CN107522237A - A kind of porous di-iron trioxide material of α phases shuttle shape and its preparation method and application - Google Patents
A kind of porous di-iron trioxide material of α phases shuttle shape and its preparation method and application Download PDFInfo
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- CN107522237A CN107522237A CN201710796372.3A CN201710796372A CN107522237A CN 107522237 A CN107522237 A CN 107522237A CN 201710796372 A CN201710796372 A CN 201710796372A CN 107522237 A CN107522237 A CN 107522237A
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- iron trioxide
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- molysite
- shuttle shape
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- 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)
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M10/00—Secondary cells; Manufacture thereof
- H01M10/05—Accumulators with non-aqueous electrolyte
- H01M10/052—Li-accumulators
- H01M10/0525—Rocking-chair batteries, i.e. batteries with lithium insertion or intercalation in both electrodes; Lithium-ion batteries
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- H—ELECTRICITY
- H01—ELECTRIC ELEMENTS
- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M4/00—Electrodes
- H01M4/02—Electrodes composed of, or comprising, active material
- H01M4/36—Selection of substances as active materials, active masses, active liquids
- H01M4/48—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides
- H01M4/52—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron
- H01M4/525—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron of mixed oxides or hydroxides containing iron, cobalt or nickel for inserting or intercalating light metals, e.g. LiNiO2, LiCoO2 or LiCoOxFy
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- 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
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- 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
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02E—REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION
- Y02E60/00—Enabling technologies; Technologies with a potential or indirect contribution to GHG emissions mitigation
- Y02E60/10—Energy storage using batteries
Abstract
The present invention relates to porous di-iron trioxide material of a kind of α phases shuttle shape and its preparation method and application, the porous di-iron trioxide material of α phases shuttle shape is prepared by molysite, fumaric acid and dimethylformamide, shape is wherein, in the molysite and fumaric acid mixing dimethyl formamide solution, molysite and fumaric mass ratio are 2~2.4:1, and concentration of the molysite in dimethylformamide is 40.58~48.70 g/L;Mixing first by molysite and fumaric acid in dimethylformamide, it is subsequently placed in solvent heat treatment in autoclave, by centrifuging and the precipitation of generation being washed with ethanol, then dried precipitation is calcined, obtains the porous di-iron trioxide material of fusiformis α phases.The advantage of the invention is that:The porous di-iron trioxide materials application of α phase shuttle shapes prepared by the present invention greatly improves the capability retention, high rate performance and cycle life of lithium battery in lithium ion battery, and technique is simple, favorable reproducibility, easy to implement.
Description
Technical field
The present invention relates to technical field of lithium ion battery negative, more particularly to a kind of porous three oxidation of α phases shuttle shape
Two iron materials and its preparation method and application.
Background technology
Lithium ion battery has high voltage, high power capacity, small volume, light weight, memory-less effect, self discharge small and the circulation longevity
The advantages that long is ordered, becomes the mechanism of new electrochemical power sources of 21 century great potential.Negative material stone in commercialization lithium battery at present
The theoretical capacity of ink only has 372 mAh/g, it is impossible to meets the application demand of heavy-duty battery.Therefore, exploitation with higher capacity,
The negative material of long circulation life and high rate capability turns into the target that domestic and international researcher is chased.Wherein, transiting metal oxidation
Thing di-iron trioxide (Fe2O3) theoretical capacity (1007 mAh/g) is 3 times of graphite, have great application prospect;But it is deposited
It is low and the shortcomings that cycle life is poor in coulombic efficiency.
In order to improve Fe2O3Chemical property, mainly account for from the following aspect:Prepare Fe2O3Hollow nanometer material
On the one hand material, the presence in hole are advantageous to the infiltration of electrolyte and the transmission of lithium ion, on the other hand can alleviate charge and discharge process
In material volume change.By such a method can significantly improve di-iron trioxide be used as negative material coulombic efficiency and
Cycle performance.The poroid Fe of the preparations such as Yansen Wang2O3Nano material, although achieve 73% coulombic efficiency first and follow
898.5 mAh/g charging capacity is achieved after ring 50 times, but the preparation method is numerous and diverse needs to use SiO2As template
(Materials Letters, 2016, 171, 125-128.).Porous microsphere shape is prepared in order to explore a kind of easy method
Fe2O3Nano structural material, the present invention are prepared for porous di-iron trioxide material using simple low-temperature solvent heat method, avoided
The use of template.The porous di-iron trioxide nanometer anode material of shuttle shape α phases is applied to lithium battery, can significantly improve lithium
The cycle life of battery(After being circulated 150 times under 1C, the charging capacity and 97.91% capacity that achieve 824.25mAh/g are kept
Rate), yet there are no relevant report.
The content of the invention
The technical problem to be solved in the present invention is to provide a kind of porous di-iron trioxide material of α phases shuttle shape and its preparation side
Method and application, to solve technical problem of the existing di-iron trioxide as lithium ion battery negative material cycle life difference.
In order to solve the above technical problems, the technical scheme is that:A kind of porous di-iron trioxide material of α phases shuttle shape
Material, its innovative point are:The porous di-iron trioxide material of α phases shuttle shape is by molysite, fumaric acid and dimethyl methyl
Acid amides is prepared, wherein, in the molysite and fumaric acid mixing dimethyl formamide solution, molysite and anti-butylene two
The mass ratio of acid is 1:1~2:1, and concentration of the molysite in dimethylformamide is 40.58~48.70 g/L.
Further, the molysite is any of iron chloride, ferric nitrate or ferric sulfate.
A kind of preparation method of the above-mentioned porous di-iron trioxide material of α phase shuttle shapes, its innovative point are:First by iron
The mixing of salt and fumaric acid in dimethylformamide, is subsequently placed in solvent heat treatment in autoclave, passes through centrifugation
Separate and the precipitation of generation is washed with ethanol, then be calcined dried precipitation, obtain the porous di-iron trioxide of fusiformis α phase shuttle shapes
Material.
Further, the preparation method specifically includes following steps:
(1)Molysite and fumaric acid are successively added in the container for filling dimethylformamide and stirred until all molten
Solution;Wherein molysite and fumaric mass ratio are 1:1~2:1, and concentration of the molysite in dimethylformamide is 40.58
~48.70 g/L;
(2)Mixing dimethyl formamide solution in step (1) is placed in autoclave, is then placed within baking oven and carries out
Solvent heat treatment, room temperature is naturally cooled to after being kept for 4 hours under 80 DEG C of > temperature conditionss;
(3)By the sample after solvent heat treatment in step (2), it is centrifuged simultaneously with 5000~8000 r/min rotating speed
Washed 3~5 times with ethanol;Finally precipitation is put into 80~100 DEG C of vacuum drying chamber and is dried, obtaining ferrous metals has
Machine skeleton nanosphere;
(4)The ferrous metals organic backbone nanosphere that step (3) obtains is placed in tube furnace, with entering for 0.2~0.8 L/min
Tolerance is passed through air conservation gas, and heating rate is 2 DEG C~5 DEG C/min, is warming up to 450~550 DEG C and is incubated 2~4 hours
After naturally cool to room temperature, obtain the porous di-iron trioxide material of shuttle shape α phases.
A kind of application of the above-mentioned porous di-iron trioxide material of α phase shuttle shapes, its innovative point are:The α phases are porous
Application of the di-iron trioxide material in lithium ion battery.
Further, the porous di-iron trioxide materials application of the α phases shuttle shape is in CR2032 fastening lithium ionic cells
Comprise the concrete steps that:
(A)According to mass ratio by the porous di-iron trioxide material of shuttle shape α phase shuttle shapes:Conductive black:Conductive agent Super P=
7:2:1 is mixed, and is stirred, and obtains solid mixture;
(B)By step(A)Obtained solid mixture is 20 according to mass ratio with 1-METHYLPYRROLIDONE:80~25:75 are carried out
Mixing, stirs, and slurry is made;
(C)By step(B)Obtained slurry coated on copper foil, be made after drying, roll-in lithium that thickness is 13~22 μm from
Sub- battery electrode piece;
(D)By step(C)Obtained lithium ion cell electrode piece uses microporous polypropylene membrane as barrier film as Electrode Negative piece,
The electrolyte used is 1 mol/L LiPF6, solvent is isometric dimethyl carbonate and dipropyl carbonate, full of argon gas
CR2032 fastening lithium ionic cells are assembled into glove box.
The advantage of the invention is that:The porous di-iron trioxide material of α phase shuttle shapes prepared by the present invention can be as excellent
Lithium ion battery negative material, the cycle life of lithium battery can be significantly improved(After being circulated 150 times under 1C, 824.5 are achieved
MAh/g charging capacity and 76% capability retention), and technique is simple, favorable reproducibility, easy to implement, is adapted to extensive raw
Production.
Brief description of the drawings
The present invention is further detailed explanation with reference to the accompanying drawings and detailed description.
Fig. 1 is the X-ray diffraction result of the porous di-iron trioxide material of α phase shuttle shapes prepared by the embodiment of the present invention 1, point
Dui Yingyu not di-iron trioxide (JCPDS cards:Peak 33-0664).
Fig. 2 is the scanning electron microscope (SEM) photograph of the porous di-iron trioxide material of α phase shuttle shapes prepared by the embodiment of the present invention 1.
Fig. 3 be the embodiment of the present invention 1 prepare the porous di-iron trioxide material of α phase shuttle shapes as negative material lithium from
Cycle performance curve of the sub- battery under 1C.
Embodiment
The following examples can make professional and technical personnel that the present invention be more fully understood, but therefore not send out this
It is bright to be limited among described scope of embodiments.
Embodiment 1
(1) 0.649g iron chloride and 0.649g fumaric acid are added in the beaker for filling 16ml dimethylformamides not
Disconnected stirring, until all dissolvings;
(2) the mixing dimethyl formamide solution in step (1) is placed in 20 mL autoclaves, is then placed within baking oven
Middle carry out solvent heat treatment, room temperature is naturally cooled to after being kept for 4 hours at 80 DEG C;
(3) by the sample after solvent heat in step (2), it is centrifuged with 5000 r/min rotating speed and is washed with ethanol
4 times;Finally by precipitation be put into vacuum drying in 80 DEG C be dried, obtain ferrous metals organic backbone nanofiber;
(4) the dried ferrous metals organic backbone nanofiber of step (3) is placed in tube furnace, with 0.15 L/min's
Air inflow is passed through air conservation gas, and heating rate is 2 DEG C/min, natural cooling after being warming up to 500 DEG C and being incubated 4 hours
To room temperature, the porous di-iron trioxide material of α phase shuttle shapes is obtained.
The porous di-iron trioxide material of the α phase shuttle shapes obtained in embodiment is subjected to X-ray diffraction and electron-microscope scanning, by
The porous di-iron trioxide material of α phases that Fig. 2 can be seen that to obtain is shuttle shape, Fig. 1 surfaces, the shuttle shape α prepared using this method
Mutually porous di-iron trioxide material purity is high, without other impurities.
The assembling and performance test of lithium ion battery:According to mass ratio 80:10:10 by the porous di-iron trioxide of fusiformis α phases
Material, conductive black and Super P are well mixed, and are 20 according to mass ratio:80 addition 1-METHYLPYRROLIDONEs simultaneously stir,
Slurry is made;Lithium ion cell electrode piece is made coated on copper foil in slurry after drying, roll-in afterwards.Then with lithium piece
As electrode anode piece, microporous polypropylene membrane is barrier film, 1 mol/L LiPF6 (solvent is isometric dimethyl carbonate and carbon
Sour dipropyl) it is electrolyte, CR2032 fastening lithium ionic cells are assembled into the glove box full of argon gas with this electrode slice.Will
After lithium ion battery stands 24 hours, charge-discharge performance test is carried out under 0.1C electric currents respectively, charge and discharge voltage is 0.01
Between~3.0 V.From figure 3, it can be seen that the porous di-iron trioxide material of fusiformis α phases prepared using this method is as electrode material
Material, applied to lithium ion battery, after the circle of circulation 150, charging and discharging capacity is respectively 824.5mAh/g and 807.9mAh/g,
Capability retention has good cycle performance, far above the graphite cathode material of Current commercial more than 76%.
Embodiment 2
(1) 0.779 g ferric nitrates and 0.389 g fumaric acid are added in the beaker for filling 16ml dimethylformamides
It is stirred continuously, until all dissolvings;
(2) the mixing dimethyl formamide solution in step (1) is placed in 20 mL autoclaves, is then placed within baking oven
Middle carry out solvent heat treatment, room temperature is naturally cooled to after being kept for 4 hours at 80 DEG C;
(3) by the sample after solvent heat in step (2), it is centrifuged with 6500 r/min rotating speed and is washed with ethanol
4 times;Finally by precipitation be put into vacuum drying in 80 DEG C be dried, obtain ferrous metals organic backbone nanofiber;
(4) the dried ferrous metals organic backbone nanofiber of step (3) is placed in tube furnace, with entering for 0.3 L/min
Tolerance is passed through air conservation gas, and heating rate is 3 DEG C/min, is warming up to 500 DEG C and naturally cools to room after being incubated 4 hours
Temperature, obtain the porous di-iron trioxide material of α phases.
In the present embodiment lithium ion battery assembling and performance test it is same as Example 1.
Embodiment 3
(1) 0.724 g ferric sulfate and 0.483 g fumaric acid are added to the beaker for filling 16 ml dimethylformamides
In be stirred continuously, until all dissolving;
(2) the mixing dimethyl formamide solution in step (1) is placed in 20 mL autoclaves, is then placed within baking oven
Middle carry out solvent heat treatment, room temperature is naturally cooled to after being kept for 4 hours at 80 DEG C;
(3) by the sample after solvent heat in step (2), it is centrifuged with 8000 r/min rotating speed and is washed with ethanol
4 times;Finally by precipitation be put into vacuum drying in 80 DEG C be dried, obtain ferrous metals organic backbone nanofiber;
(4) the dried ferrous metals organic backbone nanofiber of step (3) is placed in tube furnace, with entering for 0.4 L/min
Tolerance is passed through air conservation gas, and heating rate is 5 DEG C/min, is warming up to 500 DEG C and naturally cools to room after being incubated 4 hours
Temperature, obtain the porous di-iron trioxide material of α phase shuttle shapes.
In the present embodiment lithium ion battery assembling and performance test it is same as Example 1.
The general principle and principal character and advantages of the present invention of the present invention has been shown and described above.The skill of the industry
For art personnel it should be appreciated that the present invention is not limited to the above embodiments, described in above-described embodiment and specification is explanation
The principle of the present invention, without departing from the spirit and scope of the present invention, various changes and modifications of the present invention are possible, these
Changes and improvements all fall within the protetion scope of the claimed invention.The claimed scope of the invention by appended claims and
Its equivalent thereof.
Claims (6)
- A kind of 1. porous di-iron trioxide material of α phases shuttle shape, it is characterised in that:The porous di-iron trioxide of α phases shuttle shape Material is prepared by molysite, fumaric acid and dimethylformamide, wherein, mixed in the molysite and fumaric acid In dimethyl formamide solution, molysite and fumaric mass ratio are 1:1~2.4:1, and the molysite is in dimethyl methyl Concentration in acid amides is 40.58~48.70 g/L.
- 2. the porous di-iron trioxide material of α phases shuttle shape according to claim 1, it is characterised in that:The molysite is chlorine Change any of iron, ferric nitrate or ferric sulfate.
- A kind of 3. preparation method of the porous di-iron trioxide material of α phase shuttle shapes described in claim 1, it is characterised in that:It is first The first mixing by molysite and fumaric acid in dimethylformamide, solvent heat treatment in autoclave is subsequently placed in, led to The precipitation for centrifuging and generation being washed with ethanol is crossed, then is calcined dried precipitation, obtains porous three oxidation two of shuttle shape α phases Iron material.
- 4. the preparation method of the porous di-iron trioxide material of α phases shuttle shape according to claim 3, it is characterised in that:Institute State preparation method and specifically include following steps:(1)Molysite and fumaric acid are successively added in the container for filling dimethylformamide and stirred until all molten Solution;Wherein molysite and fumaric mass ratio are 1:1~2:1, and concentration of the molysite in dimethylformamide is 40.58 ~48.70 g/L;(2)Mixing dimethyl formamide solution in step (1) is placed in autoclave, is then placed within baking oven and carries out Solvent heat treatment, room temperature is naturally cooled to after being kept for 4 hours under 80 DEG C of > temperature conditionss;(3)By the sample after solvent heat treatment in step (2), it is centrifuged simultaneously with 5000~8000 r/min rotating speed Washed 3~5 times with ethanol;Finally precipitation is put into 80~100 DEG C of vacuum drying chamber and is dried, obtaining ferrous metals has Machine skeleton nanosphere;(4)The ferrous metals organic backbone nanosphere that step (3) obtains is placed in tube furnace, with entering for 0.2~0.8 L/min Tolerance is passed through air conservation gas, and heating rate is 2 DEG C~5 DEG C/min, is warming up to 450~550 DEG C and is incubated 2~4 hours After naturally cool to room temperature, obtain the porous di-iron trioxide material of shuttle shape α phases.
- A kind of 5. application of the porous di-iron trioxide material of α phase shuttle shapes described in claim 1, it is characterised in that:The α phases Application of the porous di-iron trioxide material in lithium ion battery.
- 6. the application of the porous di-iron trioxide material of α phases shuttle shape according to claim 5, it is characterised in that:The α phases Porous di-iron trioxide materials application comprising the concrete steps that in CR2032 fastening lithium ionic cells:(A)According to mass ratio by the porous di-iron trioxide material of shuttle shape α phases:Conductive black:Conductive agent Super P=7:2:1 enters Row mixing, stirs, obtains solid mixture;(B)By step(A)Obtained solid mixture is 20 according to mass ratio with 1-METHYLPYRROLIDONE:80~25:75 are carried out Mixing, stirs, and slurry is made;(C)By step(B)Obtained slurry coated on copper foil, be made after drying, roll-in lithium that thickness is 13~22 μm from Sub- battery electrode piece;(D)By step(C)Obtained lithium ion cell electrode piece uses microporous polypropylene membrane as barrier film as Electrode Negative piece, The electrolyte used is 1 mol/L LiPF6, solvent is isometric dimethyl carbonate and dipropyl carbonate, full of argon gas CR2032 fastening lithium ionic cells are assembled into glove box.
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Cited By (1)
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CN109728282A (en) * | 2018-12-30 | 2019-05-07 | 北京乐华锂能科技有限公司 | A kind of preparation method of Porous transition metal oxides/carbon composite |
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CN103922421A (en) * | 2014-05-13 | 2014-07-16 | 西北大学 | Method for preparing alpha-Fe2O3 |
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CN109728282A (en) * | 2018-12-30 | 2019-05-07 | 北京乐华锂能科技有限公司 | A kind of preparation method of Porous transition metal oxides/carbon composite |
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Application publication date: 20171229 |