CN105948132A - 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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- CN105948132A CN105948132A CN201610297333.4A CN201610297333A CN105948132A CN 105948132 A CN105948132 A CN 105948132A CN 201610297333 A CN201610297333 A CN 201610297333A CN 105948132 A CN105948132 A CN 105948132A
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- 238000002360 preparation method Methods 0.000 title claims abstract description 25
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 22
- 229910006297 γ-Fe2O3 Inorganic materials 0.000 title claims abstract description 22
- 239000000463 material Substances 0.000 claims abstract description 28
- 238000000137 annealing Methods 0.000 claims abstract description 17
- 239000003960 organic solvent Substances 0.000 claims abstract description 13
- 239000000758 substrate Substances 0.000 claims abstract description 9
- 238000000151 deposition Methods 0.000 claims abstract description 5
- 230000008021 deposition Effects 0.000 claims abstract description 4
- 229910001566 austenite Inorganic materials 0.000 claims description 16
- 238000001652 electrophoretic deposition Methods 0.000 claims description 14
- 239000003792 electrolyte Substances 0.000 claims description 10
- 150000002505 iron Chemical class 0.000 claims description 10
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 9
- 229910000831 Steel Inorganic materials 0.000 claims description 9
- 239000010959 steel Substances 0.000 claims description 9
- 229920000049 Carbon (fiber) Polymers 0.000 claims description 8
- 239000004917 carbon fiber Substances 0.000 claims description 8
- 239000004020 conductor Substances 0.000 claims description 8
- 239000011159 matrix material Substances 0.000 claims description 8
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical group C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 claims description 8
- 238000004062 sedimentation Methods 0.000 claims description 8
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 7
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical group CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 6
- 239000006185 dispersion Substances 0.000 claims description 6
- YEJRWHAVMIAJKC-UHFFFAOYSA-N 4-Butyrolactone Chemical compound O=C1CCCO1 YEJRWHAVMIAJKC-UHFFFAOYSA-N 0.000 claims description 5
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 5
- PXHVJJICTQNCMI-UHFFFAOYSA-N Nickel Chemical compound [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 claims description 4
- WYURNTSHIVDZCO-UHFFFAOYSA-N Tetrahydrofuran Chemical compound C1CCOC1 WYURNTSHIVDZCO-UHFFFAOYSA-N 0.000 claims description 4
- 239000002322 conducting polymer Substances 0.000 claims description 4
- 229920001940 conductive polymer Polymers 0.000 claims description 4
- 239000011521 glass Substances 0.000 claims description 4
- 229910052755 nonmetal Inorganic materials 0.000 claims description 4
- 229910000358 iron sulfate Inorganic materials 0.000 claims description 3
- BAUYGSIQEAFULO-UHFFFAOYSA-L iron(2+) sulfate (anhydrous) Chemical compound [Fe+2].[O-]S([O-])(=O)=O BAUYGSIQEAFULO-UHFFFAOYSA-L 0.000 claims description 3
- 239000004753 textile Substances 0.000 claims description 3
- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical group [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 claims description 2
- 229910052782 aluminium Inorganic materials 0.000 claims description 2
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 claims description 2
- 229930188620 butyrolactone Natural products 0.000 claims description 2
- 229910052802 copper Inorganic materials 0.000 claims description 2
- 239000010949 copper Substances 0.000 claims description 2
- 238000001962 electrophoresis Methods 0.000 claims description 2
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 2
- PVFSDGKDKFSOTB-UHFFFAOYSA-K iron(3+);triacetate Chemical compound [Fe+3].CC([O-])=O.CC([O-])=O.CC([O-])=O PVFSDGKDKFSOTB-UHFFFAOYSA-K 0.000 claims description 2
- 229910052759 nickel Inorganic materials 0.000 claims description 2
- 150000002823 nitrates Chemical class 0.000 claims description 2
- 229920000767 polyaniline Polymers 0.000 claims description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims 1
- 229910052799 carbon Inorganic materials 0.000 claims 1
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 abstract description 13
- 229910052742 iron Inorganic materials 0.000 abstract description 10
- 238000000034 method Methods 0.000 abstract description 9
- 239000007772 electrode material Substances 0.000 abstract description 8
- 230000008901 benefit Effects 0.000 abstract description 5
- 239000003990 capacitor Substances 0.000 abstract description 5
- 238000012360 testing method Methods 0.000 abstract description 4
- 239000008151 electrolyte solution Substances 0.000 abstract 1
- 238000010438 heat treatment Methods 0.000 abstract 1
- 238000010992 reflux Methods 0.000 abstract 1
- -1 iron ion salt Chemical class 0.000 description 9
- 238000004146 energy storage Methods 0.000 description 4
- 238000005516 engineering process Methods 0.000 description 4
- BASFCYQUMIYNBI-UHFFFAOYSA-N platinum Chemical compound [Pt] BASFCYQUMIYNBI-UHFFFAOYSA-N 0.000 description 4
- 239000008367 deionised water Substances 0.000 description 3
- 229910021641 deionized water Inorganic materials 0.000 description 3
- 238000000634 powder X-ray diffraction Methods 0.000 description 3
- 230000008569 process Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000033228 biological regulation Effects 0.000 description 2
- 239000003153 chemical reaction reagent Substances 0.000 description 2
- 230000005518 electrochemistry Effects 0.000 description 2
- 230000007613 environmental effect Effects 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical group [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 description 2
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 2
- 239000007788 liquid Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000011056 performance test Methods 0.000 description 2
- 229910052697 platinum Inorganic materials 0.000 description 2
- 238000011160 research Methods 0.000 description 2
- 239000000243 solution Substances 0.000 description 2
- 229910001220 stainless steel Inorganic materials 0.000 description 2
- 239000010935 stainless steel Substances 0.000 description 2
- 238000003860 storage Methods 0.000 description 2
- 241000270722 Crocodylidae Species 0.000 description 1
- 229910019897 RuOx Inorganic materials 0.000 description 1
- FAPWRFPIFSIZLT-UHFFFAOYSA-M Sodium chloride Chemical compound [Na+].[Cl-] FAPWRFPIFSIZLT-UHFFFAOYSA-M 0.000 description 1
- 239000011149 active material Substances 0.000 description 1
- 239000007864 aqueous solution Substances 0.000 description 1
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 230000008859 change Effects 0.000 description 1
- 150000001875 compounds Chemical class 0.000 description 1
- 239000013078 crystal Substances 0.000 description 1
- 238000002484 cyclic voltammetry Methods 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000005137 deposition process Methods 0.000 description 1
- LNNWVNGFPYWNQE-GMIGKAJZSA-N desomorphine Chemical compound C1C2=CC=C(O)C3=C2[C@]24CCN(C)[C@H]1[C@@H]2CCC[C@@H]4O3 LNNWVNGFPYWNQE-GMIGKAJZSA-N 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- ZOMNIUBKTOKEHS-UHFFFAOYSA-L dimercury dichloride Chemical class Cl[Hg][Hg]Cl ZOMNIUBKTOKEHS-UHFFFAOYSA-L 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000446 fuel Substances 0.000 description 1
- 229910021397 glassy carbon Inorganic materials 0.000 description 1
- 239000008187 granular material Substances 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- VRIVJOXICYMTAG-IYEMJOQQSA-L iron(ii) gluconate Chemical compound [Fe+2].OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O.OC[C@@H](O)[C@@H](O)[C@H](O)[C@@H](O)C([O-])=O VRIVJOXICYMTAG-IYEMJOQQSA-L 0.000 description 1
- YOBAEOGBNPPUQV-UHFFFAOYSA-N iron;trihydrate Chemical compound O.O.O.[Fe].[Fe] YOBAEOGBNPPUQV-UHFFFAOYSA-N 0.000 description 1
- 230000014759 maintenance of location Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 229910044991 metal oxide Inorganic materials 0.000 description 1
- 150000004706 metal oxides Chemical class 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000010298 pulverizing process Methods 0.000 description 1
- 239000012266 salt solution Substances 0.000 description 1
- 229940126680 traditional chinese medicines Drugs 0.000 description 1
- 229910000314 transition metal oxide Inorganic materials 0.000 description 1
- 238000004506 ultrasonic cleaning Methods 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G49/00—Compounds of iron
- C01G49/02—Oxides; Hydroxides
- C01G49/06—Ferric oxide [Fe2O3]
-
- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES, LIGHT-SENSITIVE OR TEMPERATURE-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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/01—Particle morphology depicted by an image
- C01P2004/03—Particle morphology depicted by an image obtained by SEM
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/30—Particle morphology extending in three dimensions
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/60—Particles characterised by their size
- C01P2004/61—Micrometer sized, i.e. from 1-100 micrometer
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Power Engineering (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Inorganic Chemistry (AREA)
- Materials Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
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, relate 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, in the development of human civilization and the progress of modern science and technology, plays an important role all the time, and it is the mankind
Eternal pursuit.Energy storage, is an important intermediate steps to the application of multi-functional, high efficient energy sources, at academia and
Industrial circle all has been a great concern.In various energy storage systems, electrochemical storage device is (such as battery and super electricity
Container) due to advantages such as its efficiency height, versatility and plasticity, conduct extensive research, and also be considered as not
Long future, the most promising green sustainable energy stored system.In electrochemical storage device, ultracapacitor is only because of it
Special high power density, have extended cycle life and the advantage such as fast charging and discharging and receive the very big concern of people.And these advantages
Also 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..But, these materials are at nature scarcity of resources, expensive, and environmental protection not, therefore, to ferrum oxygen
The demand of this kind of theoretical specific capacity of compound height, energy density height, aboundresources, environmental friendliness and cheap material is just
The most urgent.But, with regard to Fe2O3During as super capacitor material, there are some drawbacks: first, this material is at base
During body electrode does Large Copacity discharge and recharge, it is easily caused the pulverizing of electrode；Again, the resistivity that metal-oxide is high is easily led
Cause the internal resistance that device is high, have a strong impact on its using value.Therefore, prepare high-performance iron sesquioxide material and seem outstanding
For important.
Summary 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-Fe2O3The preparation of nano material
Method and application thereof.Preparation technology of the present invention is simple, and with low cost, the material obtained has three-dimensional porous structure, electrochemistry
Performance is 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, specifically comprises the following steps that
(1) it is that 0.01:1-1:1g/L mixes by iron salt and organic solvent according to mass volume ratio, obtains iron salt dispersion；
Wherein: described organic solvent selected from 1-Methyl-2-Pyrrolidone (NMP), oxolane (THF), dimethylformamide (DMF),
In butyrolactone (GBL), acetone or alcohol any one；
(2) using the iron salt dispersion of step (1) gained as the electrolyte of electrophoretic deposition, with the identical or conduction of unlike material
Substrate, respectively as the positive and negative electrode pole piece in electrophoretic deposition pond, after electrolyte is heated to backflow, carries out electrophoretic deposition；Electrophoresis
After deposition terminates, take cathode pole piece and be placed in Muffle furnace annealing, the i.e. surface at cathode pole piece and obtain γ-Fe2O3Nanometer
Material, wherein: cathode pole piece has 3D structure.
In above-mentioned steps (1), described iron salt is any in nine water ferric nitrates, Iron trichloride hexahydrate, iron sulfate or iron acetate
One or both.
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), described conductive substrates is metallic conductor matrix, non-metal conductor matrix or both combinations.
Preferably, described metallic conductor matrix is copper, aluminum, nickel or rustless steel.Described non-metal conductor matrix be carbon fiber textile product,
Glassy 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, during backflow
Between be 0.5-4h, sedimentation time is 1-60min, and annealing temperature is 200-500 DEG C, and annealing time is 1-5h.Preferably, just,
Spacing between negative plate 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 is 60V, and 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 for a kind of above-mentioned three-dimensional γ-Fe2O3Nano material application in terms of preparing ultracapacitor.
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, owing to using the method for electrophoretic deposition to prepare electrode material,
The method can be controlled on cathode pole piece i.e. conductive substrates one layer of γ-Fe of preparation2O3Nano material, deposition can be tied at 3D
Carry out in the cathode pole piece of structure i.e. conductive substrates, the γ-Fe therefore prepared2O3Nano material has loose structure.
Further, a kind of γ-Fe of the present invention2O3The preparation method of nano material, by regulation iron ion salt concentration and
Experiment condition in deposition process, can control final γ-Fe2O3Microscopic appearance, deposit thickness has controllability.
Further, a kind of γ-Fe of the present invention2O3The preparation method of nano material, has with low cost, technique simple, easily
Expanding production, simple operation and other advantages, have prospects for commercial application widely.
Further, the present invention obtains γ-Fe2O3Nano material chemical property is remarkable, can be used as super capacitor material.
Its three-dimensional porous structure is favourable to the raising of chemical property.Its structure can improve the specific surface of active material γ-Fe2O3
Long-pending, when it is used as electrode material for super capacitor, it is possible to be more beneficial for ion and quickly pass on electrode and electrolyte interface
Pass, increase its specific capacity, there is high rate performance and the cycle performance of brilliance simultaneously.
Accompanying drawing explanation
Fig. 1 is the γ-Fe of embodiment 1 gained2O3The scanning electron microscope (SEM) photograph of nano material.
Fig. 2 is the γ-Fe of embodiment 1 gained2O3The X-ray powder diffraction figure of nano material.
Fig. 3 is the γ-Fe of embodiment 1 gained2O3The cyclic voltammogram of nano material.
Fig. 4 is the γ-Fe of embodiment 2 gained2O3The scanning electron microscope (SEM) photograph of nano material.
Fig. 5 is the γ-Fe of embodiment 2 gained2O3The cycle performance figure of nano material.
Detailed description of the invention
Below by specific embodiment and combine accompanying drawing the present invention is expanded on further, it should be noted that this specific embodiment is also
Do not constitute the restriction to claimed scope.
The scanning electron microscope used is the S-3400N scanning electron microscope that Hitachi produces；
The X-ray diffractometer used is that the D8Advance x-ray powder that Bruker AXS company limited of Germany produces spreads out
Penetrate；
The electrochemical workstation used is the CHI 760D electrochemical workstation that Shanghai occasion China produces.
γ-Fe with above-mentioned gained2O3Electrode material is working electrode, using platinum electrode as to electrode, with saturated calomel electrode
For reference electrode, form three-electrode system, three electrode glass electrolyzers add 1M Na2SO3Aqueous solution as electrolyte,
Respectively by working electrode, electrode and reference electrode are put in three electrode glass electrolyzers by platinum electrode, pick out corresponding test port,
CHI 760 electrochemical workstation using Shanghai Chen Hua company limited to produce is circulated volt-ampere test, uses crocodile mouth clamping connection
Go out.
In various embodiments of the present invention, required dehydrated alcohol is analytical pure, and other reagent are chemical pure, buy in traditional Chinese medicines group
Solution on Chemical Reagents in Shanghai company.
Embodiment 1
A kind of γ-Fe2O3The preparation method of electrode material, specifically includes following steps:
(1) in iron ion salt: organic solvent is the ratio of 1g:1L, iron ion salt is dissolved in organic solvent and obtains 1g/L ferrum
Ion salt solution；
Described iron ion salt is ferric nitrate；
Described organic solvent is 1-Methyl-2-Pyrrolidone；
(2) electrolyte as electrophoretic deposition pond of the dispersion liquid prepared by 150mL step (1) is taken；It is negative with carbon fiber paper
Pole pole piece, rustless steel is that anode pole piece carries out electrophoretic deposition, obtains the cathode pole piece having deposit；
Then the cathode pole piece having deposit is placed in 200 DEG C of Muffle furnace annealing 2h, finally at the table of cathode pole piece carbon fiber paper
Face obtains one layer of γ-Fe2O3Material；
Above-mentioned cathode pole piece carbon fiber paper used is cut to 2.5 × 1.5cm2, immersing electrolyte area is 1.5 × 1.0cm2；
Rustless steel anode pole piece 6# abrasive paper for metallograph used is polished, and is washed with deionized water clean；
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 of above-described embodiment 1 gained is as it is shown in figure 1,1 it can be seen that three dimensional micron is poroid from figure
The nano-particle of structure；
Further, the material of embodiment 1 gained is carried out X-ray powder diffraction, as in figure 2 it is shown, can analyze from figure
The material drawing embodiment 1 gained is γ-Fe2O3Its crystal formation is good.
Further, the material of embodiment 1 gained is circulated a volt-ampere performance test, as it is shown on figure 3, analyze from Fig. 3
Going out when sweep speed is 5mV/s, its specific capacity is 330F/g；In addition when sweep speed increases to 100mV/s, CV
The shape of curve the most significantly changes, and illustrates that electrode material has the high rate performance of brilliance.
Embodiment 2
A kind of γ-Fe2O3The preparation method of electrode material, specifically includes following steps:
(1) in iron ion salt: organic solvent is the ratio of 0.05g:1L, iron ion salt is dissolved in organic solvent and obtains 0.05g/L
Iron ion saline solution；
Described iron ion salt is iron sulfate；
Described organic solvent is 1-Methyl-2-Pyrrolidone；
(2) electrolyte as electrophoretic deposition pond of the dispersion liquid prepared by 150mL step (1) is taken；With 400 mesh rustless steels
Net is cathode pole piece, and rustless steel is that anode pole piece carries out electrophoretic deposition, obtains the cathode pole piece having deposit；
Then the cathode pole piece having deposit is placed in 300 DEG C of Muffle furnace annealing 2h, finally at the table of cathode pole piece carbon fiber paper
Face obtains one layer of γ-Fe2O3Material；
Cathode pole piece 400 mesh stainless steel mesh used in above-mentioned electrophoretic deposition process is 316 rustless steel steel, is cut to
2.5×1.5cm2Size, successively with acetone, ethanol, deionized water ultrasonic cleaning 10min, immersing electrolyte area is
1.5×1.0cm2；
Rustless steel anode pole piece 6# abrasive paper for metallograph used is polished, and is washed with deionized water clean；
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 of examples detailed above 2 gained as shown in Figure 4, γ-Fe as can see from Figure 42O3Layer size
Even compact to be deposited on stainless steel sift online, material is the loose structure of three dimensional micron or nanometer.
Further, the material of embodiment 2 gained is circulated charge-discharge performance test, as it is shown in figure 5, from Fig. 5 be
γ-Fe2O3Material under 1A/g through the specific capacity change curve of discharge and recharge 1000 times.By calculating, γ-Fe2O3Material
Material electrode capability retention after circulating 1000 times still has 90%, shows the cycle performance of brilliance.
In sum, a kind of γ-Fe of the present invention2O3The preparation method of electrode material, can deposit and can in 3D structure
Retain conductive substrates original 3D structure, can effectively control γ-Fe by the concentration of iron ion in regulation and control solution2O3Granule
Microscopic appearance and particle diameter, scanning electron microscope and X-ray powder diffraction indicate γ-Fe the most clearly2O3Existence,
That i.e. formed on cathode pole piece i.e. conductive substrates is γ-Fe2O3, for electrochemical property test, show the electrochemistry of excellence
Performance.
The above is only the citing of embodiments of the present invention, it is noted that for those skilled in the art
For, on the premise of without departing from the technology of the present invention principle, it is also possible to make some improvement and modification, these improve and modification
Also should be regarded as protection scope of the present invention.
Claims (10)
1. a three-dimensional γ-Fe2O3The preparation method of nano material, it is characterised in that specifically comprise the following steps that
(1) it is that 0.01:1-1:1g/L mixes by iron salt and organic solvent according to mass volume ratio, obtains iron salt dispersion；Its
In: described organic solvent is selected from 1-Methyl-2-Pyrrolidone, oxolane, dimethylformamide, butyrolactone, acetone or second
In alcohol any one；
(2) using the iron salt dispersion of step (1) gained as the electrolyte of electrophoretic deposition, with the identical or conduction of unlike material
Substrate, respectively as the positive and negative electrode pole piece in electrophoretic deposition pond, after electrolyte is heated to backflow, carries out electrophoretic deposition；Electrophoresis
After deposition terminates, take cathode pole piece and be placed in Muffle furnace annealing, the i.e. surface at cathode pole piece and obtain γ-Fe2O3Nanometer
Material, wherein: cathode pole piece has 3D structure.
2. preparation method as claimed in claim 1, it is characterised in that in step (1), described 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), described conductive substrates is metallic conductor
Matrix, non-metal conductor matrix or both combinations.
4. preparation method as claimed in claim 3, it is characterised in that described metallic conductor matrix is copper, aluminum, nickel or rustless steel.
5. preparation method as claimed in claim 3, it is characterised in that described non-metal conductor matrix is carbon fiber textile product, glass
Glass 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；Described
Conducting polymer is polyaniline.
7. preparation method as claimed in claim 1, it is characterised in that in step (2), the spacing between positive and negative plate is
1-50mm, applied voltage is 10-100V, and return time is 0.5-4h, and sedimentation time is 1-60min, and annealing temperature is
200-500 DEG C, annealing time is 1-5h.
8. the preparation method as described in claim 1 or 7, it is characterised in that in step (2), between positive and negative plate between
Away from for 5-15mm, applied voltage is 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.
9. the preparation method as described in claim 1 or 7, it is characterised in that in step (2), positive and negative electrode pole piece spacing is
5-15mm, applied voltage is 60V, and return time is 1h, and sedimentation time is 10min, and annealing temperature is 300 DEG C, annealing
Time is 2h.
10. the three-dimensional γ-Fe that a preparation method according to claim 1 obtains2O3Nano material is preparing ultracapacitor side
The application in face.
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| CN110993370A (en) * | 2019-11-22 | 2020-04-10 | 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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