CN108711517B - A kind of γ-Fe2O3Nano material and its preparation method and application - Google Patents
A kind of γ-Fe2O3Nano material and its preparation method and application Download PDFInfo
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- CN108711517B CN108711517B CN201810305037.3A CN201810305037A CN108711517B CN 108711517 B CN108711517 B CN 108711517B CN 201810305037 A CN201810305037 A CN 201810305037A CN 108711517 B CN108711517 B CN 108711517B
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- nano material
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- acid iron
- glyceric acid
- presoma
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- 238000002360 preparation method Methods 0.000 title claims abstract description 20
- 239000000463 material Substances 0.000 title description 11
- 239000002086 nanomaterial Substances 0.000 claims abstract description 45
- ZECOUWLZAQNBST-UHFFFAOYSA-N 2,3-dihydroxypropanoic acid;iron Chemical compound [Fe].OCC(O)C(O)=O ZECOUWLZAQNBST-UHFFFAOYSA-N 0.000 claims abstract description 37
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims abstract description 30
- XEEYBQQBJWHFJM-UHFFFAOYSA-N Iron Chemical compound [Fe] XEEYBQQBJWHFJM-UHFFFAOYSA-N 0.000 claims abstract description 26
- 229910006297 γ-Fe2O3 Inorganic materials 0.000 claims abstract description 23
- 229910001566 austenite Inorganic materials 0.000 claims abstract description 21
- 229910052742 iron Inorganic materials 0.000 claims abstract description 13
- 235000011187 glycerol Nutrition 0.000 claims abstract description 11
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 9
- 239000004202 carbamide Substances 0.000 claims abstract description 9
- 229940044631 ferric chloride hexahydrate Drugs 0.000 claims abstract description 6
- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 15
- 239000000843 powder Substances 0.000 claims description 13
- 238000010438 heat treatment Methods 0.000 claims description 11
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 10
- 241000186216 Corynebacterium Species 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000006243 chemical reaction Methods 0.000 claims description 6
- 239000002253 acid Substances 0.000 claims description 5
- 238000002156 mixing Methods 0.000 claims description 5
- 235000019441 ethanol Nutrition 0.000 claims description 4
- 230000035484 reaction time Effects 0.000 claims description 2
- 239000002904 solvent Substances 0.000 claims description 2
- FBAFATDZDUQKNH-UHFFFAOYSA-M iron chloride Chemical compound [Cl-].[Fe] FBAFATDZDUQKNH-UHFFFAOYSA-M 0.000 claims 2
- 238000000034 method Methods 0.000 abstract description 6
- 238000001291 vacuum drying Methods 0.000 abstract description 5
- 238000005406 washing Methods 0.000 abstract description 4
- RBNPOMFGQQGHHO-UHFFFAOYSA-N -2,3-Dihydroxypropanoic acid Natural products OCC(O)C(O)=O RBNPOMFGQQGHHO-UHFFFAOYSA-N 0.000 abstract description 2
- RBNPOMFGQQGHHO-UWTATZPHSA-N D-glyceric acid Chemical compound OC[C@@H](O)C(O)=O RBNPOMFGQQGHHO-UWTATZPHSA-N 0.000 abstract description 2
- 238000005119 centrifugation Methods 0.000 abstract 1
- 238000001027 hydrothermal synthesis Methods 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 abstract 1
- PXHVJJICTQNCMI-UHFFFAOYSA-N nickel Substances [Ni] PXHVJJICTQNCMI-UHFFFAOYSA-N 0.000 description 19
- 229910052759 nickel Inorganic materials 0.000 description 10
- 239000007772 electrode material Substances 0.000 description 9
- 239000006260 foam Substances 0.000 description 9
- 239000003990 capacitor Substances 0.000 description 6
- 229910044991 metal oxide Inorganic materials 0.000 description 5
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 230000005389 magnetism Effects 0.000 description 4
- 150000004706 metal oxides Chemical class 0.000 description 4
- -1 oxygen (sulphur) compound Chemical class 0.000 description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 3
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical compound CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 description 3
- 229910052799 carbon Inorganic materials 0.000 description 3
- JEIPFZHSYJVQDO-UHFFFAOYSA-N iron(III) oxide Inorganic materials O=[Fe]O[Fe]=O JEIPFZHSYJVQDO-UHFFFAOYSA-N 0.000 description 3
- 229910052751 metal Inorganic materials 0.000 description 3
- 239000011259 mixed solution Substances 0.000 description 3
- 230000010355 oscillation Effects 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 238000001228 spectrum Methods 0.000 description 3
- 238000003786 synthesis reaction Methods 0.000 description 3
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 description 2
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 description 2
- UQSXHKLRYXJYBZ-UHFFFAOYSA-N Iron oxide Chemical compound [Fe]=O UQSXHKLRYXJYBZ-UHFFFAOYSA-N 0.000 description 2
- YTPLMLYBLZKORZ-UHFFFAOYSA-N Thiophene Chemical compound C=1C=CSC=1 YTPLMLYBLZKORZ-UHFFFAOYSA-N 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 239000002322 conducting polymer Substances 0.000 description 2
- 229920001940 conductive polymer Polymers 0.000 description 2
- 238000010586 diagram Methods 0.000 description 2
- 239000011267 electrode slurry Substances 0.000 description 2
- 239000003792 electrolyte Substances 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- SZVJSHCCFOBDDC-UHFFFAOYSA-N ferrosoferric oxide Chemical compound O=[Fe]O[Fe]O[Fe]=O SZVJSHCCFOBDDC-UHFFFAOYSA-N 0.000 description 2
- DKAGJZJALZXOOV-UHFFFAOYSA-N hydrate;hydrochloride Chemical class O.Cl DKAGJZJALZXOOV-UHFFFAOYSA-N 0.000 description 2
- 150000002500 ions Chemical class 0.000 description 2
- 229910052748 manganese Inorganic materials 0.000 description 2
- 239000011572 manganese Substances 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- UPWOEMHINGJHOB-UHFFFAOYSA-N oxo(oxocobaltiooxy)cobalt Chemical compound O=[Co]O[Co]=O UPWOEMHINGJHOB-UHFFFAOYSA-N 0.000 description 2
- 229920000767 polyaniline Polymers 0.000 description 2
- 229920000128 polypyrrole Polymers 0.000 description 2
- 239000002994 raw material Substances 0.000 description 2
- WOCIAKWEIIZHES-UHFFFAOYSA-N ruthenium(iv) oxide Chemical compound O=[Ru]=O WOCIAKWEIIZHES-UHFFFAOYSA-N 0.000 description 2
- 229920000049 Carbon (fiber) Polymers 0.000 description 1
- 239000004966 Carbon aerogel Substances 0.000 description 1
- CWYNVVGOOAEACU-UHFFFAOYSA-N Fe2+ Chemical compound [Fe+2] CWYNVVGOOAEACU-UHFFFAOYSA-N 0.000 description 1
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 description 1
- KJTLSVCANCCWHF-UHFFFAOYSA-N Ruthenium Chemical compound [Ru] KJTLSVCANCCWHF-UHFFFAOYSA-N 0.000 description 1
- 229910000835 Sweet iron Inorganic materials 0.000 description 1
- 239000006230 acetylene black Substances 0.000 description 1
- 125000000217 alkyl group Chemical group 0.000 description 1
- 239000004411 aluminium Substances 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 239000003575 carbonaceous material Substances 0.000 description 1
- 239000010941 cobalt Substances 0.000 description 1
- 229910017052 cobalt Inorganic materials 0.000 description 1
- GUTLYIVDDKVIGB-UHFFFAOYSA-N cobalt atom Chemical compound [Co] GUTLYIVDDKVIGB-UHFFFAOYSA-N 0.000 description 1
- UBEWDCMIDFGDOO-UHFFFAOYSA-N cobalt(II,III) oxide Inorganic materials [O-2].[O-2].[O-2].[O-2].[Co+2].[Co+3].[Co+3] UBEWDCMIDFGDOO-UHFFFAOYSA-N 0.000 description 1
- 239000006258 conductive agent Substances 0.000 description 1
- 238000010277 constant-current charging Methods 0.000 description 1
- 125000004122 cyclic group Chemical group 0.000 description 1
- 230000001351 cycling effect Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 239000002270 dispersing agent Substances 0.000 description 1
- 230000005611 electricity Effects 0.000 description 1
- 238000000840 electrochemical analysis Methods 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 229960004756 ethanol Drugs 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- HOIQWTMREPWSJY-GNOQXXQHSA-K iron(3+);(z)-octadec-9-enoate Chemical compound [Fe+3].CCCCCCCC\C=C/CCCCCCCC([O-])=O.CCCCCCCC\C=C/CCCCCCCC([O-])=O.CCCCCCCC\C=C/CCCCCCCC([O-])=O HOIQWTMREPWSJY-GNOQXXQHSA-K 0.000 description 1
- QSKMODRNBDHZFN-UHFFFAOYSA-N iron;propane-1,2,3-triol Chemical compound [Fe].OCC(O)CO QSKMODRNBDHZFN-UHFFFAOYSA-N 0.000 description 1
- AMWRITDGCCNYAT-UHFFFAOYSA-L manganese oxide Inorganic materials [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 description 1
- GEYXPJBPASPPLI-UHFFFAOYSA-N manganese(III) oxide Inorganic materials O=[Mn]O[Mn]=O GEYXPJBPASPPLI-UHFFFAOYSA-N 0.000 description 1
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 1
- 125000002524 organometallic group Chemical group 0.000 description 1
- 238000013021 overheating Methods 0.000 description 1
- 239000011148 porous material Substances 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 238000006479 redox reaction Methods 0.000 description 1
- 229910052707 ruthenium Inorganic materials 0.000 description 1
- 229910001925 ruthenium oxide Inorganic materials 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 229930192474 thiophene Natural products 0.000 description 1
- 238000012876 topography Methods 0.000 description 1
- 230000001988 toxicity Effects 0.000 description 1
- 231100000419 toxicity Toxicity 0.000 description 1
- 238000002604 ultrasonography Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
Classifications
-
- 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
- H01G11/24—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
-
- 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
-
- 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
- H01G11/84—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
-
- 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
- Engineering & Computer Science (AREA)
- Power Engineering (AREA)
- Microelectronics & Electronic Packaging (AREA)
- Chemical & Material Sciences (AREA)
- Materials Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Battery Electrode And Active Subsutance (AREA)
- Electric Double-Layer Capacitors Or The Like (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention belongs to supercapacitor fields, and in particular to a kind of γ-Fe2O3Nano material and its preparation method and application.The present invention prepares γ-Fe2O3The method of nano material is specific as follows: ferric chloride hexahydrate and urea being added in glycerin solution mix first, hydro-thermal reaction obtains the presoma of glyceric acid iron；Then by the washing of glyceric acid iron presoma, centrifugation, vacuum drying, glyceric acid iron is obtained；Glyceric acid iron is heat-treated in the air atmosphere of tube furnace finally, obtains γ-Fe2O3Nano material.γ-Fe prepared by the present invention2O3Nano material partial size is small, large specific surface area, when being applied in supercapacitor, has biggish specific discharge capacity and good cyclical stability.Preparation method of the invention is at low cost, simple and easy, process is shorter, easy controlled operation, is expected to be used in production.
Description
Technical field
The invention belongs to supercapacitor fields, and in particular to a kind of γ-Fe2O3It nano material and preparation method thereof and answers
With.
Background technique
Supercapacitor is that one kind compensates for traditional capacitor low energy densities and traditional storage battery low power density disadvantage
Electrochemical capacitor can be applied to science and techniques of defence, aerospace as a kind of energy storage device of new green environment protection
And electric car etc., and caused the extensive concern of scientific research personnel.According to charge storage mode, super capacitor
Device can be divided into two classes: double layer capacitor and pseudocapacitors.Electric double layer capacitance mainly relies in electrostatic attraction electrolyte
Negative ions make negative ions respectively to two electrode movements, to form electric double layer；After voltage take-off, it is adsorbed on electrode
The electronics of material ends is restored to mixed and disorderly random state again, and energy is released.This kind of capacitor electrode material is mainly carbon
Material, comprising: carbon nanotube, carbon fiber, carbon aerogels, graphene etc..But electrode material for electric double layer capacitor is in storage charge
When only lean on electrostatic attraction, be not directed to chemical reaction, therefore specific discharge capacity is smaller；And pseudocapacitors are mainly positioned against electrode material
Expect that quick faraday's redox reaction occurs for surface or near surface, so that charge is stored and is discharged, therefore have higher
Specific discharge capacity, electrode material is mainly metal oxygen (sulphur) compound and conducting polymer.
In above two electrode material, conducting polymer specifically includes that polypyrrole (PPy), polyaniline (PANI), poly- thiophene
Pheno etc.；And metal oxide specifically includes that iron type oxide (Fe2O3、Fe3O4, FeO etc.), manganese type oxide (Mn2O3、Mn3O4、
MnO etc.), cobalt type oxide (Co2O3、Co3O4, CoO etc.) and rare metal oxide ruthenium-oxide (RuO2) etc..And rare metal
Oxides ruthenium (RuO2) there is toxicity and at high price, unsuitable large-scale use；And ferrous metal oxide relative to
For other metal oxides (Mn, Co, Ni, Ti), price is cheaper, source is more abundant, to be only second to aluminium in the earth's crust
The high metallic element of content second, thus the oxide of iron have it is at low cost, it is resourceful, it is environmental-friendly the features such as, it is extensive
Substitution electrode material as pseudocapacitors.
Summary of the invention
It is an object of the invention to overcome defect existing in the prior art, such as: synthesis technology is complicated, and raw material are expensive,
Obtained sample topography is inhomogenous etc., and the present invention provides a kind of γ-Fe that rodlike glyceric acid iron is converted to2O3Nano material
Preparation method.
Specifically, the present invention adopts the following technical scheme that:
(1) presoma of synthetic glycerine acid iron:
Two kinds of solvents of glycerine and water are uniformly mixed, ferric chloride hexahydrate and urea is sequentially added, turns after mixing evenly
It moves in high-temperature high-pressure reaction kettle, reacts under hydrothermal conditions, obtain the presoma of glyceric acid iron；
(2) glyceric acid iron is prepared:
Glyceric acid iron presoma is washed with deionized water and ethyl alcohol, is centrifuged, is dried in vacuo, obtain green powder,
As glyceric acid iron；
(3) γ-Fe is prepared2O3Nano material:
Glyceric acid iron in step (2) is heat-treated in the air atmosphere of tube furnace, obtains γ-Fe2O3Nanometer material
Material.
In step 1, the volume ratio of glycerine and water is 11 ~ 12:0 ~ 1.
In step 1, the molar ratio of ferric chloride hexahydrate and urea is 1 ~ 5:1 ~ 5.
In step 1, the hydrothermal temperature is 200 DEG C ~ 250 DEG C, and the reaction time is 10h ~ 20h.
In step 3, the temperature of heat treatment is 400 DEG C ~ 500 DEG C, and heat treatment time is 2h ~ 6h, and heating rate is 1 DEG C/min
~10℃/min。
The present invention also provides a kind of γ-Fe2O3Nano material, synthesized γ-Fe2O3Nano material is in porous stub
Shape structure, length is between 150nm ~ 400nm, and width is in 50nm or so.
The present invention also provides a kind of γ-Fe2O3The purposes of nano material, prepared γ-Fe2O3Nano material is used for
In supercapacitor.
Compared with prior art, beneficial effects of the present invention embody as follows:
(1) forerunner's element of volume used in the present invention is ferro element, and abundance is cheap.Prepared presoma is short
Rodlike glyceric acid iron is the organometallic complex of a kind of glycerol and iron ion formation, and synthesis technology is simple, and pattern is equal
One.
(2) the porous rodlike γ-Fe prepared by the present invention2O3Nano material is with high purity, partial size is small, specific surface area
The features such as big, can come into full contact with the electronics in electrolyte, therefore have high specific discharge capacity, and good cycling stability etc. is excellent
Point.Nanoscale porous material has a large amount of hole and high specific surface area, and this feature makes it have more excellent ratio
Capacity.
(3) of the invention preparation method is simple, process is shorter, easy controlled operation, at low cost, is suitable for promoting the use of.This
Invention is organic with the glyceric acid ferrous metal that ferric chloride hexahydrate offer source of iron prepares nanoscale corynebacterium first to reduce cost
Complex, and as presoma, the γ-of corynebacterium porous structure has been obtained by further heat treatment in air atmosphere
Fe2O3Nano material.The material of such corynebacterium porous structure shows higher specific capacity and circulation in electro-chemical test
Stability, in the case where current density is 1A/g, specific capacity is a kind of fake capacitance electricity with applications well prospect up to 240 F/g
Pole material.
Detailed description of the invention
Fig. 1 (a) is that the X-ray diffraction (XRD) figure of glyceric acid iron prepared by the present invention is composed；Fig. 1 (b) is prepared by the present invention
γ–Fe2O3The XRD spectrum of nano material；Fig. 1 (c) is γ-Fe prepared by the present invention2O3The pictorial diagram of nano material；
Fig. 2 is the scanning electron microscope (SEM) photograph (a) and transmission electron microscope picture (b) of glyceric acid iron prepared by the present invention；
Fig. 3 is γ-Fe prepared by the present invention2O3Nano material transmission electron microscope picture；
Fig. 4 is γ-Fe prepared by the present invention2O3Nano material CV curve (a), GCD curve (b) and cyclic curve figure (c).
Specific embodiment
The invention will be further described below in conjunction with the accompanying drawings:
Embodiment 1:
Prepare γ-Fe2O3Nano material:
(1) presoma of synthetic glycerine acid iron:
The glycerine of 55mL and the deionized water of 5mL are weighed, is uniformly mixed；Sequentially add six chloride hydrates of 6 mmol
Obtained mixed solution is transferred in high-temperature high-pressure reaction kettle by iron, the urea of 6mmol after mixing evenly, at 200 DEG C, instead
10 h are answered, the presoma of glyceric acid iron is obtained.
(2) glyceric acid iron is prepared:
By the presoma cooled to room temperature of the above-mentioned glyceric acid iron being prepared, washed 3 times through deionized water, it is anhydrous
Ethanol washing 1 time, centrifuge separation, vacuum drying, obtain green powder, as glyceric acid iron；
(3) γ-Fe is prepared2O3Nano material:
0.2g glyceric acid iron is heat-treated under the air atmosphere of tube furnace, the temperature of heat treatment is 450 DEG C, at heat
The reason time is 3h, and heating rate is 1 DEG C/min, obtains red magnetism powder, as γ-Fe2O3Nano material.
Embodiment 2:
Prepare γ-Fe2O3Nano material:
(1) presoma of synthetic glycerine acid iron:
The glycerine of 60mL and the deionized water of 5mL are weighed, is uniformly mixed；Sequentially add six chloride hydrates of 1 mmol
Obtained mixed solution is transferred in high-temperature high-pressure reaction kettle by iron, the urea of 5mmol after mixing evenly, at 250 DEG C, instead
15 h are answered, the presoma of glyceric acid iron is obtained.
(2) glyceric acid iron is prepared:
By the presoma cooled to room temperature of the above-mentioned glyceric acid iron being prepared, washed 3 times through deionized water, it is anhydrous
Ethanol washing 1 time, centrifuge separation, vacuum drying, obtain green powder, as glyceric acid iron；
(3) γ-Fe is prepared2O3Nano material:
2.5g glyceric acid iron is heat-treated under the air atmosphere of tube furnace, the temperature of heat treatment is 400 DEG C, at heat
The reason time is 6h, and heating rate is 5 DEG C/min, obtains red magnetism powder, as γ-Fe2O3Nano material.
Embodiment 3:
Prepare γ-Fe2O3Nano material:
(1) presoma of synthetic glycerine acid iron:
The glycerine for weighing 55mL, sequentially adds the ferric chloride hexahydrate of 5 mmol, the urea of 1mmol, after mixing evenly,
Obtained mixed solution is transferred in high-temperature high-pressure reaction kettle, at 225 DEG C, 20h is reacted, obtains the forerunner of glyceric acid iron
Body.
(2) glyceric acid iron is prepared:
By the presoma cooled to room temperature of the above-mentioned glyceric acid iron being prepared, washed 3 times through deionized water, it is anhydrous
Ethanol washing 1 time, centrifuge separation, vacuum drying, obtain green powder, as glyceric acid iron；
(3) γ-Fe is prepared2O3Nano material:
5.0g glyceric acid iron is heat-treated under the air atmosphere of tube furnace, the temperature of heat treatment is 500 DEG C, at heat
The reason time is 2h, and heating rate is 10 DEG C/min, obtains red magnetism powder, as γ-Fe2O3Nano material.
As can be seen that (a) is the XRD spectrum of synthesized green powder in Fig. 1, the X-ray diffractogram for synthesizing presoma is aobvious
Showing, for only one apparent diffraction peak in 11 ° or so, this diffraction maximum position is attributable to the iron glycerol phase in glycerol, this
It is one kind typically using glycerol as the iron-based alkyl oxide of raw material, that is, proves that this green powder is glyceric acid iron；It (b) is sweet
Iron oleate is after Overheating Treatment, the XRD spectrum of the red magnetism powder of synthesis, these sample powders have good diffraction
Peak corresponds respectively to γ-Fe2O3(220), (311), (222), (400), (422), (511), (440) face, it was demonstrated that it is such
Material is γ-Fe2O3；It (c) is prepared by the present invention–Fe2O3The pictorial diagram of nano material, as seen from the figure, this nano material is
Red powder.
As can be seen that the pattern of glyceric acid iron is high-visible in Fig. 2, the glyceric acid iron of preparation is corynebacterium structure, size
Uniform, length is between 150nm ~ 400nm, and width is in 50nm or so.
As can be seen that synthesized γ-Fe in Fig. 32O3Nano material maintains the corynebacterium pattern of glyceric acid iron, length
Between 150nm ~ 400nm, width is in porous corynebacterium structure in 50nm or so, the appearance of porous structure mainly due to
Caused by glycerol small molecule under high temperature in glyceric acid iron is decomposed.
γ-the Fe of porous corynebacterium made from the method as described in embodiment 1-32O3Nano material is tested as follows:
Electrochemical property test:
(1) preparation of electrode slurry:
It disperses electrode material, conductive agent (acetylene black) and binder (Kynoar) according to the ratio of 75:15:10
In dispersing agent 1-Methyl-2-Pyrrolidone (NMP), it is uniformly mixed to get electrode slurry is arrived.
(2) preparation of foam nickel electrode piece:
Nickel foam is cut into the rectangular-shaped pieces of 5cm × 1cm, and is marked at 4cm, the precoating of 1cm × 1cm is obtained
Plasma-based material surface.Nickel foam is washed later, is first impregnated nickel foam in acetone, sonic oscillation 15min, then will
Nickel foam immerses in the hydrochloric acid solution of 1mol/L, sonic oscillation 15min；Nickel foam is immersed in deionized water again later, ultrasound
Vibrate 15min；Finally nickel foam is immersed in dehydrated alcohol again, sonic oscillation 15min.Nickel foam is transferred to vacuum drying again
In case, dry 12h, obtains electrode slice at 60 DEG C.
(3) preparation of electrode material:
Plasma-based material is evenly applied to foam nickel electrode on piece, is transferred in vacuum oven, dry 12h at 60 DEG C,
Obtain electrode material.
As can be seen that (a) is γ-Fe in Fig. 42O3The CV curve graph of nano material, there is apparent redox peaks, table
Bright its belongs to fake capacitance material；It (b) is γ-Fe2O3The constant current charging and discharging curve figure (GCD) of nano material, in current density
For under 1A/g, specific capacity is up to 240 F/g；It (c) is γ-Fe2O3The cycle performance figure of nano material, after circulation 2000 times, still
There is 64.5% specific capacity conservation rate.
Claims (9)
1. a kind of γ-Fe2O3The preparation method of nano material, which comprises the following steps:
(1) presoma of synthetic glycerine acid iron:
Two kinds of solvents of glycerine and water are uniformly mixed, ferric chloride hexahydrate, urea is sequentially added, after mixing evenly, will obtain
Mixed liquor be transferred in reaction kettle, react under hydrothermal conditions, obtain the presoma of glyceric acid iron；
(2) glyceric acid iron is prepared:
Glyceric acid iron presoma deionized water in step (1), ethyl alcohol are washed, is centrifuged, is dried in vacuo, obtain green
Powder, as glyceric acid iron；
(3) γ-Fe is prepared2O3Nano material:
Glyceric acid iron in step (2) is heat-treated in the air atmosphere of tube furnace, obtains γ-Fe2O3Nano material.
2. γ-Fe according to claim 12O3The preparation method of nano material, which is characterized in that in step (1), the third three
The volume ratio of alcohol and water is 11~12:0~1.
3. γ-Fe according to claim 12O3The preparation method of nano material, which is characterized in that in step (1), six water
The molar ratio for closing iron chloride and urea is 1~5:1~5.
4. γ-Fe according to claim 12O3The preparation method of nano material, which is characterized in that described in step (1)
Hydrothermal temperature is 200 DEG C~250 DEG C, and the reaction time is 10h~20h.
5. γ-Fe according to claim 12O3The preparation method of nano material, which is characterized in that in step (3), at heat
The temperature of reason is 400 DEG C~500 DEG C, and heating rate is 1 DEG C/min~10 DEG C/min.
6. γ-Fe according to claim 12O3The preparation method of nano material, which is characterized in that in step (3), at heat
The reason time is 2h~6h.
7. γ-Fe according to claim 22O3The preparation method of nano material, which is characterized in that in step (1), the third three
The volume ratio of alcohol and water is 11:1.
8. γ-Fe according to claim 32O3The preparation method of nano material, which is characterized in that in step (1), six water
The molar ratio for closing iron chloride and urea is 1:1.
9. γ-Fe prepared by the preparation method as described in claim 1-8 any one2O3Nano material, which is characterized in that institute
State γ-Fe2O3Nano material is in porous corynebacterium structure, is applied in supercapacitor.
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