CN106340621A - Ferric negative electrode material for lithium battery and preparation method thereof - Google Patents
Ferric negative electrode material for lithium battery and preparation method thereof Download PDFInfo
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- CN106340621A CN106340621A CN201610813802.3A CN201610813802A CN106340621A CN 106340621 A CN106340621 A CN 106340621A CN 201610813802 A CN201610813802 A CN 201610813802A CN 106340621 A CN106340621 A CN 106340621A
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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
- H01M4/364—Composites as mixtures
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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
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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
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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 discloses a ferric negative electrode material for a lithium battery and a preparation method thereof. The preparation method comprises the following steps: adding metal nitrate M(NO3)2, ferric nitrate Fe(NO3)3 and a combustion aid into water, then heating to volatilize water and form gel, then calcining the gel, and naturally cooling to obtain the ferric negative electrode material for the lithium battery. When the preparation method provided by the invention is used for preparing the negative electrode material, a solid-phase grinding operating step in the conventional method is omitted, so that the reaction can be easily speeded up; compared with the prior art, the reaction time is shortened. The negative electrode material prepared with the preparation method provided by the invention has excellent cycle performance, high capacity and good conductivity, and can be applied to the fields of large energy storage batteries and the like.
Description
Technical field
The present invention relates to lithium battery material field, more particularly, to a kind of lithium battery ferrum system negative material and its preparation side
Method.
Background technology
Lithium rechargeable battery (rechargeable battery, abbreviation lithium ion battery) is the electricity of a kind of high efficiency, high-energy-density
Energy storage device, has been widely used in small movable electronic equipment.As other battery systems, lithium ion battery master
To be made up of positive electrode, negative material, barrier film and the big critical material of electrolyte four, the property of the property of material and lithium ion battery
Can there is very important relation.
At present, the widely used positive electrode of lithium ion battery is mainly the transition metal of the reversible embedded-deintercalation of lithium ion
Oxide, such as with cobalt acid lithium (licoo2), ternary material (lini1/3co1/3mn1/3o2) etc. for representative layered metal oxide,
With LiMn2O4 (limn2o4) be the spinel-type metal-oxide of representative, with LiFePO4 (lifepo4) be representative olivine
Type metal-oxide etc.；Negative material predominantly reversibly embeds-compound of deintercalate lithium ions, such as lamellar graphite.These are high
The application of performance materials, determines lithium ion battery today as small sized portable communication electronic equipment (as mobile phone, portable electricity
Brain etc.) power supply can not shake status.But with social development further (as electric automobile wanting in terms of power source
Ask), existing lithium-ion battery system is all gone back at the aspect such as plentiful of price, safety, specific capacity and power-performance, raw material
Have much room for improvement.The material of exploitation higher performance and corresponding lithium ion cell electrode are important.
Using unit metal oxide as the titanio negative material representing as a class negative material, because it is with respect to gold
Belong to lithium and there is higher electrode potential it is suppressed that lithium metal separates out on negative pole, fundamentally solve that Li dendrite causes is short
Road problem, improves the safety of battery.But unit metal oxide is relatively low due to theoretical capacity, electric conductivity poor so as to
It is applied to the fields such as large-scale energy-storage battery to be greatly limited.
Therefore, prior art has yet to be improved and developed.
Content of the invention
In view of above-mentioned the deficiencies in the prior art, it is an object of the invention to provide a kind of lithium battery with ferrum system negative material and
Its preparation method it is intended to solve negative material due to theoretical capacity relatively low, electric conductivity poor so as to be applied to large-scale energy-storage battery
The problem being greatly limited in field.
Technical scheme is as follows:
A kind of lithium battery preparation method of ferrum system negative material, wherein, including step:
Metal nitrate m (no is added in water3)2, ferric nitrate fe (no3)3With comburant, then heat and so that water volatilization is formed
Then gel is calcined by gel, then natural cooling obtains described lithium battery ferrum system negative material.
Described preparation method, wherein, described comburant be one of glycine, citric acid, sucrose, glucose or
Multiple mixture.
Described preparation method, wherein, according to the molar ratio, m:fe=1:2.
Described preparation method, wherein, according to the molar ratio, comburant: fe=1:2 ~ 1:1.
Described preparation method, wherein, when being calcined, is carried out as follows: with the speed liter of 5 ~ 10 DEG C/min
Temperature is to 650 ~ 850 DEG C, and calcines 2 ~ 3 hours at this temperature.
Described preparation method, wherein, is warming up to 700 DEG C with the speed of 5 DEG C/min, and calcining 2 is little at this temperature
When.
Described preparation method, wherein, described lithium battery ferrum system negative material is micro-nano structure, particle diameter be 10 ~
200nm.
Described preparation method, wherein, described m is zn, co, mg or cu.
Described preparation method, wherein, after forming gel, first gel being positioned on electric furnace heating makes gel occur from climing
Prolong combustion reaction.
A kind of lithium battery ferrum system negative material, wherein, is made using the preparation method described in as above any one.
Beneficial effect: the negative material of the method preparation that the present invention uses, it is to avoid the behaviour of solid-phase grinding in traditional method
Make step, be conducive to accelerating response speed, compared with the existing technology, shorten the response time.The negative material of present invention preparation
There is excellent cycle performance, capacity is high, electric conductivity preferably, can be applicable to the fields such as large-scale energy-storage battery.
Brief description
Fig. 1 is znfe in the embodiment of the present invention one2o4The xrd figure of material.
Fig. 2 is znfe in the embodiment of the present invention one2o4The sem figure of material.
Fig. 3 is znfe in the embodiment of the present invention one2o4The electrochemistry cycle performance figure of material.
Fig. 4 is cofe in the embodiment of the present invention two2o4The xrd figure of material.
Fig. 5 is cofe in the embodiment of the present invention two2o4The sem figure of material.
Fig. 6 is cofe in the embodiment of the present invention two2o4The electrochemistry cycle performance figure of material.
Specific embodiment
The present invention provides a kind of lithium battery ferrum system negative material and preparation method thereof, for making the purpose of the present invention, technology
Scheme and effect are clearer, clear and definite, and the present invention is described in more detail below.It should be appreciated that it is described herein concrete
Embodiment only in order to explain the present invention, is not intended to limit the present invention.
A kind of lithium battery provided by the present invention preparation method of ferrum system negative material, it includes step:
Metal nitrate m (no is added in water3)2, ferric nitrate fe (no3)3With comburant, then heat and so that water volatilization is formed
Then gel is calcined by gel, then natural cooling obtains described lithium battery ferrum system negative material.
The present invention is by corresponding metal nitrate and comburant mix homogeneously in deionized water, is formed uniformly molten
Liquid, then volatilization moisture prepares gel (xerogel) in a heated condition.By xerogel in air atmosphere high temperature calcination reaction
After obtain mfe2o4Material.
In the prior art, be mostly with solid-phase ball milling mixing after, then calcine some hours at high temperature and be obtained.This method
The material physicochemical property of preparation is uneven and is easy to reunite, thus being unfavorable for improving product quality.The invention has the advantages that system
Preparation Method is simple, consumes energy low (calcination time≤3 hour), and yield is high, it is easy to accomplish large-scale production.
Further, described comburant is the mixture of one or more of glycine, citric acid, sucrose, glucose.
Select glycine as comburant in a preferred approach, because glycine burns more abundant during the course of the reaction, have more
Good combustion-supporting effect.
Further, according to the molar ratio, m:fe=1:2.That is, m (no3)2With fe (no3)3Mol ratio be 1:2,
Under the conditions of being somebody's turn to do, the two reaction is more abundant, can improve reaction efficiency, and the two can form the more preferable mfe of quality2o4Material, by-product
Few.
Further, according to the molar ratio, comburant: fe=1:2 ~ 1:1.I.e. comburant and the mol ratio of fe are 1:2 ~ 1:
1, under these conditions, comburant can be accelerated to make m (no3)2With fe (no3)3The two burning is more thorough, and combustion-supporting effect is good.
In addition, after forming gel, first gel being positioned over heating on electric furnace makes gel that self-propagating combustion reaction to occur.
Further, when being calcined, carry out as follows: be warming up to 650 ~ 850 with the speed of 5 ~ 10 DEG C/min
DEG C, and calcine 2 ~ 3 hours at this temperature.For example, it is warming up to 700 DEG C with the speed of 5 DEG C/min, and calcine 2 at this temperature
Hour.Under these conditions, the excellent micro-nano structure of particle size (comprising nanostructured and micrometer structure) can be prepared,
The electrochemically stable performance of prepared electrode material will be substantially better than conventional ferrous material.And the inventive method technical costss are low,
Process is simple.
Further, described lithium battery ferrum system negative material is micro-nano structure, and particle diameter is 10 ~ 200nm.
Further, described m is zn, co, mg or cu.Wherein, during m=zn, particle diameter is 100 ~ 150nm, and during m=co, particle diameter is
10~50nm.The electrode material of present invention preparation has porous micro-nano structure.Nanostructured therein, not only improves electrolyte
Infiltration, is conducive to the electronics of electrolysis material and lithium ion transport thus improving the chemical property of material again；Micrometer structure then increases
Plus material preparation, the stability of storage, reduce production and storage cost to a certain extent.
The present invention also provides a kind of lithium battery ferrum system negative material, and it adopts the as above preparation method system described in any one
Become.
The present invention compared with prior art has the advantage that
1st, the present invention uses the electrode material of gel-combustion method preparation, it is to avoid the operation of solid-phase grinding in traditional method
Step, is conducive to accelerating response speed, compared with the existing technology, shortens the response time.
2nd, using the electrode material of the inventive method preparation, there is porous micro-nano structure.Nanostructured therein, both favorably
In the infiltration of electrolyte, be conducive to the electronics of electrolysis material with lithium ion transport thus improving the chemical property of material again；Micro-
Rice structure then increases material preparation, the stability of storage, reduces production and storage cost to a certain extent.
3rd, the titanium system electrode material of present invention preparation has excellent cycle performance, znfe2o4Close in the electric current of 200ma/g
Degree is lower to circulate 80 weeks reversible capacities up to 1024mah/g.cofe2o480 weeks reversible capacities are circulated under the electric current density of 200ma/g
Up to 908mah/g.
Embodiment 1:
Add glycine, zn (no in deionized water3)2With fe (no3)3, wherein glycine and the molar ratio of fe element are 1:
The molar ratio of 1, zn element and fe element is 1:2.To be dissolved completely after, mixed solution is put into stirring in 100 DEG C of oil bath pans
Heating eliminating water, stirring 8h forms gel.Then the gel of formation is placed on heating on electric furnace, gel will occur self-propagating combustion anti-
Should.The powder obtaining reaction afterwards is put into Muffle furnace and is sintered 2 h at 700 DEG C, naturally cools to after room temperature after in-furnace temperature
Take out from Muffle furnace, you can obtain target product.
Material property characterizes: by xrd diffractometer (using philips x ' pert pro super x-ray diffractometer
With cu k alpha ray source) crystal structure of analysis of material obtains Fig. 1, and this electrode material crystal structure is spinel-type as can be seen from Figure 1
Structure and do not have impurity；The particle diameter of scanning electron microscope (hitachi s-4800) analysis of material, obtains Fig. 2, as can be seen from Figure 2
This electrode material is porous micro-nano structure granule, and particle diameter is 100 ~ 150nm.
Electrochemical property test: by obtained electrode material lithium titanate/titanium nitride and acetylene black and pvdf in mass ratio
8: 1: 1 mix homogeneously, add appropriate n- methyl pyrrolidone dissolving, slurry film are obtained on Copper Foil electrode.This is tried
Electrical verification pole 110 DEG C of dryings 24 hours in vacuum drying oven, with ec/dec/dmc=1: 1:1(body in high-purity argon atmosphere glove box
Long-pending ratio) with lipf6For electrolyte, with glass fiber filter paper for imbibition film, pp film is barrier film, and lithium metal assembles for battery cathode
Become 2016 button cells.Put charge condition: discharged into identical electric current density and after 0.02v, recharge to 3v, the electric current of selection
Density is 200ma/g.
Above-mentioned battery is tested, obtain Fig. 3 it is known that: by embodiment one method preparation electrode material 200ma/g electricity
Discharge and recharge under current density, after circulating 80 weeks, reversible capacity is maintained at 1042mah/g.
Embodiment 2:
The other conditions of preparation method and embodiment 1, simply metal nitrate selection co (no3)2.
Material property characterizes: by xrd diffractometer (using philips x ' pert pro super x-ray diffractometer
With cu k alpha ray source) crystal structure of analysis of material obtains Fig. 4, and this electrode material crystal structure is spinel-type as can be seen from Figure 4
Structure and do not have impurity；The particle diameter of scanning electron microscope (hitachi s-4800) analysis of material, obtains Fig. 5, as can be seen from Figure 5
This electrode material is porous micro-nano structure granule, and particle diameter is 10 ~ 50nm.
Electrochemical property test: electro-chemical test is identical with embodiment one, obtains Fig. 6.Electricity by the preparation of embodiment two method
The discharge and recharge under 200ma/g electric current density of pole material, after circulating 80 weeks, reversible capacity is maintained at 908mah/g.
By comparative example one to two it is known that: the stable circulation of the electrode material being obtained using technical solution of the present invention
Excellent performance.
The method of the present invention, without solid-phase grinding, simplifies preparation technology, reduces production cost；Using gel-combustion method
One-step synthesis material, shortens the response time, improves the uniformity of product physicochemical property.Additionally, the material of preparation is micro-nano structure,
Both the transmission of lithium ion electronics can have been accelerated, improved electro-chemical activity；The stability of material can be increased, that improves material can again
Processability and storage stability.
It should be appreciated that the application of the present invention is not limited to above-mentioned citing, for those of ordinary skills, can
To be improved according to the above description or to convert, all these modifications and variations all should belong to the guarantor of claims of the present invention
Shield scope.
Claims (10)
1. a kind of lithium battery with the preparation method of ferrum system negative material it is characterised in that include step:
Metal nitrate m (no is added in water3)2, ferric nitrate fe (no3)3With comburant, then heat and make water volatilization formation solidifying
Then gel is calcined by glue, then natural cooling obtains described lithium battery ferrum system negative material.
2. preparation method according to claim 1 is it is characterised in that described comburant is glycine, citric acid, sugarcane
The mixture of one or more of sugar, glucose.
3. preparation method according to claim 1 it is characterised in that according to the molar ratio, m:fe=1:2.
4. preparation method according to claim 1 it is characterised in that according to the molar ratio, comburant: fe=1:2 ~ 1:1.
5. preparation method according to claim 1 is it is characterised in that when being calcined, carry out as follows: with 5 ~
The speed of 10 DEG C/min is warming up to 650 ~ 850 DEG C, and calcines 2 ~ 3 hours at this temperature.
6. preparation method according to claim 5 is it is characterised in that be warming up to 700 DEG C with the speed of 5 DEG C/min, and
This temperature lower calcination 2 hours.
7. preparation method according to claim 1 is it is characterised in that described lithium battery ferrum system negative material is micro-nano knot
Structure, particle diameter is 10 ~ 200nm.
8. preparation method according to claim 1 is it is characterised in that described m is zn, co, mg or cu.
9., after preparation method according to claim 1 is it is characterised in that form gel, first gel is positioned on electric furnace
Heating makes gel that self-propagating combustion reaction to occur.
10. a kind of lithium battery with ferrum system negative material it is characterised in that using preparation as described in any one of claim 1 ~ 9
Method is made.
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Cited By (5)
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| CN106602037A (en) * | 2017-01-19 | 2017-04-26 | 新乡天力锂能股份有限公司 | Lithium ion battery cathode material LiVOPO4/C and synthetic method thereof |
| CN108400299A (en) * | 2018-02-08 | 2018-08-14 | 江西理工大学 | A kind of preparation method of CuFe2O4/C composite negative pole materials for sodium-ion battery |
| CN110635103A (en) * | 2019-08-29 | 2019-12-31 | 天津工业大学 | Flexible nano porous metal oxide cathode for secondary battery and preparation method thereof |
| CN114242977A (en) * | 2021-12-06 | 2022-03-25 | 桂林理工大学 | Method for preparing high-performance composite negative electrode material by using sucrose-assisted jarosite slag hydrochloric acid leaching solution |
| CN114261991A (en) * | 2021-12-24 | 2022-04-01 | 西安工业大学 | Nano-flaky ZnFe2O4Preparation method of lithium ion battery cathode material |
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| CN114261991A (en) * | 2021-12-24 | 2022-04-01 | 西安工业大学 | Nano-flaky ZnFe2O4Preparation method of lithium ion battery cathode material |
| CN114261991B (en) * | 2021-12-24 | 2023-11-14 | 西安工业大学 | Nanometer flaky ZnFe 2 O 4 Preparation method of lithium ion battery anode material |
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Application publication date: 20170118 |