CN106057501B - A kind of Ni (OH) for ultracapacitor2/ NiSe nano-bar materials and preparation method thereof - Google Patents
A kind of Ni (OH) for ultracapacitor2/ NiSe nano-bar materials and preparation method thereof Download PDFInfo
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Abstract
The Ni (OH) that the invention discloses a kind of for ultracapacitor2/ NiSe nano-bar materials and preparation method thereof.Preparation method includes:Nickel foam is pre-processed, the collector as electrode;Presoma nanometer rods are first grown in foam nickel base;Then by precursor selenizing, you can obtain Ni (OH)2/ NiSe nanometer rods.Preparation method of the present invention is easy to operate, does not need complex device, of low cost;The Ni (OH) of preparation2/ NiSe nanometer rods are evenly distributed, and nanorod surfaces form porous structure.It is tested under three-electrode system, the material is in 1 A g‑1Current density under up to 1763.68 F g‑1Height ratio capacity, material resistance can be down to 0.5 Ω, while having good high rate performance and superior electrochemical stability, is a kind of excellent electrode material for super capacitor.
Description
Technical field
The present invention relates to the field of electrode material for super capacitor, more particularly to a kind of transition gold for ultracapacitor
Belong to hydroxide and selenides combination electrode material and preparation method thereof.
Background technology
With the fast development of global economy, fossil energy constantly consumes, and environmental pollution increasingly sharpens, the future economy and society
A series of global problems of meeting sustainable development are increasingly paid high attention to by countries in the world.In this context, Ren Menzheng
Actively finding and developing various novel clean energy resourcies, such as solar energy, wind energy, tide energy, nuclear energy, biological energy source.In energy
Source domain, a kind of efficient, low cost of exploitation, long-life, environmental-friendly energy conversion and storage system have seemed increasingly
It is important.Wherein, ultracapacitor is a kind of novel energy storage device, and performance is between traditional capacitor and secondary cell, tool
It has the advantage that:Power density is high, is equivalent to 5-10 times of battery;Charge/discharge rates are fast, can be completed in several seconds to a few minutes,
And efficiency for charge-discharge is high;Temperature range is wide, can work in the environment of -40 ~ 70 DEG C;It has extended cycle life;It is non-maintaining, green ring
It protects.Therefore, ultracapacitor is increasingly subject to extensive concern, in consumer electronics, electric power energy, mechanical industry, new-energy automobile, life
There are huge application space and potentiality in the fields such as object sensing, space flight and aviation and military affairs.
Ultracapacitor is mainly made of four positive and negative two electrodes, collector, diaphragm and electrolyte parts, wherein influencing
The most crucial factor of ultracapacitor chemical property is exactly electrode material.Performance more preferably electrode material how is obtained, is section
The personnel of grinding do one's utmost the problem captured.To solve this problem, the Main way of ultracapacitor research and development should be found
Possess the new electrode materials of high power capacity and wide potential window.Electrode material for super capacitor is designed, should include following property:
(1)Specific surface area is big, to obtain more active sites;(2)There is the length of suitable pore-size distribution, gap network and hole
Degree, to promote ion high speed diffusion;(3)Internal conductance wants high in electrode, to provide effective charge transfer;(4)Electrochemistry
Energy and mechanical stability will be got well, to obtain good cycle performance.
In the way of energy stores, ultracapacitor can be divided into two kinds.First, double layer capacitor, electrode material master
If carbon material, in the electrolyte, charge are separated from each other, an electric double layer, the type are generated on carbon electrode/electrolyte interface
Capacitor stores charge and is realized by the electric double layer of electrode and electrolyte interface, only the accumulation of static electricity of surface charge, institute
It is relatively low with specific capacity of double-layer capacitor.Second, Faradic pseudo-capacitor, also referred to as pseudocapacitors, usually with transition metal
Object and conducting polymer are closed as electrode material, using the electrochemical redox reaction of quick electroactive material or in electrode table
The quick adsorption desorption in face stores charge, completes charge and discharge process, the specific capacitance of pseudocapacitors is higher.
Currently, the energy density of ultracapacitor is still relatively low, this is to restrict its widely applied crucial and bottleneck.
The key for improving super capacitor energy density is to improve the specific capacitance of electrode material, compared with double layer capacitor, fake capacitance
Device electrode material has notable higher specific capacitance, thus is the focus of people's research and development.Currently, people are for pseudocapacitors electrode
The research and development of material include mainly:Conducting polymer, transition metal oxide and hydroxide, transient metal sulfide etc..But this
A little materials respectively have disadvantage, and if conducting polymer cyclical stability is poor, oxide and hydroxide conductivity are low, and sulfide also has
The relatively low disadvantage of conductivity, it is even more important that the demand of high-energy density is still not achieved in the specific capacitance of above-mentioned material.Cause
And find a kind of high specific capacitance, high conductivity, high circulation stability electrode material for super capacitor become people and study and produce
The target of industry.
Transition metal selenides has high conductivity, or even has metalline, this characteristic is very beneficial for it and answers
For electrode material for super capacitor.Transition metal selenides is in fields such as catalysis, photocatalytic water, fuel sensitization solar batteries
It is applied, but then considerably less in the research of ultracapacitor and application.Transition metal selenide material and its in super capacitor
Application in device is a very potential research and development field, and the following high-performance super capacitor industrialized development side
To.
Invention content
The present invention is directed to be directed to practical application request, the Ni (OH) of Composite is designed2/ NiSe nano-bar materials, pass through water
Hot method is synthesized, and technological parameter is controlled, and is made it have very more pore structures, is effectively improved the specific surface area and sky of electrode
Between utilization rate, promote the specific capacitance of combination electrode material, make it have good chemical property, become a kind of excellent super
Capacitor electrode material.
Based on the above goal of the invention, technical problem to be solved by the invention is to provide a kind of Ni for ultracapacitor
(OH)2/ NiSe nano-bar materials and preparation method thereof, and the capacitor electrode material that the present invention is prepared has high ratio electricity
Appearance, good high rate performance and superior electrochemical stability;Preparation manipulation is simple, does not need complex device, of low cost.
Specific technical solution is the Ni (OH) that the present invention provides a kind of for ultracapacitor2/ NiSe nano-bars
Material is Ni (OH)2The composite material formed with NiSe has nanometer rods form, nanorod surfaces using nickel foam as growth substrate
For vesicular texture, a diameter of 30 ~ 100nm of nanometer rods, length is 1 ~ 3 μm.
Further, the Ni (OH) produced by the present invention for ultracapacitor2/ NiSe nano-bar materials are in three electrode bodies
In system's test, specific capacitance value can reach 860~1763.68 F g-1, it is 0.5 Ω to have very high specific capacitance, material resistance,
With very high conductivity.
The present invention also provides prepare above-mentioned Ni (OH)2The preparation method of/NiSe nanometer rods super capacitor materials, step
Including:
(1)Nickel foam is put into hydrochloric acid solution, is ultrasonically treated, the NiO layer on surface is removed, washs to neutrality, obtains everywhere
Nickel foam after reason is Ni (OH)2The growth substrate of/NiSe nanometer rods;
(2)Nickel dichloride hexahydrate, sodium hydroxide and water are mixed, stirring obtains Ni (OH)2Precursor solution, wherein
Nickel dichloride hexahydrate, sodium hydroxide, water ratio be 1m mol: 1m mol : 10mL;
(3)By step(2)The precursor solution of middle gained pours into reaction kettle, by step(1)In treated nickel foam
It is put into reaction kettle, carries out hydro-thermal reaction, reaction temperature is 160 ~ 200 DEG C, and time 12h is cooled to room temperature, and collection is attached with
The nickel foam of product is washed, dry.
(4)Selenium powder, sodium borohydride and water are mixed, stirring at room temperature is configured to clear aqueous solution, is the presoma of NiSe
Solution, wherein selenium powder, sodium borohydride, water ratio ratio be 1m mol: 2m mol : 40mL;
(5)By step(4)The precursor solution of middle gained is transferred in reaction kettle, by step(3)The nickel foam of middle gained
It is put into reaction kettle, carries out hydro-thermal reaction, reaction temperature is 120 ~ 180 DEG C, and the time is 6 ~ 12h, is cooled to room temperature, and is collected
It is attached with the nickel foam of final product, is washed, it is dry, obtain the Ni (OH) using nickel foam as substrate2The super electricity of/NiSe nanometer rods
Container material.
In above-mentioned processing step, the temperature and time control of the proportioning, hydro-thermal reaction of each raw material, is to form material of the present invention
The key of material final specific microscopic appearance and chemical composition.
The step(1)Middle concentration of hydrochloric acid is 3 mol L-1, sonication treatment time 30min.
The step(2)Middle mixing time is 30min.
The step(3)Middle washing is respectively with ethyl alcohol, deionized water flushing 3 ~ 5 times.
The step(4)Middle mixing time is 10min.
The step(5)Middle drying temperature is 60 DEG C, drying time 6h.
Above-mentioned growing technology and its each technological parameter are that inventor establishes through many experiments, need stringent accurate control
System, the temperature and time of the proportioning of especially each chemical reagent, order of addition and hydro-thermal reaction are even more crucial parameter, are being sent out
If exceeding above-mentioned parameter range in the experiment of a person of good sense, Ni (OH) can not be obtained2/ NiSe nanometer rod composite materials.
The beneficial effects of the present invention are:
(1)The Ni (OH) that the method for the present invention is prepared2/ NiSe electrode materials are Ni (OH)2With NiSe composite materials,
Thus Ni (OH) is had both2With the advantageous feature of two kinds of materials of NiSe, there is higher internal conductance, it is possible to provide significantly more efficient
Charge transfer.
(2)The Ni (OH) that the method for the present invention is prepared2It is in cavernous nanometer rods that/NiSe electrode materials, which have surface,
Form, the gap between nanometer rods are conducive to electrolyte and are permeated to electrode interior, and the cavernous structure of nanorod surfaces is conducive to
Increase electrode specific surface area, increases contact of the electrolyte with electrode material, obtain more active sites, this pattern and its aperture
It is very beneficial for promoting the high speed diffusion of ion with Size Distribution, and obtains high chemical property.
(3)The Ni (OH) that the method for the present invention is prepared2/ NiSe electrode materials not only have higher specific capacitance, together
When have good high rate performance and superior cyclical stability, electrochemical stability is good, is a kind of excellent super electricity
Container electrode material can be applied to the ultracapacitor product of high-energy density.
(4)The method that the present invention uses hydrothermal synthesis, does not need complex device, easy to operate, is very suitable for industrializing
Batch production.
Description of the drawings
Fig. 1 is Ni (OH) prepared by embodiment 12The scanning electron microscope of/NiSe nano-bar materials(SEM)Figure.
Fig. 2 is Ni (OH) prepared by embodiment 12The x-ray diffraction of/NiSe nano-bar materials(XRD)Figure.
Fig. 3 is Ni (OH) prepared by embodiment 12The cyclic voltammetric of/NiSe nano-bar materials(CV)Figure.
Fig. 4 is Ni (OH) prepared by embodiment 12The constant current charge-discharge curve graph of/NiSe nano-bar materials.
Fig. 5 is Ni (OH) prepared by embodiment 12Specific capacitance figure under the different current densities of/NiSe nano-bar materials.
Fig. 6 is Ni (OH) prepared by embodiment 12The AC impedance figure of/NiSe nano-bar materials.
Specific implementation mode
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment 1
(1)Nickel foam is cut into 4cm × 2cm sizes, is placed on 3 mol L-1In hydrochloric acid solution, ultrasonic reaction 30min is removed
The NiO layer on surface, and treated nickel foam deionized water and ethyl alcohol are washed to neutrality.
(2)Weigh raw material 4m mol Nickel dichloride hexahydrates, 4m mol sodium hydroxides are dissolved in 40 mL water, stirring
30min obtains precursor solution.
(3)Above-mentioned mixed solution is poured into polytetrafluoroethylene (PTFE) hydrothermal reaction kettle, it will be through step(1)The nickel foam of processing is set
In wherein, reaction kettle is put into drying box, 12h is reacted under the conditions of 180 DEG C, reaction kettle is then cooled down to room temperature, collects foam
Nickel uses ethyl alcohol, deionized water to rinse respectively, and dry.
(4)Weigh raw material 1m mol selenium powders, 2m mol sodium borohydrides are dissolved in 40mL water, stir 10min at room temperature, match
It is set to clear aqueous solution and is transferred in reaction kettle.
(5)By step(3)The nickel foam of middle gained is put into step(4)Reaction kettle in, carry out hydro-thermal reaction, reaction temperature
It it is 160 DEG C, time 8h is cooled to room temperature, and collects nickel foam, is washed, dry, obtains the Ni (OH) using nickel foam as substrate2/
NiSe nanometer rods super capacitor materials.
Embodiment 2
(1)Nickel foam is cut into 4cm × 2cm sizes, is so placed on 3 mol L-1In hydrochloric acid solution, ultrasonic reaction 30min is removed
It removes the NiO layer on surface, and treated nickel foam deionized water and ethyl alcohol is washed to neutrality.
(2)Weigh raw material 4m mol Nickel dichloride hexahydrates, 4m mol sodium hydroxides are dissolved in 40 mL water, stirring
30min obtains precursor solution.
(3)Above-mentioned mixed solution is poured into polytetrafluoroethylene (PTFE) hydrothermal reaction kettle, it will be through step(1)The nickel foam of processing is set
In wherein, reaction kettle is put into drying box, 12h is reacted under the conditions of 160 DEG C, reaction kettle is then cooled down to room temperature, collects foam
Nickel uses ethyl alcohol, deionized water to rinse respectively, and dry.
(4)Weigh raw material 1m mol selenium powders, 2m mol sodium borohydrides are dissolved in 40mL water, at room temperature stir 10min match
It is set to clear aqueous solution and is transferred in reaction kettle.
(5)By step(3)The nickel foam of middle gained is put into step(4)Reaction kettle in, carry out hydro-thermal reaction, reaction temperature
It it is 140 DEG C, time 10h is cooled to room temperature, and collects nickel foam, is washed, dry, obtains the Ni using nickel foam as substrate
(OH)2/ NiSe nanometer rods super capacitor materials.
Embodiment 3
(1)Nickel foam is cut into 4cm × 2cm sizes, is so placed on 3 mol L-1In hydrochloric acid solution, ultrasonic reaction 30min is removed
It removes the NiO layer on surface, and treated nickel foam deionized water and ethyl alcohol is washed to neutrality.
(2)Weigh raw material 4m mol Nickel dichloride hexahydrates, 4m mol sodium hydroxides are dissolved in 40 mL water, stirring
30min obtains precursor solution.
(3)Above-mentioned mixed solution is poured into polytetrafluoroethylene (PTFE) hydrothermal reaction kettle, it will be through(1)The nickel foam of processing is placed in it
In, reaction kettle is put into drying box, 12h is reacted under the conditions of 200 DEG C, postcooling reaction kettle to room temperature collects nickel foam, respectively
It is rinsed with ethyl alcohol, deionized water, and dry.
(4)Weigh raw material 1m mol selenium powders, 2m mol sodium borohydrides are dissolved in 40mL water, at room temperature stir 10min match
It is set to clear aqueous solution and is transferred in reaction kettle.
(5)By step(3)The nickel foam of middle gained is put into step(4)Reaction kettle in, carry out hydro-thermal reaction, reaction temperature
It it is 180 DEG C, time 6h is cooled to room temperature, and collects nickel foam, is washed, dry, obtains the Ni (OH) using nickel foam as substrate2/
NiSe nanometer rods super capacitor materials.
Embodiment 4
(1)Nickel foam is cut into 4cm × 2cm sizes, is so placed on 3 mol L-1In hydrochloric acid solution, ultrasonic reaction 30min is removed
It removes the NiO layer on surface, and treated nickel foam deionized water and ethyl alcohol is washed to neutrality.
(2)Weigh raw material 4m mol Nickel dichloride hexahydrates, 4m mol sodium hydroxides are dissolved in 40 mL water, stirring
30min obtains precursor solution.
(3)Above-mentioned mixed solution is poured into polytetrafluoroethylene (PTFE) hydrothermal reaction kettle, it will be through step(1)The nickel foam of processing is set
In wherein, reaction kettle is put into drying box, 12h is reacted under the conditions of 180 DEG C, postcooling reaction kettle to room temperature collects nickel foam,
Ethyl alcohol, deionized water is used to rinse respectively, and dry.
(4)Weigh raw material 1m mol selenium powders, 2m mol sodium borohydrides are dissolved in 40mL water, at room temperature stir 10min match
It is set to clear aqueous solution and is transferred in reaction kettle.
(5)By step(3)The nickel foam of middle gained is put into step(4)Reaction kettle in, carry out hydro-thermal reaction, reaction temperature
It it is 120 DEG C, time 12h is cooled to room temperature, and collects nickel foam, is washed, dry, obtains the Ni using nickel foam as substrate
(OH)2/ NiSe nanometer rods super capacitor materials.
Performance test:
1)SEM is tested:Above-mentioned each example is prepared finally obtained sample to observe under a scanning electron microscope, it is each to implement
Ni (OH) made from example2/ NiSe composite materials have nanometer rods form, and nanorod surfaces are vesicular texture.For example, Fig. 1 is
SEM figures under Sample Scan electron microscope made from embodiment 1, it can be seen that sample microscopic appearance is nanometer rods, a diameter of
30 ~ 100nm, length are 1 ~ 3 μm, nanorod surfaces cellular;Gap between nanometer rods is conducive to electrolyte to electrode interior
Infiltration, the cavernous structure of nanorod surfaces are conducive to increase electrode specific surface area, increase contact of the electrolyte with electrode material,
More active sites are obtained, this pattern and its aperture and Size Distribution are very beneficial for promoting the high speed diffusion of ion, and obtain
Obtain high chemical property.
2)XRD is tested:Above-mentioned each example is prepared into finally obtained sample and carries out XRD tests, it can be verified that each embodiment
Sample obtained is Ni (OH)2With the composite material of NiSe compositions.It is obtained for example, Fig. 2 is sample test made from embodiment 1
XRD diagram, X-ray diffraction peak and Ni (OH)2It is corresponding with the characteristic peak of NiSe, so obtaining sample by Ni (OH)2With NiSe groups
At.
3)Electrochemical property test:By material made from above-mentioned each example be assembled into respectively electrode under three-electrode system into
Row electrochemical property test, Fig. 3 are CV curve of the sample under different surface sweeping rates made from embodiment 1, it can be seen that are had
Apparent redox peaks illustrate that material has good fake capacitance characteristic.Fig. 4 is sample made from embodiment 1 in different electricity
Charging and discharging curve under current density.Fig. 5 is to calculate sample made from the embodiment 1 of gained under different current densities according to Fig. 4
860~1763.68 F g of specific capacitance value-1, show Ni (OH)2/ NiSe nano-bar materials have excellent chemical property.Figure
6 be the AC impedance figure of sample made from embodiment 1, it can be deduced that material resistance is 0.5 ohm, shows Ni (OH)2/ NiSe receives
Rice bar material has satisfactory electrical conductivity.
Claims (8)
1. a kind of Ni (OH) for ultracapacitor2/ NiSe nano-bar materials, it is characterised in that:The Ni (OH)2/ NiSe receives
Rice bar material is Ni (OH)2The composite material formed with NiSe has nanometer rods form, nanometer using nickel foam as growth substrate
Stick surface is vesicular texture, and a diameter of 30 ~ 100nm of nanometer rods, length are 1 ~ 3 μm.
2. a kind of Ni (OH) for ultracapacitor according to claim 12@NiSe nano-bar materials, feature exist
In:The Ni (OH)2/ NiSe nano-bar materials, specific capacitance value can reach 860~1763.68 F g-1, material resistance down to
0.5Ω。
3. preparing a kind of Ni (OH) for ultracapacitor described in any one of claim 1 to 22/ NiSe nano-bar materials
Method, which is characterized in that including step:
1)Nickel foam is put into hydrochloric acid solution, is ultrasonically treated, removes the NiO layer on surface, is washed to neutrality, obtains that treated
Nickel foam is Ni (OH)2The growth substrate of@NiSe nano-bar materials;
2)Nickel dichloride hexahydrate, sodium hydroxide and water are mixed, stirring obtains Ni (OH)2Precursor solution, wherein six hydration
Nickel chloride, sodium hydroxide, water ratio ratio be 1m mol: 1m mol : 10mL;
3)By step 2)The precursor solution of middle gained pours into reaction kettle, by step 1)In treated that nickel foam is put into reaction
Kettle carries out hydro-thermal reaction, and reaction temperature is 160 ~ 200 DEG C, and time 12h is cooled to room temperature, and collection is attached with product
Nickel foam is washed, dry;
4)Selenium powder, sodium borohydride and water are mixed, stirring at room temperature is configured to clear aqueous solution, is the precursor solution of NiSe,
Wherein selenium powder, sodium borohydride, water ratio ratio be 1m mol: 2m mol : 40mL;
5)By step 4)The precursor solution of middle gained is transferred in reaction kettle, by step 3)The nickel foam of middle gained is put into reaction
In kettle, hydro-thermal reaction is carried out, reaction temperature is 120 ~ 180 DEG C, and the time is 6 ~ 12h, is cooled to room temperature, and collection is attached with most
The nickel foam of final product is washed, dry, obtains the Ni (OH) using nickel foam as substrate2/ NiSe nanometer rods super capacitor equipment
Material.
4. a kind of Ni (OH) for ultracapacitor according to claim 32The preparation method of/NiSe nano-bar materials,
It is characterized in that:The step 1)Middle concentration of hydrochloric acid is 3 mol L-1, sonication treatment time 30min.
5. a kind of Ni (OH) for ultracapacitor according to claim 32The preparation method of/NiSe nano-bar materials,
It is characterized in that:The step 2)Middle mixing time is 30min.
6. a kind of Ni (OH) for ultracapacitor according to claim 32The preparation method of/NiSe nano-bar materials,
It is characterized in that:The step 3)Middle washing is respectively with ethyl alcohol, deionized water flushing 3 ~ 5 times.
7. a kind of Ni (OH) for ultracapacitor according to claim 32The preparation method of/NiSe nano-bar materials,
It is characterized in that:The step 4)Middle mixing time is 10min.
8. a kind of Ni (OH) for ultracapacitor according to claim 32The preparation method of/NiSe nano-bar materials,
It is characterized in that:The step 5)Middle drying temperature is 60 DEG C, drying time 6h.
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CN108470646A (en) * | 2018-04-19 | 2018-08-31 | 燕山大学 | Based on the different ultracapacitor and preparation method thereof of material uniformity coefficient |
CN108597899B (en) * | 2018-04-20 | 2019-11-19 | 浙江大学 | NiSe for supercapacitor2-Ni2O3Nanocomposite and preparation method thereof |
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