CN104241628A - Method for preparing titanium-dioxide-modified ferric oxide microspheres as well as produced product and use of titanium-dioxide-modified ferric oxide microspheres - Google Patents
Method for preparing titanium-dioxide-modified ferric oxide microspheres as well as produced product and use of titanium-dioxide-modified ferric oxide microspheres Download PDFInfo
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- CN104241628A CN104241628A CN201410496005.8A CN201410496005A CN104241628A CN 104241628 A CN104241628 A CN 104241628A CN 201410496005 A CN201410496005 A CN 201410496005A CN 104241628 A CN104241628 A CN 104241628A
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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
- H01M4/362—Composites
- H01M4/366—Composites as layered products
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- H—ELECTRICITY
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- 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
- H01M4/483—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides for non-aqueous cells
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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
- H01M4/523—Selection of substances as active materials, active masses, active liquids of inorganic oxides or hydroxides of nickel, cobalt or iron for non-aqueous cells
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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 invention relates to a method for preparing titanium-dioxide-modified ferric oxide microspheres. The method comprises the following steps: after putting a sucrose or glucose aqueous solution in a hydrothermal reaction kettle for hydrothermal reaction at 180-220 DEG C, carrying out suction filtration and washing with deionized water and ethanol, and drying to obtain carbon balls with uniform particle size distribution; then, ultrasonically dispersing the carbon balls in a mixed solution of a ferric nitrate ethanol solution and tetrabutyl titanate, stirring at room temperature, and stirring at 60-80 DEG C after uniformly mixing; after the reaction, carrying out suction filtration and washing with absolute ethanol and the deionized water, and drying at 100 DEG C to obtain an intermediate product; putting the intermediate product in a tube furnace for roasting for 2-4 hours in air at 400-600 DEG C to obtain the titanium-dioxide-modified ferric oxide microspheres. The method is easy and convenient to operate and easy to control in conditions and is good in repeatability. The prepared product is used as an anode material of a lithium ion battery, and the produced lithium ion battery has a good charge-discharge cycle performance and high energy storage capacity.
Description
Technical field
The present invention relates to the di-iron trioxide microballoon that a kind of titanium dioxide is modified, it can as lithium ion battery negative material.
Background technology
Be about to exhaust and can produce the problems such as a large amount of greenhouse gas in its use procedure owing to there is fossil energy, a large amount of emerging energies has come into the visual field of people, as wind energy, tidal energy, solar energy, nuclear energy, biomass energy etc.These energy mostly need to be converted into electric energy and just can be utilized.On the other hand, need by produce unstable electrical power storage get up after just can be utilized.So moveable power supply obtains and rapidly develops.Lithium rechargeable battery wherein rely on its higher specific capacity and energy density and have extended cycle life, the feature such as operating voltage is high, memory-less effect has been widely used in the portable electronic devices such as mobile phone, portable/panel computer, and in electrical source of power such as electric automobiles, and also presented its good potentiality in the large-scale accumulation power supply such as power station, be expected to replace traditional NI-G, lead-acid battery and become the leading of Green Chemistry power supply.Anode material for lithium-ion batteries commercial on market is mainly: cobalt acid lithium, LiMn2O4, LiFePO4 and cobalt nickel lithium manganate ternary material; The negative material that commercialization uses is mainly graphite material.Worldwide researcher is all carrying out deep research and development for the new material that can be applied to lithium ion cell electrode.
In commercial li-ion battery, production cost is mainly derived from electrode material.So how to prepare cheap, environmental friendliness and the electrode material of electrochemical performance becomes the most important thing of lithium ion battery development.Only with regard to negative material, the graphite that commercialization uses just occupies the market share of thumping majority with its cheap price and stable cycle performance.But due to lower (the theoretical specific capacity 372mAh/g of its specific capacity, actual specific capacity is not higher than 350mAh/g), and intercalation potential is close to the current potential of lithium metal, cause easily forming Li dendrite in long-term cyclic process, cause battery short circuit, even can cause the serious consequences such as blast on fire.Based on this, the research and development of Novel anode material have good prospect.
The metal oxide that working mechanism reacts for " transformant ", the oxides such as iron, manganese, molybdenum rely on the features such as its higher theoretical specific capacity, cheap price, environmental friendliness and rich reserves to enter the visual field of vast researcher.For di-iron trioxide, its theoretical specific capacity is 1005mAh/g, be almost three times of graphite, and ferro element is extensively present in nature as the deputy metallic element of content in the earth's crust, very easily obtains.But due to the working mechanism of its " transformant ", in lithium cyclic process, change in volume is comparatively large, easily make material structure efflorescence and its poor ion, electronic conduction performance also make the cycle performance of battery poor, finally hinder its practical application.For the problems referred to above, researcher is by having carried out exquisite structural design to material, as the people such as David Lou have obtained di-iron trioxide hollow ball (J.Am.Chem.Soc.2011 by microemulsion hydro thermal method, 133,17146 – 17148), through test, the cycle performance of the battery charging and discharging of this material obtains good lifting.
Titanium dioxide, as the metal oxide of a kind of " inserting insert-type " working mechanism, have very good lithium cycle performance, but its theoretical specific capacity is relatively low.On the spherical shell of di-iron trioxide hollow ball, embed titanium dioxide, see chemiluminescence by Jie of titanium dioxide and di-iron trioxide and suppress its structure efflorescence to be a kind of composite oxides structural design of innovation.
Summary of the invention
The preparation method of the di-iron trioxide microballoon that the object of the present invention is to provide a kind of titanium dioxide to modify and obtained product and the purposes as lithium ion battery negative material.
Technical scheme of the present invention is as follows:
A preparation method for the di-iron trioxide microballoon that titanium dioxide is modified, it comprises the following steps:
Step 1, be that the sucrose of 1.5-3mol/L or D/W put into hydrothermal reaction kettle at 180-220 DEG C of temperature after hydro-thermal reaction 1-4 hour by concentration, by deionized water and ethanol filtering and washing, dry at 80 DEG C, obtain the carbon ball that domain size distribution is homogeneous;
Step 2, by obtained carbon ball ultrasonic disperse in iron nitrate concentration is the 80ml ethanolic solution of 1.5-5mol/L and the mixed solution of 1-5ml butyl titanate, room temperature lower magnetic force stirs 0.5-2 hour, to be mixed evenly after in 60-80 DEG C of magnetic agitation 4-12 hour, reaction terminates rear absolute ethyl alcohol and deionized water filtering and washing, dries obtained intermediate product in 100 DEG C;
Step 3, intermediate product obtained for step 2 is placed in tube furnace at 400-600 DEG C of temperature, roasting 2-4 hour under air atmosphere, the di-iron trioxide microballoon that obtained titanium dioxide is modified.
The di-iron trioxide microballoon that the titanium dioxide that a kind of above-mentioned preparation method obtains is modified.
The di-iron trioxide microballoon that above-mentioned titanium dioxide is modified is preparing the application in lithium ion battery as lithium ion battery negative material.
The present invention uses carbon to go out intermediate product from sacrificing template synthesis, then intermediate product is carried out roasting in air atmosphere, generates the di-iron trioxide microballoon that titanium dioxide is modified.Method is easy, reproducible, and preparation process is nontoxic.The product made has high lithium storage content and good cycle performance.
The carbosphere pattern that the present invention prepares is unified, even particle size distribution, and its surface has a large amount of functional group and micropore can make later stage mixed solution immerse.Directly also namely the thickness of product hollow core spherical shell is closely related with the degree of depth immersing carbon spherical shell for the temperature of solution diffusion, time, concentration difference, and the thickness of spherical shell determines again the chemical property of material simultaneously.
In described mixed solution, butyl titanate and the ethanolic solution volume ratio that feeds intake is 1.25 ~ 6.25:100, this rate of charge determines the ratio of titanium dioxide and ferric oxide in final products, the electrochemical properties adding membership lifting material of appropriate titanium dioxide, if but titanium dioxide addition is too much, its specific capacity can significantly decrease.
The calcination atmosphere of described intermediate product is air, and sintering temperature is 400-600 DEG C, temperature retention time 2-4 hour.Above-mentioned condition is from removing carbon template product completely, obtaining the metal oxide products of higher crystallinity and specific area.The present invention obtains microspherulite diameter and is about 20 nanometers.
The lithium ion battery energy storage capacity that the di-iron trioxide microballoon modified using titanium dioxide of the present invention is prepared as negative material is high, and charge-discharge performance is good.
Accompanying drawing explanation
Fig. 1 is SEM and the TEM image of product, therefrom can find out that the pattern of product is the tiny balloon of diameter about 2 μm, the thick about 500nm of shell.Its pattern is homogeneous, Stability Analysis of Structures.Fig. 1 upper left is the monomer SEM image of product, can find out that it is tiny balloon.Upper right is the product SEM image condensed together, and can find out that its pattern is homogeneous.Lower-left is macroscopical SEM image that product is assembled in a large number, can find out that products together on the whole together, even size distribution.Bottom right is the monomer TEM image of product, and the outer surface of its microballoon is bobbles shape as we know from the figure.
Fig. 2 is the EDX-mapping image of product, therefrom can find out that microballoon is made up of Ti/Fe/O element, and Elemental redistribution is even.
In Fig. 3, a is within the scope of 0.005-3V for product is made half-cell at voltage, electrochemistry cycle performance curve under the speed of 200mA/g, b is common di-iron trioxide correlation curve, known according to Fig. 3, cycle performance compared by the more common di-iron trioxide of this material and capacity is greatly improved, and also has the specific capacity of nearly 1000 MAH every gram 100 circulations.
Fig. 4 is the XRD collection of illustrative plates of product, can find out that the degree of crystallinity of its di-iron trioxide is fine by collection of illustrative plates, 20 nanometers are about by Scherrer formula its crystallite dimension known, little owing to modifying titanium dioxide amount used, and its particle may be less, so the crystal information of titanium dioxide cannot be found out in XRD collection of illustrative plates.
Fig. 5 is the specific area result of product.As calculated, product roasting at 550 DEG C still has 50m in 4 hours
2the specific area of/g, and there is the mesoporous of average pore size 14nm.
Embodiment
In line with the target of the object of clear interpretation the present invention, technical scheme and product performance, below in conjunction with embodiment, the invention will be further described
Embodiment 1
1) from the synthesis of sacrificing carbon ball template: in 150ml water heating kettle, put into 100ml deionized water, after take sucrose 52g, be dissolved in deionized water, seal reactor and be placed in the baking oven of 200 DEG C, heat after 2 hours and take out, alcohol wash 5 times after suction filtration, puts into 80 DEG C of baking ovens and spends the night.
2) synthesis of intermediate product: add 80ml absolute ethyl alcohol in beaker, takes 60.2g Fe(NO3)39H2O and is dissolved in wherein, after suitably heating and magnetic agitation make it fully dissolve, add 2ml butyl titanate, magnetic agitation 30 minutes.Separately get 0.8g carbon ball and put into mixed solution, heat after 4 hours at 80 DEG C, through suction filtration and washing alcohol wash, after putting into 100 DEG C of oven for drying, obtain intermediate product.
3) acquisition of final products: intermediate product is put into tube furnace, is warming up to 500 DEG C in air atmosphere, is incubated 3 hours, afterwards with stove cooling, can obtain the di-iron trioxide microballoon that final products titanium dioxide is modified.
4) product 160mg is got, in the 20mg binding agent Kynoar (PVDF) mixed before pouring into conductive agent acetylene black 20mg ground and mixed 10min and 1ml N-methyl-pyrrolidon (NMP) solution, to obtain slurry.This slurry is applied equably on copper current collector, and dries at 80 DEG C.Carry out punching afterwards, by cathode pole piece vacuumize under 120 DEG C of conditions good for punching, after put into glove box.: by obtained lithium ion battery negative electrode, barrier film, lamination is good successively for lithium sheet, and with the ethylene carbonate of lithium hexafluoro phosphate (LiPF6) containing 1 mol/L: methyl ethyl carbonate: seal after the electrolyte that diethyl carbonate (EC/EMC/DEC) is made into for 1:1:1 by volume fully mixes, obtained 2032 type lithium-ion button batteries
Embodiment 2
1) from the synthesis of sacrificing carbon ball template: in 150ml water heating kettle, put into 100ml deionized water, after take glucose 60g, be dissolved in deionized water, seal reactor and be placed in the baking oven of 200 DEG C, heat after 3 hours and take out, alcohol wash 5 times after suction filtration, puts into 80 DEG C of baking ovens and spends the night.
2) synthesis of intermediate product: add 50ml absolute ethyl alcohol in beaker, takes 60.2g Fe(NO3)39H2O and is dissolved in wherein, after suitably heating and magnetic agitation make it fully dissolve, add 1ml butyl titanate, magnetic agitation 30 minutes.Separately get 0.6g carbon ball and put into mixed solution, heat after 4 hours at 80 DEG C, through suction filtration and washing alcohol wash, after putting into 100 DEG C of oven for drying, obtain intermediate product.
3) acquisition of final products: intermediate product is put into tube furnace, is warming up to 550 DEG C in air atmosphere, is incubated 2 hours, afterwards with stove cooling, can obtain the di-iron trioxide microballoon that final products titanium dioxide is modified.Get product 160mg, in the 20mg binding agent Kynoar (PVDF) mixed before pouring into conductive agent acetylene black 20mg ground and mixed 10min and 1ml N-methyl-pyrrolidon (NMP) solution, to obtain slurry.This slurry is applied equably on copper current collector, and dries at 80 DEG C.Carry out punching afterwards, by cathode pole piece vacuumize under 120 DEG C of conditions good for punching, after put into glove box.: by obtained lithium ion battery negative electrode, barrier film, lamination is good successively for lithium sheet, and with the ethylene carbonate of lithium hexafluoro phosphate (LiPF6) containing 1 mol/L: methyl ethyl carbonate: seal after the electrolyte that diethyl carbonate (EC/EMC/DEC) is made into for 1:1:1 by volume fully mixes, obtained 2032 type lithium-ion button batteries
Embodiment 3
1) from the synthesis of sacrificing carbon ball template: in 150ml water heating kettle, put into 100ml deionized water, after take sucrose 62g, be dissolved in deionized water, seal reactor and be placed in the baking oven of 190 DEG C, heat after 4 hours and take out, alcohol wash 5 times after suction filtration, puts into 80 DEG C of baking ovens and spends the night.
2) synthesis of intermediate product: add 100ml absolute ethyl alcohol in beaker, takes 60.2g Fe(NO3)39H2O and is dissolved in wherein, after suitably heating and magnetic agitation make it fully dissolve, add 3ml butyl titanate, magnetic agitation 30 minutes.Separately get 1g carbon ball and put into mixed solution, heat after 8 hours at 70 DEG C, through suction filtration and washing alcohol wash, after putting into 100 DEG C of oven for drying, obtain intermediate product.
3) acquisition of final products: intermediate product is put into tube furnace, is warming up to 400 DEG C in air atmosphere, is incubated 4 hours, afterwards with stove cooling, can obtain the di-iron trioxide microballoon that final products titanium dioxide is modified.
4) product 160mg is got, in the 20mg binding agent Kynoar (PVDF) mixed before pouring into conductive agent acetylene black 20mg ground and mixed 10min and 1ml N-methyl-pyrrolidon (NMP) solution, to obtain slurry.This slurry is applied equably on copper current collector, and dries at 80 DEG C.Carry out punching afterwards, by cathode pole piece vacuumize under 120 DEG C of conditions good for punching, after put into glove box.: by obtained lithium ion battery negative electrode, barrier film, lamination is good successively for lithium sheet, and with the ethylene carbonate of lithium hexafluoro phosphate (LiPF6) containing 1 mol/L: methyl ethyl carbonate: seal after the electrolyte that diethyl carbonate (EC/EMC/DEC) is made into for 1:1:1 by volume fully mixes, obtained 2032 type lithium-ion button batteries
Embodiment 4
1) from the synthesis of sacrificing carbon ball template: in 150ml water heating kettle, put into 100ml deionized water, after take glucose 90g, be dissolved in deionized water, seal reactor and be placed in the baking oven of 220 DEG C, heat after 1 hour and take out, alcohol wash 5 times after suction filtration, puts into 80 DEG C of baking ovens and spends the night.
2) synthesis of intermediate product: add 100ml absolute ethyl alcohol in beaker, takes 60.2g Fe(NO3)39H2O and is dissolved in wherein, after suitably heating and magnetic agitation make it fully dissolve, add 4ml butyl titanate, magnetic agitation 30 minutes.Separately get 1.2g carbon ball and put into mixed solution, heat after 12 hours at 60 DEG C, through suction filtration and washing alcohol wash, after putting into 100 DEG C of oven for drying, obtain intermediate product.
3) acquisition of final products: intermediate product is put into tube furnace, is warming up to 400 DEG C in air atmosphere, is incubated 4 hours, afterwards with stove cooling, can obtain the di-iron trioxide microballoon that final products titanium dioxide is modified.4) product 160mg is got, in the 20mg binding agent Kynoar (PVDF) mixed before pouring into conductive agent acetylene black 20mg ground and mixed 10min and 1ml N-methyl-pyrrolidon (NMP) solution, to obtain slurry.This slurry is applied equably on copper current collector, and dries at 80 DEG C.Carry out punching afterwards, by cathode pole piece vacuumize under 120 DEG C of conditions good for punching, after put into glove box.: by obtained lithium ion battery negative electrode, barrier film, lamination is good successively for lithium sheet, and with the ethylene carbonate of lithium hexafluoro phosphate (LiPF6) containing 1 mol/L: methyl ethyl carbonate: seal after the electrolyte that diethyl carbonate (EC/EMC/DEC) is made into for 1:1:1 by volume fully mixes, obtains 2032 type lithium-ion button batteries.
Claims (3)
1. a preparation method for the di-iron trioxide microballoon of titanium dioxide modification, is characterized in that: it comprises the following steps:
Step 1, be that the sucrose of 1.5-3mol/L or D/W put into hydrothermal reaction kettle at 180-220 DEG C of temperature after hydro-thermal reaction 1-4 hour by concentration, by deionized water and ethanol filtering and washing, dry at 80 DEG C, obtain the carbon ball that domain size distribution is homogeneous;
Step 2, by obtained carbon ball ultrasonic disperse in iron nitrate concentration is the 80ml ethanolic solution of 1.5-5mol/L and the mixed solution of 1-5ml butyl titanate, room temperature lower magnetic force stirs 0.5-2 hour, to be mixed evenly after in 60-80 DEG C of magnetic agitation 4-12 hour, reaction terminates rear absolute ethyl alcohol and deionized water filtering and washing, dries obtained intermediate product in 100 DEG C;
Step 3, intermediate product obtained for step 2 is placed in tube furnace at 400-600 DEG C of temperature, roasting 2-4 hour under air atmosphere, the di-iron trioxide microballoon that obtained titanium dioxide is modified.
2. the di-iron trioxide microballoon that the titanium dioxide that described in a claim 1, preparation method obtains is modified.
3. the di-iron trioxide microballoon that titanium dioxide according to claim 2 is modified is preparing the application in lithium ion battery as lithium ion battery negative material.
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| CN104766953A (en) * | 2015-03-31 | 2015-07-08 | 浙江大学 | Preparation method of titanium dioxide/iron oxide composite anode material |
| CN108598449A (en) * | 2018-06-28 | 2018-09-28 | 西南石油大学 | High-performance hollow silicon-carbon graphene tri compound negative material and preparation method |
| CN108914706A (en) * | 2018-07-26 | 2018-11-30 | 武汉菡美洛建筑材料有限公司 | A kind of Environment-friendlywallpaper wallpaper of formaldehyde adsorption |
| CN115057471A (en) * | 2022-05-23 | 2022-09-16 | 山东大学 | Lithium ion battery cathode material and preparation method thereof |
| CN115472801A (en) * | 2022-10-11 | 2022-12-13 | 扬州工业职业技术学院 | Preparation method and application of porous ferroferric oxide and nickel oxide with hydrogenated titanium dioxide modified core-shell structure |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN104766953A (en) * | 2015-03-31 | 2015-07-08 | 浙江大学 | Preparation method of titanium dioxide/iron oxide composite anode material |
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| CN115472801A (en) * | 2022-10-11 | 2022-12-13 | 扬州工业职业技术学院 | Preparation method and application of porous ferroferric oxide and nickel oxide with hydrogenated titanium dioxide modified core-shell structure |
| CN115472801B (en) * | 2022-10-11 | 2023-06-30 | 扬州工业职业技术学院 | Preparation method and application of hydrogenated titanium dioxide modified core-shell structure carbon coated porous ferroferric oxide and nickel oxide |
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