CN105428624A - Method for preparing lithium ferrous silicate/carbon composite cathode material by alcohol-assisted hydrothermal method - Google Patents
Method for preparing lithium ferrous silicate/carbon composite cathode material by alcohol-assisted hydrothermal method Download PDFInfo
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- CN105428624A CN105428624A CN201510893181.XA CN201510893181A CN105428624A CN 105428624 A CN105428624 A CN 105428624A CN 201510893181 A CN201510893181 A CN 201510893181A CN 105428624 A CN105428624 A CN 105428624A
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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
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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
-
- 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
- H01M4/58—Selection of substances as active materials, active masses, active liquids of inorganic compounds other than oxides or hydroxides, e.g. sulfides, selenides, tellurides, halogenides or LiCoFy; of polyanionic structures, e.g. phosphates, silicates or borates
- H01M4/5825—Oxygenated metallic salts or polyanionic structures, e.g. borates, phosphates, silicates, olivines
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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
- H01M4/62—Selection of inactive substances as ingredients for active masses, e.g. binders, fillers
- H01M4/624—Electric conductive fillers
- H01M4/625—Carbon or graphite
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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 provides a method for preparing a lithium ferrous silicate/carbon composite cathode material by an alcohol-assisted hydrothermal method. The method comprises the following steps: obtaining an amorphous-state SiO2 through silicon source pretreatment; adding the amorphous-state SiO2, a ferrous iron source, lithium hydrate and a carbon source to an alcohol/water mixed solution for stirring for 30-90 minutes, and then transferring the solution to a hydrothermal high-pressure reaction kettle for sealing; carrying out heat preservation at 120-300 DEG C for 10-72 hours; and finally carrying out washing and vacuum drying on the product in an inert atmosphere, so as to obtain the final product. The material obtained by the method is relatively high in purity, relatively good in electrochemical property, low in raw material, simple in process and short in flow; and industrial production is facilitated.
Description
Technical field
The present invention relates to battery material preparing technical field, particularly the method for Hydrothermal Synthesis, specifically a kind of alcohol helps hydro thermal method to prepare the method for lithium ferrosilicon silicate/carbon composite cathode material.
Background technology
Lithium ion battery has the advantages such as voltage is high, volume is little, quality is light, specific energy is high, memory-less effect, pollution-free, self discharge is little, cycle-index is many, the life-span is long due to it, becomes the desirable energy of current good combination property, achieves develop rapidly.The chief component of lithium ion battery is lithium intercalation compound positive electrode, and positive electrode occupies larger proportion in lithium ion battery, and the quality of positive electrode determines the performance index of lithium ion battery product.Therefore, searching exploitation has the cutting edge of a knife or a sword ion battery positive electrode of high voltage, height ratio capacity and good circulation performance is this field important research content.Lithium ion battery generally selects transition-metal oxide to be positive electrode, and transition metal exists mixed valence, and electron conduction is more satisfactory, and not easily disproportionated reaction occurs.As the newest research results of lithium ion secondary battery anode material, the research of ferrosilicon silicate of lithium becomes and solves energy problem now, manufactures the important channel of the secondary cell of high-efficient energy-saving environment friendly.As how economic environmental protection and simple mode synthetic silicic acid ferrous lithium efficiently become the most important thing.
AntonNyte ' n etc. utilized solid phase method successfully to synthesize Li in 2005
2feSiO
4.This material of current synthesis mainly contains: solid phase method, sol-gal process.Solid phase synthesis Li
2feSiO
4with ferrous salt and Li
2siO
3under being blended in protection gas by chemical ratios, high temperature sintering forms, although method is simple, the method has common shortcoming to be exactly that material grains after synthesis is large, skewness.Sol-gal process synthesis Li
2feSiO
4r.Dominko; M.Bele; under M.Gaber ek etc. were blended in protective atmosphere with ironic citrate and ferric nitrate by chemical ratios in 2006, high temperature sintering forms colloidal sol; and then add a certain proportion of lithium hydroxide and silicon dioxide be blended in protective atmosphere and hydrothermal condition under heating and thermal insulation obtain last xerogel, finally grinding forms.The advantage of the method is that the material granule obtained has good uniformity, but shortcoming to be exactly complex process wayward.
Hydro thermal method geologist's simulating nature circle mineralization and beginning one's study in the middle of the 19th century.Within 1900, post-science men establish Hydrothermal Synthesis theory, start again the research of turning function material later, have prepared over one hundred kind of crystal at present by hydro thermal method.Hydro thermal method, also known as hydrothermal method, belongs to the category of liquid chemical method.Referring in the pressure vessel of sealing, take water as solvent, the chemical reaction carried out under the condition of HTHP.Hydro-thermal reaction can be divided into the hydrolysis of hydrothermal oxidization, hydrothermal reduction, hydrothermal deposition, Hydrothermal Synthesis, hydro-thermal, hydrothermal crystallization etc. according to the difference of reaction type.
Hydro thermal method has two features, and one is higher reaction temperature (100-300 DEG C), is conducive to the raising of magnetic property; Two is carry out in closed container, produces relatively high pressure (0.3-4MPa), avoids component volatilization, is conducive to the purity and the protection of the environment that improve product.Also there is the advantages such as raw material is easy to get, particle purity is high, good dispersion, good crystalline simultaneously.Better crystallinity degree, pattern is good-looking, and be beneficial to the growth of research crystal, experimentation is fairly simple.
The present invention utilizes hydro thermal method to add appropriate alcohols can to reach between raw material and fully contact and the object stoping side reaction to occur, and products therefrom impurity is less, and pattern and granularity are comparatively even, compares additive method and is more conducive to intermediate reaction and controls.
Summary of the invention
The technical problem to be solved in the present invention is to provide a kind of preparation method of lithium ferrosilicon silicate/carbon composite cathode material.The low in raw material price of the method, technique is simple, the advantages such as be easy to suitability for industrialized production, it is good that the finished product produced has uniformity, and purity is high, and chemical property is good.
In order to solve the problems of the technologies described above, the technical solution used in the present invention is:
Alcohol helps hydro thermal method to prepare a method for lithium ferrosilicon silicate/carbon composite cathode material, it is characterized in that, comprises the steps:
(1) by silicon source, H
2o, absolute ethyl alcohol, according to after the mixed in molar ratio of 1:2:2, add at HCl regulates PH to 3-5,70-90 DEG C and add thermal agitation 30min; Drip NH
3h
2o to PH is 8-9, continues to stir 2h, and form milk white gel, ageing 12h, removes supernatant liquor, puts into baking oven 80-150 DEG C of dry 3h; Be, after powder, put into Muffle furnace 600 DEG C of roasting 6-10h by xerogel grinding, finally collect after the product grinding after roasting, give over to step (2) and use;
(2) by amorphous state SiO prepared by step (1)
2add V(alcohol with divalence source of iron, lithium hydroxide, carbon source according to the mol ratio of 1:1:2.3:0.4): V(water)=1:4 mixed solution in, stir 30-90min under an inert atmosphere, then be transferred in hydro-thermal autoclave, sealing, 120-300 DEG C of insulation 10-72h in vacuum drying chamber;
(3) step (2) products therefrom is distinguished centrifuge washing 3 times with distilled water and absolute ethyl alcohol under an inert atmosphere, then vacuumize 12h at 120 DEG C, obtains end product.
The HCl that adds described in step (1) regulates PH to 3-5, PH to be preferably 3-4.
Dropping NH described in step (1)
3h
2o to PH is that 8-9, PH are preferably 8.5-9.
Put into baking oven 80-150 DEG C of dry 3h described in step (1), oven temperature is preferably 120-135 DEG C.
Put into Muffle furnace 600 DEG C of roasting 6-10h described in step (1), roasting time is preferably 6h.
In vacuum drying chamber described in step (2), 120-300 DEG C of insulation 10-72h, is preferably 120 DEG C of dry 12h.
Silicon source described in step (1) is one or more mixture of tetraethoxysilane, positive isopropyl silicate, silicon tetrachloride, sodium metasilicate and trimethyl silanol.
Divalence source of iron described in step (2) is one or more mixture of ferrous sulfate, frerrous chloride, ferrous nitrate, ferrous phosphate, ferrous acetate and ferrous oxalate; Described carbon source is one or more mixture of glucose, sucrose, fructose, dextrin, galactolipin, lactose and maltose; Hydro thermal method needs to add a certain amount of alcohol, and the alcohol described in it is one or more mixture of ethanol, ethylene glycol, normal propyl alcohol, isopropyl alcohol and isoprene.
Step (2) and the inert atmosphere described in step (3) are the one in the gaseous mixture of nitrogen, argon gas and their arbitrary proportions.
Resulting materials purity of the present invention is higher, and chemical property is better, and raw material is cheap, technique is simple, flow process is short, is convenient to suitability for industrialized production.
Accompanying drawing explanation
Fig. 1 is step of the present invention (1) gained amorphous state SiO
2xRD collection of illustrative plates;
Fig. 2 is commodity SiO
2xRD collection of illustrative plates;
Fig. 3 is finished product of the present invention typical case XRD collection of illustrative plates;
Fig. 4 is the embodiment of the present invention 1 charge and discharge electrograph;
Fig. 5 is the embodiment of the present invention 2 charge and discharge electrograph;
Fig. 6 is the XRD collection of illustrative plates of the embodiment of the present invention 1 finished product and embodiment 3 finished product, and wherein a is embodiment 1, b is embodiment 3.
Embodiment
The present invention is described in detail below in conjunction with the drawings and specific embodiments.
X-ray powder diffraction (XRD) test completes on BrukerD8 type diffractometer, Cu target diffraction (=0.15406nm), tube voltage 40kV, tube current 40mA.Sweep limits 20-80 degree, sweep speed is 4 degree of per minutes.Charge-discharge test carries out on Neware charging-discharge tester system, by the Li of synthesis
2feSiO
4as active material, acetylene black is conductive agent, and polytetrafluoroethylene (PTFE) emulsion is as binding agent, after mixing, evenly compacting film forming does positive pole in proportion, take lithium metal as negative pole, Celgard2400 microporous barrier is barrier film, in the glove box being full of argon gas, dress up simulated battery.Under normal temperature, constant current charge-discharge test macro carries out electrochemical property test.
embodiment 1
By TEOS:H
2o: absolute ethyl alcohol is after the mixed in molar ratio of 1:2:2, adds HCl and regulates PH to 3, add thermal agitation 30min at 70 DEG C.Then NH is dripped
3h
2o to PH is 9, continues to stir 2h, forms milk white gel.Ageing 12h, removes supernatant liquor afterwards, puts into baking oven 120 DEG C of dry 3h.Be, after powder, put into Muffle furnace 600 DEG C of roasting 6h by xerogel grinding.Finally collect after the product grinding after roasting, give over to subsequent reactions and use.
Get 1mmolFeCl
2, 2.3mmolLiOH, 1mmolSiO
2(preparing above), 0.4mmol glucose is dissolved in 60ml distilled water and adds in 15ml absolute ethyl alcohol, at N
2proceed to after stirring 30min under protective atmosphere in 100ml hydrothermal reaction kettle, then put into vacuum drying oven, 200 DEG C keep 72h.Then at N
2under atmosphere, product taking-up distilled water and absolute ethyl alcohol are washed three times respectively, precipitation is put into vacuum drying oven and vacuumize 120 DEG C of dry 12h.
Fig. 1 the present embodiment gained SiO
2with Fig. 2 commodity SiO
2xRD collection of illustrative plates contrasts, and therefrom can find out gained SiO
2for amorphous state, by ESEM, prove that it is nanostructure, molecular dimension is between 20-50nm.And commodity SiO
2purity is high and degree of crystallinity is higher, and structure is more stable, does not generally participate in reaction, can not be for the synthesis of, so need to make SiO by oneself
2.
Fig. 4 is the present embodiment products therefrom charge and discharge electrograph, and therefrom can find out in battery charge and discharge process, platform is comparatively smoothly clear, and battery specific capacity is higher, can reach 140mAhg
-1, and battery special capacity fade is slower.Fig. 6 (a) is the present embodiment XRD collection of illustrative plates, and can find out that products therefrom purity is higher, impurities only has minute quantity Fe
3o
4.
embodiment 2
By positive isopropyl silicate: H
2o: absolute ethyl alcohol is after the mixed in molar ratio of 1:2:2, adds HCl and regulates PH to 4, add thermal agitation 30min at 80 DEG C.Then NH is dripped
3h
2o to PH is 8.5, continues to stir 2h, forms milk white gel.Ageing 12h, removes supernatant liquor afterwards, puts into baking oven 135 DEG C of dry 3h.Be, after powder, put into Muffle furnace 600 DEG C of roasting 6h by xerogel grinding.Finally collect after the product grinding after roasting, give over to subsequent reactions and use.
Get 1mmolFe(CH
3cOOH)
2, 2.3mmolLiOH, 1mmolSiO
2(preparing above), 0.4mmol fructose is dissolved in 60ml distilled water and adds in 15ml isopropyl alcohol, proceeds in 100ml hydrothermal reaction kettle, then put into vacuum drying oven under Ar protective atmosphere after stirring 60min, and 240 DEG C keep 60h.Then under an ar atmosphere product taking-up distilled water and absolute ethyl alcohol are washed three times respectively, precipitation is put into vacuum drying oven and vacuumize 120 DEG C of dry 12h.
Fig. 5 is the present embodiment products therefrom charge and discharge electrograph, contrast can find out that two kinds of product charge and discharge platform are substantially identical with charging and discharging curve, illustrate that embodiment 1 is identical with embodiment 2 products therefrom, also prove that the method that this invention provides has certain versatility and repeatability.
embodiment 3
By TEOS:H
2o: absolute ethyl alcohol is after the mixed in molar ratio of 1:2:2, adds HCl and regulates PH to 3, add thermal agitation 30min at 70 DEG C.Then NH is dripped
3h
2o to PH is 9, continues to stir 2h, forms milk white gel.Ageing 12h, removes supernatant liquor afterwards, puts into baking oven 120 DEG C of dry 3h.Be, after powder, put into Muffle furnace 600 DEG C of roasting 6h by xerogel grinding.Finally collect after the product grinding after roasting, give over to subsequent reactions and use.
Get 1mmolFeCl
2, 2.3mmolLiOH, 1mmolSiO
2(preparing above), 0.4mmol glucose is dissolved in 75ml distilled water, at N
2proceed to after stirring 30min under protective atmosphere in 100ml hydrothermal reaction kettle, then put into vacuum drying oven, 200 DEG C keep 72h.Then at N
2under atmosphere, product taking-up distilled water and absolute ethyl alcohol are washed three times respectively, precipitation is put into vacuum drying oven and vacuumize 120 DEG C of dry 12h.
Fig. 6 (b) is the present embodiment products therefrom XRD collection of illustrative plates, therefrom can find out that products therefrom is poor compared with embodiment 1 degree of crystallinity, have a large amount of impurity, wherein Fe
3o
4content is more, and also has a certain amount of Li
2siO
3.This illustrates that adding of absolute ethyl alcohol is conducive to reaction and carries out, and the dispersion effect of absolute ethyl alcohol can make abundant haptoreaction between raw material, and stops the generation of side reaction.
Claims (9)
1. alcohol helps hydro thermal method to prepare a method for lithium ferrosilicon silicate/carbon composite cathode material, and its feature comprises the steps:
(1) by silicon source, H
2o, absolute ethyl alcohol, according to after the mixed in molar ratio of 1:2:2, add at HCl regulates PH to 3-5,70-90 DEG C and add thermal agitation 30min; Drip NH
3h
2o to PH is 8-9, continues to stir 2h, and form milk white gel, ageing 12h, removes supernatant liquor, puts into baking oven 80-150 DEG C of dry 3h; Be, after powder, put into Muffle furnace 600 DEG C of roasting 6-10h by xerogel grinding, finally collect after the product grinding after roasting, give over to step (2) and use;
(2) by amorphous state SiO prepared by step (1)
2add V(alcohol with divalence source of iron, lithium hydroxide, carbon source according to the mol ratio of 1:1:2.3:0.4): V(water)=1:4 mixed solution in, stir 30-90min under an inert atmosphere, then be transferred in hydro-thermal autoclave, sealing, 120-300 DEG C of insulation 10-72h in vacuum drying chamber;
(3) step (2) products therefrom is distinguished centrifuge washing 3 times with distilled water and absolute ethyl alcohol under an inert atmosphere, then vacuumize 12h at 120 DEG C, obtains end product.
2. the alcohol according to claims 1 helps hydro thermal method to prepare the method for lithium ferrosilicon silicate/carbon composite cathode material, it is characterized in that, the HCl that adds described in step (1) regulates PH to 3-5, PH to be preferably 3-4.
3. the alcohol according to claims 1 helps hydro thermal method to prepare the method for lithium ferrosilicon silicate/carbon composite cathode material, it is characterized in that, the dropping NH described in step (1)
3h
2o to PH is that 8-9, PH are preferably 8.5-9.
4. the alcohol according to claims 1 helps hydro thermal method to prepare the method for lithium ferrosilicon silicate/carbon composite cathode material, it is characterized in that, puts into baking oven 80-150 DEG C of dry 3h described in step (1), and oven temperature is preferably 120-135 DEG C.
5. the alcohol according to claims 1 helps hydro thermal method to prepare the method for lithium ferrosilicon silicate/carbon composite cathode material, it is characterized in that, puts into Muffle furnace 600 DEG C of roasting 6-10h described in step (1), and roasting time is preferably 6h.
6. the alcohol according to claims 1 helps hydro thermal method to prepare the method for lithium ferrosilicon silicate/carbon composite cathode material, it is characterized in that, in the vacuum drying chamber described in step (2), 120-300 DEG C of insulation 10-72h, is preferably 120 DEG C of dry 12h.
7. the alcohol according to claims 1 helps hydro thermal method to prepare the method for lithium ferrosilicon silicate/carbon composite cathode material, it is characterized in that, the silicon source described in step (1) is one or more mixture of tetraethoxysilane, positive isopropyl silicate, silicon tetrachloride, sodium metasilicate and trimethyl silanol.
8. the alcohol according to claims 1 helps hydro thermal method to prepare the method for lithium ferrosilicon silicate/carbon composite cathode material, it is characterized in that, the divalence source of iron described in step (2) is one or more mixture of ferrous sulfate, frerrous chloride, ferrous nitrate, ferrous phosphate, ferrous acetate and ferrous oxalate; Described carbon source is one or more mixture of glucose, sucrose, fructose, dextrin, galactolipin, lactose and maltose; Hydro thermal method needs to add a certain amount of alcohol, and the alcohol described in it is one or more mixture of ethanol, ethylene glycol, normal propyl alcohol, isopropyl alcohol and isoprene.
9. the alcohol according to claims 1 helps hydro thermal method to prepare the method for lithium ferrosilicon silicate/carbon composite cathode material, it is characterized in that, step (2) and the inert atmosphere described in step (3) are the one in the gaseous mixture of nitrogen, argon gas and their arbitrary proportions.
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Citations (5)
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|---|---|---|---|---|
| CN1757598A (en) * | 2005-10-26 | 2006-04-12 | 太原理工大学 | Method for preparing super fine hydrophobic silicon dioxide |
| CN102664262A (en) * | 2012-05-18 | 2012-09-12 | 哈尔滨工业大学 | Method for preparing lithium ferrous silicate or carbon ferrous silicate cathode material for lithium ion battery |
| CN103078120A (en) * | 2013-01-22 | 2013-05-01 | 武汉理工大学 | Ferrous silicate lithium ion battery cathode material with hierarchical structure and preparation method |
| CN103326026A (en) * | 2013-06-18 | 2013-09-25 | 西安建筑科技大学 | Method for preparing porous lithium-iron silicate/carbon composite material for positive pole of lithium ion battery |
| US20140141332A1 (en) * | 2011-07-04 | 2014-05-22 | Shoei Chemical Inc. | Positive electrode material for lithium ion secondary battery, positive electrode member, lithium ion secondary battery, and production method for said positive electrode material |
-
2015
- 2015-12-08 CN CN201510893181.XA patent/CN105428624A/en active Pending
Patent Citations (5)
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|---|---|---|---|---|
| CN1757598A (en) * | 2005-10-26 | 2006-04-12 | 太原理工大学 | Method for preparing super fine hydrophobic silicon dioxide |
| US20140141332A1 (en) * | 2011-07-04 | 2014-05-22 | Shoei Chemical Inc. | Positive electrode material for lithium ion secondary battery, positive electrode member, lithium ion secondary battery, and production method for said positive electrode material |
| CN102664262A (en) * | 2012-05-18 | 2012-09-12 | 哈尔滨工业大学 | Method for preparing lithium ferrous silicate or carbon ferrous silicate cathode material for lithium ion battery |
| CN103078120A (en) * | 2013-01-22 | 2013-05-01 | 武汉理工大学 | Ferrous silicate lithium ion battery cathode material with hierarchical structure and preparation method |
| CN103326026A (en) * | 2013-06-18 | 2013-09-25 | 西安建筑科技大学 | Method for preparing porous lithium-iron silicate/carbon composite material for positive pole of lithium ion battery |
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Application publication date: 20160323 |