CN105948132B - Preparation method of three-dimensional gamma-Fe2O3 nano material and application thereof - Google Patents
Preparation method of three-dimensional gamma-Fe2O3 nano material and application thereof Download PDFInfo
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- CN105948132B CN105948132B CN201610297333.4A CN201610297333A CN105948132B CN 105948132 B CN105948132 B CN 105948132B CN 201610297333 A CN201610297333 A CN 201610297333A CN 105948132 B CN105948132 B CN 105948132B
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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
Abstract
The invention discloses a preparation method of a three-dimensional gamma-Fe2O3 nano material and application thereof. The method includes: firstly adding an iron source into an organic solvent, conducting heating to reach a reflux state, then depositing an electrolyte solution orderly on a conductive substrate with a 3D structure, and conducting annealing treatment to prepare the gamma-Fe2O3 material. The material provided by the invention has a three-dimensional micrometer or nanometer porous structure. Electrochemical testing proves that the three-dimensional gamma-Fe2O3 nano material has excellent circulation and rate capability, and can be used as the electrode material of a super capacitor. The method provided by the invention has the characteristics of simple preparation process, low cost and low equipment requirement. The obtained material has the advantages of uniform deposit and micropore structure, controllable deposition thickness, and good product uniformity.
Description
Technical field
The invention belongs to energy storage technical field of material, is related to a kind of nano material, it particularly relates to a kind of
γ-Fe2O3The preparation method and applications of nano material.
Background technology
The energy plays an important role in the development of human civilization and the progress of modern science and technology, all the time, and it is
The eternal pursuit of the mankind.Energy storage, is an important intermediate steps to multi-functional, high efficient energy sources application, in academia
All have been a great concern with industrial circle.In various energy storage systems, electrochemical storage device is (such as battery and super electricity
Container) due to advantages such as its efficiency high, versatility and plasticity, conduct extensive research, and be also considered to be soon
Most promising green sustainable energy storage system in future.In electrochemical storage device, ultracapacitor is unique because of which
High power density, to have extended cycle life receive the very big concern of people with the advantage such as fast charging and discharging.And these advantages
It has been promoted to play great function at aspects such as electric automobile, Aero-Space, hybrid fuel cells.
Currently, increasing transition metal oxide is used in the research of energy-storage system-ultracapacitor, such as
RuOx, IrOx etc..However, these materials are in nature scarcity of resources, it is expensive, and not enough environmental protection, therefore, to ferrum oxygen
The demand of this kind of theoretical specific capacity height of compound, energy density height, aboundresources, environmental friendliness and cheap material is just more
For urgent.However, with regard to Fe2O3During as super capacitor material, some drawbacks are there are：First, the material is done in base electrode
During Large Copacity discharge and recharge, the crushing of electrode is easily caused；Again, to be easily caused device high for the high resistivity of metal-oxide
Internal resistance, has had a strong impact on its using value.Therefore, prepare high-performance iron sesquioxide material to be particularly important.
The content of the invention
In order to overcome the deficiencies in the prior art, it is an object of the invention to provide a kind of three-dimensional γ-Fe2O3Nano material
Preparation method and applications.Preparation process is simple of the present invention, with low cost, the material for obtaining has three-dimensional porous structure, electrification
Learn performance remarkable, can be used as super capacitor material.
Technical scheme is specifically described as follows.
The present invention provides a kind of three-dimensional γ-Fe2O3The preparation method of nano material, comprises the following steps that：
(1) it is 0.01 according to mass volume ratio by iron salt and organic solvent：1-1:1g/L is mixed, and obtains iron salt dispersion
Liquid；Wherein：The organic solvent is selected from 1-Methyl-2-Pyrrolidone (NMP), tetrahydrofuran (THF), dimethylformamide
(DMF), in butyrolactone (GBL), acetone or alcohol any one；
(2) using the iron salt dispersion obtained by step (1) as electrophoretic deposition electrolyte, with identical or unlike material
Positive and negative electrode pole piece of the conductive substrates respectively as electrophoretic deposition pond, electrolyte is heated to after backflow, electrophoretic deposition is carried out；Electricity
After swimming deposition terminates, take cathode pole piece and be placed in annealing in Muffle furnace, i.e., γ-Fe are obtained on the surface of cathode pole piece2O3Receive
Rice material, wherein：Cathode pole piece has 3D structures.
In above-mentioned steps (1), the iron salt is any in nine water ferric nitrates, Iron trichloride hexahydrate, iron sulfate or iron acetate
One or two.
In above-mentioned steps (1), the mass volume ratio of iron salt and organic solvent is 0.03：1-1:1g/L.
In above-mentioned steps (2), the conductive substrates are metallic conductor matrix, and non-metal conductor matrix or both is combined.
Preferably, the metallic conductor matrix is copper, aluminum, nickel or rustless steel.The non-metal conductor matrix is carbon fiber textile product, glass
Glass carbon electrode or conducting polymer.It is furthermore preferred that described conducting polymer is polyaniline.
In above-mentioned steps (2), the spacing between positive and negative plate is 1-50mm, and applied voltage is 10-100V, return time
For 0.5-4h, sedimentation time is 1-60min, and annealing temperature is 200-500 DEG C, and annealing time is 1-5h.Preferably, positive and negative electrode
Spacing between piece is 5-15mm, and applied voltage is 50-70V, and return time is 0.5-4h, and sedimentation time is 5-20min, annealing
Temperature is 200-500 DEG C, and annealing time is 1-5h.It is further preferred that positive and negative electrode pole piece spacing is 5-15mm, applied voltage
For 60V, return time is 1h, and sedimentation time is 10min, and annealing temperature is 300 DEG C, and annealing time is 2h.
The present invention also provides a kind of above-mentioned three-dimensional γ-Fe2O3Application of the nano material in terms of ultracapacitor is prepared.
Compared to the prior art, the beneficial effects of the present invention is：
A kind of γ-Fe of the present invention2O3The preparation method of nano material, as the method using electrophoretic deposition prepares electrode
Material, the method can be one layer of γ-Fe of preparation controllable in conductive substrates in cathode pole piece2O3Nano material, deposition can be
The cathode pole piece of 3D structures is to carry out in conductive substrates, therefore the γ-Fe for preparing2O3Nano material has loose structure.
Further, a kind of γ-Fe of the invention2O3The preparation method of nano material, by adjust iron ion salt concentration with
And the experiment condition in deposition process, final γ-Fe can be controlled2O3Microscopic appearance, deposit thickness have controllability.
Further, a kind of γ-Fe of the invention2O3The preparation method of nano material, with low cost, process is simple, easily
Expanding production, simple operation and other advantages, with extensive prospects for commercial application.
Further, the present invention obtains γ-Fe2O3Nano material chemical property is remarkable, can be used as super capacitor equipment
Material.Raising of its three-dimensional porous structure to chemical property is favourable.Its structure can improve the specific surface of active material γ-Fe2O3
Product, when which is used as electrode material for super capacitor, can be more beneficial for ion and quickly pass on electrode and electrolyte interface
Pass, increase its specific capacity, while with remarkable high rate performance and cycle performance.
Description of the drawings
Fig. 1 is the γ-Fe obtained by embodiment 12O3The scanning electron microscope (SEM) photograph of nano material.
Fig. 2 is the γ-Fe obtained by embodiment 12O3The X-ray powder diffraction figure of nano material.
Fig. 3 is the γ-Fe obtained by embodiment 12O3The cyclic voltammogram of nano material.
Fig. 4 is the γ-Fe obtained by embodiment 22O3The scanning electron microscope (SEM) photograph of nano material.
Fig. 5 is the γ-Fe obtained by embodiment 22O3The cycle performance figure of nano material.
Specific embodiment
Below by specific embodiment and combine accompanying drawing the present invention is expanded on further, it should be noted that being originally embodied as
Example does not constitute the restriction to the claimed scope of the invention.
The scanning electron microscope for being used is the S-3400N scanning electron microscopes of Hitachi's production；
The X-ray diffractometer for being used is the D8Advance x-ray powders of German Bruker AXS company limiteies production
Diffraction；
The electrochemical workstation for being used is the CHI 760D electrochemical workstations of Shanghai occasion China production.
With the γ-Fe of above-mentioned gained2O3Electrode material is working electrode, using platinum electrode as to electrode, with saturation calomel electricity
Extremely reference electrode, constitutes three-electrode system, and 1M Na are added in three electrode glass electrolyzers2SO3Aqueous solution divides as electrolyte
Not by working electrode, platinum electrode is put into electrode and reference electrode in three electrode glass electrolyzers, is picked out corresponding test mouth, is made
760 electrochemical workstations of CHI produced with Shanghai Chen Hua company limiteies are circulated volt-ampere test, are picked out using alligator clip.
Dehydrated alcohol needed for various embodiments of the present invention for analysis it is pure, other reagents be chemistry it is pure, buy in traditional Chinese medicines
Solution on Chemical Reagents in Shanghai company of group.
Embodiment 1
A kind of γ-Fe2O3The preparation method of electrode material, specifically includes following steps：
(1) by iron ion salt:Organic solvent is 1g:The ratio of 1L, iron ion salt is dissolved in organic solvent and obtains 1g/L
Iron ion saline solution；
Described iron ion salt is ferric nitrate；
The organic solvent is 1-Methyl-2-Pyrrolidone；
(2) dispersion liquid prepared by 150mL steps (1) is taken as the electrolyte in electrophoretic deposition pond；It is negative with carbon fiber paper
Pole pole piece, rustless steel carry out electrophoretic deposition for anode pole piece, obtain the cathode pole piece of deposit；
Then the cathode pole piece for having deposit is placed in into 200 DEG C of Muffle furnace annealing 2h, finally in cathode pole piece carbon fiber paper
Surface obtain one layer of γ-Fe2O3Material；
Above-mentioned cathode pole piece carbon fiber paper used is cut to 2.5 × 1.5cm2, immersion electrolyte area is 1.5 ×
1.0cm2；
Rustless steel anode pole piece used is polished with 6# abrasive paper for metallograph, and deionized water is cleaned；
In above-mentioned electrophoretic deposition process, positive and negative plate spacing is 15mm, and DC voltage is 60V, and return time is 30min,
Sedimentation time is 10min.
The scanning electron microscope (SEM) photograph of the material obtained by above-described embodiment 1 is as shown in figure 1,1 can see three dimensional micron hole from figure
The nano-particle of shape structure；
Further, the material obtained by embodiment 1 is carried out into X-ray powder diffraction, as shown in Fig. 2 can analyze from figure
Show that the material obtained by embodiment 1 is γ-Fe2O3Its crystal formation is good.
Further, the material obtained by embodiment 1 is circulated into a volt-ampere performance test, as shown in figure 3, analyzing from Fig. 3
Go out when sweep speed is 5mV/s, its specific capacity is 330F/g；In addition when sweep speed increases to 100mV/s, CV curves
Shape does not significantly change, and illustrates that electrode material has remarkable high rate performance.
Embodiment 2
A kind of γ-Fe2O3The preparation method of electrode material, specifically includes following steps：
(1) by iron ion salt:Organic solvent is 0.05g:The ratio of 1L, iron ion salt is dissolved in organic solvent and is obtained
0.05g/L iron ion saline solution；
Described iron ion salt is iron sulfate；
The organic solvent is 1-Methyl-2-Pyrrolidone；
(2) dispersion liquid prepared by 150mL steps (1) is taken as the electrolyte in electrophoretic deposition pond；With 400 mesh stainless (steel) wires
For cathode pole piece, rustless steel carries out electrophoretic deposition for anode pole piece, obtains the cathode pole piece of deposit；
Then the cathode pole piece for having deposit is placed in into 300 DEG C of Muffle furnace annealing 2h, finally in cathode pole piece carbon fiber paper
Surface obtain one layer of γ-Fe2O3Material；
In above-mentioned electrophoretic deposition process, 400 mesh stainless steel mesh of cathode pole piece used is 316 rustless steel steel, is cut to
2.5×1.5cm2Size, is cleaned by ultrasonic 10min with acetone, ethanol, deionized water successively, and immersion electrolyte area is 1.5 ×
1.0cm2；
Rustless steel anode pole piece used is polished with 6# abrasive paper for metallograph, and deionized water is cleaned；
In above-mentioned electrophoretic deposition process, positive and negative plate spacing is 10mm, and DC voltage is 70V, and return time is 120min,
Sedimentation time is 10min.
The scanning electron microscope (SEM) photograph of the material obtained by examples detailed above 2 is as shown in figure 4, γ-Fe as can see from Figure 42O3Layer size
Even compact is deposited on that stainless steel sift is online, and material is the loose structure of three dimensional micron or nanometer.
Further, by the material obtained by embodiment 2 be circulated charge-discharge performance test, as shown in figure 5, from Fig. 5 be γ-
Fe2O3Material under 1A/g through discharge and recharge 1000 times specific capacity change curve.By calculating, γ-Fe2O3Material electrodes
After circulating 1000 times, capability retention still has 90%, shows the cycle performance of brilliance.
In sum, a kind of γ-Fe of the invention2O3The preparation method of electrode material, can deposit in 3D structures and energy
Enough retain the original 3D structures of conductive substrates, γ-Fe can effectively be controlled by the concentration for regulating and controlling iron ion in solution2O3
The microscopic appearance and particle diameter of grain, scanning electron microscope and X-ray powder diffraction all clearly indicate γ-Fe2O3Presence,
It is that formed in conductive substrates is γ-Fe i.e. in cathode pole piece2O3, for electrochemical property test, show excellent electrochemistry
Performance.
The above is only the citing of embodiments of the present invention, it is noted that for the ordinary skill of the art
For personnel, on the premise of without departing from the technology of the present invention principle, some improvement and modification can also be made, these improve and become
Type also should be regarded as protection scope of the present invention.
Claims (9)
1. a kind of three-dimensional γ-Fe2O3The preparation method of nano material, it is characterised in that comprise the following steps that：
(1) it is 0.01 according to mass volume ratio by iron salt and organic solvent：1-1:1g/L is mixed, and obtains iron salt dispersion；
Wherein：The organic solvent is selected from 1-Methyl-2-Pyrrolidone, tetrahydrofuran, dimethylformamide, butyrolactone, acetone or second
In alcohol any one；
(2) using the iron salt dispersion obtained by step (1) as electrophoretic deposition electrolyte, with the conduction of identical or unlike material
Positive and negative electrode pole piece of the substrate respectively as electrophoretic deposition pond, electrolyte is heated to after backflow, electrophoretic deposition is carried out；Electrophoresis sinks
After product terminates, take cathode pole piece and be placed in annealing in Muffle furnace, i.e., γ-Fe are obtained on the surface of cathode pole piece2O3Nanometer material
Material, wherein：Cathode pole piece has 3D structures；
In step (2), the spacing between positive and negative plate is 1-50mm, and applied voltage is 10-100V, and return time is 0.5-4h,
Sedimentation time is 1-60min, and annealing temperature is 200-500 DEG C, and annealing time is 1-5h.
2. preparation method as claimed in claim 1, it is characterised in that in step (1), the iron salt selected from nine water ferric nitrates,
Any one or two kinds in Iron trichloride hexahydrate, iron sulfate or iron acetate；The mass volume ratio of iron salt and organic solvent is 0.03：1-
1:1g/L。
3. preparation method as claimed in claim 1, it is characterised in that in step (2), the conductive substrates are metallic conductor base
Body, non-metal conductor matrix or both are combined.
4. preparation method as claimed in claim 3, it is characterised in that the metallic conductor matrix is copper, aluminum, nickel or stainless
Steel.
5. preparation method as claimed in claim 3, it is characterised in that the non-metal conductor matrix be carbon fiber textile product,
Glassy carbon electrode or conducting polymer.
6. preparation method as claimed in claim 5, it is characterised in that described carbon fiber textile product are carbon fiber paper；It is described
Conducting polymer be polyaniline.
7. preparation method as claimed in claim 1, it is characterised in that in step (2), the spacing between positive and negative plate are 5-
15mm, applied voltage are 50-70V, and return time is 0.5-4h, and sedimentation time is 5-20min, and annealing temperature is 200-500 DEG C,
Annealing time is 1-5h.
8. preparation method as claimed in claim 1, it is characterised in that in step (2), positive and negative electrode pole piece spacing are 5-15mm,
Applied voltage is 60V, and return time is 1h, and sedimentation time is 10min, and annealing temperature is 300 DEG C, and annealing time is 2h.
9. the three-dimensional γ-Fe that a kind of preparation method according to claim 1 is obtained2O3Nano material is preparing super capacitor
Application in terms of device.
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| CN106558423B (en) * | 2016-11-21 | 2018-10-16 | 华中科技大学 | Fe2O3Laminar nano array, the Fe with layer structure2O3/ PPy flexible composites and preparation and application |
| CN109052369B (en) * | 2018-08-15 | 2020-08-21 | 深圳大学 | Preparation method of nano material |
| CN110787772B (en) * | 2019-11-14 | 2022-02-18 | 山东大学 | Magnetic caramelized carbon nano material and preparation method and application thereof |
| CN110993370B (en) * | 2019-11-22 | 2022-02-18 | 南京理工大学 | Ketjen black/NiCo2O4Preparation method of mixed super capacitor electrode material |
| WO2021187019A1 (en) * | 2020-03-16 | 2021-09-23 | 株式会社クオルテック | Battery and method for manufacturing said battery |
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