CN106098402B - A kind of CoNiSe for ultracapacitor2Nano-array material and preparation method thereof - Google Patents
A kind of CoNiSe for ultracapacitor2Nano-array material and preparation method thereof Download PDFInfo
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Abstract
The invention discloses a kind of CoNiSe for ultracapacitor2Nano-array material and preparation method thereof.Preparation process includes：Nickel foam is pre-processed, the collector as electrode；Precursor nanosphere is first grown in foam nickel base；Then by precursor selenizing, you can obtain CoNiSe2Nano-array.Preparation method of the present invention is easy to operate, does not need complex device, of low cost；The CoNiSe of preparation2In nano array structure, nano-array is by CoNiSe2The surface of nanometer rods and nanotube composition, a diameter of 50 ~ 100nm of nanometer rods and nanotube, nanometer rods and nanotube is vesicular texture.CoNiSe produced by the present invention2Nano-array material is in 1 A g‑1Current density under show 1338F g‑1Height ratio capacity, while there is good high rate performance and superior electrochemical stability, be 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 binary selenides 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.The exploitation of transition metal selenide material and its super
Application in grade capacitor be international forward position research and development field and high-energy density super capacitor industrialization it is important
And very potential developing direction.
Invention content
The present invention is directed to design CoNiSe2Nano-array material, and the binary selenides is synthesized using hydrothermal method,
By technical process control, make it have significant porous structure, with reach combination electrode material obtained have specific capacitance it is high,
The good goal of the invention of high rate performance, chemical property.
The present invention provides a kind of CoNiSe for ultracapacitor2Nano-array material and preparation method thereof.This hair
The bright capacitor electrode material being prepared has high specific capacitance, good high rate performance, high conductivity；Preparation manipulation letter
It is single, complex device is not needed, it can industrialized production.
Specifically, a kind of CoNiSe for ultracapacitor2Nano-array material, using nickel foam as substrate, in vertical
The nano array structure of arrangement, the nano-array is by CoNiSe2Nanometer rods and nanotube composition, the diameter of nanometer rods and nanotube
For 50 ~ 150nm, the surface of nanometer rods and nanotube is vesicular texture.
Further, the CoNiSe produced by the present invention for ultracapacitor2Nano-array material is in three-electrode system
In test, in 1 A g-1Current density under show 1338F g-1Height ratio capacity, and material resistance is down to 0.6 Ω, table
Reveal very high conductivity.
The present invention also provides prepare above-mentioned CoNiSe2The preparation method of nano-array super capacitor material, 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 CoNiSe2The growth substrate of nano-array material；
（2）Nickelous nitrate hexahydrate, cabaltous nitrate hexahydrate and isopropanol are mixed, then a certain amount of glycerine is added in stirring,
Obtain precursor solution；
（3）By step（2）In obtained precursor solution pour into reaction kettle, by step（1）In treated nickel foam
It is put into reaction kettle, carries out hydro-thermal reaction, be cooled to room temperature, collect the nickel foam for being attached with product, wash, it is dry, it is steeping
The product adhered on foam nickel is CoNiSe2Presoma nanosphere；
（4）Selenium powder, sodium borohydride and water are mixed, stirs at room temperature, is configured to clear aqueous solution；
（5）By step（4）In obtained aqueous solution be transferred in reaction kettle, by step（3）In obtain have product
Nickel foam be put into reaction kettle, carry out hydro-thermal reaction, be cooled to room temperature, collect and be attached with the nickel foam of final product, washing,
It is dry, obtain the CoNiSe using nickel foam as substrate2Nano-array super capacitor material；
The step（2）Middle Nickelous nitrate hexahydrate, cabaltous nitrate hexahydrate molar ratio be 1:2~1:1, isopropanol and glycerine
It is added respectively according to the amount of every 0.125m mol Nickelous nitrate hexahydrates 40mL and 8mL.
The step（3）Middle reaction temperature is 160 ~ 200 DEG C, time 6h.
The step（4）Middle selenium powder, sodium borohydride, water ratio be 1m mol: 2m mol : 40mL.
The step（5）Middle reaction temperature is 120 ~ 180 DEG C, time 6h.
Above-mentioned each parameter is the key process parameter of the preparation method of the present invention, true through many experiments institute for inventor
Recognize, need strictly and accurately control, if exceeding the range of above-mentioned technological parameter in the experiment of inventor, can not be made
CoNiSe2Nano-array material.
The useful achievement of the present invention is：
（1）The CoNiSe for ultracapacitor that the method for the present invention is prepared2Nano-array material is Co, Ni
Binary selenides, with the corresponding binary oxide reported（CoNiO2）, binary sulfide（CoNiS2）Equal electrode materials phase
Than having higher conductivity, this characteristic to be very beneficial for transmission and transport of the electrode material to charge.
（2）The CoNiSe for ultracapacitor that the method for the present invention is prepared2Nano-array material, mainly by
CoNiSe2Nanometer rods form, and also include a small amount of CoNiSe2Nanotube, nanometer rods and nanotube surface are vesicular texture, are received
Gap between rice array is conducive to electrolyte and is permeated to electrode interior, and the porous structure of nanometer rods and nanotube surface is conducive to increase
Add electrode specific surface area, increase contact of the electrolyte with electrode material, obtain more active sites, this pattern and its aperture and
Size Distribution is advantageous to promote the high speed diffusion of ion, and obtains high chemical property.
（3）The CoNiSe for ultracapacitor that the method for the present invention is prepared2Nano-array material, not only has
High specific capacitance, while there is high conductivity and good high rate performance, electrochemical stability is good, is a kind of excellent surpass
Grade capacitor 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 the scanning electron microscope of presoma nanosphere prepared by embodiment 1（SEM）Figure.
Fig. 2 is CoNiSe prepared by embodiment 12The scanning electron microscope of nano-array material（SEM）Figure.
Fig. 3 is CoNiSe prepared by embodiment 12The x-ray diffraction of nano-array material（XRD）Figure.
Fig. 4 is CoNiSe prepared by embodiment 12The cyclic voltammetric of nano-array material（CV）Figure.
Fig. 5 is CoNiSe prepared by embodiment 12The constant current charge-discharge curve graph of nano-array material.
Fig. 6 is CoNiSe prepared by embodiment 12Specific capacitance figure under the different current densities of nano-array material.
Fig. 7 is CoNiSe prepared by embodiment 12The ac impedance spectroscopy of nano-array material.
Specific implementation mode
Below in conjunction with specific embodiment, the present invention is further illustrated.
Embodiment 1
（1）Nickel foam is cut into a diameter of 18mm sizes, is 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 that raw material 0.125m mol Nickelous nitrate hexahydrates, that 0.125m mol cabaltous nitrate hexahydrates are dissolved in 40 mL is different
In propyl alcohol, 8mL glycerine is then added, stirs 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, 6h is reacted under the conditions of 180 DEG C, reaction kettle is then cooled down to room temperature, collects nickel foam, point
Not Yong ethyl alcohol, deionized water rinse, and dry, the product adhered in nickel foam is CoNiSe2Presoma nanosphere.
（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 with product of middle gained is put into step（4）Reaction kettle in, carry out hydro-thermal
Reaction, reaction temperature are 160 DEG C, and time 6h is cooled to room temperature, and collect nickel foam, are washed, dry, obtain be with nickel foam
The CoNiSe of substrate2Nano-array super capacitor material.
Embodiment 2
（1）Nickel foam is cut into a diameter of 18mm sizes, is so placed on 3 mol L-1In hydrochloric acid solution, ultrasonic reaction 30min,
It removes the NiO layer on surface, and treated nickel foam deionized water and ethyl alcohol is washed to neutrality.
（2）Weigh that raw material 0.125m mol Nickelous nitrate hexahydrates, that 0. 25m mol cabaltous nitrate hexahydrates are dissolved in 40 mL is different
In propyl alcohol, 8mL glycerine is then added, stirs 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, 6h is reacted under the conditions of 180 DEG C, reaction kettle is then cooled down to room temperature, collects nickel foam, point
Not Yong ethyl alcohol, deionized water rinse, and dry, the product adhered in nickel foam is CoNiSe2Presoma nanosphere.
（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 with product of middle gained is put into step（4）Reaction kettle in, carry out hydro-thermal
Reaction, reaction temperature are 160 DEG C, and time 6h is cooled to room temperature, and collect nickel foam, are washed, dry, obtain be with nickel foam
The CoNiSe of substrate2Nano-array super capacitor material.
Embodiment 3
（1）Nickel foam is cut into a diameter of 18mm sizes, is so placed on 3 mol L-1In hydrochloric acid solution, ultrasonic reaction 30min,
It removes the NiO layer on surface, and treated nickel foam deionized water and ethyl alcohol is washed to neutrality.
（2）Weigh that raw material 0.125m mol Nickelous nitrate hexahydrates, that 0.125m mol cabaltous nitrate hexahydrates are dissolved in 40 mL is different
In propyl alcohol, 8mL glycerine is then added, stirs 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, 6h is reacted under the conditions of 160 DEG C, reaction kettle is then cooled down to room temperature, collects nickel foam, point
Not Yong ethyl alcohol, deionized water rinse, and dry, the product adhered in nickel foam is CoNiSe2Presoma nanosphere.
（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 with product of middle gained is put into step（4）Reaction kettle in, carry out hydro-thermal
Reaction, reaction temperature are 180 DEG C, and time 6h is cooled to room temperature, and collect nickel foam, are washed, dry, obtain be with nickel foam
The CoNiSe of substrate2Nano-array super capacitor material.
Embodiment 4
（1）Nickel foam is cut into a diameter of 18mm sizes, is so placed on 3 mol L-1In hydrochloric acid solution, ultrasonic reaction 30min,
It removes the NiO layer on surface, and treated nickel foam deionized water and ethyl alcohol is washed to neutrality.
（2）Weigh that raw material 0.125m mol Nickelous nitrate hexahydrates, that 0.125m mol cabaltous nitrate hexahydrates are dissolved in 40 mL is different
In propyl alcohol, 8mL glycerine is then added, stirs 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, 6h is reacted under the conditions of 200 DEG C, reaction kettle is then cooled down to room temperature, collects nickel foam, point
Not Yong ethyl alcohol, deionized water rinse, and dry, the product adhered in nickel foam is CoNiSe2Presoma nanosphere.
（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 with product of middle gained is put into step（4）Reaction kettle in, carry out hydro-thermal
Reaction, reaction temperature are 120 DEG C, and time 6h is cooled to room temperature, and collect nickel foam, are washed, dry, obtain be with nickel foam
The CoNiSe of substrate2Nano-array super capacitor material.
Performance test：
1）SEM is tested：Sample prepared by above-mentioned each example is observed under a scanning electron microscope.Fig. 1 is 1 step of embodiment
Suddenly（3）In obtained CoNiSe2The microscopic appearance figure of presoma nanosphere, it can be seen that be made of uniform nanosphere, size
About 400nm；Fig. 2 is the final CoNiSe obtained of embodiment 12Microscopic appearance, there it can be seen that sample shows as nanometer
Stick also includes a small amount of nanotube, and a diameter of 50 ~ 150nm of nanometer rods and nanotube, nanometer rods and nanotube surface are porous
Shape structure, nanometer rods and nanotube are overlapping to form nano-array, and the gap between nano-array is conducive to electrolyte to electrode interior
The porous structure of infiltration, nanometer rods and nanotube surface is conducive to increase electrode specific surface area, increases electrolyte and electrode material
Contact, obtain more active sites, this pattern and its aperture and Size Distribution are advantageous to promote the high speed of ion to expand
It dissipates, and obtains high chemical property.
2）XRD is tested：Above-mentioned each example is prepared into finally obtained sample and carries out XRD tests, Fig. 3 is made for embodiment 1
CoNiSe2The XRD diagram that nano-array testing of materials obtains, X-ray diffraction peak and CoNiSe2Characteristic spectrum it is corresponding, show
Sample composition is CoNiSe2。
3）Electrochemical property test：By CoNiSe made from above-mentioned each example2Nano-array is assembled into electrode three respectively
Electrochemical property test is carried out under electrode system, Fig. 4 is CoNiSe made from embodiment 12Nano-array is in different scanning rates
Under CV curves, it can be seen that have apparent redox peaks, illustrate material have good fake capacitance characteristic；Fig. 5 is real
Apply CoNiSe made from example 12Discharge curve of the nano-array under different current densities, discharge curve have apparent platform,
Confirm CoNiSe2With fake capacitance characteristic；Fig. 6 is to calculate CoNiSe made from the embodiment 1 of gained according to Fig. 52Nano-array
Specific capacitance value under different current densities, in 1 A g-1Current density under show 1338F g-1Height ratio capacity, table
Bright CoNiSe2Nano-array material has high specific capacitance；Fig. 7 is the AC impedance figure of sample made from embodiment 1, it can be deduced that
Material resistance is 0.6 ohm, shows material satisfactory electrical conductivity.
Claims (7)
1. a kind of CoNiSe for ultracapacitor2Nano-array material, it is characterised in that：The CoNiSe2Nano-array material
Material is using nickel foam as substrate, and in the nano array structure being vertically arranged, the nano-array is by CoNiSe2Nanometer rods and nanotube
The surface of composition, a diameter of 50 ~ 150nm of nanometer rods and nanotube, nanometer rods and nanotube is vesicular texture.
2. a kind of CoNiSe for ultracapacitor according to claim 12Nano-array material, it is characterised in that：Institute
State CoNiSe2Nano-array material, in 1 A g-1Current density under reach 1338F g-1Specific capacity, material resistance down to
0.6Ω。
3. preparing the CoNiSe for ultracapacitor described in any one of claim 1 to 22The method of nano-array material,
It is characterized in that, step includes：
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 CoNiSe2The growth substrate of nano-array material；
2）Nickelous nitrate hexahydrate, cabaltous nitrate hexahydrate and isopropanol are mixed, then stirring is added a certain amount of glycerine, obtains
Precursor solution；
3）By step 2）In obtained precursor solution pour into reaction kettle, by step 1）In treated that nickel foam is put into reaction
In kettle, hydro-thermal reaction is carried out, is then cooled to room temperature, collect the nickel foam for being attached with product, washed, it is dry, in nickel foam
The product of upper attachment is CoNiSe2Presoma nanosphere；
4）Selenium powder, sodium borohydride and water are mixed, stirs at room temperature, is configured to clear aqueous solution；
5）By step 4）In obtained aqueous solution be transferred in reaction kettle, by step 3）In obtain the nickel foam for being attached with product
It is put into reaction kettle, carries out hydro-thermal reaction, then cool to room temperature, collect the nickel foam for being attached with final product, wash, do
It is dry, obtain the CoNiSe using nickel foam as substrate2Nano-array super capacitor material.
4. a kind of CoNiSe for ultracapacitor according to claim 32The preparation method of nano-array material, it is special
Sign is：The step 2）Middle Nickelous nitrate hexahydrate, cabaltous nitrate hexahydrate molar ratio be 1:2~1:1, isopropanol and glycerine divide
It is not added according to the amount of every 0.125m mol Nickelous nitrate hexahydrates 40mL and 8mL.
5. a kind of CoNiSe for ultracapacitor according to claim 32The preparation method of nano-array material, it is special
Sign is：The step 3）Middle reaction temperature is 160 ~ 200 DEG C, time 6h.
6. a kind of CoNiSe for ultracapacitor according to claim 32The preparation method of nano-array material, it is special
Sign is：The step 4）Middle selenium powder, sodium borohydride, water ratio be 1m mol: 2m mol : 40mL.
7. a kind of CoNiSe for ultracapacitor according to claim 32The preparation method of nano-array material, it is special
Sign is：The step 5）Middle reaction temperature is 120 ~ 180 DEG C, time 6h.
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