CN109755028A - A kind of nickelous selenide applied to supercapacitor/nickel hydroxide composite material and preparation method - Google Patents
A kind of nickelous selenide applied to supercapacitor/nickel hydroxide composite material and preparation method Download PDFInfo
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- CN109755028A CN109755028A CN201910077484.2A CN201910077484A CN109755028A CN 109755028 A CN109755028 A CN 109755028A CN 201910077484 A CN201910077484 A CN 201910077484A CN 109755028 A CN109755028 A CN 109755028A
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
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- Y02E60/13—Energy storage using capacitors
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Abstract
Invention describes a kind of nickelous selenide applied to supercapacitor/nickel hydroxide composite material and preparation methods, belong to novel energy resource material technology field.The present invention has obtained the presoma of nickelous selenide using hydro-thermal reaction under aqueous conditions using inorganic nickel and hydrazine hydrate, further utilizes hydrogen peroxide, has obtained the composite material of nickelous selenide and nickel hydroxide.This strategy prepares the strategy of metal oxide and hydroxide composite material on the contrary, the composite material being prepared has excellent performance of the supercapacitor with tradition, and the electrode material for preparing high-performance super capacitor has important directive significance.
Description
Technical field
The invention belongs to new material technology fields, and in particular to a kind of nickelous selenide/hydroxide applied to supercapacitor
Nickel composite material and preparation method thereof
Background technique
Supercapacitor also known as electrochemical capacitor have the power density of superelevation, good cycle life, quickly fill
The advantages such as electricity, therefore be expected to become one of the energy storage device of next-generation highly effective and safe.Nevertheless, its relatively low energy is close
Degree still limits its practical commercial applications.Therefore, design and synthesis have excellent electrochemical performance electrode material just at
For key.
Transition metal hydroxide is due to high specific surface area and theoretical capacity (3500-4600F/g), it is considered to be answers
With one of the electrode material of prospect.By taking nickel hydroxide as an example, show than metal oxide, metal sulfide, metal phosphorizing
The higher theoretical capacity of object.However, the disadvantages of its lower electric conductivity, poor electrochemical stability, constrains transition metal hydrogen
Oxide is further applied.A kind of effective strategy be by transition metal hydroxide and other with satisfactory electrical conductivity and structure
The Material cladding of stability.Pang et al. synthesizes to have obtained Co using hydro-thermal method3O4/Co(OH)2Composite material, Co (OH)2For
2.5-3 μm of hexagonal nano lamella, Co3O4For the nanocrystalline of 60nm, which presents excellent supercapacitor
Can, under the current density of 1.2A/g with 1164F/g height ratio capacity (H.Pang, X.Li, Q.Zhao, H.Xue, W.Lai,
Z.Hu and W.Huang,Nano Energy,2017,35,138-145.).Wang et al. is using hydro-thermal method in carbon cloth substrate
The NiCo-OH presoma for having synthesized celestial being's palmate has obtained the composite material of NiCoP/NiCo-OH by high temperature phosphorization.The material
Material combines effective charge transmission, the mechanical stability of 2D nanometer sheet, the flexible advantage of 3D carbon cloth of 1D nano material, because
This capacity with 1100F/g, about the 7 of NiCo-OH times (X.Li, H.Wu, A.M.Elshahawy, L.Wang,
S.J.Pennycook,C.Guan and J.Wang,Adv.Funct.Mater.,2018,28,1800036.).Li et al. people passes through
Hydro-thermal method synthesizes to have obtained NixFe1-xS2Rodlike presoma, then utilize its pyrohydrolysis, obtained electrochemical performance
Sulfide and hydroxide composite material (T.Wang, G.Nam, Y.Jin, X.Wang, P.Ren, M.G.Kim, J.Liang,
X.Wen,H.Jang,J.Han,Y.Huang,Q.Li and J.Cho,Adv.Mater.,2018,30,1800757.).To sum up institute
It states, the composite material for synthesizing transistion metal compound and transition metal hydroxide can effectively solve transition metal hydroxide
The problem of structural stability and poorly conductive, promotes performance of the supercapacitor.Transistion metal compound and transition gold are prepared at present
Belong to hydroxide and mainly pass through two methods: first method is the presoma for first synthesizing hydroxide, then passes through oxidation, phosphorus
The means such as change, vulcanization obtain composite material；Second method is then first to synthesize transistion metal compound, then pass through suitable hand
Section generates composite material.
Nickelous selenide be it is a kind of with preferable electric conductivity and high stability material (resistivity be lower than 10-3Ω * cm), it can be by
For generating Ni (OH)2/NiSe2Composite material.However, how to be prepared by rationally effective method has excellent super capacitor
The Ni (OH) of device performance2/NiSe2Still explored, therefore significantly limit Ni (OH)2/NiSe2The big rule of composite material
Mould application.
Summary of the invention
The present invention provides a kind of new strategies, and nickelous selenide surface layer to be made to grow lamella nickel hydroxide, thus prepare nickelous selenide and
Nickel hydroxide is as electrode material for super capacitor.This method not only can effectively control the nanotopography of synthetic material, also
The boundary layer between nickelous selenide and nickel hydroxide can be constructed effectively in favor of electron transport, to improve its capacitor appearance
Amount.It is different from traditional method for first synthesizing nickel hydroxide then selenizing, we have synthesized the presoma of nickelous selenide first, in turn
Using hydrogen peroxide and aqueous slkali, nickelous selenide/nickel hydroxide composite material has been obtained by hydro-thermal reaction.We are compound by this
When material is applied to the electrode material of supercapacitor, the advantages that having shown high specific capacitance, good stability.This method
A kind of new strategy is provided for the composite material of synthesis transistion metal compound and hydroxide, there is excellent electricity for synthesis
Chemical property electrode material has great importance.
A kind of nickelous selenide applied to supercapacitor/nickel hydroxide composite material and preparation method of the present invention,
It is characterized in that, preparing NiSe first2Octahedra crystallite then converts sheet Ni (OH) for its outer layer2And it constructs conducive to electronics
The NiSe transported2/Ni(OH)2Interface.
Further, the nickelous selenide/nickel hydroxide composite material uses hydrogen peroxide and aqueous slkali hydro-thermal process selenium
Change nickel octahedron crystallite to obtain.
Further, the preparation method the following steps are included:
(1) octahedron NiSe2The preparation of crystallite: it weighs 0.5mmol (0.1454g) Nickelous nitrate hexahydrate and is dissolved in 10ml and goes
Solution A, ultrasound 30 minutes are obtained in ionized water；It weighs 3mmol (0.2369g) selenium powder to be added in 10ml hydrazine hydrate, stirs 30 points
Clock obtains solution B；Solution A is poured into solution B and stirred 30 minutes and obtains mixed solution, is placed at 120 DEG C and reacts 12h, then
It is cooled to room temperature；Above-mentioned reaction solution is filtered, precipitating deionized water and dehydrated alcohol are repeatedly washed, is obtained after 60 DEG C of dryings
NiSe with shape of octahedron2Crystallite, having a size of 50~200 nanometers.
(2)NiSe2/Ni(OH)2The preparation of composite material: 100mg NiSe is weighed2Presoma is scattered in 20ml0.1M's
In KOH solution, ultrasound is uniformly dispersed for 5 minutes, and the hydrogen peroxide of 1ml 30% is added, stirs evenly, 2h is reacted at 170 DEG C, so
After be cooled to room temperature；Above-mentioned reaction solution is filtered, gained precipitating is washed repeatedly using deionized water and dehydrated alcohol, after 60 DEG C of dryings
Obtain NiSe2/Ni(OH)2Composite material.
Further, the step (2) uses hydrogen peroxide/KOH aqueous solution hydro-thermal process NiSe2, to ensure to prepare
Lamella Ni (OH)2The NiSe of cladding2It is octahedra.
Further, the step (2) utilizes the collective effect of hydrogen peroxide and KOH, to ensure prepared Ni (OH)2It is brilliant
Lattice are directly epitaxially grown in NiSe2On lattice, in favor of electron transport.
Further, the reaction time is 2h at 170 DEG C in the step (2).
Further, nickelous selenide/nickel hydroxide composite material that the preparation method obtains.
Further, the nickelous selenide of preparation/nickel hydroxide composite material is used for the application of capacitive property material.
The present invention provides a kind of new strategies to synthesize nickelous selenide/nickel hydroxide high-performance super capacitor electrode material,
Have the following prominent advantages: (1) presoma NiSe octahedronlike2It can largely synthesize, there is further actual application prospect；
(2) the new method of one kind is utilized to have synthesized NiSe2/Ni(OH)2Composite material；(3) using derived from NiSe2 presoma
NiSe2/Ni(OH)2With good electrochemical properties, performance of the supercapacitor has biggish promotion；(4)Ni(OH)2Tool
There is good sheet hierarchical porous structure, is conducive to electrochemical reaction, NiSe2Still retain original octoploids structure, provide good
Good structural stability and good electric conductivity；(5) NiSe has been constructed2/Ni(OH)2It is special that interface provides good electron transport
Property.
Detailed description of the invention
Fig. 1: the NiSe being prepared in embodiment 12The XRD spectra and JCPDS standard spectrogram of presoma.
Fig. 2: NiSe is utilized in embodiment 12The NiSe that forerunner's syntaxy is prepared2/Ni(OH)2Composite material XRD spectra
With JCPDS standard spectrogram.
The NiSe being prepared in Fig. 3 embodiment 12The electron scanning micrograph (SEM) of presoma.
Fig. 4 embodiment 1 utilizes NiSe2The NiSe that forerunner's syntaxy is prepared2/Ni(OH)2The scanning electron of composite material
Microscopical photo (SEM).
The NiSe being prepared in Fig. 5 embodiment 12/Ni(OH)2The transmission electron microscope photo (TEM) of composite material.
Fig. 6: a corresponding NiSe being prepared2/Ni(OH)2The transmission electron microscope photo of composite material；B is corresponding
NiSe2/Ni(OH)2The Elemental redistribution of O in composite material；C corresponds to NiSe2/Ni(OH)2The Elemental redistribution of Se in composite material；d
Corresponding NiSe2/Ni(OH)2The Elemental redistribution (TEM-mapping) of Ni in composite material.
Fig. 7: a corresponds to NiSe2The CV curve of presoma；B corresponds to NiSe2The constant current charge-discharge curve of presoma；C is corresponding
NiSe2/Ni(OH)2The CV curve of composite material；D corresponds to NiSe2/Ni(OH)2The crossing current charging and discharging curve of composite material.
Capacitor of Fig. 8: a counter electrode material under different current densities；The impedance spectra of b counter electrode material.
Specific embodiment
Technical characterstic of the invention is illustrated below with reference to specific experiment scheme and attached drawing, but the present invention is not limited thereto.
Test method described in following example is unless otherwise specified conventional method；The instrument and material, unless otherwise specified,
Commercially obtain.
Embodiment 1
(1) octahedra bulk NiSe2Preparation: weigh 0.5mmol (0.1454g) Nickelous nitrate hexahydrate and be dissolved in 10ml and go
Solution A is obtained in ionized water, ultrasound 30 minutes weighs in 3mmol (0.2369g) selenium powder and 10ml hydrazine hydrate, stirs 30 minutes
Solution B is obtained, solution A is poured into solution B and stirring obtains mixed solution in 30 minutes, mixed solution is poured into 50ml polytetrafluoroethyl-ne
In alkene reaction kettle, black product is obtained after reacting 12h at 120 DEG C, is repeatedly washed with deionized water and dehydrated alcohol, is placed in drum
In wind drying box, octahedral NiSe is obtained after 60 DEG C of dryings2Presoma.
(2)NiSe2/Ni(OH)2The preparation of composite material: 100mg NiSe is weighed2Presoma is scattered in 20ml0.1M/L's
In KOH solution, ultrasound is uniformly dispersed for 5 minutes, and the hydrogen peroxide of 1ml 30% is added, stirs evenly.Above-mentioned mixed solution is poured into
In 50ml ptfe autoclave, reaction kettle is placed in air dry oven 2h at 170 DEG C, takes out reaction kettle, using go from
Sub- water and dehydrated alcohol wash products therefrom repeatedly, obtain NiSe after 60 DEG C of dryings2/Ni(OH)2Composite material.
(3) preparation of active material electrode: the NiSe for taking 16mg to synthesize2/Ni(OH)2Composite material (or NiSe2) in Ma
It is ground in Nao mortar, 2mg conductive black is added, continue grinding uniformly, the polytetrafluoroethylene (PTFE) that 40ul mass fraction 5% is added is water-soluble
Liquid uniformly, is added dehydrated alcohol and obtains homogeneous solution, ultrasound 30 minutes as binder, grinding.Then above-mentioned solution is placed in
60 DEG C of drying, are applied to 1x2cm for the mixing material after drying in air dry oven2Foamed nickel current collector on, then tabletting
It is made into electrode (pressure is less than 10 megapascal).
Attached drawing meaning
(4) in order to study the performance of the supercapacitor for preparing material, Shanghai Chen Hua electrochemical workstation has been used
(chi760e) test of chemical property has been carried out to material.All electrochemical properties of active material are in three-electrode system
Lower test, using calomel electrode as reference electrode, platinum guaze is to electrode, and active material electrode is working electrode, 6M/L KOH solution
For electrolyte solution.Under the disturbance voltage of 5mV, frequency range is 0.01 to 106Hz has carried out the test of electrochemical impedance spectroscopy.
Fig. 1: the NiSe being prepared in embodiment 12The XRD spectra and JCPDS standard spectrogram of presoma.XRD test knot
Fruit shows the NiSe of preparation2Presoma fits like a glove with standard spectrogram, and NiSe2Presoma has shown very high crystallization
Degree shows that the material has very high object phase purity.
Fig. 2: NiSe is utilized in embodiment 12The NiSe that forerunner's syntaxy is prepared2/Ni(OH)2Composite material XRD spectra
With JCPDS standard spectrogram.XRD test result shows that the composite material of synthesis contains NiSe simultaneously2With Ni (OH)2Diffraction maximum, table
It is bright that we successfully prepare NiSe2/Ni(OH)2Composite material, no other impurities.
Fig. 3: NiSe in embodiment 12The electron scanning micrograph of presoma shows our NiSe2Pattern be eight
Face body is blocky, having a size of 100-200nm.
Fig. 4: NiSe in embodiment 12/Ni(OH)2The photo of the scanning electron microscope of composite material.SEM test result table
The bright block-like NiSe of octahedron2There are many sheet substances in surface, is Ni (OH)2, and NiSe2Still maintain eight
The bulk of face body.
Fig. 5: the NiSe being prepared in embodiment 12/Ni(OH)2The transmission electron microscope photo of composite material.TEM is surveyed
Test result shows octahedra block-like NiSe2The Ni (OH) that surface occurs2Nanometer sheet, it is corresponding with SEM test result.This table
The nanometer sheet that face occurs can significantly increase the specific surface area of material, increase the electro-chemical activity site of material surface, enhance
The mass transport process of electrode material and electrolyte solution, therefore NiSe2/Ni(OH)2Composite material can have better super capacitor
Device performance.
Fig. 6: NiSe2/Ni(OH)2The TEM-mapping photo of composite material.A figure test result is opposite with Fig. 3 and Fig. 4
It answers；B figure is NiSe2/Ni(OH)2The Elemental redistribution of O in composite material shows that oxygen element is evenly distributed in sample；C figure is
NiSe2/Ni(OH)2The Elemental redistribution of Se in composite material, Selenium In Some Selenium-rich Biological Samples element are mainly evenly distributed on internal octahedra block
It is interior；D schemes NiSe2/Ni(OH)2The Elemental redistribution of Ni in composite material shows that Ni is mainly distributed in octahedra block in sample, still
Also the distribution for having a small amount of Ni on surface.
Fig. 7: NiSe2Presoma and NiSe2/Ni(OH)2The electro-chemical test of composite material, including CV curve and constant current are filled
Discharge curve.A schemes NiSe2There are apparent redox peaks in curve in the CV curve of presoma；B schemes NiSe2Presoma
Flow over charging and discharging curve, apparent platform occurs in curve, corresponding with the redox peaks in a figure；C figure is NiSe2/Ni
(OH)2The CV curve of composite material, with NiSe2CV curve compare, the curve integral area of the composite material obviously becomes larger, table
We bright material has better capacitive property；D figure is NiSe2/Ni(OH)2The constant current charge-discharge curve of composite material, with
NiSe2It compares, the charge and discharge time of composite material is obviously elongated, and it is corresponding with CV test result, show that composite material has more
Good capacitive property.
Fig. 8: a figure is NiSe2Presoma and NiSe2/Ni(OH)2Capacitor of the composite material under different current densities,
NiSe2/Ni(OH)2With higher capacitor, under the current density of 1,2,5 and 10A/g, specific capacitance is respectively 1735,
1574,1385 and 1199F/g.B figure is NiSe2Presoma and NiSe2/Ni(OH)2The impedance spectrum of composite material is opposite with a figure
It answers, shows NiSe2/Ni(OH)2Composite material has better electrochemical properties.
To disclosed in this invention the description of embodiment be not intended to limit the scope of the invention, but for describing
The present invention.Correspondingly, the scope of the present invention is not limited by embodiment of above, but is carried out by claim or its equivalent
It limits.
Claims (7)
1. a kind of nickelous selenide applied to supercapacitor/nickel hydroxide composite material and preparation method, which is characterized in that institute
The nickelous selenide stated/nickel hydroxide composite material is prepared by two step hydro-thermal reactions, anti-with hydrazine hydrate first with metal nitrate
Nickelous selenide octahedral crystal should be obtained, nickelous selenide/hydroxide is then obtained by hydrogen peroxide/potassium hydroxide aqueous solution hydro-thermal process
Nickel composite material.
2. nickelous selenide described according to claim 1/nickel hydroxide composite material and preparation method thereof, which is characterized in that prepare first
NiSe2Octahedra crystallite then converts sheet Ni (OH) for its outer layer2And the NiSe constructed conducive to electron transport2/Ni(OH)2
Interface.The preparation method the following steps are included:
(1) octahedron NiSe2The preparation of crystallite: it weighs 0.5mmol (0.1454g) Nickelous nitrate hexahydrate and is dissolved in 10ml deionization
Solution A, ultrasound 30 minutes are obtained in water；3mmol (0.2369g) selenium powder is weighed to be added in 10ml hydrazine hydrate, stirring 30 minutes
To solution B；Solution A is poured into solution B and stirred 30 minutes and obtains mixed solution, is placed at 120 DEG C and reacts 12h, then cool down
To room temperature；Above-mentioned reaction solution is filtered, precipitating deionized water and dehydrated alcohol are repeatedly washed, is had after 60 DEG C of dryings
The NiSe of shape of octahedron2Crystallite, having a size of 50~200 nanometers.
(2)NiSe2/Ni(OH)2The preparation of composite material: 100mg NiSe is weighed2The KOH that presoma is scattered in 20ml 0.1M is molten
In liquid, ultrasound is uniformly dispersed for 5 minutes, and the hydrogen peroxide of 1ml 30% is added, stirs evenly, 2h is reacted at 170 DEG C, is then cooled down
To room temperature；Above-mentioned reaction solution is filtered, gained precipitating is washed repeatedly using deionized water and dehydrated alcohol, is obtained after 60 DEG C of dryings
NiSe2/Ni(OH)2Composite material.
3. nickelous selenide according to claim 2/nickel hydroxide composite material and preparation method thereof, which is characterized in that the step
(2) hydrogen peroxide/KOH aqueous solution hydro-thermal process NiSe is used2, to ensure to prepare lamella Ni (OH)2The NiSe of cladding2Octahedral
Body.
4. nickelous selenide according to claim 2/nickel hydroxide composite material and preparation method thereof, which is characterized in that the step
(2) collective effect of hydrogen peroxide and KOH is utilized, to ensure prepared Ni (OH)2Lattice is directly epitaxially grown in NiSe2Lattice
On, it is conducive to electron transport.
5. nickelous selenide according to claim 2/nickel hydroxide composite material and preparation method thereof, which is characterized in that the step
(2) reaction time is 2h at 170 DEG C in.
6. nickelous selenide/nickel hydroxide composite material that any one of -5 preparation methods obtain according to claim 1.
7. being used for the application of capacitive property material according to nickelous selenide/nickel hydroxide composite material prepared by claim 6.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110400926A (en) * | 2019-08-07 | 2019-11-01 | 福州大学 | A kind of nitrogen-doped carbon cladding two-phase is interspersed type nickel cobalt bimetallic selenides electrode material and preparation method thereof |
| CN112614992A (en) * | 2020-12-10 | 2021-04-06 | 三峡大学 | Nickel composite positive electrode material of water-based zinc-nickel battery and preparation method of nickel composite positive electrode material |
-
2019
- 2019-01-28 CN CN201910077484.2A patent/CN109755028A/en active Pending
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110400926A (en) * | 2019-08-07 | 2019-11-01 | 福州大学 | A kind of nitrogen-doped carbon cladding two-phase is interspersed type nickel cobalt bimetallic selenides electrode material and preparation method thereof |
| CN112614992A (en) * | 2020-12-10 | 2021-04-06 | 三峡大学 | Nickel composite positive electrode material of water-based zinc-nickel battery and preparation method of nickel composite positive electrode material |
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