CN108493004A - A kind of preparation method and application of the ferric oxide nano-material of morphology controllable - Google Patents
A kind of preparation method and application of the ferric oxide nano-material of morphology controllable Download PDFInfo
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- CN108493004A CN108493004A CN201810261844.XA CN201810261844A CN108493004A CN 108493004 A CN108493004 A CN 108493004A CN 201810261844 A CN201810261844 A CN 201810261844A CN 108493004 A CN108493004 A CN 108493004A
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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 belongs to ultracapacitor and field of nanometer material technology, and in particular to a kind of preparation method of the ferric oxide nano-material of morphology controllable；The specific steps are, it weighs glycerine and deionized water is uniformly mixed, then ferric chloride hexahydrate and urea is added, stirring, then mixed solution is transferred in high-temperature high-pressure reaction kettle and carries out hydro-thermal reaction, waited after the completion of reacting, cooled to room temperature, through Magnetic Isolation or centrifuge separation, vacuum drying, the ferric oxide nano-material of morphology controllable is obtained；Ferric oxide nano-material synthetic method of the present invention is simple, cheap, when being applied in ultracapacitor, has larger specific discharge capacity and good cyclical stability.
Description
Technical field
The invention belongs to ultracapacitor fields, and in particular to a kind of system of the ferric oxide nano-material of different-shape
Preparation Method.
Background technology
21 century, the mankind are faced with the problem of the traditional energies such as coal, oil, natural gas shortage, and this requires people urgently
Develop novel energy, such as solar energy, wind energy, nuclear energy, tide energy.At the same time, some novel energy storage apparatus also come into being,
Such as solid state battery, ultracapacitor, and ultracapacitor has power density big in numerous energy storage devices, has extended cycle life
And the features such as environmentally protective, has caused the extensive concern of scientific research personnel.Ultracapacitor is also known as electrochemical capacitor, is
A kind of novel energy storage apparatus for having gathered traditional capacitor high power density and battery high energy metric density.And for ultracapacitor
For, the selection of electrode material is most important, therefore, in terms of current research hot spot is concentrated mainly on electrode material, develops one
Kind is high with energy density, power density is big, the electrode material of good cycling stability is most important to the development of ultracapacitor.
According to charge-storage mechanism, ultracapacitor can be divided into two classes：Double layer capacitor（EDLC）It is counterfeit with faraday
Capacitor.Double layer capacitor is mainly positioned against electrode material both ends and applies voltage, passes through the electronics in electrostatic attraction electrolyte
It forms electrode/electrolyte interfacial electric double layer and carries out storage charge, process is not related to chemically react；And pseudocapacitors mainly lean on
After electrode material both ends apply voltage, the redox that Rapid reversible occurs on the surface of electrode active material or near surface is anti-
It answers, and then achievees the purpose that store charge.Since pseudocapacitors electrode material stores charge mainly by redox reaction,
With high specific capacity.
The electrode material of ultracapacitor can be mainly divided into three classes, and the first kind is used as the carbon material of electric double layer capacitance,
Include mainly：Activated carbon, carbon nanotube, carbon fiber, carbon aerogels and graphene etc.；Second class is conducting polymer, main to wrap
It includes：Polyaniline, polypyrrole and polythiophene etc.；Third class is then metal oxide, includes mainly：Iron-series metal oxide, manganese systems
Metal oxide, cobalt system and nickel series metal oxide etc..Due to electrode material for electric double layer capacitor when storing charge only lean on it is quiet
Electric attraction is not directed to chemical reaction, therefore specific discharge capacity is smaller, to limit its commercial applications；And pseudocapacitors
Electrode material is mainly positioned against electrode material surface or quick faraday's redox reaction occurs near surface, enables charge
It stores and discharges, therefore there is higher specific discharge capacity.And iron series element metal oxide is compared to manganese systems, cobalt system, nickel system
For equal metal oxides, price is cheaper, source is more abundant, and content is only second to aluminium in earth's crust metallic element,
Therefore the oxide such as Fe of iron3O4, Fe2O3, FeOOH etc. is at low cost, resourceful, environmental-friendly and higher electric discharge
The features such as specific capacity, is widely used as the replacement electrode material of pseudocapacitors.
The preparation method of metal oxide nano-material mainly also has：The precipitation method, microemulsion method, thermal decomposition method.The precipitation method
Although easy to operate, product quality is not easy to control；Microemulsion method needs to use a large amount of organic solvents, surfactant etc.,
Environmental pollution is serious, and being needed by metal oxide nano-material prepared by microemulsion method can profit after being modified after carrying out
With；Thermal decomposition method is mainly under the high temperature conditions（Generally 300oC or more）, so that presoma is decomposed and generate metal oxidation
Object nano material.This method energy consumption is big, needs expensive equipment, and is modified after the product prepared difficult；Hydro-thermal method in contrast,
Easy to operate, reaction condition is mild, it is i.e. usable to prepare modification after product is generally not necessarily to.
Invention content
It is an object of the invention to overcome synthesis technology complexity in the prior art, raw material are expensive, sample topography unevenness
Defect.
The present invention solves its technical problem using following technical scheme：
Present invention firstly provides a kind of ferric oxide nano-material of morphology controllable, the shape of material is particle, microballoon, ellipse
Ball, rodlike and pie, size are micro-nano rank.
The present invention also provides a kind of preparation methods of the ferric oxide nano-material of morphology controllable, include the following steps：
The glycerine centainly matched and deionized water are weighed first, are uniformly mixed；Then, ferric chloride hexahydrate and urea is added,
Mixed solution is obtained after stirring；Mixed solution is transferred in high-temperature high-pressure reaction kettle and carries out hydro-thermal reaction, is waited after the completion of reacting,
Cooled to room temperature obtains the di-iron trioxide nanometer material of morphology controllable through Magnetic Isolation or centrifuge separation, vacuum drying
Material.
Preferably, the volume ratio of the glycerine and deionized water is 0 ~ 15:45~60.
Preferably, the molar ratio of the ferric chloride hexahydrate and urea is 1:1.
Preferably, the hydrothermal temperature is 190 DEG C ~ 220 DEG C, and the time is 6h ~ 15h.
Urea used is as precipitating reagent, and ferric chloride hexahydrate used is as source of iron.
The present invention provides the ferric oxide nano-material that source of iron prepares different-shape with ferric chloride hexahydrate, is applied to
Capacitor area is a kind of fake capacitance electrode material with applications well foreground.
Advantageous effect：
（1）The present invention provides source of iron using ferric chloride hexahydrate, and abundance is cheap；Glycerine and water are nontoxic molten
Agent has the advantages such as environmentally protective；Collectively as mixed solvent, glycerine has adjusting material surface polar for glycerine and water
Effect, the dosage of glycerine has the pattern of material, size important influence, to influence material specific capacity size.
（2）The present invention uses solvent-thermal method, is reacted under the boiling point less than glycerine, and reaction condition is mild, and anti-
It is short between seasonable, you can ferric oxide nano-material to be obtained, to save time and the cost of industrialized production.
（3）Ferric oxide nano-material prepared by the present invention has pattern uniform, and stability is good, and grain size is small, compares table
The big feature of area can come into full contact with the electronics in electrolyte, and specific capacity is up to 260 F/g, after 5000 cycles
Capacity retention ratio be 82.8%；Therefore have many advantages, such as higher specific discharge capacity, good cycling stability.
（4）Preparation method is simple, flow is shorter, easy controlled operation by the present invention, suitable for promoting the use of.
Description of the drawings
Fig. 1 is Fe prepared by embodiment 1-42O3-0、Fe2O3-5、Fe2O3- 10 and Fe2O3-15（0, it 5,10,15 respectively represents
The volumetric usage of glycerine in preparation process（mL））The XRD spectrum of nano material.
In Fig. 2,（a）With（b）For the scanning electron microscope and transmission electron microscope of ferric oxide nano-material prepared by embodiment 1
Figure；（c）With（d）For the scanning electron microscope and transmission electron microscope picture of ferric oxide nano-material prepared by embodiment 2；（e）With（f）For
The scanning electron microscope and transmission electron microscope picture of ferric oxide nano-material prepared by embodiment 3；（g）With（h）It is prepared for embodiment 4
The scanning electron microscope and transmission electron microscope picture of ferric oxide nano-material；
Fig. 3 is the Fe prepared in embodiment 1-42O3-0、Fe2O3-5、Fe2O3-10、Fe2O3The cyclic voltammetric of -15 nano materials
（CV）Curve.
Fig. 4 is the Fe prepared in embodiment 1-42O3-0、Fe2O3-5、Fe2O3-10、Fe2O3- 15 nano materials are close in electric current
Degree is 1A/g, the constant current charge and discharge under the conditions of a concentration of 1mol/L of KOH（GCD）Curve.
Fig. 5 is the Fe prepared in embodiment 1-42O3-0、Fe2O3-5、Fe2O3-10、Fe2O3- 15 nano materials are close in electric current
Degree is the stable circulation figure under the conditions of 2A/g.
Specific implementation mode
The present invention is illustrated with following implementation, but the present invention is not limited to the following embodiments, is not departing from the front and back objective
In the range of, change is included in the technical scope of the present invention.
Embodiment 1
First, the deionized water of 60mL is added as solvent；The ferric chloride hexahydrate of 6 mmol, the urea of 6mmol, stirring is added
Uniformly, mixed solution is obtained；Mixed solution is transferred in high-temperature high-pressure reaction kettle later, at 200 DEG C, reacts 10 h；Most
Cooled to room temperature afterwards, through deionized water wash 3 times, absolute ethyl alcohol wash 1 time, Magnetic Isolation or centrifuge separation, vacuum
It is dry, red di-iron trioxide nano particle is obtained, Fe is denoted as2O3-0。
Embodiment 2
First, the glycerine of 5mL and the deionized water of 55mL are weighed, is uniformly mixed；The ferric chloride hexahydrate of 6mmol is added,
The urea of 6mmol, stirs evenly, and obtains mixed solution；Mixed solution is transferred in high-temperature high-pressure reaction kettle later, 200
At DEG C, 10 h are reacted；Last cooled to room temperature, through deionized water wash 3 times, absolute ethyl alcohol wash 1 time, Magnetic Isolation or
Centrifuge separation, vacuum drying, obtain red di-iron trioxide nanoparticle, are denoted as Fe2O3-5。
Embodiment 3
First, the glycerine of 10mL and the deionized water of 50mL are weighed, is uniformly mixed；The ferric chloride hexahydrate of 6mmol is added,
The urea of 6mmol, stirs evenly, and obtains mixed solution；Mixed solution is transferred in high-temperature high-pressure reaction kettle later, 200
At DEG C, 10 h are reacted；Last cooled to room temperature, through deionized water wash 3 times, absolute ethyl alcohol wash 1 time, Magnetic Isolation or
Centrifuge separation, vacuum drying, obtain red di-iron trioxide nanometer ellipsoid, are denoted as Fe2O3-10。
Embodiment 4
First, the glycerine of 15mL and the deionized water of 45mL are weighed, is uniformly mixed；The ferric chloride hexahydrate of 6mmol is added,
The urea of 6mmol, stirs evenly, and obtains mixed solution；Mixed solution is transferred in high-temperature high-pressure reaction kettle later, 200
At DEG C, 10 h are reacted；Last cooled to room temperature, through deionized water wash 3 times, absolute ethyl alcohol wash 1 time, Magnetic Isolation or
Centrifuge separation, vacuum drying, obtain the red ferric oxide powder of two kinds of patterns of corynebacterium and pie, are denoted as Fe2O3-15。
As can be seen that the proportioning of mixed solvent glycerine and glycerine is in a certain range（0-15:45-60）Change equal
Fe can be obtained2O3Nano material, but its pattern is changed.
The XRD spectrum of material, which can be seen that the material prepared by the present invention, in Fig. 1 has good diffraction maximum, right respectively
It should be in Fe2O3(012), (104), (110), (113), (202), (024), (116), (018), (214) and (300), it was demonstrated that
Four kinds of materials of synthesis are Fe2O3Nano material.
In Fig. 2 as it can be seen that（a）With（b）, and（c）With（d）,（e）With（f）,（g）With（h）It is followed successively by Fe2O3- 0, Fe2O3- 5,
Fe2O3- 10 and Fe2O3- 15 field emission scanning electron microscope figure（FESEM）And transmission electron microscope picture（TEM）, from（a）With（b）It can see
Go out, when only using deionized water as solvent, product Fe2O3Nano particle, size is in 100 nm ~ 500nm；From（c）
With（d）As can be seen that when the glycerine of 5mL is added in deionized water, product Fe2O3Nanoparticle, size 1.5
μm ~ 2 μm, surface is more coarse；From（e）With（f）As can be seen that when the glycerine of 10mL is added in deionized water, Fe2O3
Pattern become the spheroid similar to button shape, size is 0.82 μm ~ 1.2 μm, favorable dispersibility；From（g）With（h）It can
To find out, when the glycerine of 15mL is added in deionized water, occur two kinds of patterns in sample, one kind is corynebacterium knot
Structure, length be 150nm ~ 200nm, it is another then be pie structure, a diameter of 150nm ~ 300nm.
To the Fe prepared by the present invention2O3Nano material carries out electrochemical property test：
（1）The preparation of electrode slurry：By electrode material, conductive agent（Acetylene black）And binder（Kynoar）According to 75:15:
10 ratio is scattered in dispersant 1-Methyl-2-Pyrrolidone（NMP）In, it is uniformly mixed to get to electrode slurry.
（2）The preparation of foam nickel electrode piece：Nickel foam is cut into the rectangular-shaped pieces of 5cm × 1cm, and is marked at 4cm
Note, obtains the precoating plasma-based material surface of 1cm × 1cm.Nickel foam is washed later, nickel foam is immersed in third first
In ketone, sonic oscillation 15min, then nickel foam is immersed in the hydrochloric acid solution of 1mol/L, sonic oscillation 15min；It later again will bubble
Foam nickel immerses in deionized water, sonic oscillation 15min；Finally nickel foam is immersed in absolute ethyl alcohol again, sonic oscillation 15min.
Nickel foam is transferred in vacuum drying chamber again, dry 12h, obtains electrode slice at 60 DEG C.
（3）The preparation of electrode material：Plasma-based material is evenly applied to foam nickel electrode on piece, is transferred to vacuum drying chamber
In, dry 12h, obtains electrode material at 60 DEG C.
As it can be seen that Fe in Fig. 32O3-0、Fe2O3-5、Fe2O3-10、Fe2O3- 15 nano materials all have apparent redox
Peak shows that four kinds of materials belong to fake capacitance material；And Fe2O3The area that the corresponding curve of -15 nano materials surrounds is maximum, puts
Electric specific capacity highest.
As it can be seen that the potential window of four kinds of materials is all up 0.5V, Fe in Fig. 42O3The discharge time longest of -15 nano materials,
In the case where current density is 1A/g, specific capacity has higher specific discharge capacity up to 260 F/g.This is mainly by Fe2O3-15
The size of nano material is smaller, what large specific surface area determined.Secondly it is Fe2O3- 10 specific discharge capacities with 140 F/g, this master
If since its grain size is larger, specific surface area is smaller, but resulted in since its surface texture is imperfect its in electrolyte
Electronic contact area increases, and finally determines the size of its specific capacity；Fe2O3- 0 and Fe2O3The specific capacity of -5 nanospheres is respectively about
For 100 F/g and 80 F/g, this is mainly due to its grain size is larger, and the smaller decision of specific surface area.
Fig. 5 is stable circulation figure of four kinds of materials in the case where current density is 2A/g, it can be seen that four kinds of materials pass through
Capacity retention ratio after 5000 cycles is followed successively by 62.1%, 67.1%, 73.7%, 82.8%.Therefore Fe2O3- 15 with more excellent
Different cyclical stability.
The above test result shows synthesized Fe2O3- 15 nano materials have more excellent specific discharge capacity and
There is more excellent capacity conservation rate after charge and discharge cycles 5000 times, be a kind of good electrode material for super capacitor.
Claims (7)
1. a kind of ferric oxide nano-material of morphology controllable, which is characterized in that the ferric oxide nano-material shape
Shape is particle, microballoon, ellipsoid, rodlike or pie.
2. a kind of preparation method of the ferric oxide nano-material of morphology controllable, which is characterized in that include the following steps：
The glycerine centainly matched and deionized water are weighed first, are uniformly mixed；Then, ferric chloride hexahydrate and urea is added,
Mixed solution is obtained after stirring；Mixed solution is transferred in high-temperature high-pressure reaction kettle and carries out hydro-thermal reaction, is waited after the completion of reacting,
Cooled to room temperature obtains the di-iron trioxide nanometer material of morphology controllable through Magnetic Isolation or centrifuge separation, vacuum drying
Material.
3. a kind of preparation method of the ferric oxide nano-material of morphology controllable according to claim 2, feature exist
In the volume ratio of the glycerine and deionized water is 0 ~ 15:45~60.
4. a kind of preparation method of the ferric oxide nano-material of morphology controllable according to claim 2, feature exist
In the molar ratio of the ferric chloride hexahydrate and urea is 1:1.
5. a kind of preparation method of the ferric oxide nano-material of morphology controllable according to claim 2, feature exist
In the hydrothermal temperature is 190 DEG C ~ 220 DEG C.
6. a kind of preparation method of the ferric oxide nano-material of morphology controllable according to claim 2, feature exist
In the hydro-thermal reaction time is 6h ~ 15h.
7. a kind of preparation of the ferric oxide nano-material of morphology controllable according to 1 ~ 6 any one claim of right
Ferric oxide nano-material prepared by method is applied to ultracapacitor field.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN111668445A (en) * | 2020-06-01 | 2020-09-15 | 广东轻工职业技术学院 | Shape-controllable nickel manganese oxide electrode material and preparation method and application thereof |
| CN111905689A (en) * | 2019-05-08 | 2020-11-10 | 浙江理工大学 | Flexible glass fiber cloth @ FeZn double-hydroxide adsorbing material and preparation method thereof |
| CN115159583A (en) * | 2022-07-07 | 2022-10-11 | 重庆邮电大学 | Method for preparing spherical ferric oxide material by quasi-triangular star self-assembly, product and application thereof |
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