h in temperature 50 C, most
Afterwards in 300 DEG C of roastings, heating rate is 1 DEG C/min, roasting 1h, has both obtained light green nickel oxide nano piece powder body.
Embodiment 7
Prepare nickel oxide nano piece：
A, Nickelous nitrate hexahydrate, sodium citrate are sufficiently stirred for after example 1: 2 is added in 200mL water mixing in molar ratio
2min, obtains uniform solution,
B, four cyano nickel (II) of solubility acid potassium is added in 200mL water mixing after be sufficiently stirred for 2min, obtain homogeneous
Solution,
C, the solution being added to the solution that step a is obtained in step b, then in 30 DEG C of standing 1h of temperature, are grown
There is light green to precipitate；
D then by the light green pelleting centrifugation obtained in step c, washing after, collect and simultaneously dry 12h in temperature 50 C, most
Afterwards in 300 DEG C of roastings, heating rate is 1 DEG C/min, roasting 7h, has both obtained light green nickel oxide nano piece powder body.
Claims (7)
1. a kind of preparation method of nickel oxide nano piece, it is characterised in that：Comprise the following steps：
A, soluble nickel salt, sodium citrate are proportionally added into into in water mixing after be sufficiently stirred for, obtain uniform solution,
It is sufficiently stirred for after b, mixing that solubility potassium tetracyanonickelate is added to the water, obtains uniform solution,
C, the solution solution that step a is obtained being added in step b, then in standing, obtaining growth has light green to precipitate,
D and then the light green pelleting centrifugation obtained in step c is collected, deionized water and ethanol are fully washed, products therefrom
Heat preservation and dryness in vacuum drying oven is placed in, heat treatment is subsequently carried out at different temperatures, roasting had both obtained light green nickel oxide and received
Rice piece powder body.
2. the preparation method of a kind of nickel oxide nano piece according to claim 1, it is characterised in that：In step a
The soluble nickel salt, the mol ratio of sodium citrate are 1: 2, and in step a, the amount of water is 200mL.
3. the preparation method of a kind of nickel oxide nano piece according to claim 1, it is characterised in that：Water in step b
Amount be 200mL.
4. the preparation method of a kind of nickel oxide nano piece according to claim 1, it is characterised in that：Can in step a
Insoluble nickel salt is Nickel dichloride., nickel acetate, nickel nitrate or nickel sulfate.
5. the preparation method of a kind of nickel oxide nano piece according to claim 1, it is characterised in that：In step c
Time of repose isDwell temperature in step c is
6. the preparation method of a kind of nickel oxide nano piece according to claim 1, it is characterised in that：It is true in step d
In empty drying baker heat preservation and dryness process beTemperature environment in carry out, when a length of 12 hours.
7. the preparation method of a kind of nickel oxide nano piece according to claim 1, it is characterised in that：Heat in step d
ProcessTemperature environment in carry out, ramp isAnd the time is
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| CN109187512B (en) * | 2018-09-17 | 2021-07-20 | 四川大学 | Catalytic luminescence analysis method and sensor device for detecting hydrogen sulfide based on nickel oxide |
| CN111686734B (en) * | 2020-06-05 | 2023-08-11 | 苏州机数芯微科技有限公司 | Preparation method and application of magnetic porous nickel nanosheets |
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| CN102603016A (en) * | 2012-03-08 | 2012-07-25 | 中国科学院苏州纳米技术与纳米仿生研究所 | Method for preparing nanometer nickel oxide and application of method |
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