CN102623692A - Method for preparing anode material of ferroferric oxide and carbon composite lithium battery - Google Patents
Method for preparing anode material of ferroferric oxide and carbon composite lithium battery Download PDFInfo
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Abstract
The invention relates to a method for preparing an anode material of a ferroferric oxide and carbon composite lithium battery. The method comprises the following steps of: weighing raw materials according to ferrum elements in a ferrum source and carbon elements in graphite; adding the weighed raw materials and a grinding ball into a ball grinding pot, adding a certain amount of distilled or deionized water into the ball grinding pot, and performing wet ball grinding or directly performing dry grinding; placing the ball grinding pot on a ball grinder, performing ball grinding for certain time at certain rotating speed, and discharging a product; when the ferrum source is hydroxide, chloride or various ferric salts, performing thermal treatment on the product subjected to ball grinding for several hours under the protection of inertia gas; performing magnetic separation on the product to separate out graphite particles which are not composited fully; and finally screening the graphite particles in sequence according to different apertures, drying the product subjected to wet grinding before screening, and screening to obtain the carbon-based ferroferric oxide composite material. The method has the characteristics of low cost, no pollution and simple process, and the material can be produced in a large scale.
Description
Technical field
The present invention relates to a kind of preparation method of lithium cell cathode material, that concrete is the preparation method of a kind of tri-iron tetroxide-carbon composite lithium ion battery negative material.
Background technology
As a kind of mechanism of new electrochemical power sources, it is fast that lithium ion battery has a charging rate with it, has extended cycle life; Load performance is good, and energy density and operating voltage are high, advantages such as safety non-pollution; Be widely used in various portable electric appts, its annual production date increases.Lithium ion battery negative material has worldwide obtained extensive studies as the key factor that improves lithium rechargeable battery energy and cycle life.As lithium ion battery negative material, carbon-based material has the discharge capacity height, has extended cycle life low cost and other advantages.Therefore, as a kind of economic and practical raw material, be used for the negative material great majority or the carbon-based material of lithium ion battery at present.
Carbon is a kind of very common element, extensively is present in the middle of the atmosphere and the earth's crust in a variety of forms.Carbon simple substance is very early by people understanding with utilize, and a series of compound-organic substances of carbon are life basic especially.And be applied in carbon in the lithium cell cathode material all is that form with carbon simple substance exists basically.Carbon simple substance has multiple, as: graphite, diamond, fullerene (ball carbon family) and Graphene etc.Carbon atom lumps together with plane stratiform structural bond in the graphite; Bonding is relatively fragile between layer and the layer, when applying external force, layer with layer between separated by slip easily; If separating in layer, the single atomic layer that finally obtains is called as Graphene (Graphene).Therefore, graphite material is the general name of single or multiple lift Graphene.From 2004; An Delie Jim of Univ Manchester UK and Ke Siteyanuowo two professors of Lip river husband (two people are because the outstanding contributions in Graphene research obtain 2010 annual Nobel Prizes in physics) that disappear have used successfully that tape stripping monoatomic layer graphite--since the Graphene, people have started the research boom of Graphene for the moment.The grapheme material that has several stratiforms or a multilayer according to research report is used in to have in the lithium battery than traditional material has more excellent performance.This mainly be Graphene with its unique two-dimensional network structure, have high conductance (under the room temperature, the speed of conduction electron is all faster than known conductor), high-specific surface area (2600m
2/ g) determined.
On the other hand, Nature magazine 2000, the 407th phase, 496-499 has reported that one piece is entitled as: Nano-sized transition-metal oxidesas negative-electrode materials for lithium-ion batteries.People begin utilizing transition metal oxide nano powder preparing lithium cell cathode material to produce great interest.In recent years; Continuous development along with nano combined material; Add the further investigation of people to the physicochemical characteristics of carbon single or multiple lift material; People begin to prepare and study carbon and the transition metal oxide complex desirable lithium cell cathode material of making comparisons, as in google academics search engine, importing recently: C-Fe
3O4, C-Fe
2O
3, C-FeO, C-Co
3O
4, C-CuO, C-Cu
2O, C-NiO, C-CoO, C-MnO
2, C-Mn
3O
4In a keyword and import lithium ion cells simultaneously or lithium-ion battery anodes has a large amount of bibliographical informations.Discover that negative material that this type of composite material is made has than the city with carbon electrode material or singly have the more performance of excellence with non-carbon composite.Wherein, C-Fe
3O
4Composite material, the bibliographical information of recent years: (1) Fe
3O
4Nanoparticle-integrated graphene sheets for high-performance half and full lithium ion cells, Phys. Chem. Chem. Phys; 2011,13,7170-7177; (2) Bottom-up in situ formation of Fe
3O
4Nanocrystals in a porous carbon foam for lithium-ion battery anodes J. Mater. Chem., 2011,21,17325-17330; (3) Electrospinning synthesis of C/Fe
3O
4Composite nanofibers and their application for high performance lithium-ion batteries, Journal of Power Sources, 2008,183 (2): 717-723; (4) Facile preparation of carbon coated magnetic Fe
3O
4Particles by a combined reduction/CVD process, Materials Research Bulletin, 2011,46 (5): 748-754; (5) One-step pyrolysis route to C/Fe
3O
4Hybrids from EDTA ferric sodium salt, Materials Letters, 2010,64 (7): 817 –, 819. (6) Electrospinning synthesis of C/Fe
3O
4Composite nanofibers and their application for high performance lithium-ion batteries; (7) A magnetite nanocrystal/graphene composite as high performance anode for lithium-ion batteries, Journal of Alloys and Compounds, 2012,514:76-80 (8) An Fe
3O
4-FeO-FeC composite and its application as anode for lithium-ion battery. Journal of Alloys and Compounds, 2012,513 (5): 460-465 (9) Hollow Fe
3O
4/ C spheres as superior lithium storage materials. Journal of Power Sources. 2012,197:305-309 (10) Carbon Coated Fe
3O
4Nanospindles as a Superior Anode Material for Lithium-Ion Batteries, Adv. Funct. Mater. 2008,18:3941 – 3946.(11) Structural evolution from mesoporous α-Fe
2O
3To Fe
3O
4C and γ-Fe
2O
3Nanospheres and their lithium storage performances, Cryst. Eng. Comm, 2011,13,4709-4713 or the like.
In transition metal oxide, the tri-iron tetroxide low price, thermal stability property is good, has the favorable conductive characteristic, is a kind of good lithium battery material.On Nature Materials, 2006 the 5th phases the 567th to 573 page of High rate capabilities Fe
3O
4-based Cu nano-architectured electrodes for lithium-ion battery applications just has the possibility of the complex of bibliographical information tri-iron tetroxide and copper as lithium battery material, and copper is as noble metal, and cost is high.Ferro element and carbon simple substance distribute extensively at occurring in nature, and the composite material of preparation tri-iron tetroxide and carbon is applied to lithium battery cathode material; Not only improving the electrochemical properties and the security feature of battery material, still is a kind of low pollution, material cheaply simultaneously; Both environmental friendliness, energy-conserving and environment-protective again.Yet go up report according to this, this composite material mainly adopts liquid phase method, high-temperature decomposition, or liquid phase method and high-temperature processing method combination.In preparation process, or need numerous reagent raw material, or need the technological process of complicated operation, the byproduct of product causes waste, and target product yields poorly, and highly energy-consuming so that production cost are high, difficult realization large-scale industrialization production and application.
In numerous material preparation technology, high-energy ball milling method is a kind of easy to operate, and low cost method is in the preparation that is applied to multiple functional material.The high-energy ball milling process is divided into physics and prepares two kinds of process and chemical processes.Physical process is to be milled into micron and even nano level granule through mechanical ball milling in order to reach the bulky grain fragmentation, and chemical process to be the limit mill, the process of limit reaction.Solid phase method is an example with preparation Graphene and graphite nano plate: as authorizing Chinese invention patent, the production method of (1) a kind of grapheme material, publication number: 101671015.(2) Chinese invention patent utilizes high-energy ball milling to prepare the method for Nano graphite thin slice, publication number: 101348251.More than utilizing the graphite raw material ball milling to go out multilayer or single-layer graphene and graphite nano plate is to utilize the physical process of high-energy ball milling.The English report that utilizes physical process to prepare the nano-graphite material also has document: (1) Nanostructure Evolution of Expanded Graphite during High-Energy Ball-Milling; Journal Applied Mechanics and Materials; 2011,80-81:229-232.(2)?Highly?curved?carbon?nanostructures?produced?by?ball-milling,?Chemical?Physics?Letters,?1999，303(1–2):130
–134.?(3)?Transformation?of?carbon?nanotubes?to?nanoparticles?by?ball?milling?process,?Carbon,?1999,?37(?3):?493–497。Above document description is explained and is adopted the mechanism of high-energy ball milling ability can graphite be peeled off the nano-graphite material that becomes to have the excellent electrochemical characteristic.
In addition, with the preparation nanometer Fe
3O
4Be example:, report in the 42-45 page or leaf that (α-Fe2O3) dry grinding reflects the ferriferrous oxide nano powder to the method that adopts high-energy ball milling with steel ball with di-iron trioxide as in " Journal of Alloy and Compounds " the 475th phase in 2009.And for example " China Particuology " 2007, mentions in the 357-358 page or leaf and utilizes reduced iron powder (α-Fe) obtain ferroferric oxide nano granules with deionized water wet-milling reaction the 5th phase.More than utilizing reduced iron powder to add deionized water perhaps utilizes iron shot and di-iron trioxide successfully to prepare Fe
3O
4Process, explain that high-energy ball milling can provide enough energy to make and have only the chemical reaction that at high temperature could take place to carry out smoothly usually.In industry was also used, the method can also successfully be prepared other a large amount of oxide functional materials, and bibliographical information has in the recent period: Mechanochemistry:opportunities for new and cleaner synthesis; Chem. Soc. Rev.; 2012,41,413-447.
At present, the report that utilizes high-energy ball milling to prepare electrode of lithium cell composite carbon base alloy material is arranged also, as: Composite anode material of silicon/graphite/carbon nanotubes for Li-ion batteries; Electrochimica Acta; 2006,51 (23): 4994 – 5000, Synthesis and electrochemical performance of Si/Cu and Si/Cu/graphite composite anode; Materials Chemistry and Physics; 2007,104 (2 – 3): 444 –, 447. Graphite-Tin composites as anode materials for lithium-ion batteries, Journal of Power Sources; 2001,97 – 98:211 – 215.
But up to the present, also there are not document and patent report to adopt high-energy ball milling method to prepare the composite material of tri-iron tetroxide and carbon.
Summary of the invention
Comprehensive production cost of this patent and material property, employing high-energy ball milling method utilize the physical process and the chemical process that produce in the mechanical milling process to act on the composite material for preparing carbon and transition metal oxide simultaneously.
Specifically realize through following scheme is concrete:
The first step takes by weighing raw material by carbon in ferro element in the source of iron and the graphite with 1:1 ~ 1:100.
Second step was that 1:1 ~ 10:1 joins in the ball grinder with raw material that takes by weighing and abrading-ball by mass ratio, in ball grinder, added the distilled water or the deionized water wet ball grinding of certain mass again, perhaps directly dry grinding.Ball grinder is put on the ball mill, with rotating speed be 300 ~ 800 rev/mins or more than, after ball milling 3-100 hour, discharging obtains product.For source of iron is iron powder, or during the mixture of iron powder and ferriferous oxide, the product behind the ball milling is target product, need not to heat-treat.For source of iron is the hydroxide of iron, chloride, and carbonate, sulfate is when nitrate or acetate, to the product after the ball milling discharging, at inert gas Ar or N
2Protection under, 350 ~ 1000
oThe processing of C 0.5 ~ 4 hour.
The 3rd step, product is carried out magnetic separate, isolate not fully compound graphite granule.
The 4th step, sieve successively by different apertures at last, need oven dry handle before sieving for the product of wet-milling, sieve and choose the carbon back ferric oxide composite material that obtains in this patent invention.The isolated graphite granule of magnetic with sieve after the bulky grain that obtains, recycling.
Preferable, described iron powder is reduction Fe powder;
Preferable, described ferriferous oxide is artificial synthetic Fe
2O
3, Fe
3O
4, FeO, natural bloodstone, a kind of or many in magnetic iron ore and the siderite;
Preferable, described carbon simple substance is elected graphite as, Graphene, one or more in CNT and the fullerene;
Preferable, described wet ball grinding, used deionized water is 1:1 ~ 5:1 with raw material cumulative volume ratio;
Preferable, described mill pearl and ball grinder cavity material are stainless steel, agate, zirconia ceramics body.
Physical process in this method is that raw material is milled, and reduces particle size, increases its specific area, makes it have bigger surface energy simultaneously; Especially to the ball milling of graphite in the raw material, to a certain extent large-sized graphite flake is peeled off the multilayer graphite flake that becomes to have nanostructure, or the single-layer graphene structure, it is had than the better electrochemical properties of graphite.Chemical process in this method is the energy that utilizes high-energy ball milling to produce; Make carbon and selected raw material carry out the part chemical reaction; Form with weak bond power combines, and this being combined in physically mainly is mutual coating, and the form that embeds is each other carried out; Arrive compound effect, thereby arrive the purpose that its electrochemical properties is provided.This method has low cost, and is pollution-free, and technology is simple, the characteristics that can produce in enormous quantities.
Description of drawings
Fig. 1 is that source of iron is an iron powder, or the mixture of iron powder and ferriferous oxide and graphite nodule grind the artwork of carbon back ferriferous oxide fully,
Fig. 2 is that source of iron is the hydroxide of iron, and insoluble salt or soluble-salt and graphite nodule grind the artwork of carbon back ferriferous oxide fully.
Embodiment
Further set forth the present invention below in conjunction with specific embodiment, should be understood that these embodiment only are used to the present invention is described and are not used in restriction protection scope of the present invention.
Embodiment 1
Take by weighing 11.6g Fe3O4 powder, 6g expanded graphite powder, 20g stainless steel abrading-ball; The 50ml deionized water is put into stainless steel jar mill, starts ball mill, and regulating rotating speed is 500 rev/mins; Behind the ball milling 6 hours, pour out product and abrading-ball, with deionized water rotating wash bowl mill chamber inwall and abrading-ball.The product of collecting is separated with the magnetic field that permanent magnet produces, collect magnetic particle 40 ~ 110
oC presses the different-grain diameter needs after drying down, sieves by the aperture is descending successively, obtains the combination product of the tri-iron tetroxide-carbon in the patent of the present invention.The bulky grain that collection does not meet the particle diameter demand repeats the ball milling utilization.
Embodiment 2
Take by weighing 11.6g Fe
3O
4Powder, the 1g CNT, 15g stainless steel abrading-ball, the 30ml deionized water is put into stainless steel jar mill, starts ball mill, and regulating rotating speed is 500 rev/mins, and ball milling was poured out product and abrading-ball after 8 hours, with deionized water rotating wash bowl mill chamber inwall and abrading-ball.The product of collecting is separated with the magnetic field that permanent magnet produces, collect magnetic particle 40 ~ 110
oC presses the different-grain diameter needs after drying down, sieves by the aperture is descending successively, obtains the combination product of the tri-iron tetroxide-carbon in the patent of the present invention.
Embodiment 3
Take by weighing 8g Fe
2O
3, 0.7gFe powder, 6g expanded graphite powder, 20g stainless steel abrading-ball; The 50ml deionized water is put into stainless steel jar mill, starts ball mill, and regulating rotating speed is 500 rev/mins; Behind the ball milling 12 hours, pour out product and abrading-ball, with deionized water rotating wash bowl mill chamber inwall and abrading-ball.The product of collecting is separated with the magnetic field that permanent magnet produces, collect magnetic particle 40 ~ 110
oC presses the different-grain diameter needs after drying down, sieves by the aperture is descending successively, obtains the combination product of the tri-iron tetroxide-carbon in the patent of the present invention.
Embodiment 4
Take by weighing 8g Fe
2O
3, 0.9gFeO powder, 6g expanded graphite powder, 20g stainless steel abrading-ball; The 50ml deionized water is put into stainless steel jar mill, starts ball mill, and regulating rotating speed is 500 rev/mins; Behind the ball milling 8 hours, pour out product and abrading-ball, with deionized water rotating wash bowl mill chamber inwall and abrading-ball.The product of collecting is separated with the magnetic field that permanent magnet produces, collect magnetic particle 40 ~ 110
oC presses the different-grain diameter needs after drying down, sieves by the aperture is descending successively, obtains the combination product of the tri-iron tetroxide-carbon in the patent of the present invention.
Embodiment 5
Take by weighing 27gFeCl
3.6H
2O, 17.6g FeCl
2.4H
2O, 6g expanded graphite powder, 50g ceramic grinding ball; Put into agate mill jar, start ball mill, regulating rotating speed is 400 rev/mins; Behind the ball milling 6 hours; Pour out product and abrading-ball,, collect product and be positioned in the alumina crucible under protection of nitrogen gas 800 then with deionized water rotating wash bowl mill chamber inwall and abrading-ball
oC handled 1 hour.Naturally cool to room temperature, remove product and separate with the magnetic field that permanent magnet produces, collecting belt magnetic is pressed the different-grain diameter needs, sieves by the aperture is descending successively, obtains the combination product of the tri-iron tetroxide-carbon in the patent of the present invention.
Embodiment 6
Take by weighing 27gFeCl
3.6H
2O, 2.8g Fe powder, the 8g expanded graphite powder, the 50g ceramic grinding ball is put into agate mill jar, starts ball mill, and regulating rotating speed is 500 rev/mins, and ball milling was poured out product and abrading-ball after 8 hours, with deionized water rotating wash bowl mill chamber inwall and abrading-ball.Pour out product and abrading-ball,, collect product and be positioned in the alumina crucible under protection of nitrogen gas 600 then with deionized water rotating wash bowl mill chamber inwall and abrading-ball
oC handled 0.5 hour.Naturally cool to room temperature, remove product and separate with the magnetic field that permanent magnet produces, collecting belt magnetic is pressed the different-grain diameter needs, sieves by the aperture is descending successively, obtains the combination product of the tri-iron tetroxide-carbon in the patent of the present invention.
Claims (7)
1. a tri-iron tetroxide--preparation method, this method of carbon composite lithium ion battery negative material realize through following simple process process: at first, take by weighing raw material by carbon in ferro element in the source of iron and the graphite with 1:1 ~ 1:100, then; Is that 1:1 ~ 10:1 joins in the ball grinder with raw material that takes by weighing and abrading-ball by mass ratio, in ball grinder, adds a certain amount of distilled water or deionized water wet ball grinding again, perhaps directly dry grinding; Ball grinder is put on the ball mill, with rotating speed be 300 ~ 800 rev/mins or more than, after ball milling 3-100 hour; Discharging obtains product, is the hydroxide of iron for source of iron, chloride; Carbonate, sulfate is when nitrate or acetate; To the product after the ball milling discharging, under the protection of inert gas, 350 ~ 1000
oThe processing of C 0.5 ~ 4 hour is carried out magnetic with product and is separated, and isolates not fully compound graphite granule; Sieve successively by different apertures at last, before sieving, need oven dry handle, sieve and choose the carbon back ferric oxide composite material that obtains in this patent invention for the product of wet-milling.
2. the method for claim 1 is characterized in that, used source of iron is an iron powder, or the mixture of iron powder and ferriferous oxide, the hydroxide of iron, chloride, carbonate, sulfate, nitrate or acetate.
3. the method for claim 1 is characterized in that, in the source of iron in ferro element and the graphite carbon with 1:1 ~ 1:100.
4. the method for claim 1 is characterized in that, raw material that takes by weighing and abrading-ball are 1:1 ~ 10:1 by mass ratio
5. the method for claim 1 is characterized in that, rotating speed be 300 ~ 800 rev/mins or more than, ball milling 3-100 hour.
6. method as claimed in claim 2 is characterized in that, is iron powder for source of iron, or during the mixture of iron powder and ferriferous oxide, the product behind the ball milling is target product, need not to heat-treat.
7. the method for claim 1 is characterized in that, is the hydroxide of iron for source of iron, chloride, and carbonate, sulfate is when nitrate or acetate, to the product after the ball milling discharging, at inert gas Ar or N
2Protection under, 350 ~ 1000
oThe processing time of C is 0.5 ~ 4 hour.
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Cited By (11)
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|---|---|---|---|---|
| CN103219510A (en) * | 2013-03-21 | 2013-07-24 | 华中科技大学 | Lithium battery negative electrode material preparation method and its product |
| CN105047863A (en) * | 2015-06-09 | 2015-11-11 | 北京大学深圳研究生院 | Cathode material for lithium battery and preparation method thereof |
| CN105098172A (en) * | 2015-09-01 | 2015-11-25 | 扬州大学 | Preparation method of porous graphitic carbon-coated ferroferric oxide nanofiber product and application of porous graphitic carbon-coated ferroferric oxide nanofiber product in lithium ion battery |
| CN106299290A (en) * | 2016-09-12 | 2017-01-04 | 华南理工大学 | A kind of amorphous Mn oxide/graphite composite nano materials and preparation method thereof and the application in lithium ion battery |
| CN107248454A (en) * | 2017-06-06 | 2017-10-13 | 唐春霞 | A kind of graphene crystalline material and preparation method and application |
| CN107731557A (en) * | 2017-08-23 | 2018-02-23 | 温州大学 | The preparation method and applications of electrode for super capacitor nitrogen oxygen codope porous carbon/ferriferrous oxide composite material |
| CN109841795A (en) * | 2019-03-14 | 2019-06-04 | 电子科技大学 | A kind of preparation method of negative electrode of lithium ion battery |
| CN110323442A (en) * | 2019-07-17 | 2019-10-11 | 中国科学院福建物质结构研究所 | A kind of carbon coating Fe3O4Composite material and preparation method and application |
| CN111330544A (en) * | 2020-03-26 | 2020-06-26 | 安徽工业大学 | Metallurgical dust and sludge modified activated carbon for degrading formaldehyde gas and preparation method thereof |
| CN111952555A (en) * | 2020-07-07 | 2020-11-17 | 华南理工大学 | Lithium ion battery cathode material based on fine iron powder and preparation |
| CN114436389A (en) * | 2022-02-11 | 2022-05-06 | 盐城工学院 | Preparation method and application of magnetically separable zero-valent aluminum-ferroferric oxide compound |
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| CN103219510A (en) * | 2013-03-21 | 2013-07-24 | 华中科技大学 | Lithium battery negative electrode material preparation method and its product |
| CN103219510B (en) * | 2013-03-21 | 2015-06-17 | 华中科技大学 | Lithium battery negative electrode material preparation method and its product |
| CN105047863A (en) * | 2015-06-09 | 2015-11-11 | 北京大学深圳研究生院 | Cathode material for lithium battery and preparation method thereof |
| CN105098172A (en) * | 2015-09-01 | 2015-11-25 | 扬州大学 | Preparation method of porous graphitic carbon-coated ferroferric oxide nanofiber product and application of porous graphitic carbon-coated ferroferric oxide nanofiber product in lithium ion battery |
| CN106299290B (en) * | 2016-09-12 | 2020-01-14 | 华南理工大学 | Amorphous manganese oxide/graphite composite nanomaterial, preparation method thereof and application thereof in lithium ion battery |
| CN106299290A (en) * | 2016-09-12 | 2017-01-04 | 华南理工大学 | A kind of amorphous Mn oxide/graphite composite nano materials and preparation method thereof and the application in lithium ion battery |
| CN107248454A (en) * | 2017-06-06 | 2017-10-13 | 唐春霞 | A kind of graphene crystalline material and preparation method and application |
| CN107731557A (en) * | 2017-08-23 | 2018-02-23 | 温州大学 | The preparation method and applications of electrode for super capacitor nitrogen oxygen codope porous carbon/ferriferrous oxide composite material |
| CN109841795A (en) * | 2019-03-14 | 2019-06-04 | 电子科技大学 | A kind of preparation method of negative electrode of lithium ion battery |
| CN110323442A (en) * | 2019-07-17 | 2019-10-11 | 中国科学院福建物质结构研究所 | A kind of carbon coating Fe3O4Composite material and preparation method and application |
| CN111330544A (en) * | 2020-03-26 | 2020-06-26 | 安徽工业大学 | Metallurgical dust and sludge modified activated carbon for degrading formaldehyde gas and preparation method thereof |
| CN111952555A (en) * | 2020-07-07 | 2020-11-17 | 华南理工大学 | Lithium ion battery cathode material based on fine iron powder and preparation |
| CN114436389A (en) * | 2022-02-11 | 2022-05-06 | 盐城工学院 | Preparation method and application of magnetically separable zero-valent aluminum-ferroferric oxide compound |
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| CN102623692B (en) | 2017-04-05 |
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