CN110040787A - A kind of nano whiskers FeCo2O4The preparation method and application of electrode material - Google Patents
A kind of nano whiskers FeCo2O4The preparation method and application of electrode material Download PDFInfo
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- CN110040787A CN110040787A CN201910324018.XA CN201910324018A CN110040787A CN 110040787 A CN110040787 A CN 110040787A CN 201910324018 A CN201910324018 A CN 201910324018A CN 110040787 A CN110040787 A CN 110040787A
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- C01G51/00—Compounds of cobalt
- C01G51/40—Cobaltates
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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
- H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
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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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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
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- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
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- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
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- 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
A kind of nano whiskers FeCo2O4The preparation method and application of electrode material, preparation method include: by frerrous chloride (FeCl2·4H2O), cobalt nitrate (Co (NO3)2·6H2O), urea (Co (NH2)2), ammonium fluoride (NH4F it) is mixed, hydro-thermal reaction obtains FeCo2O4Nano material, then by FeCo2O4Nano material is prepared into FeCo2O4Electrode；The present invention has preparation process simple, and process control, cost is relatively low, the FeCo of nano whiskers2O4The features such as pattern is uniform, large specific surface area, electric conductivity are good, electrochemical performance, is conducive to the application in energy storage fields such as lithium ion battery, supercapacitors.
Description
Technical field
The invention belongs to Nano-function thin films and energy storage material preparation technical fields, and in particular to a kind of nano whiskers
FeCo2O4The preparation method and application of electrode material.
Background technique
In today of the increasingly developed growth of global economy, problem of environmental pollution is increasingly violent, and fuel cell consumption is huge, high
Effect, cleaning and the research and development of sustainable energy storage device are brought into schedule with application.Battery, fuel cell and electrochemical capacitor quilt
It is widely used in multiple fields.Wherein, supercapacitor (SCs) has safety, simple process, capacitance density height, high rate performance
Good, invertibity is well, the cycle life (> 100 ten thousand times) of overlength, assembly is simple, is readily integrated into electronic product and chemical heat
Yield it is less the advantages that and receive the great concern of researcher.
Bimetallic transition metal oxide is very heavy in supercapacitor large family as the electrode material haveing excellent performance
The a member wanted.Bimetallic transition oxide such as MCo2O4, wherein M is Zn, Ni, Mn or Cu etc., because of it with better electric conductivity and
Higher electro-chemical activity, therefore can get high specific capacitance, good high rate performance and excellent cyclical stability.Numerous studies
Show that the higher conductivity of transition metal oxide can accelerate electron-transport and charge and discharge process in electrochemical reaction process
In ion diffusion.Zhang et al. by co-precipitation hydroxide precursor and at a certain temperature progress subsequent heat treatment come
Ni-Co oxide is prepared, the composition of the primitive reaction object of hydroxide precursor is used to prepare by adjusting, can easily be controlled
The ratio of Ni and Co in oxide, and have studied Ni/Co molar ratio the fake capacitance performance of binary metal oxide is influenced, when
When Ni:Co molar ratio=0.8:1, after binary Ni/Co metal oxide precursor is annealed at 300 DEG C, its electrochemistry is tested
Energy specific capacitance can achieve 750F/g.
Co oxide and Fe oxide all have good chemical property, furthermore Fe-Co oxide (FeCo2O4) it is property
The more excellent electrode material of energy, because it provides richer electro-chemical activity site and more Fe than single component2+/
Fe3+And Co2+/Co3+Redox reaction electronics pair.In recent years, due to Fe-Co oxide (FeCo2O4) inexpensive and good with it
Good chemical property provides infusive chance for electrode material, therefore many scientists have been devoted to it and storing up
The application study in the fields such as energy, catalysis, sensor.For example, Chodankar et al. is prepared on carbon cloth substrate by hydro-thermal method
FeCo2O4Nano material obtains FeCo2O4Film, specific capacitance of the constant current charge-discharge curve under the current density of 3A/g are
1329F/g is recycled 5000 times under the sweep speed of 100mV/s, and capacity retention is up to 70.27%, shows good
Chemical property.
It is documented that not yet someone makes the FeCo of nano whiskers structure by the hydro-thermal reaction of easy green so far2O4
Material.
Summary of the invention
In order to overcome the defects of the prior art described above, the purpose of the present invention is to provide a kind of nano whiskers FeCo2O4Electrode
The preparation method and application of material utilizes hydro-thermal process growth in situ FeCo2O4Nano material, this method and process is controllable, cost
It is low, environmentally friendly, more active sites are provided for charge transmission and ion diffusion, are stored up to extend it in supercapacitor etc.
The application in energy field.
To achieve the goals above, the technical solution adopted by the present invention is that:
A kind of nano whiskers FeCo2O4The preparation method of electrode material, comprising the following steps:
Step 1: powder mixing
Weigh 50-150mg frerrous chloride FeCl2·4H2O, 200-500mg cobalt nitrate Co (NO3)2·6H2O, 20-60mg urine
Plain Co (NH2)2, 100-200mg ammonium fluoride NH470mL deionized water, magnetic agitation 1-3h is added in F；
Step 2: hydro-thermal reaction
The mixed solution that step 1 is obtained is transferred in 100mL water heating kettle, keeps the temperature 5-10h at 100-200 DEG C；It has reacted
Washed 3 times, then be dried in vacuo respectively with deionized water and dehydrated alcohol afterwards, 60 DEG C of heat preservation 10-15h to get arrive nano whiskers
FeCo2O4Material.
A kind of nano whiskers FeCo2O4Nickel foam is cut into 1*2cm by the application of electrode material2The rectangle of size, according to
It is secondary to weigh 16-20mg nano whiskers FeCo2O4The conductive acetylene of material, 1-5mg is black, the polyvinylidene fluoride of 1-5mg, in agate
1-3h is ground in mortar；It is added in agate mortar and is regrind with the NMP that liquid-transfering gun draws 300 μ L, obtain uniform slurry；Slurry
Material mean droplet is added in the nickel foam cut, and by the nickel foam being added dropwise 60 DEG C of dry 10-15h in a vacuum drying oven；
Finally, by the electrode slice made under tablet press machine 8-15Mpa pressure maintaining 1-3min up to FeCo2O4Electrode.
Product verifying
It is to electrode with Pt electrode, Ag/AgCl is reference electrode, and 3M KOH uses Shanghai Chen Hua as electrolyte
CHI660E electrochemical workstation tests FeCo2O4The chemical property of electrode, such as cyclic voltammetry curve, constant current charge-discharge, friendship
Flow impedance.The result shows that nano whiskers FeCo2O4Electrode is demonstrated by good chemical property, has apparent redox peaks to go out
It is existing, show FeCo2O4Electrode material has fake capacitance characteristic；When sweep speed is 2mV s-1When, specific capacity is about 1080.7F g-1；And cyclic curve is formed by region and increases with the increase of sweep speed, but the general shape of figure is basically unchanged, table
Good high rate performance is revealed.
Beneficial effects of the present invention
The FeCo of nano whiskers is prepared using hydro-thermal method2O4Electrode material, preparation method is simple and effective, and prepares a wiener
The FeCo of rice acicular texture2O4Specific surface area is bigger, provides richer electro-chemical activity site and more Fe2+/Fe3+And
Co2+/Co3+Redox reaction electronics pair, so that nano whiskers FeCo2O4The chemical property of electrode material is substantially better than randomly
Graininess FeCo2O4Chemical property, for its further supercapacitor research and application lay a good foundation.
The present invention is with FeCl2·4H2O is source of iron, Co (NO3)2·6H2O is cobalt source, CO (NH2)2、NH4F is precipitating reagent, is adopted
The FeCo of nano whiskers is prepared with hydro-thermal method2O4Electrode material successfully prepares FeCo2O4Nano material.Preparation method simply has
Effect, and prepare the FeCo of 1-dimention nano acicular texture2O4Specific surface area is bigger, provides richer electro-chemical activity site and more
More Fe2+/Fe3+And Co2+/Co3+Redox reaction electronics pair, so that nano whiskers FeCo2O4The electrochemistry of electrode material
Irregular granules shape FeCo can be substantially better than2O4Chemical property, for its further supercapacitor research and application establish
Basis.
It is applied on electrochemical capacitor, experiment shows FeCo2O4Nano material has excellent specific capacity and change
Learn stability.And experimentation of the present invention is simple, easy to operate, safety and environmental protection, is it further in supercapacitor and lithium ion
The application of the energy storage fields such as battery is laid a good foundation.
Detailed description of the invention
Fig. 1 is one nano whiskers FeCo of embodiment2O4XRD spectrum.
Fig. 2 is one nano whiskers FeCo of embodiment2O4Sample SEM figure.
Fig. 3 is one nano whiskers FeCo of embodiment2O4Electrode material different scanning rates under three electrode test systems are corresponding
Cyclic voltammetry curve figure.
Specific embodiment
The present invention is described in further details with embodiment with reference to the accompanying drawing.
Embodiment one
A kind of nano whiskers FeCo of the present embodiment2O4The preparation method of electrode material, comprising the following steps:
Step 1: powder mixing
Weigh 50mg frerrous chloride (FeCl2·4H2O), 200mg cobalt nitrate (Co (NO3)2·6H2O), 20mg urea (Co
(NH2)2), 100mg ammonium fluoride (NH4F), 70mL deionized water, magnetic agitation 1h is added.
Step 2: hydro-thermal reaction
The mixed solution that step 1 is obtained is transferred in 100mL water heating kettle, keeps the temperature 5h at 200 DEG C；It is spent after having reacted
Ionized water and dehydrated alcohol wash 3 times respectively, then are dried in vacuo, 60 DEG C of heat preservation 10h to get arrive nano whiskers FeCo2O4Material.
Fig. 1 is the XRD spectrum of nano whiskers FeCo2O4, and Fig. 2 is nano whiskers FeCo2O4 sample SEM figure, can from figure
By find out to get to maximum gauge about 250nm, about 6 μm of length, in cluster in the form of FeCo2O4 nano whiskers material.
A kind of nano whiskers FeCo of the present embodiment2O4Nickel foam is cut into 1*2cm by the application of electrode material2The length of size
It is rectangular, successively weigh the nano whiskers FeCo of 20mg2O4The conductive acetylene of material, 5mg is black, the polyvinylidene fluoride of 5mg, in Ma
3h is ground in Nao mortar；It is added in agate mortar and is regrind with the NMP (N-Methyl pyrrolidone) that liquid-transfering gun draws 300 μ L,
Obtain uniform slurry；Slurry mean droplet is added in the nickel foam cut, and by the nickel foam being added dropwise in vacuum oven
In 60 DEG C of dry 15h；Finally, by the electrode slice made under tablet press machine 15Mpa pressure maintaining 3min to get FeCo2O4Electrode.
Pt electrode is to electrode, and Ag/AgCl is reference electrode, and 3M KOH is as electrolyte, with Shanghai Chen Hua CHI660E electricity
The test of chem workstation progress capacitor performance.It can be obtained from Fig. 3, FeCo2O4It is demonstrated by good chemical property, is had obvious
Redox peaks occur, show composite material have fake capacitance characteristic and stored energy capacitance；And cyclic voltammetry curve is formed by
Region increases with the increase of sweep speed, but the general shape of figure is basically unchanged, and shows good high rate performance.
Embodiment two
A kind of nano whiskers FeCo of the present embodiment2O4The preparation method of electrode material, comprising the following steps:
Step 1: powder mixing
Weigh 150mg frerrous chloride (FeCl2·4H2O), 500mg cobalt nitrate (Co (NO3)2·6H2O), 60mg urea (Co
(NH2)2), 200mg ammonium fluoride (NH4F), 70mL deionized water, magnetic agitation 3h is added.
Step 2: hydro-thermal reaction
The mixed solution that step 1 is obtained is transferred in 100mL water heating kettle, keeps the temperature 5h at 200 DEG C；It is spent after having reacted
Ionized water and dehydrated alcohol wash 3 times respectively, then are dried in vacuo, 60 DEG C of heat preservation 10h to get arrive nano whiskers FeCo2O4Material.
A kind of nano whiskers FeCo of the present embodiment2O4Nickel foam is cut into 1*2cm by the application of electrode material2The length of size
It is rectangular, successively weigh the nano whiskers FeCo of 16mg2O4The conductive acetylene of material, 1mg is black, the polyvinylidene fluoride of 1mg, in Ma
1h is ground in Nao mortar；It is added in agate mortar and is regrind with the NMP (N-Methyl pyrrolidone) that liquid-transfering gun draws 300 μ L,
Obtain uniform slurry；Slurry mean droplet is added in the nickel foam cut, and by the nickel foam being added dropwise in vacuum oven
In 60 DEG C of dry 10h；Finally, by the electrode slice made under tablet press machine 8Mpa pressure maintaining 1min to get FeCo2O4Electrode.
Pt electrode is to electrode, and Ag/AgCl is reference electrode, and 3M KOH is as electrolyte, using Shanghai Chen Hua CHI660E
Electrochemical workstation carries out the test of capacitor performance, such as cyclic voltammetry curve, constant current charge-discharge, AC impedance.
Embodiment three
A kind of nano whiskers FeCo of the present embodiment2O4The preparation method of electrode material, comprising the following steps:
Step 1: powder mixing
Weigh 50mg frerrous chloride (FeCl2·4H2O), 200mg cobalt nitrate (Co (NO3)2·6H2O), 20mg urea (Co
(NH2)2), 100mg ammonium fluoride (NH4F), 70mL deionized water, magnetic agitation 1h is added.
Step 2: hydro-thermal reaction
The mixed solution that step 1 is obtained is transferred in 100mL water heating kettle, keeps the temperature 10h at 100 DEG C；It is spent after having reacted
Ionized water and dehydrated alcohol wash 3 times respectively, then are dried in vacuo, 60 DEG C of heat preservation 15h to get arrive nano whiskers FeCo2O4Material.
A kind of nano whiskers FeCo of the present embodiment2O4Nickel foam is cut into 1*2cm by the application of electrode material2The length of size
It is rectangular, successively weigh the nano whiskers FeCo of 20mg2O4The conductive acetylene of material, 5mg is black, the polyvinylidene fluoride of 5mg, in Ma
3h is ground in Nao mortar；It is added in agate mortar and is regrind with the NMP (N-Methyl pyrrolidone) that liquid-transfering gun draws 300 μ L,
Obtain uniform slurry；Slurry mean droplet is added in the nickel foam cut, and by the nickel foam being added dropwise in vacuum oven
In 60 DEG C of dry 15h；Finally, by the electrode slice made under tablet press machine 15Mpa pressure maintaining 3min to get FeCo2O4Electrode.
Pt electrode is to electrode, and Ag/AgCl is reference electrode, and 3M KOH is as electrolyte, with Shanghai Chen Hua CHI660E electricity
Chem workstation carries out the test of capacitor performance, such as cyclic voltammetry curve, constant current charge-discharge, AC impedance.
Example IV
Step 1: powder mixing
Weigh 150mg frerrous chloride (FeCl2·4H2O), 500mg cobalt nitrate (Co (NO3)2·6H2O), 60mg urea (Co
(NH2)2), 200mg ammonium fluoride (NH4F), 70mL deionized water, magnetic agitation 3h is added.
Step 2: hydro-thermal reaction
The mixed solution that step 2 is obtained is transferred in 100mL water heating kettle, keeps the temperature 10h at 100 DEG C；It is spent after having reacted
Ionized water and dehydrated alcohol wash 3 times respectively, then are dried in vacuo, 60 DEG C of heat preservation 15h to get arrive FeCo2O4Nanoneedle.
A kind of nano whiskers FeCo of the present embodiment2O4Nickel foam is cut into 1*2cm by the application of electrode material2The length of size
It is rectangular, successively weigh FeCo obtained by the active material i.e. step 3 of 16mg2O4The conductive acetylene of nano-powder, 1mg is black, and 1mg's is poly-
Vinylidene fluoride grinds 1h in the agate mortar；Agate is added with the NMP (N-Methyl pyrrolidone) that liquid-transfering gun draws 300 μ L
It is regrind in mortar, obtains uniform slurry；Slurry mean droplet is added in the nickel foam cut, and the foam that will be added dropwise
Nickel 60 DEG C of dry 10h in a vacuum drying oven；Finally, by the electrode slice made under tablet press machine 8Mpa pressure maintaining 1min to get
FeCo2O4Electrode.
Pt electrode is to electrode, and Ag/AgCl is reference electrode, and 3M KOH is as electrolyte, with Shanghai Chen Hua CHI660E electricity
Chem workstation carries out the test of capacitor performance, such as cyclic voltammetry curve, constant current charge-discharge, AC impedance.
Claims (8)
1. a kind of nano whiskers FeCo2O4The preparation method of electrode material, which comprises the following steps:
Step 1: powder mixing
Weigh 50-150mg frerrous chloride FeCl2·4H2O, 200-500mg cobalt nitrate Co (NO3)2·6H2O, 20-60mg urea Co
(NH2)2, 100-200mg ammonium fluoride NH470mL deionized water, magnetic agitation 1-3h is added in F；
Step 2: hydro-thermal reaction
The mixed solution that step 1 is obtained is transferred in 100mL water heating kettle, keeps the temperature 5-10h at 100-200 DEG C；Use after having reacted
Deionized water and dehydrated alcohol wash 3 times respectively, then are dried in vacuo, 60 DEG C of heat preservation 10-15h to get arrive nano whiskers FeCo2O4
Material.
2. a kind of nano whiskers FeCo according to claim 12O4The preparation method of electrode material, which is characterized in that step
The time of one magnetic agitation is 1h.
3. a kind of nano whiskers FeCo according to claim 12O4The preparation method of electrode material, which is characterized in that step
Two the hydro-thermal reaction times are 6h.
4. a kind of nano whiskers FeCo according to claim 12O4The preparation method of electrode material, which is characterized in that step
Two vacuum drying times are 12h.
5. a kind of nano whiskers FeCo according to claim 12O4The preparation method of electrode material, which is characterized in that step
Three mortar grinder time be 1h.
6. a kind of nano whiskers FeCo according to claim 12O4The preparation method of electrode material, which is characterized in that step
Four tablet press machine pressure are 10Mpa.
7. a kind of nano whiskers FeCo according to claim 12O4The preparation method of electrode material, which is characterized in that step
Four tablet press machine dwell times were 1min.
8. a kind of nano whiskers FeCo2O4The application of electrode material, which is characterized in that nickel foam is cut into 1*2cm2Size
Rectangle successively weighs 16-20mg nano whiskers FeCo2O4The conductive acetylene of material, 1-5mg is black, the poly- inclined difluoro second of 1-5mg
Alkene grinds 1-3h in the agate mortar；It is added in agate mortar and is regrind with the NMP that liquid-transfering gun draws 300 μ L, obtained uniformly
Slurry；Slurry mean droplet is added in the nickel foam cut, and the nickel foam being added dropwise is done for 60 DEG C in a vacuum drying oven
Dry 10-15h；Finally, by the electrode slice made under tablet press machine 8-15Mpa pressure maintaining 1-3min to get FeCo2O4Electrode.
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Cited By (4)
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| CN110563049B (en) * | 2019-09-30 | 2021-11-02 | 淮阴师范学院 | Cobalt zinc sulfide nano material and preparation method and application thereof |
| CN110808172A (en) * | 2019-10-31 | 2020-02-18 | 上海应用技术大学 | Fe-Co-S nanosheet material and preparation method and application thereof |
| CN116759241A (en) * | 2023-04-20 | 2023-09-15 | 长沙理工大学 | FeCo for electrochemical energy storage 2 O 4 -Ti 3 C 2 Preparation method of MXene nanocomposite |
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