CN105869907A - Preparation method of carbon-nitrogen-codoped NiFe2O4-Ni nanocomposite material with cubic structure - Google Patents
Preparation method of carbon-nitrogen-codoped NiFe2O4-Ni nanocomposite material with cubic structure Download PDFInfo
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- CN105869907A CN105869907A CN201610296483.3A CN201610296483A CN105869907A CN 105869907 A CN105869907 A CN 105869907A CN 201610296483 A CN201610296483 A CN 201610296483A CN 105869907 A CN105869907 A CN 105869907A
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/32—Carbon-based
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/22—Electrodes
- H01G11/30—Electrodes characterised by their material
- H01G11/46—Metal oxides
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
- H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
- H01G11/84—Processes for the manufacture of hybrid or EDL capacitors, or components thereof
- H01G11/86—Processes for the manufacture of hybrid or EDL capacitors, or components thereof specially adapted for electrodes
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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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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 invention relates to a preparation method of a carbon-nitrogen-codoped NiFe2O4-Ni nanocomposite material with the cubic structure. The preparation method comprises the steps that firstly, a NiAc2 solution and a K3[Fe(CN)6]2 solution are prepared separately, the NiAc2 solution and the K3[Fe(CN)6]2 solution are stirred and mixed and then subjected to standing for a period of time, precipitates are generated, and centrifuging, washing and drying are conducted to obtain a Ni3[Fe(CN)6]2 nano cube material; secondly, the obtained material is put into a porcelain boat, the porcelain boat is placed in a tubular furnace, protective gas is introduced into the tubular furnace, calcining is conducted by setting a program and increasing the temperature, and after the temperature is decreased, the carbon-nitrogen-codoped NiFe2O4-Ni nanocomposite material with the cubic structure is taken out and obtained. The carbon-nitrogen-codoped NiFe2O4-Ni nanocomposite material with the cubic structure has the excellent properties when the composite material is used for a supercapacitor electrode material. Compared with the prior art, the synthesizing method is simple and easy to operate, and control over the product morphology is achieved.
Description
Technical field
The invention belongs to technical field of inorganic nanometer material, especially relate to a kind of nitrogen co-doped NiFe of carbon2O4/Ni
The preparation method of nano cubic structural composite material.
Background technology
The fast development of modern society, the continuous propelling of Process of Urbanization Construction, promote energy problem to become what people faced
One of ultimate challenge.The energy is the primary demand meeting economic high speed sustainable development, and energy problem is not only in that to be sought
Look for sufficient energy supply or improve efficiency of energy utilization, being more the many environmental problems involved.Therefore,
Research and development for new and effective green energy resource have become one of current energy field study hotspot.Super capacitor
Device, as a kind of novel energy-storing material, has that charge/discharge rates is fast, power density is high, have extended cycle life, work temperature
The degree advantage such as wide ranges, environmental protection, therefore has compared to traditional chemical battery product and is more widely applied,
And have the trend substituting conventional batteries product.But, often there is the shortcoming that energy density is low in current ultracapacitor,
And the selling price in the face of declining again and again is needed badly and is reduced the cost at aspects such as the energy, material, environmental protection.Now,
The Novel super capacitor material of design high-performance and easily prepared production is that related scientific research worker provides new moving
Power.
The mechanism that ultracapacitor produces according to its electric capacity can be divided into electric double layer capacitance and fake capacitance.Traditional double electric layer
Electric capacity predominantly has the material with carbon element of high-specific surface area, its feature show as stability superior in structure and performance,
High and good the most forthright of good conductivity, cycle life, simultaneously wide material sources, cheap, be readily synthesized,
And its shortcoming more relatively low than electric capacity limits its application and development.Fake capacitance material mainly have metal oxide or
Hydroxide etc., its feature shows as height ratio capacity, but electric conductivity and the most forthright less than material with carbon element.Therefore, by height
The metal hydroxides of specific capacity with processability excellent hybrid supercapacitor material compound with material with carbon element has non-
The biggest using value.
Organic metal framework material has the three-D pore structure of uniqueness, and the novel porous materials important as a class is being urged
The fields such as change, energy storage and separation have and is widely applied.In prior art, Prussian blue and derivative such as iron
Cyanides etc. can be replaced by methods such as converted in-situ as precursor, or it is many to construct synthesis as template
The nano composite material of sample.
Summary of the invention
The purpose of the present invention is contemplated to provide a kind of nitrogen co-doped from iron cyanide precursor converted in-situ synthesis carbon
The preparation method of bimetallic oxide.Preparation method of the present invention, for first to prepare Nickel hexacyanoferrate precursor, is then calcined
It is converted into nickel ferrite based magnetic loaded/nickel composite material, retains carbon nitrogen to improve its performance simultaneously.This composite is as super electric
Pole material has the performance of excellence.
The purpose of the present invention can be achieved through the following technical solutions:
A kind of nitrogen co-doped NiFe of carbon2O4The preparation method of/Ni nano cubic structural composite material, comprises the following steps:
(1) synthesis of calcining precursor is with preparation: prepare NiAc the most respectively2、K3[Fe(CN)6]2Solution, while stir
Mix limit to be slowly mixed together, be centrifuged after standing a period of time, wash, be dried, obtain Ni3[Fe(CN)6]2Nano cubic block
Material；
(2) calcining: gained precursor is placed in porcelain boat and puts into tube furnace, be passed through protective gas, setting program
Intensification is calcined, and takes out and obtain the nitrogen co-doped NiFe of carbon after cooling2O4/ Ni nano cubic block structural composite material.
NiAc described in step (1)2、K3[Fe(CN)6]2Solution, NiAc2Solution concentration scope is 0.01～0.1mol/L,
K3[Fe(CN)6]2Solution concentration scope is 0.01～0.1mol/L.
NiAc in step (1)2In solution, surfactant 1 used is PVP (K-30), and concentration range is 1～5g/100
ML。
NiAc in step (1)2In solution, surfactant 2 used is anhydrous citric acid sodium, and concentration range is 1
～5g/100ML.
In step (1), NiAc2、K3[Fe(CN)6]2Solution hybrid mode is K3[Fe(CN)6]2Solution is added dropwise over
NiAc2In solution, Ni Yu Fe mol ratio controls, at 3:2 5:1, just to meet when Ni with Fe mol ratio controls at 3:2
Ratio in product formula, Ni can be little over amount to improve conversion ratio.Time for adding is 10～30min, and mixing time is
10～30min.
In step (1), dwell temperature is room temperature, and the time of standing is 12～24h.
In step (2), protection gas used is nitrogen.
Step (2) Program heating rate is 0.5～5 DEG C/min.
Step (2) Program warming temperature is 300～400 DEG C, and temperature retention time is 1～2h.
Regulation and control precursor reaction condition or calcination condition can synthesize the nitrogen co-doped NiFe of different carbon2O4/ Ni nanometer is stood
Box structure composite.
A kind of nitrogen co-doped NiFe of carbon using above-mentioned preparation method to prepare2O4/ Ni composite, this composite is
By carbon-nitrogen doped NiFe2O4The nano cubic block that/Ni is constituted.
The nitrogen co-doped NiFe of described carbon2O4/ Ni composite has the performance of excellence for electrode material for super capacitor.
Bimetallic oxide produces fake capacitance effect and the process of redox reaction usually occurs.Based on carbon-nitrogen doped
NiFe2O4/ Ni composite has the chemical property of excellence, is mainly due to precursor uniform and monodispersed
The reservation of structure, Ni simple substance is for the enhancing of material conductivity, and the introducing of carbon nitrogen element.Precursor uniformly and
The reservation of monodispersed cubic block nanostructured so that product morphology has higher specific surface area, it is easier to occur
Reaction.And raising chemical property is also had very great help by the advantage of precursor short texture.Ni simple substance enhances material
Electric conductivity within Liao so that electronics is smooth in the conduction of cubic block material internal.Additionally, the introducing of carbon nitrogen element
Enhance electric conductivity and the stability of material greatly, and the electric double layer capacitance character that material with carbon element itself has is also to material
The performance of material has certain lifting.
Compared with prior art, the present invention has the following advantages and beneficial effect:
1, present invention achieves the organometallic complex Ni that synthesis pattern is uniform and stable3[Fe(CN)6]2Nano cubic
Block, and it is thermally treated resulting in carbon nitrogen co-doped NiFe for precursor by specific condition with it2O4/ Ni composite.
2, the method for the present invention has controllability to the pattern of product in building-up process, mainly by precursor
Synthesis regulation and control and calcination condition is regulated and controled.
3, the method for sending out of the present invention only obtains precursor by simple solution deposit, then carries out calcination processing i.e.
Can synthetic sample, synthesis step is few, and method of operating is simple.
4, product prepared by the present invention can be as electrode material for super capacitor, at KOH electrolyte, three electrodes
System shows the chemical property of excellence, has more vast potential for future development and actual application space.
Accompanying drawing explanation
Fig. 1 is the SEM photograph of the product that embodiment 1 products therefrom obtains under the multiple of 500nm.
Fig. 2 is the SEM photograph of the product that embodiment 2 products therefrom obtains under the multiple of 500nm.
Fig. 3 is the SEM photograph of the product that embodiment 3 products therefrom obtains under the multiple of 1 μm.
Fig. 4 is X-ray diffraction (XRD) collection of illustrative plates and the EDS elementary analysis collection of illustrative plates of embodiment 1 synthetic sample.
Fig. 5 is the EDS elementary analysis collection of illustrative plates of embodiment 1 synthetic sample.
Fig. 6 be embodiment 1 sample under KOH electrolyte three-electrode system, as electrode material for super capacitor
Charging and discharging curve under different size of current.
Detailed description of the invention
The present invention is described in detail with specific embodiment below in conjunction with the accompanying drawings.
Embodiment 1
A kind of nitrogen co-doped NiFe of carbon2O4The preparation method of/Ni nano cubic structural composite material, specifically comprises the following steps that
(1) precursor synthesis is with preparation: takes the 100ML aqueous solution and adds 0.267g nickel acetate, 4g PVP, 0.1g
Sodium citrate is sufficiently stirred for dissolving.Separately take the 100ML aqueous solution and add 1.3g potassium ferricyanate solid, be sufficiently stirred for molten
Solve.Slowly being added dropwise in nickel acetate solution by potassium ferricyanate solution, stirring 30min is placed on room temperature and stands.
Centrifugation after 24h, washing, alcohol are dried after washing each three times, standby.
(2) calcination process: assay balance weighs a certain amount of precursor, is placed in porcelain boat and puts into tube furnace, be passed through
Nitrogen protection gas, arranges heating schedule.Heating rate is 1 DEG C/min.Lower the temperature after being warming up to 300 DEG C of insulation 2h
To room temperature.Obtain the nitrogen co-doped NiFe of carbon2O4/ Ni nano cubic block structural composite material.
The nitrogen co-doped NiFe of this example gained carbon2O4SEM photograph such as Fig. 1 of/Ni nano cubic block structural composite material
Shown in.As seen from the figure, material is that nano cubic of uniform size is block-shaped under a scanning electron microscope, surface in
Loose porous shape, nano cubic block size is about 150nm.
Fig. 4 is X-ray diffraction (XRD) collection of illustrative plates and the EDS elementary analysis of the present embodiment 1 synthetic sample.
The peak occurred in Fig. 4 is produced after standard PDF card (NO.10-0235,06-0697,10-0280) comparison
The peak that goes out of thing corresponds to NiFe2O4And metallic nickel simple substance, but owing to metallic nickel simple substance goes out with carbonization nickel, nickel oxide etc.
Wind position is identical, can not determine the composition of this Diversity system product only according to XRD spectrum.
Fig. 5 is the EDS elementary analysis collection of illustrative plates of the present embodiment 1 synthetic sample.
XRD spectrum is combined, containing NiFe in product from EDS elementary analysis2O4, iron oxygen in EDS collection of illustrative plates
Atomic ratio is combined the molecular formula of nickel ferrite based magnetic loaded.It addition, from EDS, in system in addition to Ni, Fe element,
Possibly together with a large amount of carbon, nitrogen element, compose it may be speculated that carbon nitrogen element may be with Ni simple substance/NiC/NiN in conjunction with XRD
Presented in mixture.It can be said that bright precursor, during calcining, remains original to a certain extent
Carbon nitrogen element, be present in product with doped forms.
Fig. 6 products therefrom is under KOH electrolyte three-electrode system, as electrode material for super capacitor at different electricity
Charging and discharging curve under stream size.
Fig. 6 is under KOH electrolyte three-electrode system, and product is big at different electric currents as electrode material for super capacitor
Charging and discharging curve under little.It can be seen that along with electric current reduces, electrode charge and discharge capacity increases, when electric current is 0.5
1201F/g is reached during A/g.
Embodiment 2
A kind of nitrogen co-doped NiFe of carbon2O4The preparation method of/Ni nano cubic structural composite material, specifically comprises the following steps that
(1) precursor synthesis is with preparation: takes the 100ML aqueous solution and adds 0.267g nickel acetate, 4g PVP, 0.1g
Sodium citrate is sufficiently stirred for dissolving.Separately take the 100ML aqueous solution and add 1.3g potassium ferricyanate solid, be sufficiently stirred for molten
Solve.Slowly being added dropwise in nickel acetate solution by potassium ferricyanate solution, stirring 30min is placed on room temperature and stands.
Centrifugation after 24h, washing, alcohol are dried after washing each three times, standby.
(2) calcination process: assay balance weighs a certain amount of precursor, is placed in porcelain boat and puts into tube furnace, be passed through
Nitrogen protection gas, arranges heating schedule.Heating rate is 1 DEG C/min.Be warming up to respectively 300 DEG C, 350 DEG C,
It is cooled to room temperature after 400 DEG C of insulation 2h.Obtain the nitrogen co-doped NiFe of carbon2O4/ Ni nano cubic block structure composite material
Material.
The nitrogen co-doped NiFe of carbon of this example difference calcining heat synthesis2O4/ Ni nano cubic block structural composite material
SEM photograph is as shown in Figure 2.Fig. 2 (a-c) respectively corresponding for calcining heat at 300 DEG C, 350 DEG C, 400 DEG C.
When temperature is low, pattern keeps good, but converts not exclusively, and temperature converts completely after raising, but pattern is to a certain extent
Destroyed.
Embodiment 3
A kind of nitrogen co-doped NiFe of carbon2O4The preparation method of/Ni nano cubic structural composite material, specifically comprises the following steps that
(1) precursor synthesis is with preparation: weigh 0.142g nickel acetate and 0.25g sodium citrate is dissolved in 100ML
Solution becomes solution A；Weigh 0.07g potassium ferricyanate and 0.3g PVP is dissolved in 100ML solution
Solution B.Slowly solution B is joined in solution A under agitation, drips complete follow-up continuous stirring 30min,
Stop stirring, be placed in room temperature and stand 20h.Centrifugation, washing, ethanol is dried after washing each three times, standby.
(2) calcination process: assay balance weighs a certain amount of precursor, is placed in porcelain boat and puts into tube furnace, be passed through
Nitrogen protection gas, arranges heating schedule.Heating rate be respectively 0.5 DEG C/min, 1 DEG C/min, 5 DEG C/min.Rise
Temperature is cooled to room temperature to 400 DEG C of insulation 2h.Obtain the nitrogen co-doped NiFe of carbon2O4/ Ni nano cubic block structure is multiple
Condensation material.
The present embodiment is the nitrogen co-doped NiFe of gained carbon under different ramp rate conditions2O4/ Ni nano cubic block structure is multiple
Shown in the SEM photograph of condensation material such as Fig. 3 (a-c), in Fig. 3, a, b, c represent that heating rate is 0.5 DEG C respectively
/ min, 1 DEG C/min, the situation of 5 DEG C/min.Visible along with temperature rising, under the retentivity of product morphology from figure
Fall, heating rate reaches 5 DEG C/min afterproduct cubic block structure and is difficult to be kept.
The above-mentioned description to embodiment is to be understood that for ease of those skilled in the art and use invention.
These embodiments obviously easily can be made various amendment by person skilled in the art, and explanation at this
General Principle be applied in other embodiments without through performing creative labour.Therefore, on the invention is not restricted to
State embodiment, those skilled in the art according to the announcement of the present invention, the improvement made without departing from scope and
Amendment all should be within protection scope of the present invention.
Claims (9)
1. the nitrogen co-doped NiFe of carbon2O4The preparation method of/Ni nano cubic structural composite material, it is characterised in that
Comprise the following steps:
(1) synthesis of calcining precursor is with preparation: prepare NiAc the most respectively2、K3[Fe(CN)6]2Solution, while stir
Mix limit to be slowly mixed together, be centrifuged after standing a period of time, wash, be dried, obtain Ni3[Fe(CN)6]2Nano cubic block
Material；
(2) calcining: gained precursor is placed in porcelain boat and puts into tube furnace, be passed through protective gas, setting program
Intensification is calcined, and takes out and obtain the nitrogen co-doped NiFe of carbon after cooling2O4/ Ni nano cubic block structural composite material.
A kind of nitrogen co-doped NiFe of carbon the most according to claim 12O4/ Ni nano cubic structural composite material
Preparation method, it is characterised in that the NiAc described in step (1)2、K3[Fe(CN)6]2Solution, NiAc2Solution is dense
Degree scope is 0.01～0.1mol/L, K3[Fe(CN)6]2Solution concentration scope is 0.01～0.1mol/L.
A kind of nitrogen co-doped NiFe of carbon the most according to claim 12O4/ Ni nano cubic structural composite material
Preparation method, it is characterised in that NiAc in step (1)2In solution, surfactant 1 used is PVP (K-30),
Concentration range is 1～5g/100ML.
A kind of nitrogen co-doped NiFe of carbon the most according to claim 12O4/ Ni nano cubic structural composite material
Preparation method, it is characterised in that NiAc in step (1)2In solution, surfactant 2 used is anhydrous citric acid
Sodium, concentration range is 1～5g/100ML.
A kind of nitrogen co-doped NiFe of carbon the most according to claim 12O4/ Ni nano cubic structural composite material
Preparation method, it is characterised in that in step (1), NiAc2、K3[Fe(CN)6]2Solution hybrid mode is K3[Fe(CN)6]2
Solution is added dropwise over NiAc2In solution, time for adding is 10～30min, and mixing time is 10～30min.
A kind of nitrogen co-doped NiFe of carbon the most according to claim 12O4/ Ni nano cubic structural composite material
Preparation method, it is characterised in that in step (1), dwell temperature is room temperature, and the time of standing is 12～24h.
A kind of nitrogen co-doped NiFe of carbon the most according to claim 12O4/ Ni nano cubic structural composite material
Preparation method, it is characterised in that in step (2), protection gas used is nitrogen.
Step (2) Program heating rate scope is 0.5～5 DEG C/min.
Step (2) Program warming temperature scope is 300～400 DEG C, and temperature retention time is 1～2h.
8. the carbon that the preparation method used according to any one of claim 1-7 prepares is nitrogen co-doped
NiFe2O4/ Ni nano cubic structural composite material.
9. the nitrogen co-doped NiFe of carbon as claimed in claim 82O4Answering of/Ni nano cubic structural composite material
With, it is characterised in that the nitrogen co-doped NiFe of described carbon2O4/ Ni nano cubic block structural composite material is for super
Electrode for capacitors active material has the performance of excellence.
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| CN107597124A (en) * | 2017-09-22 | 2018-01-19 | 常州大学 | A kind of preparation method of Nano Carbon nickel ferrite based magnetic loaded |
| CN108597895A (en) * | 2018-06-05 | 2018-09-28 | 哈尔滨工程大学 | A kind of bimetallic oxide and graphene composite material and preparation method thereof |
| CN109585825A (en) * | 2018-11-28 | 2019-04-05 | 成都理工大学 | The Ni/NiFe of bimetallic MOF precursor synthesis2O4Lithium ion battery negative material and preparation method thereof |
| CN109647458A (en) * | 2019-01-11 | 2019-04-19 | 河南师范大学 | The method that self-template methods synthesis has the double-metal phosphide elctro-catalyst of hollow structure |
| CN113097499A (en) * | 2021-03-29 | 2021-07-09 | 江苏科技大学 | FeNi/NiFe2O4@ NC composite material and preparation method and application thereof |
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| CN105869907B (en) | 2018-07-24 |
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