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 PDF

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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
preparation
acid iron
glyceric acid
presoma
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CN108711517A (en
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朱脉勇
陈齐
申小娟
吴述平
张侃
李松军
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Jiangsu University
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    • H—ELECTRICITY
    • H01—ELECTRIC ELEMENTS
    • H01G—CAPACITORS; CAPACITORS, RECTIFIERS, DETECTORS, SWITCHING DEVICES OR LIGHT-SENSITIVE DEVICES, OF THE ELECTROLYTIC TYPE
    • H01G11/00—Hybrid capacitors, i.e. capacitors having different positive and negative electrodes; Electric double-layer [EDL] capacitors; Processes for the manufacture thereof or of parts thereof
    • H01G11/22—Electrodes
    • H01G11/24—Electrodes characterised by structural features of the materials making up or comprised in the electrodes, e.g. form, surface area or porosity; characterised by the structural features of powders or particles used therefor
    • 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
    • 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
    • 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

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  • 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

A kind of γ-Fe2O3Nano material and its preparation method and application
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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